Phosphorus-carbon(pyridyl) bond cleavage on reacting diphenyl-2- pyridylphosphine with triiron dodecacarbonyl

Article abstract of DOI:10.1016/j.ica.2011.06.035

The reaction of [Fe₃(CO)₁₂] with diphenyl-2- pyridylphosphine (PPh₂Py) in refluxing toluene for 1 h afforded three compounds, [Fe₂(CO)₆(μ-PPh₂)(μ- κ²-C,N-C₅H₄N)] (1), [Fe(CO) ₄(κ¹-P-PPh₂Py)] (2), and [Fe(CO) ₃(κ¹-P-PPh₂Py)₂] (3) in 23%, 10% and 3.5% yields after work-up, respectively. The PPh₂Py ligand acts as a terminal P-donor ligand in 2 and 3, while in 1 it underwent a selective phosphorus-carbon(pyridyl) bond cleavage to afford phosphido- and pyridyl-bridged ligands. The complexes were characterized by elemental analysis, FAB-mass, FTIR, ¹H and ³¹P-{¹H}NMR spectroscopies. Compounds 1 and 2 were also characterized by X-ray single crystal.

Full text of DOI:10.1016/j.ica.2011.06.035

Inorganica Chimica Acta 376 (2011) 641–644
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Note
Phosphorus–carbon(pyridyl) bond cleavage on reacting
diphenyl-2-pyridylphosphine with triiron dodecacarbonyl
Pankaj Das a, , Malabika Borah a, Francois Michaud b, François Y. Pétillon c, Philippe Schollhammer c,
⇑
⇑
a Department of Chemistry, Dibrugarh University, Dibrugarh, 786004 Assam, India
b Centre Commun d’Analyse par Diffraction des Rayons X, University of Bretagne Occidentale, France
c CNRS, UMR 6521, Chimie, Electrochimie Moleculaires et Chimie Analytique, University of Bretagne Occidentale, C.S. 93837, 29238 Brest Cedex 3, France
a r t i c l e i n f o
a b s t r a c t
Article history:
The reaction of [Fe3(CO)12] with diphenyl-2-pyridylphosphine (PPh2Py) in refluxing toluene for 1 h affor-
ded three compounds, [Fe2(CO)6( -PPh2)(
2-C,N-C5H4N)] (1), [Fe(CO)4( 1-P-PPh2Py)] (2), and
[Fe(CO)3(
1-P-PPh2Py)2] (3) in 23%, 10% and 3.5% yields after work-up, respectively. The PPh2Py ligand
acts as a terminal P-donor ligand in 2 and 3, while in 1 it underwent a selective phosphorus–carbon(pyr-
idyl) bond cleavage to afford phosphido- and pyridyl-bridged ligands. The complexes were characterized
by elemental analysis, FAB-mass, FTIR, 1H and 31P–{1H}NMR spectroscopies. Compounds 1 and 2 were
also characterized by X-ray single crystal.
Received 19 May 2011
Accepted 22 June 2011
Available online 2 July 2011
l
l
-
j
j
j
Keywords:
Iron complexes
Bimetallic
Phosphorus–carbon bond cleavage
X-ray crystal structures
Pyridylphosphine
Ó 2011 Elsevier B.V. All rights reserved.
1. Introduction
are known. Homo- and hetero binuclear complexes with PPh2Py
have been reported [12]. However, to the best of our knowledge,
The chemistry of poly-ironhexacarbonyl complexes with various
bridging phosphine ligands has been an intense area of research
since 1980s, as such ligands often undergo P–C bond cleavages to
generate phosphido- or thiophosphinito-bridged complexes, and
thus an extensive range of such compounds have been reported in
literature [1]. During last few years, the iron-carbonyl chemistry
has got a renewed interest, because the X-ray crystal structure of
the [FeFe] hydrogenase revealed that the active site of the enzyme
contains a diiron unit bridged by two sulfur atoms, with CO/CN as
terminal ligands [2], thus producing several studies of models of this
active system [3]. Efforts have been made to introduce different
phosphines in bridging [4] or terminal [5] positions, because such
phosphines increase the electron density at the diiron core which,
in turn, increases the possibility of proton binding capacity at the
metal center. In this context and in view to extent the scope of such
a chemistry, we have reacted triiron-dodecacarbonyl with diaryl-
pyridylphosphine. For many years, the diphenyl-2-pyridylphos-
phine (PPh2Py) has been widely used as a bridging ligand because
of its rigidity, induced by the small bite angle of the ligand in che-
lated mode, favouring the formation of a metal–metal bond [6,7].
Several coordination modes of this ligand, including P-monodentate
[8], P,N-chelate [8b,9], P,N-bridging [10], and N-monodentate [11],
there is no report on diironcarbonyl complexes with PPh2Py in a
bridging position. So far, in one case the ligand was found to occupy
a terminal position in a diironcarbonyl system [13].
Thus, here we report our findings on the reactivity of PPh2Py
with [Fe3CO12] to give a new diironhexacarbonyl complex resulting
from a carbon–phosphorus bond cleavage, along with two known
mononuclear complexes.
2. Results and discussion
Heating a toluene solution of [Fe3(CO)12] and PPh2Py at reflux
resulted in the formation of a new binuclear complex, [Fe2(-
CO)6(
mononuclear derivatives [Fe(CO)4(
[Fe(CO)3(
1-P-PPh2Py)2] (3) [15] (Scheme 1; Chart 1) in 23%, 10%
l-PPh2)(l-j
2-C,N-C5H4N)] (1), together with the known
j
1-P-PPh2Py)] (2) [8a,14] and
j
and 3.5% yields, respectively, after work-up by chromatography
and recrystallizations. The presence of 3% of PPh3 in the commer-
cial diphenyl-2-pyridylphosphine induced the formation of very
small amounts of the known [Fe(CO)4(PPh3)] complex (4) that
was eluted together with 1 with a mixture of hexane–CH2Cl2
(4:1); this monosubstituted complex was separated from 1 by frac-
tional crystallization and characterized by NMR and X-ray diffrac-
tion studies. By monitoring the IR spectra during the reaction, we
observed the progressive disappearance of the
starting ironcarbonyl compound together with the appearance of
new (CO) bands, indicating that the reaction was complete after
m(CO) bands of the
⇑
Corresponding authors.
E-mail addresses: pankajd29@yahoo.com (P. Das), schollha@univ-brest.fr
(P. Schollhammer).
m
0020-1693/$ - see front matter Ó 2011 Elsevier B.V. All rights reserved.
doi:10.1016/j.ica.2011.06.035

642
P. Das et al. / Inorganica Chimica Acta 376 (2011) 641–644
Toluene
1 + 2 + 3
[Fe3(CO)12] + 1.5 eq PPh2Py
Scheme 1. Synthesis of complexes 1–3 by the reaction of [Fe3(CO)12] with PPh2Py.
Ph
Ph
Ph
Py
Ph
P
Py
Ph
P
Ph
OC
P
N
OC
OC
Ph
OC
OC
Fe CO
CO
Fe CO
Fe
Fe
OC
P
CO
CO
CO
Py
OC
Ph
3
2
1
Ph
Ph
P
Fe CO
Ph
OC
OC
CO
4
Chart 1.
Fig. 1. View of the molecule of [Fe2(CO)6(l-PPh2)(l-j
2-C,N-C5H4N)] (1) showing
1 h. Products 1, 2 and 3 were also formed in time-dependent yields,
when the reaction was conducted in refluxing THF instead of
toluene.
30% probability ellipsoids. Selected bond lengths (Å) and angles (°): Fe1–Fe2,
2.6292(4); Fe1–P1, 2.2172(6); Fe2–P1, 2.2068(5); Fe1–N1, 1.9852(17); Fe2–C19,
1.9876(19); C19–N1, 1.347(2); C23–N1, 1.359(3); Fe1–P1–Fe2, 72.99(2); C1–Fe1–
C2, 93.24(10); C1–Fe1–N1, 99.68(8); C2–Fe1–N1, 166.67(9); C1–Fe1–C3,
101.78(10); C5–Fe2–C19, 170.55(10); C19–Fe2–P1, 83.22(5); C5–Fe2–P1,
91.68(7); C5–Fe2–Fe1, 100.01(8); C6–Fe2–C19, 86.86(9); C6–Fe2–P1, 144.70(8).
Compound 1 has been fully characterized from analytical, FAB
mass, and spectroscopic data. The chemical shifts coupled with
an HMBC experiment permitted an unambiguous assignment of
all the hydrogen and carbon atoms in the 1H and 13C NMR spectra
of 1 (see Section 3). The 1H NMR pattern indicates that the pyridyl
ring of 1 lacks any P–H coupling. This strongly suggests that this Py
group is no more attached to phosphorus atom, what implies P–C
(pyridyl) bond cleavage giving rise to the formation of a bridging
PPh2 group. The 31P–{1H} NMR data confirm this hypothesis since
a characteristic signal of a phosphido-bridging group is detected
at 181.51 ppm in the spectra of 1 [16]. Moreover, a resonance char-
acteristic of the Fe-bound 13C atom of a carbene-like species ap-
pears at low-field (d 193.67), indicating that the pyridyl group is
bound directly to an iron atom through one of its carbon atoms.
In order to establish without any ambiguity the molecular struc-
ture of 1, an X-ray analysis of a single crystal of that complex
was undertaken. This structure is shown in Fig. 1, in which the well
known {(CO)3FeFe(CO)3} unit is bridged on the one hand by a phos-
phido group and on the other hand by a pyridyl group through
both nitrogen and carbon atoms [Fe1–N1 = 1.9852(17) Å, and
Fe2–C19 = 1.9876(19) Å]. The iron–carbon length is consistent
with multiple-bond character. Each iron atom adopts a distorted
trigonal bipyramidal configuration. In agreement with the 1H and
13C NMR spectra, the X-ray results indicate the presence of two
inequivalent phenyl groups in 1. Thus, that set of information is
in accord with a metal-promoted cleavage of a phosphorus–carbon
bond upon heating. Cluster-promoted cleavages of P–C bonds in di-
phenyl-2-pyridylphosphine are already known, but they mainly in-
volved P–C(phenyl) bond scissions in reactions of PPh2Py with
[Ru3(CO)12] [12c,17]. In this work, P–C(Py) bond cleavage is selec-
tively observed in reactions involving, for the first time, an iron
cluster. Thus, formation of 1 occurred via PPh2 transfer through a
selective P–C(pyridyl) bond scission, but at this stage of the work
no detailed mechanism can be proposed. What can only be said
is that the monosubstituted compound [Fe(CO)4(PPh2Py)] (2) is
not an intermediate of 1, since no alteration of 2 was observed after
prolonged heating of this complex is toluene.
literature, we therefore add them in Section 3. Moreover, as no
molecular structure of this compound has been reported before,
we have determined the structure of 2 by an X-ray analysis of a
single crystal (Fig. 2). It shows that the iron atom adopts a trigonal
bipyramidal configuration where one and three carbonyl groups
occupy axial and equatorial positions, respectively. The other axial
position is occupied by the PPh2Py, which is coordinated to iron
Fig. 2. View of the molecule of [Fe(CO)4(j
1-P-PPh2Py)] (2) showing 30% proba-
bility ellipsoids. Selected bond lengths (Å) and angles (°): average Fe1–C(O),
1.788(2); Fe1–P1, 2.2216(6); C4–Fe1–P1, 177.54(17); average (O)Cax–Fe1–Ceq(O),
91.48(10); average P1–Fe1–Ceq(O), 88.58(7); C3–Fe1–C2, 115.77(10); C3–Fe1–C1,
119.06(10); C1–Fe1–C2, 124.98(9).
The mononuclear complex 2 was previously synthesised [8a,14]
but its spectroscopic data are different from those reported in the

P. Das et al. / Inorganica Chimica Acta 376 (2011) 641–644
643
through the phosphorus atom. The Fe–Cax bond distance in 2
(1.788(2) Å) is close to that found for analogous complexes, e.g.
[Fe(CO)4PPh3] (1.796(4) Å) [18], indicating that the substitution
of a phenyl by a pyridyl group does not have any influence on
the axial Fe–C length. The average (O)Cax–Fe–Ceq(O) bond angles
of 91.48° and C4–Fe–P1 angle of 177.54(7)° indicates little devia-
tion from the C3v symmetry (Table 1).
Sigma–Aldrich and ACROS Organics, respectively. Solvents were
distilled immediately before use under nitrogen from appropriate
drying agents. Infrared spectra were recorded on a Nicolet-Nexus
FT-IR spectrophotometer in CH2Cl2 solution. Elemental analyses
were performed either on a Perkin–Elmer 2400 elemental analyser
or by the ‘‘Service de Microanalyse’’ ICSN–CNRS at Gif/Yvette
(France). Yields of all products are relative to the starting triiron
dodecacarbonyl complex. The FAB mass spectra were recorded on
a JEOL SX 102/DA-6000 mass spectrometer. The NMR spectra (1H,
31P, 13C) were recorded at room temperature or 303.2 K in CDCl3
solution on either a Bruker AC300 or DRX 500 spectrometers; the
Compound 3 has also been prepared previously by Zhang et al.
[15], but our spectroscopic data are somewhat different from those
reported by these authors; therefore, we have completed the spec-
troscopic analysis and included the results in Section 3. In order to
get a trusty characterization of 3, we decided to undergo an X-ray
analysis of single crystals of this disubstituted compound. Three
sorts of crystals of 3 gave reliable X-ray data, i.e. [Fe(CO)3(PPh2-
Py)2], and two solvated polymorphic derivatives [Fe(CO)3(PPh2
Py)2]Á1/2 CH2Cl2. These results confirm the proposed structure
(Chart 1), which is in agreement with our spectroscopic data and
with the molecular structure reported by Zhang et al. for
[Fe(CO)3(PPh2Py)2]Á1/2 C6H6 [19]. Thus, the molecular structure
of 3 will no more be discussed here, but as their crystal data
slightly differ from those reported by these authors they are given
in the ‘‘Supplementary material’’ for the non-solvated compound.
In summary, both the mediated-metal oxidative cleavage of a
P–C(pyridyl) bond of the PPh2Py ligand, and the subsequent migra-
tion of the PPh2 fragment to give a pyridyl-, diphenylphosphino-
bridged dinuclear complex 1 was obtained for the first time with
a dironhexacarbonyl system.
references were SiMe4 (1H, 13C) and H3PO4
(
31P).
Single-crystal X-ray diffraction data were collected at 170 K on an
X-CALIBUR-2 CCD diffractometer (Oxford diffraction) with graph-
ite-monochromated Mo Ka radiation (k = 0.71073 Å), and by using
an Oxford-Instrument nitrogen device to get low temperature.
3.2. Reaction of [Fe3(CO)12] with PPh2Py
To a toluene (70 mL) solution of [Fe3(CO)12] (500 mg, 0.993
mmol), 395 mg of PPh2Py (1.572 mmol) were added. The reaction
mixture was then refluxed. IR monitoring of the solution indicated
that the reaction was complete after 1 h, after which time the color
of the solution changed from green to light-brown. After evapora-
tion of the toluene, the residue was analyzed by 31P NMR spectros-
copy, which indicated that three complexes (1, 2 and 3) were
mainly obtained in the 1:1.5:0.5 ratio. The crude products were
then dissolved in the minimum of the mixture CH2Cl2/hexane
(1:1), and chromatographed on a silica gel column. Elution with
a mixture of CH2Cl2/hexane (1:4) afforded a canary-yellow solution
of a mixture of 1 (88%) and 4 (12%), which was evaporated under
vacuum. Compound 1 was separated from 4 (small amount of col-
orless crystals) by fractional crystallization in pentane/CH2Cl2
(95:5), and obtained as yellow crystals (184 mg, 23% yield). Further
elution with a mixture of hexane/CH2Cl2 (1:1) gave a light-yellow
band, which after evaporation of the solution afforded a pure light-
yellow powder of 2 (124 mg, 10% yield). Finally, elution with
CH2Cl2/diethylether (95:5) removed a yellow band which gave,
after evaporation of the solvents and recrystallization in hexane/
CH2Cl2, complex 3 as light-yellow crystals (70 mg, 3.5% yield).
When the reaction was conducted in tetrahydrofuran instead of
toluene by refluxing, the same complexes 1, 2, 3, and small amount
of 4 were formed in time-dependent yields, but in all cases 1 was
obtained as the major product.
3. Experimental
3.1. General procedures
The reactions were routinely carried out under a nitrogen atmo-
sphere using standard Schlenk techniques. [Fe3(CO)12] was pre-
pared according to reported procedures [20]. [Fe(CO)5] and
diphenyl-2-pyridylphosphine (PPh2Py) were purchased from
Table 1
Crystal data and structure refinement parameters of the complexes 1 and 2.
1
2
Formula
C
23H14Fe2NO6P
C21H14FeNO4P
431.15
triclinic
Formula weight
Crystal system
Space group
a (Å)
b (Å)
c (Å)
543.02
orthorhombic
P21 21 21
11.3304 (3)
12.4050 (3)
16.3801 (4)°
90
P-1
9.5442 (5)
13.2930 (5)
10.6569 (5)
89.923 (4)
111.236 (5)
95.321 (4)
971.04 (8)
2
1: Anal. Calc. for C23H14Fe2NO6P: C, 50.87; H, 2.60; N, 2.58.
Found: C, 51.13; H, 2.58; N, 2.60%. MS-FAB m/z: 542 [MÀ1]+, 486
[MÀ2COÀ1]+, 431 [MÀ4CO], 374 [MÀ6COÀ1]+. IR (cmÀ1, CH2Cl2):
a
(°)
m(CO) 2060 (s), 2015 (vs), 1992 (s), 1970 (ms), 1952 (m, sh). 1H
b (°)
90
90
NMR(CDCl3): d 7.79, 7.50, 7.33, and 7.01 (m, 10H, Ph), 7.31 (d,
c
(°)
V (Å3)
2302.28 (10)
4
1.567
170 (2)
1.369
JH–H = 8.3 Hz, 1H, C(23)H-Py), 6.93 (d, JH–H = 8.3 Hz, 1H, C(20)H-Py),
6.75 (m, 1H,
{1H}NMR (CDCl3): d 214.07, 213.80, 213.78, 213.72 (s,CO), 213.39
C(21)/(22)H-Py, 6.31 (m, 1H, C
(22)/(21)H-Py). 13C–
Z
Dcalc (Mg/m3)
T (K)
1.475
170 (2)
0.886
2
2
(mmÀ1
)
(d, JP–C = 19.0 Hz, CO), 211.30 (d, JP–C = 16.1 Hz, CO), 193.67 (d,
l
2JP–C = 22.7 Hz, C(19)-Py), 154.01 (s, C(23)-Py), 140.19 (d,
Crystal size (mm)
Crystal color
F(0 0 0)
0.28 Â 0.21 Â 0.05 0.21 Â 0.08 Â 0.04
1JP–C = 30.6 Hz, Cipso-Ph), 138.81 (s, C(21)-Py), 136.85 (d, JP–
1
yellow
1096
light yellow
440
3
C = 26.9 Hz, Cipso-Ph), 133.11 (d, JP–C = 9.4 Hz, Cmeta-Ph), 133.04
Reflections collected
Independent reflections (Rint
hmax
23 325
6917
30.50
99.4%
7550
3948
26.37
99.7%
3
(d, JP–C = 8.9 Hz,C meta-Ph), 132.20 (s, C(20)-Py), 129.82 (s, Cpara-
)
2
Ph), 128.89 (s, Cpara-Ph), 128.46 (d, JP–C = 9.3 Hz, Cortho-Ph),
127.42 (d, JP–C = 9.4 Hz, Cortho-Ph), 119.67 (s,C(22)-Py). 31P–
2
Completeness to hmax
{1H}NMR CDCl3): d 187.51s.
Absorption correction Tmin and Tmax 0.7005 and
0.8358 and
0.9654
253
0.934
0.0336
0.0696
0.9347
2: Anal. Calc. for C21H14FeNO4P: C, 58.50; H, 3.27; N, 3.25. Found:
Parameters refined
298
C, 58.73; H, 3.30; N, 3.27%. IR (CH2Cl2; cmÀ1):
m(CO) 2050 (s), 1975
Goodness-of-fit (GOF) on F2
0.944
0.0308
0.0616
(ms), 1941 (s). MS-FAB m/z: 431 [M]+, 402 [MÀCOÀ1]+, 374
[MÀ2COÀ1]+, 346 [MÀ3COÀ1]+, 318 [MÀ4COÀ1]+. 1H NMR
(CDCl3): d 8.82 (s-br, 1H, Py), 7.73 (s-br, 2H, Py), 7.65 (s-br, 5H, Ph),
7.47 (s-br, 5H, Ph), 7.34 (s-br, 1H, Py). 31P–{1H}(CDCl3): d 74.48 s.
Final R1 [I > 2
Final wR2 [I > 2
Largest difference electron density
(e ÅÀ3
r
(I)]
r(I)]
0.518 and À0.239 0.440 and À0.217
)

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P. Das et al. / Inorganica Chimica Acta 376 (2011) 641–644
[2] (a) J.W. Peters, W.N. Lanzilotta, B.J. Lemon, L.C. Seefeldt, Science 282 (1998)
3: Anal. Calc. for C37H28FeN2O3P2: C, 66.68; H, 4.24, N, 4.20.
1853;
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m(CO) 1889
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2528.
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Acknowledgments
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2029;
This work is funded by the DST, India (Grant No. SR/FTP/CS-119/
2005). SAIF, CDRI (Lucknow) is acknowledged for Mass spectros-
copy. We also thank Mrs. J. L’Helgouarc’h, and Miss L. Beaume,
PhD student (University of Brest) for technical assistance. P.D.
acknowledges the University of Bretagne Occidentale (France) for
a visiting faculty programme and UGC (India) for a travel Grant.
Appendix A. Supplementary material
(b) P. Das, P.P. Sarmah, M. Borah, A.K. Phukan, Inorg. Chim. Acta 362 (2009)
5001;
(c) A.J. Deeming, M.B. Smith, J. Chem. Soc., Dalton Trans. (1993) 2041 (and
3383).
CCDC 825963, 825964, and 825965 contain the supplementary
crystallographic data for complexes 1, 2, and 3, respectively. These
data can be obtained free of charge from The Cambridge Crystallo-
graphic Data Centre via www.ccdc.cam.ac.uk/data_request/cif.
Supplementary data associated with this article can be found, in
the online version, at doi:10.1016/j.ica.2011.06.035.
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