Easy Preparation of the Tris(2-fluoro-6-pyridylmethyl)amine Ligand and Instantaneous Reaction of the Corresponding Dichloroferrous Complex with Molecular Dioxygen: New Access to Dinuclear Species
Ahmed Machkour; Dominique Mandon; Mohamed Lachkar; Richard Welter; Inorganic Chemistry 43 (2004) 1545–1550; doi:10.1021/ic034485e

data_4310591
_publ_section_title
;
 Easy Preparation of the Tris(2-fluoro-6-pyridylmethyl)amine Ligand and
 Instantaneous Reaction of the Corresponding Dichloroferrous Complex with
 Molecular Dioxygen: New Access to Dinuclear Species
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1545
_journal_page_last               1550
_journal_paper_doi               10.1021/ic034485e
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety         'C18 H15 Cl4 F3 Fe2 N4 O0.50'
_chemical_formula_sum            'C18 H15 Cl4 F3 Fe2 N4 O0.5'
_chemical_formula_weight         605.84
_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                102.621(5)
_cell_angle_beta                 93.289(5)
_cell_angle_gamma                105.610(5)
_cell_formula_units_Z            2
_cell_length_a                   9.343(5)
_cell_length_b                   9.569(5)
_cell_length_c                   13.696(5)
_cell_measurement_reflns_used    7814
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     1142.0(10)
_computing_cell_refinement       'Denzo (Nonius B.V., 1998)'
_computing_data_collection       'Collect (Nonius B.V., 1998)'
_computing_data_reduction        'Denzo (Nonius B.V., 1998)'
_computing_molecular_graphics    'ATOMS V6 (Dowty, 2002)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '\p scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1707
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5173
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         2.72
_exptl_absorpt_coefficient_mu    1.779
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.762
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             604
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.644
_refine_diff_density_min         -0.551
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         5172
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.1516
_refine_ls_R_factor_gt           0.0829
_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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1290
_refine_ls_wR_factor_ref         0.1481
_reflns_number_gt                3392
_reflns_number_total             5172
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034485esi20030509_060339.cif
_cod_data_source_block           Compound3
_cod_original_formula_sum        'C18 H15 Cl4 F3 Fe2 N4 O0.50'
_cod_database_code               4310591