Molecular and Electronic Structures of Iron(II)/(III) Complexes Containing N,S-Coordinated, Closed-Shello-Aminothiophenolato(1-) and o-Iminothiophenolato(2-) Ligands
Prasanta Ghosh; Ameerunisha Begum; Eckhard Bill; Thomas Weyhermüller; Karl Wieghardt; Inorganic Chemistry 42 (2003) 3208–3215; doi:10.1021/ic020617c

data_4313592
_publ_section_title
;
 Molecular and Electronic Structures of Iron(II)/(III) Complexes
 Containing N,S-Coordinated, Closed-Shello-Aminothiophenolato(1-) and
 o-Iminothiophenolato(2-) Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3208
_journal_page_last               3215
_journal_paper_doi               10.1021/ic020617c
_journal_volume                  42
_journal_year                    2003
_chemical_formula_structural     '3[C28 H24 Fe2 N4 S4], 2.5 CH2CL2'
_chemical_formula_sum            'C28.83 H25.67 Cl1.67 Fe2 N4 S4'
_chemical_formula_weight         727.22
_chemical_name_systematic
;
 ?
;
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                70.96(1)
_cell_angle_beta                 75.89(1)
_cell_angle_gamma                75.30(1)
_cell_formula_units_Z            6
_cell_length_a                   13.9882(8)
_cell_length_b                   16.4986(10)
_cell_length_c                   20.688(2)
_cell_measurement_reflns_used    6844
_cell_measurement_temperature    100(2)
_cell_volume                     4297.3(6)
_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-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measurement_device       'Nonius Kappa-CCD'
_diffrn_measurement_method       '392 images at 1 deg. in \w and 160 sec.'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating Mo-anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0732
_diffrn_reflns_av_sigmaI/netI    0.1144
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            24954
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         3.81
_exptl_absorpt_coefficient_mu    1.489
_exptl_absorpt_correction_T_max  0.9659
_exptl_absorpt_correction_T_min  0.9109
_exptl_absorpt_correction_type   'Gaussian, face-indexed'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.686
_exptl_crystal_description       'opaque parallelepiped'
_exptl_crystal_F_000             2226
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.820
_refine_diff_density_min         -0.966
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.027
_refine_ls_goodness_of_fit_obs   1.121
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1097
_refine_ls_number_reflns         10969
_refine_ls_number_restraints     18
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_refine_ls_restrained_S_obs      1.121
_refine_ls_R_factor_all          0.1229
_refine_ls_R_factor_obs          0.0671
_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^)+(0.0426P)^2^+25.3249P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1604
_refine_ls_wR_factor_obs         0.1327
_reflns_number_observed          7136
_reflns_number_total             11052
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic020617c_6.cif
_cod_data_source_block           8
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0426P)^2^+25.3249P] 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^)+(0.0426P)^2^+25.3249P] 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        4297.3(5)
_cod_database_code               4313592