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_4112103
_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            'C92 H132 Al4 Cl2 Fe2 N6'
_chemical_formula_weight         1612.56
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                82.262(6)
_cell_angle_beta                 89.088(6)
_cell_angle_gamma                87.984(6)
_cell_formula_units_Z            2
_cell_length_a                   10.676(4)
_cell_length_b                   19.708(7)
_cell_length_c                   21.150(7)
_cell_measurement_reflns_used    249
_cell_measurement_temperature    207(2)
_cell_measurement_theta_max      21.97
_cell_measurement_theta_min      2.09
_cell_volume                     4406(3)
_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      207(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_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  0.0499
_diffrn_reflns_av_sigmaI/netI    0.0565
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            31293
_diffrn_reflns_theta_full        21.97
_diffrn_reflns_theta_max         21.97
_diffrn_reflns_theta_min         2.09
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    0.477
_exptl_absorpt_correction_T_max  0.9106
_exptl_absorpt_correction_T_min  0.8508
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker (2000)'
_exptl_crystal_colour            dk_red
_exptl_crystal_density_diffrn    1.215
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1728
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.753
_refine_diff_density_min         -0.316
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     928
_refine_ls_number_reflns         10504
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.1016
_refine_ls_R_factor_gt           0.0673
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0971P)^2^+5.1489P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1660
_refine_ls_wR_factor_ref         0.1880
_reflns_number_gt                7222
_reflns_number_total             10504
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja056135ssi20051019_111023.cif
_cod_data_source_block           sg2714
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'n/a' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        4407(3)
_cod_database_code               4112103