#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:38:41 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179196 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/35/4313590.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_4313590
loop_
_publ_author_name
'Prasanta Ghosh'
'Ameerunisha Begum'
'Eckhard Bill'
'Thomas Weyhermüller'
'Karl Wieghardt'
_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     '[C56 H84 Fe2 N4 S4], hexane'
_chemical_formula_sum            'C62 H98 Fe2 N4 S4'
_chemical_formula_weight         1139.38
_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                103.94(2)
_cell_angle_beta                 101.98(2)
_cell_angle_gamma                99.29(2)
_cell_formula_units_Z            1
_cell_length_a                   10.539(5)
_cell_length_b                   11.343(5)
_cell_length_c                   14.532(6)
_cell_measurement_reflns_used    1972
_cell_measurement_temperature    100(2)
_cell_volume                     1607.9(13)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SAINT'
_computing_data_reduction        'Siemens SAINT'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measurement_device       'Siemens SMART CCD-Detector'
_diffrn_measurement_method       'ω, 0.3 deg./frame'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0558
_diffrn_reflns_av_sigmaI/netI    0.1102
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6322
_diffrn_reflns_theta_max         23.27
_diffrn_reflns_theta_min         1.90
_exptl_absorpt_coefficient_mu    0.619
_exptl_absorpt_correction_T_max  0.940
_exptl_absorpt_correction_T_min  0.838
_exptl_absorpt_correction_type   'Gaussian, face indexed'
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    1.177
_exptl_crystal_description       'transparent parallelepiped'
_exptl_crystal_F_000             614
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.880
_refine_diff_density_min         -0.378
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.039
_refine_ls_goodness_of_fit_obs   1.185
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         4519
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.174
_refine_ls_restrained_S_obs      1.194
_refine_ls_R_factor_all          0.1272
_refine_ls_R_factor_obs          0.0757
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0957P)²+4.3310P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2364
_refine_ls_wR_factor_obs         0.1897
_reflns_number_observed          2891
_reflns_number_total             4533
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic020617c_4.cif
_cod_data_source_block           6
_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^)+(0.0957P)^2^+4.3310P] 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^)+(0.0957P)^2^+4.3310P] 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        1607.9(12)
_cod_database_code               4313590
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Fe1 Fe 0.51868(10) 0.57972(10) 0.44086(8) 0.0275(4) Uani 1 d . .
S1 S 0.5464(2) 0.6384(2) 0.60273(14) 0.0288(5) Uani 1 d . .
N1 N 0.7032(6) 0.5952(6) 0.4721(4) 0.029(2) Uani 1 d D .
H1 H 0.7525(66) 0.5911(70) 0.4361(49) 0.035 Uiso 1 d D .
C1 C 0.7233(7) 0.6783(7) 0.6418(5) 0.028(2) Uani 1 d . .
C2 C 0.7851(7) 0.6468(7) 0.5650(5) 0.030(2) Uani 1 d . .
C3 C 0.9231(7) 0.6719(7) 0.5836(6) 0.032(2) Uani 1 d . .
H3 H 0.9617(7) 0.6502(7) 0.5318(6) 0.038 Uiso 1 calc R .
C4 C 1.0038(7) 0.7278(7) 0.6765(6) 0.038(2) Uani 1 d . .
C5 C 0.9387(7) 0.7621(7) 0.7522(6) 0.039(2) Uani 1 d . .
H5 H 0.9920(7) 0.8033(7) 0.8150(6) 0.047 Uiso 1 calc R .
C6 C 0.8015(7) 0.7388(7) 0.7397(5) 0.033(2) Uani 1 d . .
C7 C 0.7437(8) 0.7837(7) 0.8263(6) 0.039(2) Uani 1 d . .
C8 C 0.6613(9) 0.6701(8) 0.8460(6) 0.052(2) Uani 1 d . .
H8A H 0.6250(9) 0.6986(8) 0.9006(6) 0.079 Uiso 1 calc R .
H8B H 0.7178(9) 0.6152(8) 0.8608(6) 0.079 Uiso 1 calc R .
H8C H 0.5901(9) 0.6264(8) 0.7888(6) 0.079 Uiso 1 calc R .
C9 C 0.8495(8) 0.8510(9) 0.9221(6) 0.052(2) Uani 1 d . .
H9A H 0.8071(8) 0.8768(9) 0.9736(6) 0.078 Uiso 1 calc R .
H9B H 0.9034(8) 0.9228(9) 0.9142(6) 0.078 Uiso 1 calc R .
H9C H 0.9046(8) 0.7956(9) 0.9387(6) 0.078 Uiso 1 calc R .
C10 C 0.6557(9) 0.8745(8) 0.8072(6) 0.057(3) Uani 1 d . .
H10A H 0.6207(9) 0.9012(8) 0.8628(6) 0.086 Uiso 1 calc R .
H10B H 0.5835(9) 0.8338(8) 0.7500(6) 0.086 Uiso 1 calc R .
H10C H 0.7075(9) 0.9456(8) 0.7968(6) 0.086 Uiso 1 calc R .
C11 C 1.1550(7) 0.7509(7) 0.6966(5) 0.047(2) Uani 1 d D .
C12 C 1.2209(12) 0.8808(10) 0.7596(11) 0.126(9) Uani 0.70 d PD 1
H12A H 1.3156(12) 0.8921(10) 0.7708(11) 0.189 Uiso 0.70 calc PR 1
H12B H 1.1979(12) 0.8940(10) 0.8213(11) 0.189 Uiso 0.70 calc PR 1
H12C H 1.1913(12) 0.9395(10) 0.7271(11) 0.189 Uiso 0.70 calc PR 1
C13 C 1.2004(13) 0.6587(12) 0.7517(9) 0.073(5) Uani 0.70 d PD 1
H13A H 1.1589(13) 0.5749(12) 0.7122(9) 0.110 Uiso 0.70 calc PR 1
H13B H 1.1752(13) 0.6736(12) 0.8126(9) 0.110 Uiso 0.70 calc PR 1
H13C H 1.2953(13) 0.6699(12) 0.7647(9) 0.110 Uiso 0.70 calc PR 1
C14 C 1.2045(11) 0.7241(13) 0.6038(8) 0.063(4) Uani 0.70 d PD 1
H14A H 1.1622(11) 0.6409(13) 0.5636(8) 0.094 Uiso 0.70 calc PR 1
H14B H 1.2992(11) 0.7322(13) 0.6214(8) 0.094 Uiso 0.70 calc PR 1
H14C H 1.1834(11) 0.7823(13) 0.5680(8) 0.094 Uiso 0.70 calc PR 1
C12X C 1.1951(30) 0.8355(23) 0.6352(18) 0.065(9) Uiso 0.30 d PD 2
H12D H 1.1603(30) 0.9090(23) 0.6503(18) 0.097 Uiso 0.30 calc PR 2
H12E H 1.1598(30) 0.7919(23) 0.5667(18) 0.097 Uiso 0.30 calc PR 2
H12F H 1.2904(30) 0.8588(23) 0.6498(18) 0.097 Uiso 0.30 calc PR 2
C13X C 1.2198(32) 0.8225(24) 0.8039(10) 0.073(12) Uiso 0.30 d PD 2
H13D H 1.1851(32) 0.8957(24) 0.8208(10) 0.109 Uiso 0.30 calc PR 2
H13E H 1.3143(32) 0.8463(24) 0.8136(10) 0.109 Uiso 0.30 calc PR 2
H13F H 1.2008(32) 0.7704(24) 0.8448(10) 0.109 Uiso 0.30 calc PR 2
C14X C 1.2109(36) 0.6362(21) 0.6714(22) 0.106(15) Uiso 0.30 d PD 2
H14D H 1.1708(36) 0.5902(21) 0.6040(22) 0.159 Uiso 0.30 calc PR 2
H14E H 1.1919(36) 0.5847(21) 0.7127(22) 0.159 Uiso 0.30 calc PR 2
H14F H 1.3054(36) 0.6606(21) 0.6815(22) 0.159 Uiso 0.30 calc PR 2
S2 S 0.5323(2) 0.6432(2) 0.31184(14) 0.0308(5) Uani 1 d . .
N2 N 0.3498(6) 0.6113(6) 0.4169(5) 0.033(2) Uani 1 d D .
H2 H 0.2986(67) 0.5933(72) 0.4485(52) 0.039 Uiso 1 d D .
C21 C 0.3755(7) 0.6706(6) 0.2761(5) 0.028(2) Uani 1 d . .
C22 C 0.2941(7) 0.6491(6) 0.3389(5) 0.027(2) Uani 1 d . .
C23 C 0.1627(7) 0.6675(7) 0.3221(5) 0.030(2) Uani 1 d . .
H23 H 0.1110(7) 0.6546(7) 0.3650(5) 0.035 Uiso 1 calc R .
C24 C 0.1124(7) 0.7049(7) 0.2412(6) 0.037(2) Uani 1 d . .
C25 C 0.1964(7) 0.7250(7) 0.1791(6) 0.038(2) Uani 1 d . .
H25 H 0.1618(7) 0.7508(7) 0.1250(6) 0.045 Uiso 1 calc R .
C26 C 0.3229(7) 0.7095(7) 0.1926(5) 0.031(2) Uani 1 d . .
C27 C 0.4085(7) 0.7365(7) 0.1214(5) 0.035(2) Uani 1 d . .
C28 C 0.3284(9) 0.7753(8) 0.0357(6) 0.049(2) Uani 1 d . .
H28A H 0.2518(9) 0.7098(8) -0.0003(6) 0.073 Uiso 1 calc R .
H28B H 0.3836(9) 0.7900(8) -0.0071(6) 0.073 Uiso 1 calc R .
H28C H 0.3003(9) 0.8500(8) 0.0616(6) 0.073 Uiso 1 calc R .
C29 C 0.4499(9) 0.6193(8) 0.0736(6) 0.049(2) Uani 1 d . .
H29A H 0.3721(9) 0.5539(8) 0.0404(6) 0.074 Uiso 1 calc R .
H29B H 0.5056(9) 0.5941(8) 0.1230(6) 0.074 Uiso 1 calc R .
H29C H 0.4980(9) 0.6358(8) 0.0271(6) 0.074 Uiso 1 calc R .
C30 C 0.5275(8) 0.8435(8) 0.1750(6) 0.045(2) Uani 1 d . .
H30A H 0.4975(8) 0.9156(8) 0.2042(6) 0.067 Uiso 1 calc R .
H30B H 0.5764(8) 0.8621(8) 0.1295(6) 0.067 Uiso 1 calc R .
H30C H 0.5841(8) 0.8204(8) 0.2254(6) 0.067 Uiso 1 calc R .
C31 C -0.0298(8) 0.7276(8) 0.2159(6) 0.046(2) Uani 1 d . .
C32 C -0.1094(9) 0.6252(10) 0.1211(8) 0.076(3) Uani 1 d . .
H32A H -0.1111(9) 0.5448(10) 0.1319(8) 0.113 Uiso 1 calc R .
H32B H -0.0680(9) 0.6309(10) 0.0690(8) 0.113 Uiso 1 calc R .
H32C H -0.1988(9) 0.6362(10) 0.1035(8) 0.113 Uiso 1 calc R .
C33 C -0.0990(9) 0.7192(10) 0.2980(7) 0.068(3) Uani 1 d . .
H33A H -0.1022(9) 0.6387(10) 0.3089(7) 0.102 Uiso 1 calc R .
H33B H -0.1879(9) 0.7309(10) 0.2792(7) 0.102 Uiso 1 calc R .
H33C H -0.0502(9) 0.7827(10) 0.3572(7) 0.102 Uiso 1 calc R .
C34 C -0.0261(9) 0.8555(9) 0.2002(7) 0.064(3) Uani 1 d . .
H34A H 0.0169(9) 0.8624(9) 0.1490(7) 0.096 Uiso 1 calc R .
H34B H 0.0223(9) 0.9184(9) 0.2598(7) 0.096 Uiso 1 calc R .
H34C H -0.1154(9) 0.8666(9) 0.1818(7) 0.096 Uiso 1 calc R .
C41 C 0.7983(12) 0.9581(10) 0.5228(10) 0.098(4) Uani 1 d . .
H41A H 0.8612(12) 0.9391(10) 0.5721(10) 0.148 Uiso 1 calc R .
H41B H 0.8360(12) 1.0355(10) 0.5129(10) 0.148 Uiso 1 calc R .
H41C H 0.7774(12) 0.8928(10) 0.4624(10) 0.148 Uiso 1 calc R .
C42 C 0.6720(13) 0.9690(10) 0.5561(8) 0.080(3) Uani 1 d . .
H42A H 0.6367(13) 0.8911(10) 0.5678(8) 0.096 Uiso 1 calc R .
H42B H 0.6951(13) 1.0335(10) 0.6182(8) 0.096 Uiso 1 calc R .
C43 C 0.5656(10) 0.9984(9) 0.4864(8) 0.070(3) Uani 1 d . .
H43A H 0.5478(10) 0.9372(9) 0.4232(8) 0.084 Uiso 1 calc R .
H43B H 0.5998(10) 1.0789(9) 0.4784(8) 0.084 Uiso 1 calc R .
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'
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
N2 Fe1 N1 164.2(3) . . ?
N2 Fe1 S2 84.4(2) . . ?
N1 Fe1 S2 89.0(2) . . ?
N2 Fe1 S1 92.5(2) . . ?
N1 Fe1 S1 84.7(2) . . ?
S2 Fe1 S1 145.26(9) . . ?
N2 Fe1 S1 97.3(2) . 2_666 ?
N1 Fe1 S1 98.4(2) . 2_666 ?
S2 Fe1 S1 110.66(9) . 2_666 ?
S1 Fe1 S1 104.06(7) . 2_666 ?
N2 Fe1 Fe1 98.1(2) . 2_666 ?
N1 Fe1 Fe1 92.8(2) . 2_666 ?
S2 Fe1 Fe1 160.73(9) . 2_666 ?
S1 Fe1 Fe1 53.96(6) . 2_666 ?
S1 Fe1 Fe1 50.10(6) 2_666 2_666 ?
C1 S1 Fe1 99.7(2) . . ?
C1 S1 Fe1 107.1(2) . 2_666 ?
Fe1 S1 Fe1 75.94(7) . 2_666 ?
C2 N1 Fe1 124.0(5) . . ?
C2 C1 C6 120.4(7) . . ?
C2 C1 S1 113.6(5) . . ?
C6 C1 S1 126.0(6) . . ?
N1 C2 C3 122.4(7) . . ?
N1 C2 C1 116.9(6) . . ?
C3 C2 C1 120.6(7) . . ?
C4 C3 C2 121.8(7) . . ?
C3 C4 C5 116.4(7) . . ?
C3 C4 C11 121.3(7) . . ?
C5 C4 C11 122.3(7) . . ?
C6 C5 C4 125.2(7) . . ?
C5 C6 C1 115.6(7) . . ?
C5 C6 C7 120.2(7) . . ?
C1 C6 C7 124.1(7) . . ?
C6 C7 C9 113.4(7) . . ?
C6 C7 C10 111.3(7) . . ?
C9 C7 C10 106.6(7) . . ?
C6 C7 C8 109.6(7) . . ?
C9 C7 C8 105.9(7) . . ?
N2 C22 C21 116.3(6) . . ?
N2 C22 C23 122.1(7) . . ?
C21 C22 C23 121.6(7) . . ?
C24 C23 C22 118.9(7) . . ?
C23 C24 C25 118.1(7) . . ?
C23 C24 C31 123.2(7) . . ?
C25 C24 C31 118.7(7) . . ?
C26 C25 C24 125.1(7) . . ?
C25 C26 C21 117.1(7) . . ?
C25 C26 C27 121.3(7) . . ?
C21 C26 C27 121.5(6) . . ?
C30 C27 C29 111.9(7) . . ?
C30 C27 C28 106.8(6) . . ?
C29 C27 C28 105.6(6) . . ?
C30 C27 C26 110.5(6) . . ?
C29 C27 C26 110.2(6) . . ?
C28 C27 C26 111.7(6) . . ?
C34 C31 C33 108.4(7) . . ?
C34 C31 C32 110.2(8) . . ?
C33 C31 C32 108.9(8) . . ?
C34 C31 C24 110.6(7) . . ?
C33 C31 C24 111.5(7) . . ?
C32 C31 C24 107.3(7) . . ?
C43 C42 C41 115.2(10) . . ?
C42 C43 C43 117.0(11) . 2_676 ?
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 N2 1.851(6) . ?
Fe1 N1 1.872(6) . ?
Fe1 S2 2.187(2) . ?
Fe1 S1 2.227(2) . ?
Fe1 S1 2.347(2) 2_666 ?
Fe1 Fe1 2.816(2) 2_666 ?
S1 C1 1.780(7) . ?
S1 Fe1 2.347(2) 2_666 ?
N1 C2 1.373(9) . ?
C1 C2 1.408(10) . ?
C1 C6 1.426(10) . ?
C2 C3 1.391(10) . ?
C3 C4 1.372(10) . ?
C4 C5 1.423(11) . ?
C4 C11 1.526(10) . ?
C5 C6 1.392(10) . ?
C6 C7 1.525(10) . ?
C7 C9 1.528(10) . ?
C7 C10 1.529(11) . ?
C7 C8 1.554(11) . ?
C11 C12 1.499(9) . ?
C11 C14X 1.511(10) . ?
C11 C13X 1.525(10) . ?
C11 C14 1.527(9) . ?
C11 C12X 1.529(10) . ?
C11 C13 1.540(9) . ?
S2 C21 1.727(7) . ?
N2 C22 1.360(9) . ?
C21 C22 1.412(10) . ?
C21 C26 1.426(10) . ?
C22 C23 1.414(9) . ?
C23 C24 1.377(10) . ?
C24 C25 1.420(10) . ?
C24 C31 1.546(10) . ?
C25 C26 1.352(10) . ?
C26 C27 1.559(10) . ?
C27 C30 1.517(11) . ?
C27 C29 1.520(11) . ?
C27 C28 1.549(10) . ?
C31 C34 1.517(12) . ?
C31 C33 1.536(12) . ?
C31 C32 1.545(12) . ?
C41 C42 1.521(15) . ?
C42 C43 1.485(13) . ?
C43 C43 1.52(2) 2_676 ?
