Magnetic Interactions in the High-Spin Iron(III) Oxooctaethylchlorinato Derivative [Fe(oxoOEC)(Cl)] and Its π-Cation Radical [Fe(oxoOEC.)(Cl)]SbCl6
Teresa J. Neal; Seong-Joo Kang; Ilona Turowska-Tyrk; Charles E. Schulz; W. Robert Scheidt; Inorganic Chemistry 39 (2000) 872–880; doi:10.1021/ic991052w

data_4300184
_publ_section_title
;
Magnetic Interactions in the High-Spin Iron(III) Oxooctaethylchlorinato
Derivative [Fe(oxoOEC)(Cl)] and Its \p-Cation Radical
[Fe(oxoOEC.)(Cl)]SbCl6
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              872
_journal_page_last               880
_journal_paper_doi               10.1021/ic991052w
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C37 H46 Cl9 Fe N4 O Sb'
_chemical_formula_weight         1059.43
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 96.13(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.8419(13)
_cell_length_b                   10.027(2)
_cell_length_c                   22.417(4)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    127(2)
_cell_measurement_theta_max      11.5
_cell_measurement_theta_min      5
_cell_volume                     4434.5(12)
_computing_cell_refinement       MADNES
_computing_data_collection       MADNES
_computing_data_reduction        'MADNES (Messerschmitt & Pflugrath, 1987)'
_computing_molecular_graphics    'ORTEPIII (Burnett, Johnson, 1996)'
_computing_publication_material  'SHELXL-93, CIFTAB'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      127(2)
_diffrn_measurement_device       'ENRAF-NONIUS FAST AREA DETECTOR'
_diffrn_measurement_method       'ellipsoid-mask fitting'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2043
_diffrn_reflns_av_sigmaI/netI    0.0875
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            17600
_diffrn_reflns_theta_max         29.97
_diffrn_reflns_theta_min         2.28
_diffrn_standards_decay_%        'No measurable crystal decay'
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.513
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.751
_exptl_absorpt_correction_type   DIFABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.587
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2136
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.974
_refine_diff_density_min
;
-1.149  0.68 Angstroms away from Sb1
;
_refine_diff_density_rms         0.150
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.045
_refine_ls_goodness_of_fit_obs   0.775
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         9218
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.342
_refine_ls_restrained_S_obs      0.774
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_obs          0.0411
_refine_ls_shift/esd_max         -0.050
_refine_ls_shift/esd_mean        0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0741P)^2^+44.1212P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2061
_refine_ls_wR_factor_obs         0.1104
_reflns_number_observed          7897
_reflns_number_total             9238
_reflns_observed_criterion       >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'Not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0741P)^2^+44.1212P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0741P)^2^+44.1212P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        4434.6(12)
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               4300184