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_4307413
_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         'C24 H24 Cl18 Fe3 O16'
_chemical_formula_sum            'C24 H24 Cl18 Fe3 O16'
_chemical_formula_weight         1374.08
_chemical_name_systematic
;
Tris(N,N-tetrahydrofurane)(\m~3~-oxo)
hexakis(\m~2~-trichloroacetate)diiron(iii)iron(ii)
;
_space_group_IT_number           166
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3 2"'
_symmetry_space_group_name_H-M   'R -3 m :H'
_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                120.00
_cell_formula_units_Z            6
_cell_length_a                   18.3606(5)
_cell_length_b                   18.3606(5)
_cell_length_c                   26.0896(9)
_cell_measurement_reflns_used    315
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.15
_cell_measurement_theta_min      2.01
_cell_volume                     7616.8(4)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker P4'
_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  0.0793
_diffrn_reflns_av_sigmaI/netI    0.0327
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            33624
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         1.50
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.850
_exptl_absorpt_correction_T_max  0.645
_exptl_absorpt_correction_T_min  0.538
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.797
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             4080
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.590
_refine_diff_density_min         -0.434
_refine_diff_density_rms         0.086
_refine_ls_extinction_coef       0.00015(12)
_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   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     121
_refine_ls_number_reflns         2704
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.1186
_refine_ls_R_factor_gt           0.0614
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1193P)^2^+19.2374P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1825
_refine_ls_wR_factor_ref         0.2343
_reflns_number_gt                1393
_reflns_number_total             2704
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061903hsi20061005_084356.cif
_cod_data_source_block           fetri1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal' 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 
;
_cod_original_sg_symbol_H-M      'R -3 m'
_cod_database_code               4307413