N,N-Coordinated π Radical Anions of S-Methyl-1-phenyl-isothiosemicarbazide in Two Five-Coordinate Ferric Complexes [FeIII(LMe.)2X] (X = CH3S-, Cl-)
Sebastien Blanchard; Eckhard Bill; Thomas Weyhermüller; Karl Wieghardt; Inorganic Chemistry 43 (2004) 2324–2329; doi:10.1021/ic030285r

data_4310774
_publ_section_title
;
 N,N-Coordinated \p Radical Anions of
 S-Methyl-1-phenyl-isothiosemicarbazide in Two Five-Coordinate Ferric
 Complexes [FeIII(LMe.)2X] (X = CH3S-, Cl-)
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2324
_journal_page_last               2329
_journal_paper_doi               10.1021/ic030285r
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C17 H21 Fe N6 S3'
_chemical_formula_weight         461.43
_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                 98.50(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.5163(4)
_cell_length_b                   9.6966(4)
_cell_length_c                   22.3302(8)
_cell_measurement_temperature    100(2)
_cell_volume                     2037.90(15)
_computing_cell_refinement       'DENZO, Nonius Collect Software'
_computing_data_collection       'DENZO, Nonius Collect Software'
_computing_data_reduction        'DENZO, Nonius 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 0.948
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device_type  'Nonius Kappa-CCD'
_diffrn_measurement_method       '1381 images at 1.0 deg. in \w and 20 sec.'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
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_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
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_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            68068
_diffrn_reflns_theta_full        31.02
_diffrn_reflns_theta_max         31.02
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    1.062
_exptl_absorpt_correction_T_max  0.8743
_exptl_absorpt_correction_T_min  0.8400
_exptl_absorpt_correction_type   'Gaussian, face-indexed'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'transparent parallelepiped'
_exptl_crystal_F_000             956
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.443
_refine_diff_density_min         -0.448
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
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_refine_ls_number_parameters     253
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_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0255P)^2^+1.2492P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0616
_refine_ls_wR_factor_ref         0.0629
_reflns_number_gt                6062
_reflns_number_total             6493
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic030285r_1.cif
_cod_data_source_block           1(ST4409)
_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:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0255P)^2^+1.2492P] 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^)+(0.0255P)^2^+1.2492P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_original_cell_volume        2037.9(2)
_cod_database_code               4310774