metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

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ISSN: 2056-9890

Tetra­phenyl­phospho­nium [μ3-(4-methyl­phen­yl)tellurolato]tris­­[tetra­carbonyl­iron(0)]

aSchool of Chemistry and Pharmaceutical Engineering, Institute of Functional Materials, Sichuan University of Science & Engineering, Zigong, Sichuan 643000, People's Republic of China
*Correspondence e-mail: yu_longli@yahoo.cn

(Received 24 April 2013; accepted 13 May 2013; online 18 May 2013)

In the anion of the title compound, (C24H20P)[Fe3(C7H7Te)(CO)12], each Fe0 atom is coordinated by four CO ligands and a Te atom, resulting in a trigonal–bipyramidal coordination environment. The Te atom is coordinated by a 4-methyl­phenyl group and the Fe0 atoms in a distorted tetra­hedral geometry. The average Te—Fe bond length is 2.574 (4) Å.

Related literature

For related structures, see: Seyferth et al. (1985[Seyferth, D., Womack, G. B. & Dewan, J. C. (1985). Organometallics, 4, 398-400.]); Nicolet et al. (1999[Nicolet, Y., Piras, C., Legrand, P., Hatchikian, C. E. & Fontecilla-Camps, J. C. (1999). Structure, 7, 13-23.]); Shieh & Shieh (1994[Shieh, M. & Shieh, M.-H. (1994). Organometallics, 13, 920-924.]).

[Scheme 1]

Experimental

Crystal data
  • (C24H20P)[Fe3(C7H7Te)(CO)12]

  • Mr = 1061.77

  • Triclinic, [P \overline 1]

  • a = 12.367 (7) Å

  • b = 12.558 (6) Å

  • c = 13.626 (7) Å

  • α = 89.802 (17)°

  • β = 87.964 (13)°

  • γ = 86.312 (18)°

  • V = 2110.5 (19) Å3

  • Z = 2

  • Mo Kα radiation

  • μ = 1.80 mm−1

  • T = 113 K

  • 0.20 × 0.18 × 0.12 mm

Data collection
  • Rigaku Saturn724 CCD diffractometer

  • Absorption correction: multi-scan (CrystalClear; Rigaku/MSC, 2005[Rigaku/MSC (2005). CrystalClear and CrystalStructure. Rigaku/MSC Inc. The Woodlands, Texas, USA.]) Tmin = 0.715, Tmax = 0.813

  • 22136 measured reflections

  • 9949 independent reflections

  • 7690 reflections with I > 2σ(I)

  • Rint = 0.040

Refinement
  • R[F2 > 2σ(F2)] = 0.038

  • wR(F2) = 0.068

  • S = 1.02

  • 9949 reflections

  • 542 parameters

  • H-atom parameters constrained

  • Δρmax = 1.07 e Å−3

  • Δρmin = −0.96 e Å−3

Data collection: CrystalClear (Rigaku/MSC, 2005[Rigaku/MSC (2005). CrystalClear and CrystalStructure. Rigaku/MSC Inc. The Woodlands, Texas, USA.]); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: SHELXTL/PC (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); software used to prepare material for publication: CrystalStructure (Rigaku/MSC, 2005[Rigaku/MSC (2005). CrystalClear and CrystalStructure. Rigaku/MSC Inc. The Woodlands, Texas, USA.]).

Supporting information


Comment top

Fe/S cluster complexes containing µ-CO ligands have received considerable attention owing to their unique strucutre and particularly their apparent close relationship to the active site of [FeFe] hydrogenases (Seyferth et al., 1985; Nicolet et al., 1999). Herein, we report the synthesis and crystal struture of the title compound (Fig. 1). Each iron atom is coordinated by four CO ligands and Te1 resulting in a trigonal bipyramidal coordination environment. Tellurium is bonded to the 4-methylphenyl group and the iron atoms in a tetrahedral coordination mode. The average Te—Fe bond distances is 2.574 (1) Å is comparable to those found in the related structure [Et4N][BrFe2O6Te2] (Fe(1)—Te(1) = 2.524 (3) Å, Shieh & Shieh, 1994).

Related literature top

For related structures, see: Seyferth et al. (1985); Nicolet et al. (1999); Shieh & Shieh (1994).

Experimental top

The reaction was carried out under nitrogen atmosphere. Te (0.128 g, 1.0 mmol) and p-tolylmagnesium bromide (1.0 ml, 1.0 M in THF) were added to THF (30 ml) in a Schlenk flask and stirred for 1.0 h at room temperature. Fe3(CO)12 (0.504 g, 1.0 mmol) was then added. After stirring for 0.5 h, Ph4PBr (0.420 g, 1.0 mmol) was added, the resulting mixture was stirred for 12 h, then volatiles were removed and the title compound was recrystallized from CH2Cl2/hexane (v/v = 1:1) to afford crystals. Yield: 10%. Anal. Calcd (%) for C43H27Fe3O12PTe (Mr = 1061.78): C, 48.64; H, 2.56; Found (%): C, 48.52; H, 2.61.

Refinement top

All H atoms were placed in geometrically idealized positions and constrained to ride on their parent atoms, with phenyl and methyl C—H distances of 0.95 and 0.98 Å, respecively. Uiso(H) values were set to 1.2 (phenyl) and 1.5Ueq(C) (methyl).

Computing details top

Data collection: CrystalClear (Rigaku/MSC, 2005); cell refinement: CrystalClear (Rigaku/MSC, 2005); data reduction: CrystalClear (Rigaku/MSC, 2005); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL/PC (Sheldrick, 2008); software used to prepare material for publication: CrystalStructure (Rigaku/MSC, 2005).

Figures top
[Figure 1] Fig. 1. Molecular structure of the title compound, showing 30% probability displacement ellipsoids. H atoms have been omitted for clarity.
[Figure 2] Fig. 2. Packing diagram of the title compound.
Tetraphenylphosphonium [µ3-(4-methylphenyl)tellurolato]tris[tetracarbonyliron(0)] top
Crystal data top
(C24H20P)[Fe3(C7H7Te)(CO)12]Z = 2
Mr = 1061.77F(000) = 1052
Triclinic, P1Dx = 1.671 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 12.367 (7) ÅCell parameters from 7686 reflections
b = 12.558 (6) Åθ = 1.5–28.0°
c = 13.626 (7) ŵ = 1.80 mm1
α = 89.802 (17)°T = 113 K
β = 87.964 (13)°Prism, colorless
γ = 86.312 (18)°0.20 × 0.18 × 0.12 mm
V = 2110.5 (19) Å3
Data collection top
Rigaku Saturn724 CCD
diffractometer
9949 independent reflections
Radiation source: rotating anode7690 reflections with I > 2σ(I)
Multilayer monochromatorRint = 0.040
Detector resolution: 14.22 pixels mm-1θmax = 27.9°, θmin = 1.5°
ω and ϕ scansh = 1616
Absorption correction: multi-scan
(CrystalClear; Rigaku/MSC, 2005)
k = 1614
Tmin = 0.715, Tmax = 0.813l = 1717
22136 measured reflections
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)] = 0.038Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.068H-atom parameters constrained
S = 1.02 w = 1/[σ2(Fo2) + (0.018P)2]
where P = (Fo2 + 2Fc2)/3
9949 reflections(Δ/σ)max = 0.005
542 parametersΔρmax = 1.07 e Å3
0 restraintsΔρmin = 0.96 e Å3
Crystal data top
(C24H20P)[Fe3(C7H7Te)(CO)12]γ = 86.312 (18)°
Mr = 1061.77V = 2110.5 (19) Å3
Triclinic, P1Z = 2
a = 12.367 (7) ÅMo Kα radiation
b = 12.558 (6) ŵ = 1.80 mm1
c = 13.626 (7) ÅT = 113 K
α = 89.802 (17)°0.20 × 0.18 × 0.12 mm
β = 87.964 (13)°
Data collection top
Rigaku Saturn724 CCD
diffractometer
9949 independent reflections
Absorption correction: multi-scan
(CrystalClear; Rigaku/MSC, 2005)
7690 reflections with I > 2σ(I)
Tmin = 0.715, Tmax = 0.813Rint = 0.040
22136 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0380 restraints
wR(F2) = 0.068H-atom parameters constrained
S = 1.02Δρmax = 1.07 e Å3
9949 reflectionsΔρmin = 0.96 e Å3
542 parameters
Special details top

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. 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, with F set to zero for negative F2. 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*/Ueq
Te10.691679 (15)0.758534 (15)0.266548 (13)0.01634 (5)
Fe10.89752 (3)0.77509 (3)0.27611 (3)0.01900 (10)
Fe20.60360 (4)0.69476 (3)0.42882 (3)0.02299 (11)
Fe30.64378 (3)0.64786 (3)0.11779 (3)0.01782 (10)
P10.00221 (6)0.76504 (6)0.75476 (5)0.01717 (17)
O10.88942 (18)0.78268 (17)0.49180 (15)0.0343 (6)
O21.13180 (19)0.79072 (19)0.27970 (18)0.0438 (6)
O30.93297 (18)0.56280 (17)0.18610 (16)0.0358 (6)
O40.87619 (18)0.96158 (18)0.14596 (17)0.0397 (6)
O50.7700 (2)0.51627 (18)0.42636 (16)0.0406 (6)
O60.65189 (19)0.88384 (18)0.54154 (16)0.0389 (6)
O70.5086 (2)0.6040 (2)0.60572 (18)0.0514 (7)
O80.3964 (2)0.6788 (3)0.33252 (19)0.0706 (10)
O90.42183 (19)0.74524 (18)0.11968 (17)0.0396 (6)
O100.60419 (18)0.52660 (16)0.05756 (15)0.0322 (6)
O110.81703 (19)0.74332 (18)0.00161 (15)0.0378 (6)
O120.68476 (19)0.44626 (17)0.22563 (16)0.0370 (6)
C10.8880 (2)0.7808 (2)0.4075 (2)0.0249 (7)
C21.0394 (3)0.7854 (2)0.2783 (2)0.0278 (7)
C30.9171 (2)0.6449 (2)0.2214 (2)0.0242 (7)
C40.8830 (2)0.8892 (3)0.1975 (2)0.0261 (7)
C50.7045 (3)0.5864 (3)0.4247 (2)0.0289 (8)
C60.6334 (3)0.8114 (3)0.4946 (2)0.0288 (8)
C70.5452 (3)0.6398 (3)0.5365 (2)0.0330 (8)
C80.4788 (3)0.6861 (3)0.3673 (2)0.0387 (9)
C90.5090 (3)0.7069 (2)0.1223 (2)0.0261 (7)
C100.6190 (2)0.5735 (2)0.0122 (2)0.0238 (7)
C110.7505 (3)0.7075 (2)0.0494 (2)0.0250 (7)
C120.6694 (2)0.5273 (2)0.1866 (2)0.0245 (7)
C130.6250 (2)0.9165 (2)0.2345 (2)0.0173 (6)
C140.6116 (3)0.9927 (2)0.3076 (2)0.0335 (8)
H140.63140.97490.37260.040*
C150.5699 (3)1.0939 (2)0.2870 (2)0.0327 (8)
H150.56211.14520.33820.039*
C160.5388 (2)1.1234 (2)0.1926 (2)0.0247 (7)
C170.5556 (3)1.0475 (2)0.1210 (2)0.0298 (8)
H170.53721.06550.05560.036*
C180.5986 (3)0.9451 (2)0.1406 (2)0.0292 (8)
H180.60980.89460.08880.035*
C190.4883 (3)1.2327 (2)0.1721 (2)0.0365 (8)
H19A0.46861.23730.10310.055*
H19B0.54031.28620.18530.055*
H19C0.42321.24600.21450.055*
C200.0707 (2)0.6535 (2)0.71677 (19)0.0179 (6)
C210.1683 (2)0.6338 (2)0.7639 (2)0.0269 (7)
H210.19780.68100.81380.032*
C220.2239 (3)0.5452 (3)0.7388 (2)0.0307 (8)
H220.29140.53250.77070.037*
C230.1801 (3)0.4762 (2)0.6671 (2)0.0299 (8)
H230.21730.41530.65030.036*
C240.0828 (3)0.4949 (2)0.6195 (2)0.0283 (8)
H240.05360.44740.56980.034*
C250.0275 (2)0.5836 (2)0.6444 (2)0.0236 (7)
H250.03970.59630.61200.028*
C260.0972 (2)0.8696 (2)0.7888 (2)0.0183 (6)
C270.1827 (2)0.8945 (2)0.7263 (2)0.0246 (7)
H270.18600.85800.66560.030*
C280.2623 (2)0.9723 (2)0.7529 (2)0.0281 (7)
H280.32030.98980.71070.034*
C290.2568 (3)1.0245 (2)0.8419 (2)0.0287 (8)
H290.31171.07760.86070.034*
C300.1730 (3)1.0004 (2)0.9032 (2)0.0285 (8)
H300.17021.03730.96370.034*
C310.0921 (2)0.9225 (2)0.8776 (2)0.0212 (7)
H310.03430.90560.92030.025*
C320.0834 (2)0.7279 (2)0.85719 (19)0.0171 (6)
C330.0495 (2)0.6507 (2)0.9234 (2)0.0221 (7)
H330.01500.61570.91280.027*
C340.1104 (3)0.6253 (2)1.0050 (2)0.0266 (7)
H340.08830.57171.04940.032*
C350.2029 (2)0.6774 (2)1.0217 (2)0.0263 (7)
H350.24390.66061.07790.032*
C360.2357 (2)0.7546 (2)0.9557 (2)0.0234 (7)
H360.29940.79040.96710.028*
C370.1771 (2)0.7798 (2)0.8741 (2)0.0209 (7)
H370.20040.83250.82930.025*
C380.0915 (2)0.8065 (2)0.65763 (19)0.0178 (6)
C390.1806 (2)0.7382 (2)0.6292 (2)0.0236 (7)
H390.19500.67300.66330.028*
C400.2480 (3)0.7657 (3)0.5512 (2)0.0289 (8)
H400.30770.71860.53080.035*
C410.2285 (3)0.8614 (3)0.5029 (2)0.0316 (8)
H410.27410.87910.44840.038*
C420.1435 (3)0.9315 (2)0.5329 (2)0.0266 (7)
H420.13240.99870.50140.032*
C430.0741 (2)0.9031 (2)0.6099 (2)0.0219 (7)
H430.01440.95040.62980.026*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Te10.01614 (11)0.01721 (11)0.01579 (10)0.00058 (8)0.00307 (7)0.00083 (7)
Fe10.0173 (2)0.0202 (2)0.0198 (2)0.00153 (19)0.00379 (18)0.00052 (17)
Fe20.0226 (3)0.0266 (3)0.0199 (2)0.0029 (2)0.00044 (19)0.00009 (18)
Fe30.0196 (2)0.0169 (2)0.0172 (2)0.00067 (18)0.00419 (17)0.00139 (17)
P10.0166 (4)0.0184 (4)0.0164 (4)0.0003 (3)0.0012 (3)0.0007 (3)
O10.0375 (15)0.0433 (15)0.0229 (13)0.0049 (11)0.0083 (11)0.0015 (10)
O20.0220 (14)0.0529 (17)0.0578 (17)0.0086 (12)0.0094 (12)0.0114 (13)
O30.0358 (15)0.0288 (14)0.0419 (15)0.0091 (11)0.0081 (11)0.0114 (11)
O40.0329 (15)0.0355 (15)0.0523 (16)0.0102 (11)0.0097 (12)0.0227 (12)
O50.0505 (17)0.0358 (15)0.0338 (14)0.0138 (13)0.0083 (12)0.0006 (11)
O60.0508 (17)0.0374 (15)0.0287 (13)0.0038 (12)0.0020 (11)0.0077 (11)
O70.0589 (19)0.0588 (18)0.0367 (15)0.0127 (14)0.0124 (13)0.0067 (13)
O80.0275 (17)0.141 (3)0.0466 (18)0.0261 (18)0.0046 (14)0.0042 (18)
O90.0290 (15)0.0432 (16)0.0461 (15)0.0111 (12)0.0155 (11)0.0121 (12)
O100.0366 (14)0.0345 (14)0.0261 (12)0.0049 (11)0.0041 (10)0.0121 (10)
O110.0463 (16)0.0428 (15)0.0258 (13)0.0200 (12)0.0076 (12)0.0010 (11)
O120.0557 (17)0.0238 (14)0.0312 (13)0.0028 (12)0.0083 (12)0.0037 (10)
C10.0196 (18)0.0237 (18)0.0317 (19)0.0018 (14)0.0059 (14)0.0020 (14)
C20.031 (2)0.0255 (19)0.0273 (18)0.0022 (15)0.0034 (15)0.0033 (13)
C30.0202 (18)0.0293 (19)0.0233 (17)0.0009 (14)0.0052 (13)0.0032 (13)
C40.0176 (17)0.030 (2)0.0316 (18)0.0047 (14)0.0055 (14)0.0006 (14)
C50.038 (2)0.028 (2)0.0214 (17)0.0037 (16)0.0011 (15)0.0017 (14)
C60.030 (2)0.033 (2)0.0238 (18)0.0021 (16)0.0001 (14)0.0022 (14)
C70.032 (2)0.037 (2)0.0293 (19)0.0058 (16)0.0022 (16)0.0002 (15)
C80.029 (2)0.061 (3)0.0265 (19)0.0095 (19)0.0018 (16)0.0038 (17)
C90.030 (2)0.0238 (18)0.0248 (17)0.0021 (15)0.0089 (14)0.0071 (13)
C100.0209 (17)0.0219 (18)0.0287 (18)0.0015 (14)0.0020 (14)0.0003 (13)
C110.034 (2)0.0257 (18)0.0162 (16)0.0022 (15)0.0055 (14)0.0057 (13)
C120.0256 (19)0.0279 (19)0.0201 (16)0.0009 (15)0.0046 (13)0.0074 (14)
C130.0113 (15)0.0140 (16)0.0261 (16)0.0032 (12)0.0032 (12)0.0011 (12)
C140.051 (2)0.0256 (19)0.0227 (18)0.0107 (17)0.0064 (16)0.0038 (14)
C150.049 (2)0.0210 (19)0.0268 (18)0.0114 (16)0.0013 (16)0.0059 (14)
C160.0188 (17)0.0211 (18)0.0343 (19)0.0000 (14)0.0024 (14)0.0043 (14)
C170.042 (2)0.0213 (18)0.0274 (18)0.0015 (15)0.0150 (15)0.0055 (13)
C180.044 (2)0.0194 (18)0.0249 (17)0.0003 (15)0.0115 (15)0.0025 (13)
C190.038 (2)0.030 (2)0.041 (2)0.0018 (16)0.0048 (17)0.0037 (16)
C200.0180 (16)0.0189 (16)0.0167 (15)0.0018 (13)0.0057 (12)0.0002 (11)
C210.0259 (19)0.034 (2)0.0211 (17)0.0023 (15)0.0013 (14)0.0084 (14)
C220.0251 (19)0.040 (2)0.0285 (18)0.0105 (16)0.0006 (14)0.0002 (15)
C230.039 (2)0.0277 (19)0.0253 (18)0.0120 (16)0.0103 (15)0.0010 (14)
C240.036 (2)0.0248 (19)0.0246 (17)0.0032 (15)0.0029 (15)0.0038 (13)
C250.0254 (18)0.0257 (18)0.0197 (16)0.0021 (14)0.0003 (13)0.0003 (13)
C260.0179 (17)0.0172 (16)0.0194 (15)0.0015 (13)0.0012 (12)0.0002 (12)
C270.0257 (19)0.0254 (18)0.0224 (17)0.0015 (14)0.0011 (13)0.0022 (13)
C280.0179 (18)0.034 (2)0.0315 (19)0.0045 (15)0.0039 (14)0.0028 (14)
C290.0232 (19)0.0237 (18)0.038 (2)0.0076 (14)0.0042 (15)0.0005 (14)
C300.033 (2)0.0241 (19)0.0280 (18)0.0014 (15)0.0013 (15)0.0046 (14)
C310.0183 (17)0.0233 (17)0.0223 (16)0.0017 (13)0.0019 (13)0.0024 (12)
C320.0167 (16)0.0176 (16)0.0163 (15)0.0040 (13)0.0019 (12)0.0036 (11)
C330.0204 (17)0.0238 (18)0.0225 (16)0.0020 (14)0.0040 (13)0.0017 (13)
C340.033 (2)0.0241 (18)0.0227 (17)0.0004 (15)0.0017 (14)0.0064 (13)
C350.0291 (19)0.0281 (19)0.0216 (17)0.0041 (15)0.0104 (14)0.0010 (13)
C360.0181 (17)0.0276 (19)0.0247 (17)0.0001 (14)0.0040 (13)0.0046 (13)
C370.0204 (17)0.0198 (17)0.0224 (16)0.0004 (13)0.0015 (13)0.0015 (12)
C380.0194 (17)0.0188 (16)0.0153 (14)0.0015 (13)0.0017 (12)0.0004 (11)
C390.0239 (18)0.0225 (18)0.0242 (17)0.0006 (14)0.0003 (13)0.0017 (13)
C400.0233 (19)0.031 (2)0.0320 (19)0.0019 (15)0.0075 (14)0.0012 (15)
C410.035 (2)0.035 (2)0.0251 (18)0.0067 (17)0.0068 (15)0.0031 (14)
C420.033 (2)0.0200 (18)0.0273 (18)0.0035 (15)0.0027 (14)0.0065 (13)
C430.0210 (17)0.0195 (17)0.0249 (17)0.0022 (13)0.0038 (13)0.0030 (12)
Geometric parameters (Å, º) top
Te1—C132.148 (3)C19—H19C0.9800
Te1—Fe32.5693 (11)C20—C211.384 (4)
Te1—Fe12.5754 (14)C20—C251.391 (4)
Te1—Fe22.5780 (12)C21—C221.395 (4)
Fe1—C21.769 (4)C21—H210.9500
Fe1—C41.790 (3)C22—C231.382 (4)
Fe1—C11.791 (3)C22—H220.9500
Fe1—C31.797 (3)C23—C241.380 (4)
Fe2—C71.770 (3)C23—H230.9500
Fe2—C61.784 (3)C24—C251.392 (4)
Fe2—C51.786 (4)C24—H240.9500
Fe2—C81.792 (4)C25—H250.9500
Fe3—C101.765 (3)C26—C311.388 (4)
Fe3—C91.780 (3)C26—C271.401 (4)
Fe3—C111.790 (3)C27—C281.381 (4)
Fe3—C121.794 (3)C27—H270.9500
P1—C261.791 (3)C28—C291.386 (4)
P1—C381.791 (3)C28—H280.9500
P1—C321.791 (3)C29—C301.372 (4)
P1—C201.801 (3)C29—H290.9500
O1—C11.150 (3)C30—C311.390 (4)
O2—C21.150 (4)C30—H300.9500
O3—C31.142 (3)C31—H310.9500
O4—C41.147 (4)C32—C371.392 (4)
O5—C51.158 (4)C32—C331.396 (4)
O6—C61.154 (3)C33—C341.390 (4)
O7—C71.136 (4)C33—H330.9500
O8—C81.148 (4)C34—C351.380 (4)
O9—C91.153 (4)C34—H340.9500
O10—C101.146 (3)C35—C361.391 (4)
O11—C111.145 (3)C35—H350.9500
O12—C121.155 (3)C36—C371.373 (4)
C13—C181.372 (4)C36—H360.9500
C13—C141.382 (4)C37—H370.9500
C14—C151.371 (4)C38—C431.382 (4)
C14—H140.9500C38—C391.397 (4)
C15—C161.397 (4)C39—C401.384 (4)
C15—H150.9500C39—H390.9500
C16—C171.367 (4)C40—C411.380 (4)
C16—C191.501 (4)C40—H400.9500
C17—C181.389 (4)C41—C421.378 (4)
C17—H170.9500C41—H410.9500
C18—H180.9500C42—C431.392 (4)
C19—H19A0.9800C42—H420.9500
C19—H19B0.9800C43—H430.9500
C13—Te1—Fe3103.91 (8)C16—C19—H19C109.5
C13—Te1—Fe1105.46 (8)H19A—C19—H19C109.5
Fe3—Te1—Fe1112.05 (2)H19B—C19—H19C109.5
C13—Te1—Fe2108.79 (8)C21—C20—C25119.5 (3)
Fe3—Te1—Fe2112.82 (4)C21—C20—P1119.4 (2)
Fe1—Te1—Fe2113.06 (3)C25—C20—P1121.0 (2)
C2—Fe1—C491.25 (14)C20—C21—C22120.5 (3)
C2—Fe1—C190.42 (14)C20—C21—H21119.8
C4—Fe1—C1124.22 (14)C22—C21—H21119.8
C2—Fe1—C390.69 (14)C23—C22—C21119.4 (3)
C4—Fe1—C3118.77 (14)C23—C22—H22120.3
C1—Fe1—C3116.96 (14)C21—C22—H22120.3
C2—Fe1—Te1178.03 (10)C24—C23—C22120.6 (3)
C4—Fe1—Te187.96 (10)C24—C23—H23119.7
C1—Fe1—Te191.52 (10)C22—C23—H23119.7
C3—Fe1—Te188.11 (10)C23—C24—C25119.9 (3)
C7—Fe2—C690.84 (15)C23—C24—H24120.1
C7—Fe2—C589.61 (15)C25—C24—H24120.1
C6—Fe2—C5117.33 (15)C20—C25—C24120.1 (3)
C7—Fe2—C890.40 (16)C20—C25—H25120.0
C6—Fe2—C8121.94 (16)C24—C25—H25120.0
C5—Fe2—C8120.73 (16)C31—C26—C27120.3 (3)
C7—Fe2—Te1175.13 (11)C31—C26—P1120.6 (2)
C6—Fe2—Te193.60 (10)C27—C26—P1119.1 (2)
C5—Fe2—Te186.58 (10)C28—C27—C26119.9 (3)
C8—Fe2—Te188.95 (11)C28—C27—H27120.0
C10—Fe3—C991.86 (14)C26—C27—H27120.0
C10—Fe3—C1188.46 (13)C27—C28—C29119.4 (3)
C9—Fe3—C11121.47 (15)C27—C28—H28120.3
C10—Fe3—C1290.79 (14)C29—C28—H28120.3
C9—Fe3—C12117.38 (14)C30—C29—C28120.8 (3)
C11—Fe3—C12121.14 (14)C30—C29—H29119.6
C10—Fe3—Te1176.36 (10)C28—C29—H29119.6
C9—Fe3—Te190.85 (9)C29—C30—C31120.6 (3)
C11—Fe3—Te188.05 (9)C29—C30—H30119.7
C12—Fe3—Te190.11 (10)C31—C30—H30119.7
C26—P1—C38111.26 (13)C26—C31—C30118.9 (3)
C26—P1—C32110.38 (13)C26—C31—H31120.5
C38—P1—C32107.57 (14)C30—C31—H31120.5
C26—P1—C20106.86 (14)C37—C32—C33119.8 (3)
C38—P1—C20110.75 (13)C37—C32—P1120.3 (2)
C32—P1—C20110.05 (13)C33—C32—P1119.9 (2)
O1—C1—Fe1175.3 (3)C34—C33—C32119.7 (3)
O2—C2—Fe1179.2 (3)C34—C33—H33120.2
O3—C3—Fe1177.8 (3)C32—C33—H33120.2
O4—C4—Fe1178.3 (3)C35—C34—C33120.3 (3)
O5—C5—Fe2177.1 (3)C35—C34—H34119.9
O6—C6—Fe2176.4 (3)C33—C34—H34119.9
O7—C7—Fe2179.3 (4)C34—C35—C36119.6 (3)
O8—C8—Fe2176.4 (3)C34—C35—H35120.2
O9—C9—Fe3176.3 (3)C36—C35—H35120.2
O10—C10—Fe3178.6 (3)C37—C36—C35120.8 (3)
O11—C11—Fe3176.6 (3)C37—C36—H36119.6
O12—C12—Fe3175.7 (3)C35—C36—H36119.6
C18—C13—C14118.6 (3)C36—C37—C32119.8 (3)
C18—C13—Te1120.9 (2)C36—C37—H37120.1
C14—C13—Te1120.5 (2)C32—C37—H37120.1
C15—C14—C13120.5 (3)C43—C38—C39119.5 (3)
C15—C14—H14119.7C43—C38—P1122.0 (2)
C13—C14—H14119.7C39—C38—P1118.5 (2)
C14—C15—C16121.7 (3)C40—C39—C38119.8 (3)
C14—C15—H15119.1C40—C39—H39120.1
C16—C15—H15119.1C38—C39—H39120.1
C17—C16—C15116.7 (3)C41—C40—C39120.1 (3)
C17—C16—C19122.1 (3)C41—C40—H40119.9
C15—C16—C19121.2 (3)C39—C40—H40119.9
C16—C17—C18122.2 (3)C42—C41—C40120.6 (3)
C16—C17—H17118.9C42—C41—H41119.7
C18—C17—H17118.9C40—C41—H41119.7
C13—C18—C17120.2 (3)C41—C42—C43119.5 (3)
C13—C18—H18119.9C41—C42—H42120.3
C17—C18—H18119.9C43—C42—H42120.3
C16—C19—H19A109.5C38—C43—C42120.4 (3)
C16—C19—H19B109.5C38—C43—H43119.8
H19A—C19—H19B109.5C42—C43—H43119.8
C13—Te1—Fe1—C292 (3)C12—Fe3—C11—O1199 (5)
Fe3—Te1—Fe1—C221 (3)Te1—Fe3—C11—O11172 (5)
Fe2—Te1—Fe1—C2150 (3)C10—Fe3—C12—O121 (4)
C13—Te1—Fe1—C425.31 (12)C9—Fe3—C12—O1293 (4)
Fe3—Te1—Fe1—C487.09 (10)C11—Fe3—C12—O1288 (4)
Fe2—Te1—Fe1—C4144.06 (10)Te1—Fe3—C12—O12176 (4)
C13—Te1—Fe1—C198.89 (12)Fe3—Te1—C13—C1818.1 (3)
Fe3—Te1—Fe1—C1148.71 (10)Fe1—Te1—C13—C1899.9 (2)
Fe2—Te1—Fe1—C119.86 (10)Fe2—Te1—C13—C18138.6 (2)
C13—Te1—Fe1—C3144.19 (12)Fe3—Te1—C13—C14164.4 (2)
Fe3—Te1—Fe1—C331.79 (10)Fe1—Te1—C13—C1477.6 (2)
Fe2—Te1—Fe1—C397.06 (10)Fe2—Te1—C13—C1444.0 (2)
C13—Te1—Fe2—C7152.3 (14)C18—C13—C14—C151.8 (5)
Fe3—Te1—Fe2—C737.5 (14)Te1—C13—C14—C15179.4 (3)
Fe1—Te1—Fe2—C790.9 (14)C13—C14—C15—C160.6 (5)
C13—Te1—Fe2—C652.05 (14)C14—C15—C16—C172.3 (5)
Fe3—Te1—Fe2—C6166.80 (11)C14—C15—C16—C19177.0 (3)
Fe1—Te1—Fe2—C664.75 (11)C15—C16—C17—C181.7 (5)
C13—Te1—Fe2—C5169.24 (13)C19—C16—C17—C18177.6 (3)
Fe3—Te1—Fe2—C576.01 (11)C14—C13—C18—C172.4 (5)
Fe1—Te1—Fe2—C552.45 (11)Te1—C13—C18—C17180.0 (2)
C13—Te1—Fe2—C869.89 (14)C16—C17—C18—C130.6 (5)
Fe3—Te1—Fe2—C844.86 (12)C26—P1—C20—C2135.4 (3)
Fe1—Te1—Fe2—C8173.31 (12)C38—P1—C20—C21156.8 (2)
C13—Te1—Fe3—C1092.7 (16)C32—P1—C20—C2184.4 (3)
Fe1—Te1—Fe3—C1020.6 (16)C26—P1—C20—C25148.0 (2)
Fe2—Te1—Fe3—C10149.6 (16)C38—P1—C20—C2526.7 (3)
C13—Te1—Fe3—C945.43 (13)C32—P1—C20—C2592.2 (3)
Fe1—Te1—Fe3—C9158.79 (10)C25—C20—C21—C220.5 (5)
Fe2—Te1—Fe3—C972.23 (11)P1—C20—C21—C22177.2 (3)
C13—Te1—Fe3—C1176.03 (13)C20—C21—C22—C230.8 (5)
Fe1—Te1—Fe3—C1137.33 (10)C21—C22—C23—C240.8 (5)
Fe2—Te1—Fe3—C11166.31 (10)C22—C23—C24—C250.6 (5)
C13—Te1—Fe3—C12162.81 (12)C21—C20—C25—C240.3 (5)
Fe1—Te1—Fe3—C1283.83 (10)P1—C20—C25—C24176.9 (2)
Fe2—Te1—Fe3—C1245.15 (10)C23—C24—C25—C200.4 (5)
C2—Fe1—C1—O118 (3)C38—P1—C26—C31108.6 (2)
C4—Fe1—C1—O1110 (3)C32—P1—C26—C3110.7 (3)
C3—Fe1—C1—O173 (3)C20—P1—C26—C31130.4 (2)
Te1—Fe1—C1—O1161 (3)C38—P1—C26—C2774.0 (3)
C4—Fe1—C2—O2141 (19)C32—P1—C26—C27166.6 (2)
C1—Fe1—C2—O295 (19)C20—P1—C26—C2747.0 (3)
C3—Fe1—C2—O222 (19)C31—C26—C27—C280.3 (4)
Te1—Fe1—C2—O274 (20)P1—C26—C27—C28177.6 (2)
C2—Fe1—C3—O311 (7)C26—C27—C28—C290.4 (5)
C4—Fe1—C3—O380 (7)C27—C28—C29—C300.5 (5)
C1—Fe1—C3—O3102 (7)C28—C29—C30—C310.4 (5)
Te1—Fe1—C3—O3167 (7)C27—C26—C31—C300.2 (4)
C2—Fe1—C4—O435 (10)P1—C26—C31—C30177.5 (2)
C1—Fe1—C4—O4126 (10)C29—C30—C31—C260.3 (4)
C3—Fe1—C4—O457 (10)C26—P1—C32—C3789.0 (2)
Te1—Fe1—C4—O4143 (10)C38—P1—C32—C3732.5 (3)
C7—Fe2—C5—O536 (6)C20—P1—C32—C37153.3 (2)
C6—Fe2—C5—O555 (6)C26—P1—C32—C3387.4 (2)
C8—Fe2—C5—O5126 (6)C38—P1—C32—C33151.0 (2)
Te1—Fe2—C5—O5147 (6)C20—P1—C32—C3330.3 (3)
C7—Fe2—C6—O617 (5)C37—C32—C33—C340.9 (4)
C5—Fe2—C6—O673 (5)P1—C32—C33—C34177.4 (2)
C8—Fe2—C6—O6108 (5)C32—C33—C34—C351.3 (4)
Te1—Fe2—C6—O6161 (5)C33—C34—C35—C360.9 (4)
C6—Fe2—C7—O794 (30)C34—C35—C36—C370.1 (4)
C5—Fe2—C7—O723 (30)C35—C36—C37—C320.3 (4)
C8—Fe2—C7—O7144 (30)C33—C32—C37—C360.1 (4)
Te1—Fe2—C7—O762 (30)P1—C32—C37—C36176.6 (2)
C7—Fe2—C8—O85 (6)C26—P1—C38—C437.1 (3)
C6—Fe2—C8—O886 (6)C32—P1—C38—C43128.1 (2)
C5—Fe2—C8—O895 (6)C20—P1—C38—C43111.6 (2)
Te1—Fe2—C8—O8179 (100)C26—P1—C38—C39173.5 (2)
C10—Fe3—C9—O936 (4)C32—P1—C38—C3952.5 (3)
C11—Fe3—C9—O953 (4)C20—P1—C38—C3967.8 (3)
C12—Fe3—C9—O9128 (4)C43—C38—C39—C402.6 (4)
Te1—Fe3—C9—O9141 (4)P1—C38—C39—C40176.8 (2)
C9—Fe3—C10—O10108 (13)C38—C39—C40—C411.3 (5)
C11—Fe3—C10—O1013 (13)C39—C40—C41—C421.4 (5)
C12—Fe3—C10—O10134 (13)C40—C41—C42—C432.8 (5)
Te1—Fe3—C10—O1030 (14)C39—C38—C43—C421.1 (4)
C10—Fe3—C11—O119 (5)P1—C38—C43—C42178.2 (2)
C9—Fe3—C11—O1183 (5)C41—C42—C43—C381.6 (5)

Experimental details

Crystal data
Chemical formula(C24H20P)[Fe3(C7H7Te)(CO)12]
Mr1061.77
Crystal system, space groupTriclinic, P1
Temperature (K)113
a, b, c (Å)12.367 (7), 12.558 (6), 13.626 (7)
α, β, γ (°)89.802 (17), 87.964 (13), 86.312 (18)
V3)2110.5 (19)
Z2
Radiation typeMo Kα
µ (mm1)1.80
Crystal size (mm)0.20 × 0.18 × 0.12
Data collection
DiffractometerRigaku Saturn724 CCD
diffractometer
Absorption correctionMulti-scan
(CrystalClear; Rigaku/MSC, 2005)
Tmin, Tmax0.715, 0.813
No. of measured, independent and
observed [I > 2σ(I)] reflections
22136, 9949, 7690
Rint0.040
(sin θ/λ)max1)0.659
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.038, 0.068, 1.02
No. of reflections9949
No. of parameters542
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)1.07, 0.96

Computer programs: CrystalClear (Rigaku/MSC, 2005), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL/PC (Sheldrick, 2008), CrystalStructure (Rigaku/MSC, 2005).

 

Acknowledgements

The authors are grateful to Sichuan Science and Technology Department (2012JY0115, 2011JY0052, 2010GZ0130) and the start-up foundation of Sichuan University of Science & Engineering (2011RC06) for financial support.

References

First citationNicolet, Y., Piras, C., Legrand, P., Hatchikian, C. E. & Fontecilla-Camps, J. C. (1999). Structure, 7, 13–23.  Web of Science CrossRef PubMed CAS
First citationRigaku/MSC (2005). CrystalClear and CrystalStructure. Rigaku/MSC Inc. The Woodlands, Texas, USA.
First citationSeyferth, D., Womack, G. B. & Dewan, J. C. (1985). Organometallics, 4, 398–400.  CSD CrossRef CAS Web of Science
First citationSheldrick, G. M. (2008). Acta Cryst. A64, 112–122.  Web of Science CrossRef CAS IUCr Journals
First citationShieh, M. & Shieh, M.-H. (1994). Organometallics, 13, 920–924.  CSD CrossRef CAS Web of Science

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