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_4106033
_publ_contact_author_address
;
Institut f\"ur Anorganische Chemie,
Universit\"at T\"ubingen, 
Auf der Morgenstelle 18, 
D-72076 T\"ubingen, 
Germany
;
_publ_contact_author_name
;
C\"acilia Maichle-M\"ossmer
;
_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         'C12 H36 Al3 Yb'
_chemical_formula_sum            'C12 H36 Al3 Yb'
_chemical_formula_weight         434.39
_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                 92.52(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   7.3860(13)
_cell_length_b                   17.683(6)
_cell_length_c                   32.230(11)
_cell_measurement_temperature    213(2)
_cell_volume                     4205(2)
_computing_cell_refinement       EXPRESS
_computing_data_collection       EXPRESS
_computing_data_reduction        HELENA
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.944
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_device_type  CAD4
_diffrn_measurement_method       omega/2Theta
_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  0.0446
_diffrn_reflns_av_sigmaI/netI    0.0431
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            9450
_diffrn_reflns_theta_full        24.73
_diffrn_reflns_theta_max         24.73
_diffrn_reflns_theta_min         2.30
_exptl_absorpt_coefficient_mu    4.556
_exptl_absorpt_correction_T_max  0.9357
_exptl_absorpt_correction_T_min  0.5168
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
; 
Rigoult, J., Tomas, A. & Guidi Morosini, C. (1979). Acta Cryst. A35, 587-590. 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_description       plate
_exptl_crystal_F_000             1736
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.829
_refine_diff_density_min         -1.866
_refine_diff_density_rms         0.275
_refine_ls_extinction_coef       0.0044(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         7045
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0778
_refine_ls_R_factor_gt           0.0626
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1184P)^2^+13.9569P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1698
_refine_ls_wR_factor_ref         0.1826
_reflns_number_gt                5723
_reflns_number_total             7045
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja2001049_si_007.cif
_cod_data_source_block           Compound4c_HT
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1184P)^2^+13.9569P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1184P)^2^+13.9569P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4106033