A Mixed-Valence Octanuclear Iron-Oxo Pyrazolate: Assessment of Electronic Delocalization by Structural and Spectroscopic Analysis
Indranil Chakraborty; Peter Baran; Yiannis Sanakis; Athanassios Simopoulos; Esteban Fachini; Raphael G. Raptis; Inorganic Chemistry 47 (2008) 11734–11737; doi:10.1021/ic801459s

data_4306646
_publ_section_title
;
A Mixed-Valence Octanuclear Iron-Oxo Pyrazolate: Assessment of Electronic
Delocalization by Structural and Spectroscopic Analysis
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11734
_journal_page_last               11737
_journal_paper_doi               10.1021/ic801459s
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         (Bu4N)[Fe8(mu4-O)4(mu-4Clpz)12Cl4]
_chemical_formula_sum            'C52 H60 Cl16 Fe8 N25 O4'
_chemical_formula_weight         2113.25
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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            4
_cell_length_a                   18.078(4)
_cell_length_b                   26.212(5)
_cell_length_c                   18.023(4)
_cell_measurement_reflns_used    989
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      51.72
_cell_measurement_theta_min      5.28
_cell_volume                     8540(3)
_computing_cell_refinement       'BRUKER SMART-NT V5.0'
_computing_data_collection       'BRUKER SMART-NT V5.0'
_computing_data_reduction        'BRUKER SAINT-NT V5/6.0'
_computing_molecular_graphics    'BRUKER SHELXTL-NT V5.1'
_computing_publication_material  'BRUKER SHELXTL-NT V5.1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.935
_diffrn_measured_fraction_theta_max 0.935
_diffrn_measurement_device_type  'Bruker AXS SMART CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0733
_diffrn_reflns_av_sigmaI/netI    0.0815
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            53521
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         1.55
_exptl_absorpt_coefficient_mu    1.875
_exptl_absorpt_correction_T_max  0.386
_exptl_absorpt_correction_T_min  0.302
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   XPREP
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.644
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4236
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.418
_refine_diff_density_min         -0.349
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.858
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     476
_refine_ls_number_reflns         9905
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      0.863
_refine_ls_R_factor_all          0.1306
_refine_ls_R_factor_gt           0.0399
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0614P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0883
_refine_ls_wR_factor_ref         0.1206
_reflns_number_gt                4353
_reflns_number_total             9905
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801459s_si_001.cif
_cod_data_source_block           ic004f
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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               4306646