Unusual mixed valent FeIIIFeII complex (St = 3/2) stabilised by a reduced bulky 1,2-diketone.
Spikes, Geoffrey H; Bill, Eckhard; Weyhermüller, Thomas; Wieghardt, Karl; Chemical communications (Cambridge, England)  (2007) 4339–4341; doi:10.1039/b713062g

data_7102243
_publ_section_title
;
 Unusual mixed valent FeIIIFeII complex (St = 3/2) stabilised by a
 reduced bulky 1,2-diketone.
;
_journal_issue                   42
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              4339
_journal_page_last               4341
_journal_paper_doi               10.1039/b713062g
_journal_year                    2007
_chemical_formula_moiety
'[C12 H30 O6 Na]+, [C56 H78 Br2 Fe2 O6]-, 0.5 (C5 H12)'
_chemical_formula_sum            'C70.5 H114 Br2 Fe2 Na O12'
_chemical_formula_weight         1448.13
_chemical_name_systematic
;
?
;
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_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            16
_cell_length_a                   38.156(2)
_cell_length_b                   50.415(3)
_cell_length_c                   15.8144(8)
_cell_measurement_temperature    100(2)
_cell_volume                     30421(3)
_computing_cell_refinement       'Bruker AXS Collect Software'
_computing_data_collection       'Bruker AXS Collect Software'
_computing_data_reduction        'Bruker AXS Collect Software'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker-Nonius Kappa-CCD'
_diffrn_measurement_method
'1750 images at 0.3 deg. stepwise rotation in omega and phi, 54 sec./frame'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode, 50 kV, 80 mA'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0732
_diffrn_reflns_av_sigmaI/netI    0.0927
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_h_min       -49
_diffrn_reflns_limit_k_max       65
_diffrn_reflns_limit_k_min       -65
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            53720
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.99
_exptl_absorpt_coefficient_mu    1.492
_exptl_absorpt_correction_T_max  0.9562
_exptl_absorpt_correction_T_min  0.8118
_exptl_absorpt_correction_type   gaussian
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.265
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'transparent block'
_exptl_crystal_F_000             12256
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.500
_refine_diff_density_min         -0.322
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.042(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     807
_refine_ls_number_reflns         16048
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0882
_refine_ls_R_factor_gt           0.0494
_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^)+(0.0353P)^2^+25.5639P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0872
_refine_ls_wR_factor_ref         0.0990
_reflns_number_gt                11475
_reflns_number_total             16048
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b713062g.txt
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Gaussian' changed to 'gaussian'
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_sg_symbol_H-M      Fdd2
_cod_original_formula_sum        'C70.50 H114 Br2 Fe2 Na O12'
_cod_database_code               7102243