Synthesis and Reactivity of Bi-, Tri-, and Hexametallic and Zwitterionic Methyl Aluminum Complexes Containing a Phenoxide/Imine Ligand System
Andrew Cottone, III; Dolores Morales; Jennifer L. Lecuivre; Michael J. Scott; Organometallics 21 (2002) 418–428; doi:10.1021/om010773b

data_4060761
_publ_section_title
;
 Synthesis and Reactivity of Bi-, Tri-, and Hexametallic and
 Zwitterionic Methyl Aluminum Complexes Containing a Phenoxide/Imine
 Ligand System
;
_journal_name_full               Organometallics
_journal_page_first              418
_journal_page_last               428
_journal_paper_doi               10.1021/om010773b
_journal_volume                  21
_journal_year                    2002
_chemical_formula_sum            'C44.25 H59.5 Al2 Cl2.5 N O4 S'
_chemical_formula_weight         844.07
_chemical_name_common            121CH2Cl2
_chemical_name_systematic
; 
 [(5){AlMe2}{AlMe(OSMe2)}] 
;
_space_group_IT_number           14
_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                 99.9510(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.7251(8)
_cell_length_b                   15.7782(10)
_cell_length_c                   23.4282(14)
_cell_measurement_temperature    173(2)
_cell_volume                     4633.1(5)
_computing_cell_refinement       'Bruker AXS SMART'
_computing_data_collection       'Bruker AXS SMART'
_computing_data_reduction        'Bruker AXS SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_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  0.0893
_diffrn_reflns_av_sigmaI/netI    0.1060
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            32324
_diffrn_reflns_theta_full        28.34
_diffrn_reflns_theta_max         28.34
_diffrn_reflns_theta_min         1.56
_exptl_absorpt_coefficient_mu    0.292
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.593566
_exptl_absorpt_correction_type   'Corrected by SADABS'
_exptl_crystal_density_diffrn    1.210
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1794
_refine_diff_density_max         0.418
_refine_diff_density_min         -0.364
_refine_diff_density_rms         0.059
_refine_ls_extinction_coef       0.0014(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   0.903
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     475
_refine_ls_number_reflns         11290
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.903
_refine_ls_R_factor_all          0.1076
_refine_ls_R_factor_gt           0.0549
_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^)+(0.0662P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1289
_refine_ls_wR_factor_ref         0.1419
_reflns_number_gt                6103
_reflns_number_total             11290
_reflns_threshold_expression     >2sigma(I)
_cod_original_sg_symbol_H-M      P12(1)/n1
_cod_original_formula_sum        'C44.25 H59.50 Al2 Cl2.50 N O4 S'
_cod_database_code               4060761