Formation of a Paramagnetic Al Complex and Extrusion of Fe during the Reaction of (Diiminepyridine)Fe with AlR3 (R = Me, Et)
Jennifer Scott; Sandro Gambarotta; Ilia Korobkov; Quinten Knijnenburg; Bas de Bruin; Peter H. M. Budzelaar; Journal of the American Chemical Society 127 (2005) 17204–17206; doi:10.1021/ja056135s

data_4112102
_publ_section_title
;
 Formation of a Paramagnetic Al Complex and Extrusion of Fe during the
 Reaction of (Diiminepyridine)Fe with AlR3 (R = Me, Et)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17204
_journal_page_last               17206
_journal_paper_doi               10.1021/ja056135s
_journal_volume                  127
_journal_year                    2005
_chemical_formula_sum            'C49 H65 Al N3'
_chemical_formula_weight         723.02
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yc'
_symmetry_space_group_name_H-M   'P 1 c 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                 98.068(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.727(6)
_cell_length_b                   12.871(7)
_cell_length_c                   16.300(9)
_cell_measurement_reflns_used    353
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      17.53
_cell_measurement_theta_min      2.91
_cell_volume                     2228(2)
_computing_cell_refinement       'SMART, Bruker (2000)'
_computing_data_collection       'SMART, Bruker (2000)'
_computing_data_reduction        'XPREP, Bruker (2000)'
_computing_molecular_graphics    'SHELXTL, Bruker (2000)'
_computing_publication_material  'SHELXTL, Bruker (2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and 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  0.1378
_diffrn_reflns_av_sigmaI/netI    0.1738
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8193
_diffrn_reflns_theta_full        18.86
_diffrn_reflns_theta_max         18.86
_diffrn_reflns_theta_min         2.49
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    0.080
_exptl_absorpt_correction_T_max  0.9984
_exptl_absorpt_correction_T_min  0.9920
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker (2000)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.078
_exptl_crystal_description       block
_exptl_crystal_F_000             786
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.200
_refine_diff_density_min         -0.204
_refine_diff_density_rms         0.048
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   1.1(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     297
_refine_ls_number_reflns         3453
_refine_ls_number_restraints     357
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.1492
_refine_ls_R_factor_gt           0.0758
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'calc w=1/[\s^2^(Fo^2^)+(0.0505P)^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1360
_refine_ls_wR_factor_ref         0.1612
_reflns_number_gt                1925
_reflns_number_total             3453
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja056135ssi20051019_111002.cif
_cod_data_source_block           sg2378
_cod_database_code               4112102