#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:33:47 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179146 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/07/4310775.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4310775
loop_
_publ_author_name
'Sebastien Blanchard'
'Eckhard Bill'
'Thomas Weyhermüller'
'Karl Wieghardt'
_publ_section_title
;
 N,N-Coordinated π Radical Anions of
 S-Methyl-1-phenyl-isothiosemicarbazide in Two Five-Coordinate Ferric
 Complexes [FeIII(LMe.)2X] (X = CH3S-, Cl-)
;
_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            'C16 H18 Cl Fe N6 S2'
_chemical_formula_weight         449.78
_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-97
_cell_angle_alpha                108.72(1)
_cell_angle_beta                 100.12(1)
_cell_angle_gamma                98.56(1)
_cell_formula_units_Z            2
_cell_length_a                   8.9628(6)
_cell_length_b                   9.8292(6)
_cell_length_c                   12.0455(6)
_cell_measurement_temperature    100(2)
_cell_volume                     965.13(13)
_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 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Nonius Kappa-CCD'
_diffrn_measurement_method       '740 images at 1.0 deg. in ω and 90 sec.'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_av_sigmaI/netI    0.0467
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            17694
_diffrn_reflns_theta_full        31.01
_diffrn_reflns_theta_max         31.01
_diffrn_reflns_theta_min         3.37
_exptl_absorpt_coefficient_mu    1.149
_exptl_absorpt_correction_T_max  0.9663
_exptl_absorpt_correction_T_min  0.8286
_exptl_absorpt_correction_type   'Gaussian, face-indexed'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'transparent needle'
_exptl_crystal_F_000             462
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.668
_refine_diff_density_min         -1.333
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         6088
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0568
_refine_ls_R_factor_gt           0.0462
_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/[σ²(Fo²)+(0.0297P)²+1.8204P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1050
_refine_ls_wR_factor_ref         0.1106
_reflns_number_gt                5220
_reflns_number_total             6088
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic030285r_2.cif
_cod_data_source_block           2(ST4422)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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^)+(0.0297P)^2^+1.8204P] 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^)+(0.0297P)^2^+1.8204P] 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        965.13(10)
_cod_database_code               4310775
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.79567(3) 0.92935(3) 1.77593(3) 0.01604(8) Uani 1 d . . .
Cl1 Cl 0.60231(6) 0.99398(6) 1.66581(5) 0.01623(10) Uani 1 d . . .
C1 C 1.2075(3) 0.9722(4) 1.5675(3) 0.0384(7) Uani 1 d . . .
H1A H 1.1274 1.0249 1.5493 0.058 Uiso 1 calc R . .
H1B H 1.2785 0.9714 1.5142 0.058 Uiso 1 calc R . .
H1C H 1.2659 1.0218 1.6517 0.058 Uiso 1 calc R . .
S2 S 1.11754(8) 0.78660(10) 1.54445(6) 0.03732(18) Uani 1 d . . .
C3 C 0.9783(3) 0.8141(3) 1.6300(2) 0.0227(5) Uani 1 d . . .
N4 N 0.8707(2) 0.6922(2) 1.61136(19) 0.0242(4) Uani 1 d . . .
N5 N 0.7691(2) 0.7308(2) 1.67795(18) 0.0191(4) Uani 1 d . . .
C6 C 0.6516(3) 0.6101(3) 1.6681(2) 0.0220(4) Uani 1 d . . .
C7 C 0.6836(4) 0.4720(3) 1.6518(3) 0.0334(6) Uani 1 d . . .
H7 H 0.7848 0.4564 1.6473 0.040 Uiso 1 calc R . .
C8 C 0.5653(4) 0.3567(3) 1.6422(3) 0.0432(8) Uani 1 d . . .
H8 H 0.5861 0.2619 1.6316 0.052 Uiso 1 calc R . .
C9 C 0.4183(4) 0.3788(3) 1.6479(3) 0.0426(8) Uani 1 d . . .
H9 H 0.3383 0.2991 1.6407 0.051 Uiso 1 calc R . .
C10 C 0.3864(4) 0.5166(3) 1.6639(3) 0.0353(6) Uani 1 d . . .
H10 H 0.2849 0.5314 1.6683 0.042 Uiso 1 calc R . .
C11 C 0.5030(3) 0.6331(3) 1.6737(2) 0.0257(5) Uani 1 d . . .
H11 H 0.4816 0.7276 1.6842 0.031 Uiso 1 calc R . .
N12 N 0.9691(2) 0.9395(2) 1.70691(18) 0.0204(4) Uani 1 d . . .
H12 H 1.045(4) 1.018(3) 1.720(3) 0.025 Uiso 1 d . . .
C21 C 0.5471(3) 0.8188(3) 2.0746(2) 0.0239(5) Uani 1 d . . .
H21A H 0.4692 0.7984 1.9998 0.036 Uiso 1 calc R . .
H21B H 0.4949 0.8084 2.1373 0.036 Uiso 1 calc R . .
H21C H 0.6154 0.7491 2.0602 0.036 Uiso 1 calc R . .
S22 S 0.66089(6) 1.00401(7) 2.12314(5) 0.02015(12) Uani 1 d . . .
C23 C 0.7398(2) 0.9974(3) 1.9991(2) 0.0172(4) Uani 1 d . . .
N24 N 0.8341(2) 1.1250(2) 2.01174(17) 0.0184(4) Uani 1 d . . .
N25 N 0.8753(2) 1.1094(2) 1.90752(17) 0.0169(3) Uani 1 d . . .
C26 C 0.9800(2) 1.2354(2) 1.9110(2) 0.0180(4) Uani 1 d . . .
C27 C 1.0841(2) 1.3304(3) 2.0185(2) 0.0204(4) Uani 1 d . . .
H27 H 1.0842 1.3134 2.0918 0.024 Uiso 1 calc R . .
C28 C 1.1871(3) 1.4496(3) 2.0169(2) 0.0246(5) Uani 1 d . . .
H28 H 1.2585 1.5139 2.0895 0.029 Uiso 1 calc R . .
C29 C 1.1869(3) 1.4761(3) 1.9104(3) 0.0261(5) Uani 1 d . . .
H29 H 1.2587 1.5574 1.9101 0.031 Uiso 1 calc R . .
C30 C 1.0812(3) 1.3830(3) 1.8039(2) 0.0261(5) Uani 1 d . . .
H30 H 1.0803 1.4016 1.7311 0.031 Uiso 1 calc R . .
C31 C 0.9771(3) 1.2631(3) 1.8040(2) 0.0223(4) Uani 1 d . . .
H31 H 0.9044 1.2002 1.7316 0.027 Uiso 1 calc R . .
N32 N 0.7113(2) 0.8859(2) 1.89685(18) 0.0178(3) Uani 1 d . . .
H32 H 0.649(3) 0.803(3) 1.892(3) 0.021 Uiso 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N5 Fe1 N32 94.60(9) . . ?
N5 Fe1 N12 79.05(9) . . ?
N32 Fe1 N12 146.75(9) . . ?
N5 Fe1 N25 160.04(9) . . ?
N32 Fe1 N25 79.11(8) . . ?
N12 Fe1 N25 95.77(8) . . ?
N5 Fe1 Cl1 99.99(6) . . ?
N32 Fe1 Cl1 105.35(6) . . ?
N12 Fe1 Cl1 107.89(7) . . ?
N25 Fe1 Cl1 99.94(6) . . ?
C3 S2 C1 101.65(14) . . ?
N12 C3 N4 118.6(2) . . ?
N12 C3 S2 126.2(2) . . ?
N4 C3 S2 115.19(18) . . ?
N5 N4 C3 108.48(19) . . ?
N4 N5 C6 113.6(2) . . ?
N4 N5 Fe1 119.35(16) . . ?
C6 N5 Fe1 126.99(15) . . ?
C7 C6 C11 120.6(2) . . ?
C7 C6 N5 120.9(2) . . ?
C11 C6 N5 118.5(2) . . ?
C6 C7 C8 119.1(3) . . ?
C9 C8 C7 120.6(3) . . ?
C8 C9 C10 120.4(3) . . ?
C9 C10 C11 119.9(3) . . ?
C10 C11 C6 119.5(3) . . ?
C3 N12 Fe1 114.51(17) . . ?
C23 S22 C21 101.48(11) . . ?
N32 C23 N24 118.76(19) . . ?
N32 C23 S22 126.87(17) . . ?
N24 C23 S22 114.30(17) . . ?
N25 N24 C23 108.32(18) . . ?
N24 N25 C26 113.61(18) . . ?
N24 N25 Fe1 119.13(15) . . ?
C26 N25 Fe1 127.25(15) . . ?
C31 C26 C27 120.2(2) . . ?
C31 C26 N25 118.5(2) . . ?
C27 C26 N25 121.4(2) . . ?
C28 C27 C26 119.4(2) . . ?
C27 C28 C29 120.7(2) . . ?
C28 C29 C30 119.8(2) . . ?
C31 C30 C29 120.1(2) . . ?
C30 C31 C26 119.7(2) . . ?
C23 N32 Fe1 114.45(15) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N5 1.882(2) . ?
Fe1 N32 1.8887(19) . ?
Fe1 N12 1.8917(18) . ?
Fe1 N25 1.892(2) . ?
Fe1 Cl1 2.2863(6) . ?
C1 S2 1.793(4) . ?
S2 C3 1.751(2) . ?
C3 N12 1.307(3) . ?
C3 N4 1.350(3) . ?
N4 N5 1.335(3) . ?
N5 C6 1.423(3) . ?
C6 C7 1.389(4) . ?
C6 C11 1.393(4) . ?
C7 C8 1.391(4) . ?
C8 C9 1.376(5) . ?
C9 C10 1.386(5) . ?
C10 C11 1.390(4) . ?
C21 S22 1.802(3) . ?
S22 C23 1.749(2) . ?
C23 N32 1.313(3) . ?
C23 N24 1.352(3) . ?
N24 N25 1.339(3) . ?
N25 C26 1.422(3) . ?
C26 C31 1.397(3) . ?
C26 C27 1.399(3) . ?
C27 C28 1.388(3) . ?
C28 C29 1.388(4) . ?
C29 C30 1.393(4) . ?
C30 C31 1.391(3) . ?
