#------------------------------------------------------------------------------
#$Date: 2016-03-23 14:16:56 +0100 (Wed 23 de Mar de 2016) $
#$Revision: 179320 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/17/4321780.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_4321780
loop_
_publ_author_name
'Dieter Sellmann'
'Jürgen Utz'
'Frank W. Heinemann'
_publ_contact_author
; 
        Prof. Dr. D. Sellmann 
        Institut für Anorganische Chemie II 
        Universität Erlangen-Nürnberg 
        Egerlandstr. 1 
        D-91058 Erlangen 
        Bundesrepublik Deutschland 
;
_publ_contact_author_email       SELLMANN@ANORGANIK.CHEMIE.UNI-ERLANGEN.DE
_publ_contact_author_fax         '049 9131 85-7367'
_publ_contact_author_phone       '049 9131 85-7360'
_publ_section_title
;
 Transition-Metal Complexes with Sulfur Ligands. 132.1 Electron-Rich Fe
 and Ru Complexes with [MN₂S₃] Cores Containing the New Pentadentate
 Ligand 'N₂H₂S₃'²⁻ (= 2,2'-Bis(2-mercaptophenylamino)diethyl
 Sulfide(2-))
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              459
_journal_page_last               466
_journal_paper_doi               10.1021/ic980383q
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C36 H52 Fe2 N4 O4 S6'
_chemical_formula_weight         908.88
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                114.01(4)
_cell_angle_beta                 95.03(3)
_cell_angle_gamma                95.23(3)
_cell_formula_units_Z            1
_cell_length_a                   9.763(3)
_cell_length_b                   10.255(4)
_cell_length_c                   11.607(6)
_cell_measurement_reflns_used    18
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      17.6
_cell_measurement_theta_min      16.7
_cell_volume                     1047.1(8)
_computing_cell_refinement       'P3 (Siemens Analytical X-Ray Instr., 1989)'
_computing_data_collection       'P3 (Siemens Analytical X-Ray Instr., 1989)'
_computing_data_reduction
'XDISK (Siemens Analytical X-Ray Instr. , 1989)'
_computing_molecular_graphics
'XP 5.03 (Siemens Analytical X-Ray Instr, 1994)'
_computing_publication_material  'CIFTAB (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution
'SHELTL PLUS 4.21/V (Siemens An. X-Ray Instr., 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       'profile data from ω-scans'
_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  0.0230
_diffrn_reflns_av_sigmaI/netI    0.0370
_diffrn_reflns_limit_h_max       3
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4287
_diffrn_reflns_theta_max         24.05
_diffrn_reflns_theta_min         2.20
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.034
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_description       column
_exptl_crystal_F_000             476
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.50
_refine_diff_density_max         0.626
_refine_diff_density_min         -0.689
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.081
_refine_ls_goodness_of_fit_obs   1.183
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     339
_refine_ls_number_reflns         3291
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_restrained_S_obs      1.183
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_obs          0.0360
_refine_ls_shift/esd_max         4.143
_refine_ls_shift/esd_mean        0.071
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0693P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1052
_refine_ls_wR_factor_obs         0.1026
_reflns_number_observed          2677
_reflns_number_total             3291
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic980383q_2.cif
_cod_data_source_block           ju36
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0693P)^2^+0.0000P] 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^)+(0.0693P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4321780
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 0.04415(4) 0.15500(4) 0.12951(4) 0.0250(2) Uani 1 d . .
S1 S -0.18166(8) 0.19513(9) 0.19918(8) 0.0324(2) Uani 1 d . .
S2 S 0.02311(8) -0.09568(8) 0.10250(7) 0.0261(2) Uani 1 d . .
S3 S 0.15793(9) 0.39824(8) 0.14354(9) 0.0362(2) Uani 1 d . .
O1 O -0.3369(4) 0.4760(3) 0.2665(3) 0.0680(9) Uani 1 d . .
O2 O 0.3893(4) 0.3326(4) 0.4919(4) 0.0711(9) Uani 1 d . .
N1 N 0.1076(3) 0.2750(3) 0.3415(3) 0.0290(6) Uani 1 d . .
N2 N 0.2640(3) 0.0983(3) 0.0855(3) 0.0267(6) Uani 1 d . .
C1 C -0.2848(8) 0.5284(7) 0.1830(6) 0.0727(15) Uani 1 d . .
C2 C 0.4393(7) 0.2172(8) 0.5133(6) 0.090(2) Uani 1 d . .
C10 C -0.1328(3) 0.1860(3) 0.3449(3) 0.0301(7) Uani 1 d . .
C11 C -0.2289(4) 0.1375(4) 0.4068(3) 0.0363(8) Uani 1 d . .
C12 C -0.1879(4) 0.1262(4) 0.5194(4) 0.0413(9) Uani 1 d . .
C13 C -0.0520(4) 0.1636(4) 0.5745(4) 0.0405(9) Uani 1 d . .
C14 C 0.0454(4) 0.2133(4) 0.5161(3) 0.0360(8) Uani 1 d . .
C15 C 0.0060(3) 0.2236(3) 0.4020(3) 0.0264(7) Uani 1 d . .
C16 C 0.1173(4) 0.4331(3) 0.3836(3) 0.0341(8) Uani 1 d . .
C17 C 0.2176(4) 0.4849(4) 0.3126(4) 0.0410(9) Uani 1 d . .
C20 C 0.2010(3) -0.1136(3) 0.1256(3) 0.0259(7) Uani 1 d . .
C21 C 0.2380(4) -0.2276(3) 0.1514(3) 0.0324(7) Uani 1 d . .
C22 C 0.3771(4) -0.2379(4) 0.1800(3) 0.0379(8) Uani 1 d . .
C23 C 0.4789(4) -0.1346(4) 0.1829(3) 0.0380(8) Uani 1 d . .
C24 C 0.4443(4) -0.0234(4) 0.1528(3) 0.0328(7) Uani 1 d . .
C25 C 0.3061(3) -0.0119(3) 0.1235(3) 0.0253(6) Uani 1 d . .
C26 C 0.3705(4) 0.2248(3) 0.1191(4) 0.0334(8) Uani 1 d . .
C27 C 0.3127(4) 0.3327(4) 0.0763(4) 0.0393(8) Uani 1 d . .
H1B H -0.2987(60) 0.3971(62) 0.2618(53) 0.104(20) Uiso 1 d . .
H2B H 0.3948(82) 0.4131(88) 0.5680(77) 0.182(33) Uiso 1 d . .
H1A H 0.1768(33) 0.2568(31) 0.3549(28) 0.010(8) Uiso 1 d . .
H2A H 0.2415(34) 0.0642(33) 0.0104(33) 0.020(9) Uiso 1 d . .
H1C H -0.2983(64) 0.4666(66) 0.0975(62) 0.104(21) Uiso 1 d . .
H1D H -0.3022(69) 0.6213(76) 0.2015(61) 0.127(24) Uiso 1 d . .
H1E H -0.1843(63) 0.5500(58) 0.1904(52) 0.090(19) Uiso 1 d . .
H2C H 0.4454(83) 0.1451(87) 0.4234(80) 0.169(32) Uiso 1 d . .
H2D H 0.5361(80) 0.2435(72) 0.5463(66) 0.138(25) Uiso 1 d . .
H2E H 0.3689(67) 0.1936(62) 0.5873(57) 0.210(22) Uiso 1 d . .
H11 H -0.3202(44) 0.1077(40) 0.3685(36) 0.048(11) Uiso 1 d . .
H12 H -0.2494(42) 0.0892(40) 0.5543(36) 0.046(11) Uiso 1 d . .
H13 H -0.0160(48) 0.1526(44) 0.6447(41) 0.062(13) Uiso 1 d . .
H14 H 0.1418(41) 0.2470(38) 0.5533(35) 0.045(10) Uiso 1 d . .
H16A H 0.0267(41) 0.4489(36) 0.3596(33) 0.039(10) Uiso 1 d . .
H16B H 0.1450(38) 0.4876(37) 0.4826(36) 0.044(10) Uiso 1 d . .
H17A H 0.2226(40) 0.5883(43) 0.3385(35) 0.050(11) Uiso 1 d . .
H17B H 0.3074(42) 0.4656(39) 0.3273(35) 0.042(10) Uiso 1 d . .
H21 H 0.1632(40) -0.3004(40) 0.1523(35) 0.047(10) Uiso 1 d . .
H22 H 0.4036(36) -0.3203(37) 0.1996(33) 0.040(10) Uiso 1 d . .
H23 H 0.5658(42) -0.1379(38) 0.2001(34) 0.039(10) Uiso 1 d . .
H24 H 0.5094(38) 0.0416(37) 0.1518(33) 0.036(10) Uiso 1 d . .
H26A H 0.3987(33) 0.2667(33) 0.2147(32) 0.027(8) Uiso 1 d . .
H26B H 0.4511(36) 0.1988(34) 0.0761(32) 0.032(9) Uiso 1 d . .
H27A H 0.3870(42) 0.4177(43) 0.1043(36) 0.050(11) Uiso 1 d . .
H27B H 0.2861(49) 0.2949(48) -0.0153(46) 0.072(15) 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'
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 94.92(11) . . ?
N1 Fe1 S1 79.79(9) . . ?
N2 Fe1 S1 170.58(7) . . ?
N1 Fe1 S2 101.52(8) . . ?
N2 Fe1 S2 78.34(7) . . ?
S1 Fe1 S2 94.98(4) . . ?
N1 Fe1 S2 163.04(7) . 2 ?
N2 Fe1 S2 88.84(8) . 2 ?
S1 Fe1 S2 98.48(4) . 2 ?
S2 Fe1 S2 95.44(5) . 2 ?
N1 Fe1 S3 79.41(8) . . ?
N2 Fe1 S3 80.37(7) . . ?
S1 Fe1 S3 106.05(4) . . ?
S2 Fe1 S3 158.70(3) . . ?
S2 Fe1 S3 84.94(5) 2 . ?
C10 S1 Fe1 93.79(11) . . ?
C20 S2 Fe1 99.88(10) . . ?
C20 S2 Fe1 107.95(11) . 2 ?
Fe1 S2 Fe1 84.56(5) . 2 ?
C17 S3 C27 103.0(2) . . ?
C17 S3 Fe1 98.79(12) . . ?
C27 S3 Fe1 96.01(12) . . ?
C15 N1 C16 111.2(3) . . ?
C15 N1 Fe1 107.1(2) . . ?
C16 N1 Fe1 111.8(2) . . ?
C25 N2 C26 115.3(3) . . ?
C25 N2 Fe1 113.9(2) . . ?
C26 N2 Fe1 114.3(2) . . ?
C15 C10 C11 117.3(3) . . ?
C15 C10 S1 120.7(2) . . ?
C11 C10 S1 122.0(3) . . ?
C12 C11 C10 121.3(3) . . ?
C13 C12 C11 120.8(3) . . ?
C12 C13 C14 119.2(4) . . ?
C13 C14 C15 120.6(3) . . ?
C14 C15 C10 120.8(3) . . ?
C14 C15 N1 120.4(3) . . ?
C10 C15 N1 118.8(3) . . ?
N1 C16 C17 110.9(3) . . ?
C16 C17 S3 109.8(3) . . ?
C21 C20 C25 118.9(3) . . ?
C21 C20 S2 119.4(2) . . ?
C25 C20 S2 121.6(2) . . ?
C20 C21 C22 120.7(3) . . ?
C23 C22 C21 119.9(3) . . ?
C22 C23 C24 120.3(3) . . ?
C23 C24 C25 120.5(3) . . ?
C24 C25 C20 119.6(3) . . ?
C24 C25 N2 122.9(3) . . ?
C20 C25 N2 117.4(3) . . ?
N2 C26 C27 110.0(3) . . ?
C26 C27 S3 114.7(2) . . ?
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 2.254(3) . ?
Fe1 N2 2.321(3) . ?
Fe1 S1 2.4271(12) . ?
Fe1 S2 2.4466(13) . ?
Fe1 S2 2.517(2) 2 ?
Fe1 S3 2.5720(14) . ?
S1 C10 1.758(3) . ?
S2 C20 1.771(3) . ?
S2 Fe1 2.517(2) 2 ?
S3 C17 1.807(4) . ?
S3 C27 1.819(4) . ?
O1 C1 1.396(6) . ?
O2 C2 1.423(7) . ?
N1 C15 1.443(4) . ?
N1 C16 1.482(4) . ?
N2 C25 1.449(4) . ?
N2 C26 1.478(4) . ?
C10 C15 1.401(5) . ?
C10 C11 1.403(5) . ?
C11 C12 1.387(5) . ?
C12 C13 1.370(5) . ?
C13 C14 1.388(5) . ?
C14 C15 1.395(5) . ?
C16 C17 1.524(5) . ?
C20 C21 1.390(4) . ?
C20 C25 1.404(4) . ?
C21 C22 1.393(5) . ?
C22 C23 1.372(5) . ?
C23 C24 1.382(5) . ?
C24 C25 1.389(5) . ?
C26 C27 1.517(5) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 Fe1 S1 C10 -32.05(13) . . . . ?
N2 Fe1 S1 C10 24.4(5) . . . . ?
S2 Fe1 S1 C10 68.79(11) . . . . ?
S2 Fe1 S1 C10 165.06(10) 2 . . . ?
S3 Fe1 S1 C10 -107.80(11) . . . . ?
N1 Fe1 S2 C20 -73.08(13) . . . . ?
N2 Fe1 S2 C20 19.63(13) . . . . ?
S1 Fe1 S2 C20 -153.66(10) . . . . ?
S2 Fe1 S2 C20 107.31(11) 2 . . . ?
S3 Fe1 S2 C20 17.29(14) . . . . ?
N1 Fe1 S2 Fe1 179.60(8) . . . 2 ?
N2 Fe1 S2 Fe1 -87.68(9) . . . 2 ?
S1 Fe1 S2 Fe1 99.03(5) . . . 2 ?
S2 Fe1 S2 Fe1 0.0 2 . . 2 ?
S3 Fe1 S2 Fe1 -90.02(10) . . . 2 ?
N1 Fe1 S3 C17 3.9(2) . . . . ?
N2 Fe1 S3 C17 -93.0(2) . . . . ?
S1 Fe1 S3 C17 79.94(14) . . . . ?
S2 Fe1 S3 C17 -90.7(2) . . . . ?
S2 Fe1 S3 C17 177.33(14) 2 . . . ?
N1 Fe1 S3 C27 108.1(2) . . . . ?
N2 Fe1 S3 C27 11.2(2) . . . . ?
S1 Fe1 S3 C27 -175.91(14) . . . . ?
S2 Fe1 S3 C27 13.5(2) . . . . ?
S2 Fe1 S3 C27 -78.53(15) 2 . . . ?
N2 Fe1 N1 C15 -132.8(2) . . . . ?
S1 Fe1 N1 C15 39.3(2) . . . . ?
S2 Fe1 N1 C15 -53.7(2) . . . . ?
S2 Fe1 N1 C15 124.9(2) 2 . . . ?
S3 Fe1 N1 C15 147.9(2) . . . . ?
N2 Fe1 N1 C16 105.1(2) . . . . ?
S1 Fe1 N1 C16 -82.8(2) . . . . ?
S2 Fe1 N1 C16 -175.9(2) . . . . ?
S2 Fe1 N1 C16 2.8(4) 2 . . . ?
S3 Fe1 N1 C16 25.8(2) . . . . ?
N1 Fe1 N2 C25 72.8(2) . . . . ?
S1 Fe1 N2 C25 17.4(6) . . . . ?
S2 Fe1 N2 C25 -27.9(2) . . . . ?
S2 Fe1 N2 C25 -123.7(2) 2 . . . ?
S3 Fe1 N2 C25 151.2(2) . . . . ?
N1 Fe1 N2 C26 -62.7(2) . . . . ?
S1 Fe1 N2 C26 -118.1(4) . . . . ?
S2 Fe1 N2 C26 -163.5(2) . . . . ?
S2 Fe1 N2 C26 100.7(2) 2 . . . ?
S3 Fe1 N2 C26 15.7(2) . . . . ?
Fe1 S1 C10 C15 27.6(2) . . . . ?
Fe1 S1 C10 C11 -150.5(3) . . . . ?
C15 C10 C11 C12 -0.5(5) . . . . ?
S1 C10 C11 C12 177.7(3) . . . . ?
C10 C11 C12 C13 0.6(5) . . . . ?
C11 C12 C13 C14 0.0(5) . . . . ?
C12 C13 C14 C15 -0.7(5) . . . . ?
C13 C14 C15 C10 0.9(5) . . . . ?
C13 C14 C15 N1 -179.8(3) . . . . ?
C11 C10 C15 C14 -0.3(4) . . . . ?
S1 C10 C15 C14 -178.5(2) . . . . ?
C11 C10 C15 N1 -179.6(3) . . . . ?
S1 C10 C15 N1 2.2(4) . . . . ?
C16 N1 C15 C14 -91.6(4) . . . . ?
Fe1 N1 C15 C14 146.0(2) . . . . ?
C16 N1 C15 C10 87.7(3) . . . . ?
Fe1 N1 C15 C10 -34.7(3) . . . . ?
C15 N1 C16 C17 -176.2(3) . . . . ?
Fe1 N1 C16 C17 -56.5(3) . . . . ?
N1 C16 C17 S3 60.1(4) . . . . ?
C27 S3 C17 C16 -130.8(3) . . . . ?
Fe1 S3 C17 C16 -32.5(3) . . . . ?
Fe1 S2 C20 C21 163.3(2) . . . . ?
Fe1 S2 C20 C21 -109.3(2) 2 . . . ?
Fe1 S2 C20 C25 -14.1(3) . . . . ?
Fe1 S2 C20 C25 73.3(3) 2 . . . ?
C25 C20 C21 C22 2.7(5) . . . . ?
S2 C20 C21 C22 -174.8(3) . . . . ?
C20 C21 C22 C23 0.0(5) . . . . ?
C21 C22 C23 C24 -2.5(5) . . . . ?
C22 C23 C24 C25 2.2(5) . . . . ?
C23 C24 C25 C20 0.5(5) . . . . ?
C23 C24 C25 N2 -177.0(3) . . . . ?
C21 C20 C25 C24 -2.9(5) . . . . ?
S2 C20 C25 C24 174.5(2) . . . . ?
C21 C20 C25 N2 174.8(3) . . . . ?
S2 C20 C25 N2 -7.8(4) . . . . ?
C26 N2 C25 C24 -19.1(4) . . . . ?
Fe1 N2 C25 C24 -154.2(2) . . . . ?
C26 N2 C25 C20 163.3(3) . . . . ?
Fe1 N2 C25 C20 28.2(3) . . . . ?
C25 N2 C26 C27 -179.0(3) . . . . ?
Fe1 N2 C26 C27 -44.1(3) . . . . ?
N2 C26 C27 S3 58.4(4) . . . . ?
C17 S3 C27 C26 61.1(3) . . . . ?
Fe1 S3 C27 C26 -39.3(3) . . . . ?
