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_4300183
_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            'C36.78 H46 Cl2.57 Fe N4 O'
_chemical_formula_weight         707.15
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                95.79(3)
_cell_angle_beta                 92.03(3)
_cell_angle_gamma                104.84(3)
_cell_formula_units_Z            2
_cell_length_a                   9.174(2)
_cell_length_b                   13.522(3)
_cell_length_c                   14.838(3)
_cell_measurement_reflns_used    231
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      20.5
_cell_measurement_theta_min      -20.5
_cell_volume                     1766.6(7)
_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  SHELXL93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      130(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  0.0992
_diffrn_reflns_av_sigmaI/netI    0.1195
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            16498
_diffrn_reflns_theta_max         29.77
_diffrn_reflns_theta_min         2.21
_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    0.656
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'flat plate'
_exptl_crystal_F_000             745
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.925
_refine_diff_density_min         -0.880
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
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_refine_ls_goodness_of_fit_obs   1.080
_refine_ls_hydrogen_treatment    constr
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_refine_ls_restrained_S_obs      1.080
_refine_ls_R_factor_all          0.1657
_refine_ls_R_factor_obs          0.0950
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+13.5049P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2163
_refine_ls_wR_factor_obs         0.1687
_reflns_number_observed          5266
_reflns_number_total             8848
_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^)+(0.0000P)^2^+13.5049P] 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^)+(0.0000P)^2^+13.5049P] 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        1766.6(6)
_cod_database_code               4300183