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The neutral title complex, [{Fe({SCH2CH2}3N)(CO)-S,S′}2(μ-Fe)]·C6H6 or [Fe3(C6H12NS3)2(CO)2]·C6H6, contains two trigonal bipyramidally coordinated FeII atoms bridged by a tetrahedral FeII atom. There is disorder in one {SCH2CH2}3N ligand and in the solvent benzene present in the crystal structure. Dimensions in the complex are comparable to those in other five-coordinate metal–({SCH2CH2}3N) complexes.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802018573/ci6145sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536802018573/ci6145Isup2.hkl
Contains datablock I

CCDC reference: 200734

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.014 Å
  • Disorder in solvent or counterion
  • R factor = 0.057
  • wR factor = 0.144
  • Data-to-parameter ratio = 15.0

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


Amber Alert Alert Level B:
THETM_01 Alert B The value of sine(theta_max)/wavelength is less than 0.575 Calculated sin(theta_max)/wavelength = 0.5723
Author response: ... Data were collected to theta max. of 25deg., but those with theta greater than 24deg. were found to be unreliable and were not used in the final refinement.

Yellow Alert Alert Level C:
PLAT_202 Alert C Isotropic non-H Atoms in Anion/Solvent = 6 PLAT_302 Alert C Anion/Solvent Disorder ....................... 50.00 Perc. General Notes
ABSTM_02 When printed, the submitted absorption T values will be replaced by the scaled T values. Since the ratio of scaled T's is identical to the ratio of reported T values, the scaling does not imply a change to the absorption corrections used in the study. Ratio of Tmax expected/reported 0.851 Tmax scaled 0.817 Tmin scaled 0.778
0 Alert Level A = Potentially serious problem
1 Alert Level B = Potential problem
2 Alert Level C = Please check

Computing details top

Data collection: CAD-4 EXPRESS (Enraf-Nonius, 1992); cell refinement: CAD-4 EXPRESS; data reduction: CAD4 Processing Program (Hursthouse, 1976); program(s) used to solve structure: SHELXS86 (Sheldrick, 1986); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: SHELXL97.

µ-Ferrio-bis{carbonyl[µ-2,2',2''-nitrilotriethanethiolato(3-)- N,S,S',S'':S,S']iron(II)} benzene solvate top
Crystal data top
[Fe3(C6H12NS3)2(CO)2]·C6H6F(000) = 1416
Mr = 690.37Dx = 1.655 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71069 Å
Hall symbol: -P 2ynCell parameters from 24 reflections
a = 14.1644 (12) Åθ = 10–11°
b = 11.0663 (15) ŵ = 2.02 mm1
c = 17.820 (2) ÅT = 293 K
β = 97.226 (8)°Rectangular prism, orange–brown
V = 2771.1 (6) Å30.74 × 0.13 × 0.10 mm
Z = 4
Data collection top
Enraf-Nonius CAD-4
diffractometer
1873 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.058
Graphite monochromatorθmax = 24.0°, θmin = 1.5°
scintillation counter; ω/2θ scansh = 116
Absorption correction: ψ scan
(EMPABS; Sheldrick et al., 1977)
k = 112
Tmin = 0.914, Tmax = 0.960l = 2020
5226 measured reflections3 standard reflections every 300 reflections
4356 independent reflections intensity decay: none
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.057Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.144H-atom parameters constrained
S = 0.98 w = 1/[σ2(Fo2) + (0.036P)2]
where P = (Fo2 + 2Fc2)/3
4356 reflections(Δ/σ)max = 0.001
291 parametersΔρmax = 0.59 e Å3
0 restraintsΔρmin = 0.47 e Å3
Special details top

Experimental. Data were collected to θmax of 25° giving maximum h k l indices of 16, 13 and 21, and 4865 unique reflections, but those with θ greater than 24° were found to be unreliable and were not used in the final refinement, leaving data to maximum indices of 16, 12 and 20 and 4356 unique reflections with 1899 observed.

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Data were corrected for Lorentz-polarization effects, (Hursthouse, 1976), absorption using EMPABS, (Sheldrick et al., 1977), and negative intensities were eliminated using BAYES, (French et al., 1978), before structure solution and refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Fe10.40244 (10)0.91111 (11)0.63558 (7)0.0442 (4)
S10.35667 (19)0.7549 (2)0.70546 (13)0.0526 (7)
S20.4050 (2)0.8431 (2)0.51728 (13)0.0545 (7)
S30.4500 (2)1.0903 (2)0.68099 (14)0.0597 (7)
N40.5399 (5)0.8531 (7)0.6593 (4)0.050 (2)
C140.4738 (7)0.7026 (9)0.7429 (5)0.061 (3)
H14A0.49440.74380.79020.073*
H14B0.47140.61670.75340.073*
C410.5450 (8)0.7256 (9)0.6877 (6)0.074 (3)
H41A0.60870.70950.71250.089*
H41B0.53260.67070.64520.089*
C240.5299 (7)0.8001 (10)0.5235 (5)0.068 (3)
H24A0.53550.71300.52860.082*
H24B0.55480.82340.47730.082*
C420.5879 (7)0.8599 (11)0.5902 (5)0.074 (3)
H42A0.64950.82070.59970.089*
H42B0.59830.94390.57820.089*
C340.5772 (7)1.0631 (9)0.7032 (6)0.066 (3)
H34A0.60991.08680.66080.079*
H34B0.60261.11030.74700.079*
C430.5920 (8)0.9311 (9)0.7192 (6)0.075 (3)
H43A0.65940.91310.72320.090*
H43B0.57050.91220.76740.090*
C10.2916 (9)0.9729 (9)0.6158 (6)0.069 (3)
O10.2190 (6)1.0200 (8)0.6028 (7)0.129 (4)
Fe20.33136 (10)0.69828 (12)0.58149 (7)0.0455 (4)
Fe30.23887 (10)0.52547 (12)0.49710 (7)0.0518 (4)
S40.17006 (19)0.6872 (2)0.54539 (14)0.0570 (7)
S50.39107 (18)0.5158 (2)0.55223 (14)0.0535 (7)
S60.1667 (3)0.3880 (3)0.42039 (16)0.0873 (11)
N70.2024 (5)0.4255 (7)0.5862 (4)0.048 (2)
C470.1181 (7)0.6135 (9)0.6231 (6)0.071 (3)
H47A0.11670.66960.66480.085*0.541 (15)
H47B0.05340.58840.60600.085*0.541 (15)
H47C0.15530.63330.67100.085*0.459 (15)
H47D0.05370.64260.62440.085*0.459 (15)
C74A0.1801 (13)0.5015 (15)0.6496 (9)0.046 (5)*0.541 (15)
H74A0.23910.52880.67810.056*0.541 (15)
H74B0.14660.45300.68310.056*0.541 (15)
C74B0.1170 (16)0.4798 (19)0.6118 (12)0.053 (7)*0.459 (15)
H74C0.10690.44190.65920.063*0.459 (15)
H74D0.06280.45980.57500.063*0.459 (15)
C570.3757 (7)0.4138 (8)0.6320 (5)0.062 (3)
H57A0.42730.35570.63930.074*0.541 (15)
H57B0.37540.45990.67830.074*0.541 (15)
H57C0.38230.33050.61660.074*0.459 (15)
H57D0.42440.43030.67410.074*0.459 (15)
C75A0.2799 (12)0.3483 (17)0.6121 (10)0.051 (6)*0.541 (15)
H75A0.28680.28870.57330.061*0.541 (15)
H75B0.26490.30540.65660.061*0.541 (15)
C75B0.2808 (13)0.432 (2)0.6560 (11)0.049 (6)*0.459 (15)
H75C0.27840.51040.68030.059*0.459 (15)
H75D0.26910.37050.69240.059*0.459 (15)
C670.1251 (8)0.2859 (10)0.4893 (6)0.079 (4)
H67A0.06460.25100.46860.095*0.541 (15)
H67B0.17040.22060.50020.095*0.541 (15)
H67C0.05930.30380.49460.095*0.459 (15)
H67D0.12840.20320.47180.095*0.459 (15)
C76A0.1141 (16)0.350 (2)0.5586 (11)0.077 (7)*0.541 (15)
H76A0.10270.29260.59750.092*0.541 (15)
H76B0.05910.40300.54990.092*0.541 (15)
C76B0.1870 (18)0.300 (2)0.5669 (12)0.066 (8)*0.459 (15)
H76C0.15560.26030.60570.079*0.459 (15)
H76D0.24780.26020.56520.079*0.459 (15)
C20.2663 (8)0.6038 (10)0.4178 (6)0.069 (3)
O20.2819 (7)0.6534 (8)0.3642 (4)0.117 (4)
C81A0.0452 (17)1.119 (2)0.3078 (13)0.059 (7)*0.61 (3)
H81A0.02531.18000.27340.070*0.61 (3)
C82A0.1288 (18)1.080 (3)0.3086 (15)0.082 (8)*0.61 (3)
H82A0.16981.11660.27870.099*0.61 (3)
C83A0.1600 (17)0.982 (2)0.3539 (15)0.080 (7)*0.61 (3)
H83A0.21790.94450.34970.096*0.61 (3)
C84A0.1037 (18)0.944 (2)0.4035 (16)0.072 (9)*0.61 (3)
H84A0.12850.89000.44050.086*0.61 (3)
C85A0.0073 (15)0.9827 (19)0.4034 (10)0.054 (6)*0.61 (3)
H85A0.03380.94660.43350.064*0.61 (3)
C86A0.0199 (16)1.0778 (19)0.3551 (12)0.062 (6)*0.61 (3)
H86A0.07961.11310.35400.075*0.61 (3)
C81B0.013 (2)1.117 (3)0.3223 (17)0.043 (9)*0.39 (3)
H81B0.03311.17380.30650.052*0.39 (3)
C82B0.097 (3)1.086 (3)0.282 (2)0.067 (11)*0.39 (3)
H82B0.10501.12810.23800.081*0.39 (3)
C83B0.160 (2)1.000 (3)0.307 (2)0.071 (11)*0.39 (3)
H83B0.21180.98550.28090.086*0.39 (3)
C84B0.147 (3)0.927 (4)0.376 (2)0.080 (12)*0.39 (3)
H84B0.18750.86460.39290.096*0.39 (3)
C85B0.069 (3)0.960 (3)0.4126 (17)0.047 (10)*0.39 (3)
H85B0.05620.91860.45550.057*0.39 (3)
C86B0.017 (2)1.047 (3)0.3871 (16)0.045 (8)*0.39 (3)
H86B0.02871.06830.41800.054*0.39 (3)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe10.0621 (9)0.0286 (7)0.0429 (7)0.0003 (7)0.0108 (7)0.0012 (6)
S10.0786 (19)0.0424 (15)0.0400 (13)0.0059 (14)0.0196 (13)0.0030 (12)
S20.087 (2)0.0389 (15)0.0382 (13)0.0060 (14)0.0087 (13)0.0057 (11)
S30.087 (2)0.0354 (14)0.0577 (16)0.0029 (15)0.0127 (14)0.0044 (13)
N40.059 (5)0.042 (5)0.049 (5)0.001 (4)0.006 (4)0.003 (4)
C140.084 (8)0.050 (7)0.047 (6)0.012 (6)0.000 (5)0.014 (5)
C410.092 (9)0.055 (8)0.071 (7)0.002 (6)0.000 (7)0.023 (6)
C240.095 (9)0.058 (7)0.058 (7)0.004 (7)0.032 (6)0.008 (6)
C420.076 (8)0.086 (9)0.065 (7)0.013 (7)0.026 (6)0.021 (7)
C340.074 (8)0.058 (7)0.061 (7)0.020 (6)0.009 (6)0.010 (6)
C430.089 (9)0.051 (7)0.081 (8)0.002 (6)0.004 (7)0.017 (6)
C10.069 (8)0.039 (7)0.096 (9)0.011 (6)0.001 (7)0.012 (6)
O10.062 (6)0.074 (7)0.244 (12)0.023 (5)0.002 (7)0.001 (7)
Fe20.0684 (10)0.0311 (7)0.0387 (7)0.0036 (7)0.0131 (7)0.0003 (6)
Fe30.0777 (11)0.0412 (8)0.0377 (7)0.0092 (8)0.0126 (7)0.0001 (7)
S40.0692 (18)0.0381 (15)0.0641 (16)0.0054 (13)0.0097 (14)0.0122 (13)
S50.0628 (18)0.0411 (15)0.0600 (16)0.0003 (13)0.0205 (13)0.0134 (13)
S60.131 (3)0.076 (2)0.0520 (17)0.034 (2)0.0005 (18)0.0125 (16)
N70.060 (5)0.036 (5)0.050 (5)0.009 (4)0.011 (4)0.008 (4)
C470.075 (8)0.061 (8)0.085 (8)0.012 (6)0.047 (6)0.020 (6)
C570.085 (8)0.029 (5)0.067 (7)0.001 (6)0.006 (6)0.007 (5)
C670.096 (9)0.061 (8)0.076 (8)0.026 (7)0.013 (7)0.002 (6)
C20.101 (9)0.055 (7)0.053 (7)0.012 (7)0.014 (6)0.002 (6)
O20.203 (10)0.111 (7)0.043 (4)0.052 (7)0.038 (5)0.011 (5)
Geometric parameters (Å, º) top
Fe1—C11.708 (13)S5—C571.850 (10)
Fe1—N42.043 (8)S6—C671.820 (10)
Fe1—S32.214 (3)N7—C75A1.422 (17)
Fe1—S22.243 (3)N7—C76B1.45 (2)
Fe1—S12.272 (3)N7—C74B1.47 (2)
Fe1—Fe22.6917 (18)N7—C74A1.474 (17)
S1—C141.805 (10)N7—C76A1.53 (2)
S1—Fe22.281 (3)N7—C75B1.56 (2)
S2—C241.822 (10)C47—C74B1.49 (2)
S2—Fe22.295 (3)C47—C74A1.558 (18)
S3—C341.820 (10)C57—C75B1.47 (2)
N4—C421.481 (11)C57—C75A1.540 (18)
N4—C431.493 (12)C67—C76A1.45 (2)
N4—C411.498 (11)C67—C76B1.55 (2)
C14—C411.516 (13)C2—O21.148 (11)
C24—C421.510 (12)C81A—C82A1.26 (3)
C34—C431.498 (13)C81A—C86A1.40 (3)
C1—O11.150 (12)C82A—C83A1.39 (3)
Fe2—S52.276 (3)C83A—C84A1.33 (3)
Fe2—S42.298 (3)C84A—C85A1.43 (3)
Fe2—Fe32.6721 (18)C85A—C86A1.38 (3)
Fe3—C21.743 (11)C81B—C82B1.50 (5)
Fe3—N72.054 (7)C81B—C86B1.38 (4)
Fe3—S62.209 (3)C82B—C83B1.34 (5)
Fe3—S52.256 (3)C83B—C84B1.50 (5)
Fe3—S42.260 (3)C84B—C85B1.40 (5)
S4—C471.838 (9)C85B—C86B1.26 (4)
C1—Fe1—N4174.7 (4)N7—Fe3—Fe295.9 (2)
C1—Fe1—S387.0 (3)S6—Fe3—Fe2175.95 (11)
N4—Fe1—S388.1 (2)S5—Fe3—Fe254.20 (7)
C1—Fe1—S293.6 (4)S4—Fe3—Fe254.77 (8)
N4—Fe1—S287.8 (2)C47—S4—Fe399.7 (3)
S3—Fe1—S2127.13 (11)C47—S4—Fe2106.9 (4)
C1—Fe1—S195.7 (4)Fe3—S4—Fe271.79 (9)
N4—Fe1—S188.7 (2)C57—S5—Fe399.5 (3)
S3—Fe1—S1125.14 (11)C57—S5—Fe2106.4 (3)
S2—Fe1—S1107.43 (10)Fe3—S5—Fe272.26 (9)
C1—Fe1—Fe289.1 (3)C67—S6—Fe3100.0 (3)
N4—Fe1—Fe295.9 (2)C75A—N7—C76B65.5 (12)
S3—Fe1—Fe2175.77 (10)C75A—N7—C74B140.8 (12)
S2—Fe1—Fe254.52 (7)C76B—N7—C74B111.2 (14)
S1—Fe1—Fe253.91 (7)C75A—N7—C74A108.9 (11)
C14—S1—Fe197.7 (3)C76B—N7—C74A133.7 (13)
C14—S1—Fe2107.2 (3)C74B—N7—C74A42.9 (9)
Fe1—S1—Fe272.48 (8)C75A—N7—C76A110.1 (13)
C24—S2—Fe199.3 (3)C76B—N7—C76A46.1 (11)
C24—S2—Fe2106.6 (3)C74B—N7—C76A69.6 (12)
Fe1—S2—Fe272.75 (8)C74A—N7—C76A108.1 (12)
C34—S3—Fe1100.3 (3)C75A—N7—C75B47.7 (9)
C42—N4—C43109.2 (8)C76B—N7—C75B107.8 (13)
C42—N4—C41108.7 (8)C74B—N7—C75B105.3 (12)
C43—N4—C41107.7 (7)C74A—N7—C75B64.0 (10)
C42—N4—Fe1109.7 (6)C76A—N7—C75B138.7 (12)
C43—N4—Fe1109.8 (6)C75A—N7—Fe3108.4 (8)
C41—N4—Fe1111.7 (6)C76B—N7—Fe3112.4 (10)
C41—C14—S1111.2 (7)C74B—N7—Fe3108.4 (9)
N4—C41—C14111.7 (9)C74A—N7—Fe3112.6 (8)
C42—C24—S2111.2 (7)C76A—N7—Fe3108.6 (9)
N4—C42—C24111.8 (8)C75B—N7—Fe3111.6 (8)
C43—C34—S3108.2 (7)C74B—C47—C74A41.2 (9)
N4—C43—C34112.5 (8)C74B—C47—S4109.6 (10)
O1—C1—Fe1176.6 (10)C74A—C47—S4108.5 (8)
S5—Fe2—S1116.63 (11)N7—C74A—C47112.9 (12)
S5—Fe2—S2107.48 (10)N7—C74B—C47116.8 (15)
S1—Fe2—S2105.37 (10)C75B—C57—C75A47.4 (9)
S5—Fe2—S4105.88 (11)C75B—C57—S5109.8 (9)
S1—Fe2—S4108.38 (11)C75A—C57—S5107.2 (8)
S2—Fe2—S4113.33 (10)N7—C75A—C57114.4 (13)
S5—Fe2—Fe353.54 (8)C57—C75B—N7110.2 (14)
S1—Fe2—Fe3138.41 (9)C76A—C67—C76B45.7 (10)
S2—Fe2—Fe3116.15 (8)C76A—C67—S6110.4 (11)
S4—Fe2—Fe353.44 (8)C76B—C67—S6110.3 (10)
S5—Fe2—Fe1136.53 (9)C67—C76A—N7111.7 (15)
S1—Fe2—Fe153.61 (7)N7—C76B—C67111.0 (16)
S2—Fe2—Fe152.73 (7)O2—C2—Fe3177.7 (10)
S4—Fe2—Fe1117.44 (9)C82A—C81A—C86A125 (2)
Fe3—Fe2—Fe1164.28 (7)C81A—C82A—C83A120 (2)
C2—Fe3—N7176.5 (4)C84A—C83A—C82A117 (3)
C2—Fe3—S688.5 (3)C83A—C84A—C85A124 (2)
N7—Fe3—S688.0 (2)C86A—C85A—C84A114.7 (18)
C2—Fe3—S594.5 (4)C85A—C86A—C81A118.0 (18)
N7—Fe3—S587.5 (2)C86B—C81B—C82B109 (3)
S6—Fe3—S5125.40 (13)C83B—C82B—C81B122 (3)
C2—Fe3—S493.8 (4)C82B—C83B—C84B120 (3)
N7—Fe3—S488.3 (2)C85B—C84B—C83B116 (3)
S6—Fe3—S4126.39 (14)C86B—C85B—C84B119 (3)
S5—Fe3—S4107.83 (11)C85B—C86B—C81B133 (3)
C2—Fe3—Fe287.5 (3)
Fe2—S1—C14—C4142.9 (8)S4—C47—C74B—N741.9 (19)
Fe1—S1—C14—C4131.1 (7)C47—C74B—N7—Fe347.6 (18)
S1—C14—C41—N449.3 (10)Fe2—S5—C57—C75A92.8 (9)
C14—C41—N4—Fe141.7 (10)Fe3—S5—C57—C75A18.7 (9)
Fe2—S2—C24—C4293.0 (7)S5—C57—C75A—N748.4 (14)
Fe1—S2—C24—C4218.4 (8)C57—C75A—N7—Fe354.1 (14)
S2—C24—C42—N444.8 (11)Fe2—S5—C57—C75B42.8 (11)
C24—C42—N4—Fe150.1 (10)Fe3—S5—C57—C75B31.4 (10)
Fe1—S3—C34—C4327.2 (8)S5—C57—C75B—N750.6 (15)
S3—C34—C43—N449.8 (11)C57—C75B—N7—Fe346.2 (15)
C34—C43—N4—Fe148.0 (10)Fe3—S6—C67—C76A25.3 (12)
Fe2—S4—C47—C74A45.4 (10)S6—C67—C76A—N749.2 (18)
Fe3—S4—C47—C74A28.4 (10)C67—C76A—N7—Fe349.2 (18)
S4—C47—C74A—N747.3 (15)Fe3—S6—C67—C76B23.6 (13)
C47—C74A—N7—Fe342.7 (14)S6—C67—C76B—N745.4 (19)
Fe2—S4—C47—C74B89.1 (12)C67—C76B—N7—Fe345.5 (19)
Fe3—S4—C47—C74B15.3 (12)
 

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