#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:38:41 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179196 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/35/4313591.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_4313591
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] * 5 MeOH'
_chemical_formula_sum            'C61 H104 Fe2 N4 O5 S4'
_chemical_formula_weight         1213.42
_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                73.80(2)
_cell_angle_beta                 76.29(2)
_cell_angle_gamma                66.93(2)
_cell_formula_units_Z            1
_cell_length_a                   10.6112(9)
_cell_length_b                   10.6514(9)
_cell_length_c                   16.910(2)
_cell_measurement_reflns_used    13640
_cell_measurement_temperature    100(2)
_cell_volume                     1670.8(4)
_computing_cell_refinement       'Nonius Collect'
_computing_data_collection       'Nonius Collect'
_computing_data_reduction        'Nonius Collect'
_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 ω and 180 sec.'
_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  0.0446
_diffrn_reflns_av_sigmaI/netI    0.0800
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            13640
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.63
_exptl_absorpt_coefficient_mu    0.601
_exptl_absorpt_correction_T_max  0.9705
_exptl_absorpt_correction_T_min  0.8997
_exptl_absorpt_correction_type   'Gaussian, face indexed'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.207
_exptl_crystal_description       'opaque parallelepiped'
_exptl_crystal_F_000             654
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.921
_refine_diff_density_min         -0.385
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.040
_refine_ls_goodness_of_fit_obs   1.095
_refine_ls_matrix_type           full
_refine_ls_number_parameters     378
_refine_ls_number_reflns         7442
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.056
_refine_ls_restrained_S_obs      1.094
_refine_ls_R_factor_all          0.0936
_refine_ls_R_factor_obs          0.0595
_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)+(0.0587P)²+2.7416P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1608
_refine_ls_wR_factor_obs         0.1405
_reflns_number_observed          5408
_reflns_number_total             7506
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic020617c_5.cif
_cod_data_source_block           7
_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^)+(0.0587P)^2^+2.7416P] 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^)+(0.0587P)^2^+2.7416P] 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        1670.8(3)
_cod_database_code               4313591
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 0.48044(5) 0.40807(5) 0.46898(3) 0.02015(14) Uani 1 d . .
S1 S 0.38479(8) 0.36039(9) 0.38456(5) 0.0222(2) Uani 1 d . .
S2 S 0.32662(8) 0.35002(10) 0.57090(5) 0.0245(2) Uani 1 d . .
N1 N 0.6430(3) 0.3675(3) 0.3875(2) 0.0247(6) Uani 1 d D .
H1 H 0.7004(35) 0.3865(43) 0.3888(26) 0.030 Uiso 1 d D .
N2 N 0.5867(3) 0.3752(3) 0.5552(2) 0.0192(6) Uani 1 d D .
H2 H 0.6609(29) 0.3537(39) 0.5474(24) 0.023 Uiso 1 d D .
C1 C 0.5158(3) 0.3372(3) 0.2997(2) 0.0210(7) Uani 1 d . .
C2 C 0.6393(3) 0.3491(3) 0.3102(2) 0.0220(7) Uani 1 d . .
C3 C 0.7524(3) 0.3370(4) 0.2466(2) 0.0221(7) Uani 1 d . .
H3 H 0.8339(3) 0.3453(4) 0.2552(2) 0.027 Uiso 1 calc R .
C4 C 0.7470(3) 0.3134(3) 0.1718(2) 0.0226(7) Uani 1 d . .
C5 C 0.6246(3) 0.2969(3) 0.1635(2) 0.0226(7) Uani 1 d . .
H5 H 0.6212(3) 0.2782(3) 0.1124(2) 0.027 Uiso 1 calc R .
C6 C 0.5099(3) 0.3060(3) 0.2241(2) 0.0195(7) Uani 1 d . .
C7 C 0.3858(3) 0.2777(4) 0.2104(2) 0.0237(7) Uani 1 d . .
C8 C 0.4056(4) 0.2499(4) 0.1234(2) 0.0299(8) Uani 1 d . .
H8A H 0.3239(12) 0.2348(26) 0.1164(6) 0.045 Uiso 1 calc R .
H8B H 0.4877(15) 0.1667(15) 0.1168(6) 0.045 Uiso 1 calc R .
H8C H 0.4179(26) 0.3304(11) 0.0814(2) 0.045 Uiso 1 calc R .
C9 C 0.3688(4) 0.1490(4) 0.2740(3) 0.0316(8) Uani 1 d . .
H9A H 0.2910(17) 0.1304(17) 0.2642(11) 0.047 Uiso 1 calc R .
H9B H 0.3508(27) 0.1661(11) 0.3303(3) 0.047 Uiso 1 calc R .
H9C H 0.4538(11) 0.0683(7) 0.2681(11) 0.047 Uiso 1 calc R .
C10 C 0.2507(3) 0.4042(4) 0.2173(2) 0.0261(8) Uani 1 d . .
H10A H 0.1727(5) 0.3799(9) 0.2133(15) 0.039 Uiso 1 calc R .
H10B H 0.2579(10) 0.4830(9) 0.1720(9) 0.039 Uiso 1 calc R .
H10C H 0.2358(13) 0.4302(16) 0.2709(7) 0.039 Uiso 1 calc R .
C11 C 0.8641(3) 0.3023(4) 0.0987(2) 0.0254(7) Uani 1 d . .
C12 C 0.9078(4) 0.1622(4) 0.0732(2) 0.0314(8) Uani 1 d . .
H12A H 0.9828(19) 0.1561(12) 0.0261(11) 0.047 Uiso 1 calc R .
H12B H 0.8285(8) 0.1549(12) 0.0570(16) 0.047 Uiso 1 calc R .
H12C H 0.9399(26) 0.0858(4) 0.1202(6) 0.047 Uiso 1 calc R .
C13 C 0.9918(4) 0.3132(4) 0.1195(2) 0.0339(9) Uani 1 d . .
H13A H 1.0652(10) 0.3028(28) 0.0715(6) 0.051 Uiso 1 calc R .
H13B H 1.0245(17) 0.2392(17) 0.1674(10) 0.051 Uiso 1 calc R .
H13C H 0.9674(8) 0.4044(11) 0.1329(16) 0.051 Uiso 1 calc R .
C14 C 0.8135(4) 0.4222(4) 0.0246(2) 0.0337(9) Uani 1 d . .
H14A H 0.8873(10) 0.4139(16) -0.0232(6) 0.051 Uiso 1 calc R .
H14B H 0.7892(26) 0.5118(4) 0.0401(6) 0.051 Uiso 1 calc R .
H14C H 0.7320(17) 0.4170(17) 0.0099(11) 0.051 Uiso 1 calc R .
C21 C 0.4147(3) 0.2993(3) 0.6574(2) 0.0206(7) Uani 1 d . .
C22 C 0.5441(3) 0.3149(3) 0.6385(2) 0.0199(7) Uani 1 d . .
C23 C 0.6280(3) 0.2764(3) 0.6998(2) 0.0206(7) Uani 1 d . .
H23 H 0.7164(3) 0.2859(3) 0.6853(2) 0.025 Uiso 1 calc R .
C24 C 0.5828(3) 0.2246(3) 0.7816(2) 0.0206(7) Uani 1 d . .
C25 C 0.4529(3) 0.2107(3) 0.7995(2) 0.0218(7) Uani 1 d . .
H25 H 0.4219(3) 0.1748(3) 0.8556(2) 0.026 Uiso 1 calc R .
C26 C 0.3657(3) 0.2457(4) 0.7409(2) 0.0209(7) Uani 1 d . .
C27 C 0.2239(3) 0.2258(4) 0.7668(2) 0.0236(7) Uani 1 d . .
C28 C 0.2187(4) 0.1197(4) 0.7234(2) 0.0296(8) Uani 1 d . .
H28A H 0.1258(8) 0.1141(19) 0.7369(13) 0.044 Uiso 1 calc R .
H28B H 0.2865(18) 0.0279(7) 0.7425(12) 0.044 Uiso 1 calc R .
H28C H 0.2405(25) 0.1494(14) 0.6630(3) 0.044 Uiso 1 calc R .
C29 C 0.1965(4) 0.1704(4) 0.8607(2) 0.0332(9) Uani 1 d . .
H29A H 0.1053(12) 0.1607(27) 0.8753(3) 0.050 Uiso 1 calc R .
H29B H 0.1990(27) 0.2358(14) 0.8907(2) 0.050 Uiso 1 calc R .
H29C H 0.2678(16) 0.0792(13) 0.8763(3) 0.050 Uiso 1 calc R .
C30 C 0.1075(3) 0.3663(4) 0.7455(2) 0.0300(8) Uani 1 d . .
H30A H 0.0178(4) 0.3531(6) 0.7628(15) 0.045 Uiso 1 calc R .
H30B H 0.1198(15) 0.4032(13) 0.6853(3) 0.045 Uiso 1 calc R .
H30C H 0.1105(17) 0.4323(9) 0.7748(13) 0.045 Uiso 1 calc R .
C31 C 0.6640(3) 0.1910(4) 0.8532(2) 0.0233(7) Uani 1 d . .
C32 C 0.8082(3) 0.2002(4) 0.8214(2) 0.0272(8) Uani 1 d . .
H32A H 0.8564(10) 0.1799(26) 0.8688(2) 0.041 Uiso 1 calc R .
H32B H 0.7996(4) 0.2944(8) 0.7890(13) 0.041 Uiso 1 calc R .
H32C H 0.8610(9) 0.1323(18) 0.7861(13) 0.041 Uiso 1 calc R .
C33 C 0.5827(4) 0.2974(4) 0.9085(2) 0.0334(9) Uani 1 d . .
H33A H 0.6317(15) 0.2770(17) 0.9555(9) 0.050 Uiso 1 calc R .
H33B H 0.4903(10) 0.2916(19) 0.9295(13) 0.050 Uiso 1 calc R .
H33C H 0.5739(24) 0.3915(5) 0.8760(5) 0.050 Uiso 1 calc R .
C34 C 0.6819(4) 0.0436(4) 0.9048(2) 0.0356(9) Uani 1 d . .
H34A H 0.7318(26) 0.0254(11) 0.9510(10) 0.053 Uiso 1 calc R .
H34B H 0.7347(25) -0.0245(5) 0.8695(5) 0.053 Uiso 1 calc R .
H34C H 0.5907(4) 0.0354(10) 0.9269(14) 0.053 Uiso 1 calc R .
O40 O 0.8892(3) 0.2722(4) 0.4939(3) 0.0759(12) Uani 1 d . .
H40 H 0.9362(7) 0.1916(29) 0.4855(47) 0.114 Uiso 1 calc R .
C41 C 0.9787(7) 0.3377(8) 0.5005(7) 0.140(4) Uani 1 d . .
H41A H 1.0571(43) 0.3231(70) 0.4555(29) 0.210 Uiso 1 calc R .
H41B H 1.0129(64) 0.2973(58) 0.5543(20) 0.210 Uiso 1 calc R .
H41C H 0.9279(23) 0.4379(16) 0.4963(51) 0.210 Uiso 1 calc R .
C51 C 0.3533(15) -0.0196(9) 0.5082(6) 0.093(5) Uani 0.50 d P .
C61 C 0.0485(11) 0.0494(10) 0.3453(6) 0.065(3) Uani 0.60 d P .
O50 O 0.2434(12) -0.0630(12) 0.5270(7) 0.051(3) Uiso 0.30 d P 1
O60 O 0.0374(18) 0.0163(17) 0.4299(11) 0.111(5) Uiso 0.35 d P 1
O50X O 0.2625(18) 0.0928(19) 0.4914(11) 0.060(5) Uiso 0.20 d P 2
O60X O 0.0406(21) 0.1696(21) 0.3772(13) 0.099(6) Uiso 0.25 d P 2
O60Y O 0.0041(18) -0.0405(19) 0.3738(12) 0.144(6) Uiso 0.40 d P 3
C61Y C -0.0767(31) -0.0020(29) 0.4633(18) 0.153(10) Uiso 0.40 d P 3
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'
O O 0.0106 0.0060 '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
N1 Fe1 N2 92.39(12) . . ?
N1 Fe1 N2 100.90(13) . 2_666 ?
N2 Fe1 N2 96.67(11) . 2_666 ?
N1 Fe1 S1 84.83(9) . . ?
N2 Fe1 S1 158.51(9) . . ?
N2 Fe1 S1 104.79(8) 2_666 . ?
N1 Fe1 S2 153.61(10) . . ?
N2 Fe1 S2 85.74(9) . . ?
N2 Fe1 S2 105.46(9) 2_666 . ?
S1 Fe1 S2 87.39(4) . . ?
N1 Fe1 Fe1 100.24(9) . 2_666 ?
N2 Fe1 Fe1 50.83(9) . 2_666 ?
N2 Fe1 Fe1 45.83(7) 2_666 2_666 ?
S1 Fe1 Fe1 150.60(4) . 2_666 ?
S2 Fe1 Fe1 98.89(4) . 2_666 ?
C1 S1 Fe1 101.47(11) . . ?
C21 S2 Fe1 101.12(11) . . ?
C2 N1 Fe1 121.8(2) . . ?
C22 N2 Fe1 120.0(2) . . ?
C22 N2 Fe1 113.5(2) . 2_666 ?
Fe1 N2 Fe1 83.33(11) . 2_666 ?
C2 C1 C6 119.1(3) . . ?
C2 C1 S1 114.6(2) . . ?
C6 C1 S1 126.4(2) . . ?
N1 C2 C3 122.3(3) . . ?
N1 C2 C1 116.4(3) . . ?
C3 C2 C1 121.3(3) . . ?
C4 C3 C2 120.8(3) . . ?
C3 C4 C5 117.1(3) . . ?
C3 C4 C11 124.1(3) . . ?
C5 C4 C11 118.7(3) . . ?
C6 C5 C4 125.0(3) . . ?
C5 C6 C1 116.6(3) . . ?
C5 C6 C7 120.6(3) . . ?
C1 C6 C7 122.7(3) . . ?
C8 C7 C9 107.8(3) . . ?
C8 C7 C6 111.7(3) . . ?
C9 C7 C6 109.9(3) . . ?
C8 C7 C10 106.0(3) . . ?
C9 C7 C10 109.8(3) . . ?
C6 C7 C10 111.6(3) . . ?
C4 C11 C13 112.2(3) . . ?
C4 C11 C12 110.1(3) . . ?
C13 C11 C12 108.1(3) . . ?
C4 C11 C14 109.0(3) . . ?
C13 C11 C14 108.0(3) . . ?
C12 C11 C14 109.4(3) . . ?
C22 C21 C26 119.7(3) . . ?
C22 C21 S2 114.3(3) . . ?
C26 C21 S2 126.0(2) . . ?
C23 C22 C21 121.3(3) . . ?
C23 C22 N2 120.6(3) . . ?
C21 C22 N2 118.1(3) . . ?
C24 C23 C22 120.3(3) . . ?
C23 C24 C25 117.6(3) . . ?
C23 C24 C31 123.2(3) . . ?
C25 C24 C31 119.1(3) . . ?
C26 C25 C24 124.6(3) . . ?
C25 C26 C21 116.5(3) . . ?
C25 C26 C27 120.7(3) . . ?
C21 C26 C27 122.8(3) . . ?
C28 C27 C29 107.1(3) . . ?
C28 C27 C30 110.3(3) . . ?
C29 C27 C30 107.3(3) . . ?
C28 C27 C26 110.6(3) . . ?
C29 C27 C26 111.5(3) . . ?
C30 C27 C26 109.9(3) . . ?
C32 C31 C34 107.8(3) . . ?
C32 C31 C33 109.0(3) . . ?
C34 C31 C33 109.5(3) . . ?
C32 C31 C24 111.7(3) . . ?
C34 C31 C24 111.0(3) . . ?
C33 C31 C24 107.8(3) . . ?
C61 O60Y C61Y 101.3(17) . . ?
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 N1 1.919(3) . ?
Fe1 N2 1.924(3) . ?
Fe1 N2 2.080(3) 2_666 ?
Fe1 S1 2.1956(9) . ?
Fe1 S2 2.2089(11) . ?
Fe1 Fe1 2.6644(10) 2_666 ?
S1 C1 1.742(3) . ?
S2 C21 1.765(3) . ?
N1 C2 1.386(4) . ?
N2 C22 1.422(4) . ?
N2 Fe1 2.080(3) 2_666 ?
C1 C2 1.420(4) . ?
C1 C6 1.429(5) . ?
C2 C3 1.400(5) . ?
C3 C4 1.374(5) . ?
C4 C5 1.421(4) . ?
C4 C11 1.525(5) . ?
C5 C6 1.383(5) . ?
C6 C7 1.540(4) . ?
C7 C8 1.530(5) . ?
C7 C9 1.532(5) . ?
C7 C10 1.542(5) . ?
C11 C13 1.531(5) . ?
C11 C12 1.533(5) . ?
C11 C14 1.541(5) . ?
C21 C22 1.398(4) . ?
C21 C26 1.423(5) . ?
C22 C23 1.397(4) . ?
C23 C24 1.384(5) . ?
C24 C25 1.397(4) . ?
C24 C31 1.532(4) . ?
C25 C26 1.391(4) . ?
C26 C27 1.546(4) . ?
C27 C28 1.532(5) . ?
C27 C29 1.532(5) . ?
C27 C30 1.536(5) . ?
C31 C32 1.529(5) . ?
C31 C34 1.531(5) . ?
C31 C33 1.532(5) . ?
O40 C41 1.419(7) . ?
C51 O50X 1.22(2) . ?
C51 O50 1.36(2) . ?
C61 O60Y 1.17(2) . ?
C61 O60 1.36(2) . ?
C61 O60X 1.49(2) . ?
O60Y C61Y 1.63(3) . ?
