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_4106030
_publ_contact_author_address
;
Department of Chemistry,
University of Bergen,
All\'egaten 41,
N-5007 Bergen,
Norway
;
_publ_contact_author_name
;
Prof. Karl Wilhelm T\"ornroos
;
_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_formula_moiety         'C24 H60 Al3 Nd O3'
_chemical_formula_sum            'C24 H60 Al3 Nd O3'
_chemical_formula_weight         621.90
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           159
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 3 -2c'
_symmetry_space_group_name_H-M   'P 3 1 c'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   16.1210(4)
_cell_length_b                   16.1210(4)
_cell_length_c                   8.6164(5)
_cell_measurement_reflns_used    14337
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      30.51
_cell_measurement_theta_min      2.02
_cell_volume                     1939.28(13)
_computing_cell_refinement
;
Bruker (2004). SAINT, version 6.45a, Bruker AXS Inc., Madison, 
Wisconsin, USA.
;
_computing_data_collection
;
Bruker (1999). SMART, version 5.054, Bruker AXS Inc., Madison, 
Wisconsin, USA.
;
_computing_data_reduction
;
Bruker (2004). SAINT, version 6.45a, Bruker AXS Inc., Madison, 
Wisconsin, USA.
;
_computing_molecular_graphics
;
Brandenburg, K. (2005). DIAMOND. Version 3.1. Crystal Impact GbR, Bonn, 
Germany.; Farrugia, L. J. (1997). ORTEP-3. J. Appl. Cryst. 30, 565.
;
_computing_publication_material
;
Bruker AXS (2003). SHELXTL. Version 6.14. Bruker AXS Inc., Madison, 
Wisconsin, USA.
;
_computing_structure_refinement
;
Sheldrick, G. M. (2008). Acta Cryst. A64, 112--122.
;
_computing_structure_solution
;     
Sheldrick, G. M. (2008). Acta Cryst. A64, 112--122.
;
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean '48 \um'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker-AXS SMART 2K CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_av_sigmaI/netI    0.0222
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            32758
_diffrn_reflns_theta_full        30.56
_diffrn_reflns_theta_max         30.56
_diffrn_reflns_theta_min         2.53
_exptl_absorpt_coefficient_mu    1.423
_exptl_absorpt_correction_T_max  0.89429
_exptl_absorpt_correction_T_min  0.62112
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
Bruker AXS (2003). SHELXTL. Version 6.14. Bruker AXS Inc., Madison, 
Wisconsin, USA.
;
_exptl_crystal_colour            'pale blue'
_exptl_crystal_density_diffrn    1.065
_exptl_crystal_description       needle
_exptl_crystal_F_000             654
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
;
_refine_diff_density_max         0.509
_refine_diff_density_min         -0.393
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.013(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     108
_refine_ls_number_reflns         3959
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.136
_refine_ls_R_factor_all          0.0160
_refine_ls_R_factor_gt           0.0153
_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^)+(0.0221P)^2^+0.0263P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0417
_refine_ls_wR_factor_ref         0.0419
_reflns_number_gt                3840
_reflns_number_total             3959
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja2001049_si_004.cif
_cod_data_source_block           Compound3b
_cod_database_code               4106030