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_4319495
_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         'C36 H36 N12 O8 Fe2'
_chemical_formula_sum            'C40.5 H54 Fe2 N14 O18.5'
_chemical_formula_weight         1144.68
_chemical_melting_point          612
_chemical_name_common            '[Fe2(HPTB)(OCH3)(ONO2)2](NO3)2*4.5CH3OH'
_chemical_name_systematic
; 
(mu-N,N,N',N'-tetrakis(2-benzimidazolylmethyl)-2-hydroxy-1,3-diaminopropane)
-(mu-methoxo)-bis(nitrato-O)di-iron(iii) dinitrate penta methanol solvent
;
_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                65.95(3)
_cell_angle_beta                 72.08(3)
_cell_angle_gamma                74.22(3)
_cell_formula_units_Z            2
_cell_length_a                   12.435(2)
_cell_length_b                   15.383(3)
_cell_length_c                   16.053(3)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      25.9
_cell_measurement_theta_min      4.3
_cell_volume                     2629.9(11)
_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      213(2)
_diffrn_measured_fraction_theta_full 0.927
_diffrn_measured_fraction_theta_max 0.927
_diffrn_measurement_device_type  'STOE IPDS'
_diffrn_measurement_method       phi-Rotation
_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  0.1148
_diffrn_reflns_av_sigmaI/netI    0.1275
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            20634
_diffrn_reflns_theta_full        25.87
_diffrn_reflns_theta_max         25.87
_diffrn_reflns_theta_min         4.28
_exptl_absorpt_coefficient_mu    0.635
_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            red
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needles
_exptl_crystal_F_000             1190
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.779
_refine_diff_density_min         -0.631
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    'H atoms refined as riding models'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     690
_refine_ls_number_reflns         9449
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.1299
_refine_ls_R_factor_gt           0.0725
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0798P)^2^+1.2571P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1617
_refine_ls_wR_factor_ref         0.1887
_reflns_number_gt                5685
_reflns_number_total             9449
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0009371_1.cif
_cod_data_source_block           '[Fe2(HPTB)(OCH3)(ONO2)2](NO3)2*4.5CH3OH'
_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        2629.9(8)
_cod_original_formula_sum        'C40.50 H54 Fe2 N14 O18.50'
_cod_database_code               4319495