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_4304390
_publ_contact_author
'Prof. Dr. Dietmar Stalke; Prof. Dr. Herbert Roesky'
_publ_contact_author_email
'dstalke@chemie.uni-goettingen.de, hroesky@gwdg.de'
_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 H55 Al Cl N3'
_chemical_formula_weight         580.25
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 97.4050(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.0276(8)
_cell_length_b                   20.3125(16)
_cell_length_c                   16.7958(13)
_cell_measurement_reflns_used    9863
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.16
_cell_measurement_theta_min      2.46
_cell_volume                     3392.5(5)
_computing_cell_refinement       'SAINT V7.23A'
_computing_data_collection       'APEX2 v2.1.0'
_computing_data_reduction        'SAINT V7.23A'
_computing_molecular_graphics    'XP in SHELXTL ver. 6.12'
_computing_publication_material  'XP in SHELXTL ver. 6.12'
_computing_structure_refinement  'SHELXL in SHELXTL ver. 6.12'
_computing_structure_solution    'SHELXS in SHELXTL ver. 6.12'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Smart Apex II with D8-Goniometer'
_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  0.0264
_diffrn_reflns_av_sigmaI/netI    0.0162
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            38060
_diffrn_reflns_theta_full        25.21
_diffrn_reflns_theta_max         25.21
_diffrn_reflns_theta_min         2.64
_exptl_absorpt_coefficient_mu    0.165
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.894196
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS v2.10'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.136
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.286
_refine_diff_density_min         -0.282
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     375
_refine_ls_number_reflns         6089
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0329
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0472P)^2^+1.4306P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0877
_refine_ls_wR_factor_ref         0.0918
_reflns_number_gt                5390
_reflns_number_total             6089
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701896r-file002_2.cif
_cod_data_source_block           LAl(Cl)NiPr2
_cod_database_code               4304390