Synthesis, Characterization, and Reaction of Aluminum Halide Amides Supported by a Bulky β-Diketiminato Ligand
Ying Yang; Thomas Schulz; Michael John; Arne Ringe; Herbert W. Roesky; Dietmar Stalke; Jörg Magull; Hongqi Ye; Inorganic Chemistry 47 (2008) 2585–2592; doi:10.1021/ic701896r

data_4304391
_publ_contact_author_address
;Institut fuer Anorganische Chemie
Universitaet Goettingen
Tammannstr. 4
D-37077 Goettingen, Germany
;
_publ_contact_author_email       hroesky@gwdg.de
_publ_contact_author_fax         0049/551/39-3373
_publ_contact_author_name        'Herber W. Roesky'
_publ_contact_author_phone       0049/551/39-3001
_publ_section_title
;
Synthesis, Characterization, and Reaction of Aluminum Halide Amides
Supported by a Bulky \b-Diketiminato Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2585
_journal_page_last               2592
_journal_paper_doi               10.1021/ic701896r
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C35 H59 Al Cl N3 Si2'
_chemical_formula_weight         640.46
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.3830(5)
_cell_length_b                   18.1958(4)
_cell_length_c                   20.0821(5)
_cell_measurement_temperature    133(2)
_cell_volume                     7448.1(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0394
_diffrn_reflns_av_sigmaI/netI    0.0147
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            72208
_diffrn_reflns_theta_full        24.84
_diffrn_reflns_theta_max         24.84
_diffrn_reflns_theta_min         1.50
_exptl_absorpt_coefficient_mu    0.218
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.142
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2784
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.218
_refine_diff_density_min         -0.253
_refine_diff_density_rms         0.036
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     395
_refine_ls_number_reflns         6420
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0294
_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^)+(0.0494P)^2^+1.9061P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0823
_refine_ls_wR_factor_ref         0.0845
_reflns_number_gt                5675
_reflns_number_total             6420
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701896r-file002_3.cif
_cod_data_source_block           LAl(Cl)N(SiMe3)2
_cod_database_code               4304391