Synthesis and Reactivity of Haloacetato Derivatives of Iron(II) Including the Crystal and the Molecular Structure of [Fe(CF3COOH)2(μ-CF3COO)2]n
Fabio Marchetti; Fabio Marchetti; Bernardo Melai; Guido Pampaloni; Stefano Zacchini; Inorganic Chemistry 46 (2007) 3378–3384; doi:10.1021/ic061903h

data_4307416
_publ_section_title
;
Synthesis and Reactivity of Haloacetato Derivatives of Iron(II) Including
the Crystal and the Molecular Structure of [Fe(CF3COOH)2(\m-CF3COO)2]n
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3378
_journal_page_last               3384
_journal_paper_doi               10.1021/ic061903h
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         'C28 H28 F24 Fe4 N4 O22'
_chemical_formula_sum            'C28 H28 F24 Fe4 N4 O22'
_chemical_formula_weight         1451.94
_chemical_name_systematic
;
Tetrakis(N,N-dimethylformamide)bis(\m~3~-oxo)
hexakis(\m~2~-trifluoroacetate)bis(O-acetate)tetrairon(iii)
;
_space_group_IT_number           122
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4 2bw'
_symmetry_space_group_name_H-M   'I -4 2 d'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.0900(10)
_cell_length_b                   16.0900(10)
_cell_length_c                   48.867(4)
_cell_measurement_reflns_used    35
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      10.96
_cell_measurement_theta_min      6.63
_cell_volume                     12651.1(15)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Ital-Structures XCS'
_computing_data_reduction        'Darx 2000'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'WINGX-1.64 (Farrugia, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.607
_diffrn_measured_fraction_theta_max 0.607
_diffrn_measurement_device_type  Ital-Structures
_diffrn_measurement_method       '2\q/\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0218
_diffrn_reflns_av_sigmaI/netI    0.0387
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       57
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            4027
_diffrn_reflns_theta_full        24.90
_diffrn_reflns_theta_max         24.90
_diffrn_reflns_theta_min         2.44
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.033
_exptl_absorpt_correction_T_max  0.6166
_exptl_absorpt_correction_T_min  0.5143
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'Deep red'
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             5760
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.539
_refine_diff_density_min         -0.396
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.04(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     294
_refine_ls_number_reflns         2113
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0668
_refine_ls_R_factor_gt           0.0617
_refine_ls_shift/su_max          0.085
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0911P)^2^+61.9362P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1580
_refine_ls_wR_factor_ref         0.1644
_reflns_number_gt                1972
_reflns_number_total             2113
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             4307415
_cod_data_source_file            ic061903hsi20061005_084432.cif
_cod_data_source_block           ferox_rs
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
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_cod_database_code               4307416