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_4311618
_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            'C22.5 H17.5 Cl8 Mn N3 O5'
_chemical_formula_weight         748.43
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 114.986(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.061(6)
_cell_length_b                   15.918(5)
_cell_length_c                   18.498(3)
_cell_measurement_temperature    93(2)
_cell_volume                     5621(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      93(2)
_diffrn_measured_fraction_theta_full 0.932
_diffrn_measured_fraction_theta_max 0.932
_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  0.0418
_diffrn_reflns_av_sigmaI/netI    0.0434
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            24648
_diffrn_reflns_theta_full        29.28
_diffrn_reflns_theta_max         29.28
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    1.272
_exptl_absorpt_correction_T_max  0.928083
_exptl_absorpt_correction_T_min  0.759179
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.769
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2996
_refine_diff_density_max         0.474
_refine_diff_density_min         -0.339
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         7152
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0348
_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^)+(0.0348P)^2^+4.1089P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0715
_refine_ls_wR_factor_ref         0.0779
_reflns_number_gt                5450
_reflns_number_total             7152
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049579isi20040331_044943.cif
_cod_data_source_block           pbmn2m
_cod_depositor_comments
;
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        5621(2)
_cod_original_formula_sum        'C22.50 H17.50 Cl8 Mn N3 O5'
_cod_database_code               4311618