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_4106028
_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         'C20 H58 N3 O2 Si6 Yb'
_chemical_formula_sum            'C20 H58 N3 O2 Si6 Yb'
_chemical_formula_weight         714.27
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.304(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.0353(9)
_cell_length_b                   16.0013(7)
_cell_length_c                   16.8519(11)
_cell_measurement_temperature    173(2)
_cell_volume                     3512.2(4)
_computing_cell_refinement       X-AREA
_computing_data_collection       X-AREA
_computing_data_reduction        X-AREA
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.959
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       'omega scans'
_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  0.1231
_diffrn_reflns_av_sigmaI/netI    0.0595
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            59549
_diffrn_reflns_theta_full        29.26
_diffrn_reflns_theta_max         29.26
_diffrn_reflns_theta_min         3.20
_exptl_absorpt_coefficient_mu    2.887
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_description       bloc
_exptl_crystal_F_000             1476
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.110
_refine_diff_density_min         -2.844
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.228
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     323
_refine_ls_number_reflns         9472
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.228
_refine_ls_R_factor_all          0.0849
_refine_ls_R_factor_gt           0.0612
_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^)+(0.0001P)^2^+13.6940P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0859
_refine_ls_wR_factor_ref         0.0906
_reflns_number_gt                7510
_reflns_number_total             9472
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja2001049_si_002.cif
_cod_data_source_block           Compound2b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0001P)^2^+13.6940P] 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^)+(0.0001P)^2^+13.6940P] 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               4106028