Syntheses and Structural Characterization of Dinuclear and Tetranuclear Iron(III) Complexes with Dinucleating Ligands and Their Reactions with Hydrogen Peroxide
Lars Westerheide; Felizitas K. Müller; Roberto Than; Bernt Krebs; Jens Dietrich; Siegfried Schindler; Inorganic Chemistry 40 (2001) 1951–1961; doi:10.1021/ic0009371

data_4319499
_publ_contact_author
;
Bernt Krebs
Anorganisch-Chemisches Institut
Westfaelische Wilhelms-Universitaet Muenster
Wilhelm-Klemm-Strasse 8
D-48149 Muenster
Germany
;
_publ_contact_author_email       krebs@.uni-muenster.de
_publ_contact_author_fax         '0049 251 83 383 66'
_publ_contact_author_phone       '0049 251 83 331 31'
_publ_section_title
;
 Syntheses and Structural Characterization of Dinuclear and Tetranuclear
 Iron(III) Complexes with Dinucleating Ligands and Their Reactions with
 Hydrogen Peroxide
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1951
_journal_page_last               1961
_journal_paper_doi               10.1021/ic0009371
_journal_volume                  40
_journal_year                    2001
_chemical_formula_moiety         'C70 H70 N20 O6 F2 Fe4'
_chemical_formula_sum            'C76 H85 Cl4 F2 Fe4 N21 O24'
_chemical_formula_weight         2079.87
_chemical_melting_point          429
_chemical_name_common
'[Fe4(HPTB)2(OH)4(F)2](ClO4)4*CH3CN*C2H5OC2H5*H2O'
_chemical_name_systematic
; 
bis(mu-Fluoro)-bis(mu-N,N,N',N'-tetrakis(2-benzimidazolylmethyl)-2-hydroxy-
1,3-diaminopropane)-tetrahydroxo-tetra-iron(iii) tetraperchlorate
 acetonitrile diethyl ether solvate monohydrate
;
_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     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                84.49(3)
_cell_angle_beta                 79.66(3)
_cell_angle_gamma                88.32(3)
_cell_formula_units_Z            2
_cell_length_a                   14.620(3)
_cell_length_b                   14.851(3)
_cell_length_c                   22.141(4)
_cell_measurement_reflns_used    20135
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      27.0
_cell_measurement_theta_min      2.0
_cell_volume                     4707.0(17)
_computing_cell_refinement       SHELX-PLUS
_computing_data_collection       SHELX-PLUS
_computing_data_reduction        SHELX-PLUS
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      170(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Siemens P3/V'
_diffrn_measurement_method       omega-scan
_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  0.0438
_diffrn_reflns_av_sigmaI/netI    0.1553
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            20911
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.01
_diffrn_standards_decay_%        'not measured'
_diffrn_standards_interval_count 99
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.802
_exptl_absorpt_correction_T_max  none
_exptl_absorpt_correction_T_min  none
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.465
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2110
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.411
_refine_diff_density_min         -0.615
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.929
_refine_ls_hydrogen_treatment    'H atoms refined as riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1183
_refine_ls_number_reflns         20135
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.929
_refine_ls_R_factor_all          0.1618
_refine_ls_R_factor_gt           0.0749
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1198P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2003
_refine_ls_wR_factor_ref         0.2332
_reflns_number_gt                9235
_reflns_number_total             20135
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0009371_5.cif
_cod_data_source_block
'[Fe4(HPTB)2(OH)4(F)2](ClO4)4*CH3CN*C2H5OC2H5*H2O'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' 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        4707.0(16)
_cod_database_code               4319499