Remarkable Room-Temperature Insertion of Carbon Monoxide into an Aluminum-Carbon Bond of Tri-tert-butylaluminum
Mark R. Mason; Bingxu Song; Kristin Kirschbaum; Journal of the American Chemical Society 126 (2004) 11812–11813; doi:10.1021/ja046411n

data_4112963
_publ_contact_author
;
     Professor Mark R. Mason
     Department of Chemistry
     MS 602
     University of Toledo
     Toledo
     OH 43606
     USA
;
_publ_contact_author_email       mmason5@uoft02.utoledo.edu
_publ_contact_author_fax         '(419) 530-4033'
_publ_contact_author_phone       '(419) 530-1532'
_publ_section_title
;
 Remarkable Room-Temperature Insertion of Carbon Monoxide into an
 Aluminum-Carbon Bond of Tri-tert-butylaluminum
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11812
_journal_page_last               11813
_journal_paper_doi               10.1021/ja046411n
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C26 H54 Al2 O2'
_chemical_formula_weight         452.65
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.712(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.5511(9)
_cell_length_b                   11.6180(13)
_cell_length_c                   14.657(2)
_cell_measurement_reflns_used    639
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      17.5
_cell_measurement_theta_min      2.7
_cell_volume                     1456.0(3)
_computing_cell_refinement       'Saintplus 6.22'
_computing_data_collection       Smart5.57
_computing_data_reduction        'Saintplus 6.22'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(1)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker platform with 1K CCD'
_diffrn_measurement_method       \w-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  0.0276
_diffrn_reflns_av_sigmaI/netI    0.0324
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8377
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.24
_exptl_absorpt_coefficient_mu    0.118
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.823
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
Sheldrick, G.M. (1996). SADABS, Univ. G\"ottingen. 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.032
_exptl_crystal_description       'parallel pipet'
_exptl_crystal_F_000             504
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.375
_refine_diff_density_min         -0.286
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.322
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         2858
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.322
_refine_ls_R_factor_all          0.0695
_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
'calc w=1/[\s^2^(Fo^2^)+(0.0253P)^2^+1.3073P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1156
_refine_ls_wR_factor_ref         0.1186
_reflns_number_gt                2593
_reflns_number_total             2858
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja046411nsi20040824_045053.cif
_cod_data_source_block           1
_cod_database_code               4112963