Synthesis, Characterization, and Study of Octanuclear Iron-Oxo Clusters Containing a Redox-Active Fe4O4-Cubane Core
Peter Baran; Roman Boča; Indranil Chakraborty; John Giapintzakis; Radovan Herchel; Qing Huang; John E. McGrady; Raphael G. Raptis; Yiannis Sanakis; Athanasios Simopoulos; Inorganic Chemistry 47 (2008) 645–655; doi:10.1021/ic7020337

data_4304535
_publ_section_title
;
Synthesis, Characterization, and Study of Octanuclear Iron-Oxo Clusters
Containing a Redox-Active Fe4O4-Cubane Core
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              645
_journal_page_last               655
_journal_paper_doi               10.1021/ic7020337
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         '[Fe8(mu4-O)4(mu-pz)12Br4]'
_chemical_formula_sum            'C36 H36 Br4 Fe8 N24 O4'
_chemical_formula_weight         1635.33
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 93.492(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.847(2)
_cell_length_b                   21.517(4)
_cell_length_c                   20.030(4)
_cell_measurement_temperature    298(2)
_cell_volume                     5526.6(17)
_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      298(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.1233
_diffrn_reflns_av_sigmaI/netI    0.1683
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            27721
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         1.39
_exptl_absorpt_coefficient_mu    4.991
_exptl_absorpt_correction_T_max  0.9777
_exptl_absorpt_correction_T_min  0.4329
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.965
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3200
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.737
_refine_diff_density_min         -0.498
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.933
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     685
_refine_ls_number_reflns         9938
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.933
_refine_ls_R_factor_all          0.1786
_refine_ls_R_factor_gt           0.0589
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0579P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1058
_refine_ls_wR_factor_ref         0.1465
_reflns_number_gt                4290
_reflns_number_total             9938
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic7020337-file004_4.cif
_cod_data_source_block           for_compound_[Fe8(m4-O)4(m-pz)12Br4],_4.
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_cell_volume        5526.5(17)
_cod_database_code               4304535