New Route to the Mixed Valence Semiquinone-Catecholate Based Mononuclear FeIII and Catecholate Based Dinuclear MnIII Complexes: First Experimental Evidence of Valence Tautomerism in an Iron Complex
Nizamuddin Shaikh; Sanchita Goswami; Anangamohan Panja; Xin-Yi Wang; Song Gao; Ray J. Butcher; Pradyot Banerjee; Inorganic Chemistry 43 (2004) 5908–5918; doi:10.1021/ic049579i

data_4311617
_publ_section_title
;
 New Route to the Mixed Valence Semiquinone-Catecholate Based Mononuclear
 FeIII and Catecholate Based Dinuclear MnIII Complexes: First Experimental
 Evidence of Valence Tautomerism in an Iron Complex
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5908
_journal_page_last               5918
_journal_paper_doi               10.1021/ic049579i
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C27.5 H21.5 Cl8 Fe N4.5 O4.5'
_chemical_formula_weight         826.44
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 92.19(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.33(2)
_cell_length_b                   28.72(8)
_cell_length_c                   10.81(2)
_cell_measurement_temperature    93(2)
_cell_volume                     2895(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      93(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  '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  0.0863
_diffrn_reflns_av_sigmaI/netI    0.0542
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            19443
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.01
_exptl_absorpt_coefficient_mu    1.310
_exptl_absorpt_correction_T_max  0.862156
_exptl_absorpt_correction_T_min  0.222036
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.897
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chunk
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.64
_refine_diff_density_max         1.329
_refine_diff_density_min         -2.600
_refine_diff_density_rms         0.203
_refine_ls_extinction_coef       0.0023(8)
_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   1.155
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         5823
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.155
_refine_ls_R_factor_all          0.0923
_refine_ls_R_factor_gt           0.0777
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1112P)^2^+16.3337P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1986
_refine_ls_wR_factor_ref         0.2139
_reflns_number_gt                4910
_reflns_number_total             5823
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049579isi20040331_044854.cif
_cod_data_source_block           pbsg2m
_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 

The following automatic conversions were performed:

'_exptl_absorpt_correction_type' tag value 'multi-scans' was replaced
with 'multi-scan' value.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        2894(12)
_cod_original_formula_sum        'C27.50 H21.50 Cl8 Fe N4.50 O4.50'
_cod_database_code               4311617