Ureato(1-) complexes of palladium(II) and platinum(II): Crystal structure of [NBu4][(C6F5)2Pt{PhNC(O)NPr 2i}]

Article abstract of DOI:10.1016/S0020-1693(03)00200-7

The reaction of [NBu₄]₂[{M(C₆F₅)₂ (μ-OH)}₂] (M=Pd, Pt) with amines R₂NH in the presence of the heterocumulene phenylisocyanate, PhNCO, leads to the synthesis of the ureato(1-) complexes [NBu₄][M(C₆F₅)₂{PhNC(O)NR ₂}] (M=Pd, Pt). The single-crystal structure of [NBu₄][(C₆F₅)₂Pt{PhNC(O)NPr ₂ⁱ}] revealed the presence of a N,N′-chelating ureato(1-) with a N(1)-Pt-N(2) bite angle of 64.0(3)°.

Full text of DOI:10.1016/S0020-1693(03)00200-7

Inorganica Chimica Acta 351 (2003) 114ꢂ118
/
www.elsevier.com/locate/ica
Ureato(1ꢀ
/
) complexes of palladium(II) and platinum(II)
Crystal structure of [NBu4][(C6F5)2Pt{PhNC(O)NPri2}]
Jose´ Ruiz a,*, Venancio Rodr´ıguez a, Consuelo Vicente a, Jose´ Pe´rez b, Gregorio Lo´pez a,
Penny A. Chaloner c, Peter B. Hitchcock c
a Departamento de Qu´ımica Inorga´nica, Universidad de Murcia, 30071 Murcia, Spain
´
Departamento de Ingenier´ıa Minera, Geolo´gica y Cartogra´fica, Area de Qu´ımica Inorga´nica, Universidad Polite´cnica de Cartagena, 30203 Cartagena,
b
Spain
c School of Chemistry, Physics and Environmental Sciences, University of Sussex, Brighton BN1 9QJ, UK
Received 23 October 2002; accepted 17 February 2003
Abstract
The reaction of [NBu4]2[{M(C6F5)2(m-OH)}2] (Mꢁ
phenylisocyanate, PhNCO, leads to the synthesis of the ureato(1ꢀ
The single-crystal structure of [NBu4][(C6F5)2Pt{PhNC(O)NPri2}] revealed the presence of a N,N?-chelating ureato(1ꢀ
N(2) bite angle of 64.0(3)8.
/
Pd, Pt) with amines R2NH in the presence of the heterocumulene
) complexes [NBu4][M(C6F5)2{PhNC(O)NR2}] (MꢁPd, Pt).
) with a
/
/
/
N(1)Ã
/
PtÃ
/
# 2003 Elsevier B.V. All rights reserved.
Keywords: Palladium complexes; Platinum complexes; Ureato complexes; Phenylisocyanate; Crystal structures
1. Introduction
heterocumulene phenylisocyanate, PhCNO, to form the
ureato(1ꢀ
complexes [M(C6F5)2{PhNC(O)NR2}]ꢀ
(MꢁPd, Pt), including the first crystal structure of a
mononuclear chelate ureato(1ꢀ) platinum complex.
Urea is a final product of the nitrogen cycle in the
human body and many bio-chemically important sub-
stances have an N(CO)N skeleton, such as uracil,
cytosine and thymine. Urea and its alkyl or aryl
derivatives act as weak N- or O-donor [9,10], and so
/)
Dimeric hydroxo complexes M(m-OH)2M of palladiu-
m(II) and platinum(II) [1] have shown to be excellent
precursors in organic and organometallic synthesis of
/
/
new compounds [2]. The acidꢂbase reaction of these
/
hydroxo complexes with a protic electrophile (HL) leads
to the formation of mono- or binuclear complexes
depending on the nature of the deprotonated (L)ꢀ
ligand [3ꢂ
[M2(C6F5)4(m-OH)2]2ꢀ with amines in the presence of
CS2, CÃN bonds are formed to give the corresponding
dithiocarbamate complexes [M(C6F5)2(S2CNR2)]ꢀ
(MꢁPd, Pt) [8].
Following our systematic study of the reactivity of
hydroxo complexes of Pd and Pt, we have now
investigated the chemical behavior of [M2(C6F5)4(m-
OH)2]2ꢀ with amines R2NH in the presence of the
/
7]. Furthermore, in the reaction of
far the ureato(1ꢀ
monodentate terminal group [11ꢂ
monodentate bridging group between two metal centres
[14], an N,O-chelating ligand (generating highly
strained, four-membered rings) [15], an N,O-bridging
ligand between two metal centres [16] or an N,N?,O-
/
) anion functions as an N-bonded
/13], an N-bonded
/
/
bonded ureato(1ꢀ
To the best of our knowledge, no crystal structure of any
N,N?-chelated ureato(1ꢀ) complex of any transition
metal is available so far. Mononuclear ureato(2ꢀ
/
) anion bridging three metal ions [17].
/
/)
palladium [18] and platinum(II) complexes [19], and a
number of tri- and tetranuclear palladium complexes
containing urea dianions have also been reported [14].
* Corresponding author. Tel.: ꢃ
148.
E-mail address: jruiz@um.es (J. Ruiz).
/
34-968-367 455; fax: ꢃ34-968-364
/
0020-1693/03/$ - see front matter # 2003 Elsevier B.V. All rights reserved.
doi:10.1016/S0020-1693(03)00200-7

J. Ruiz et al. / Inorganica Chimica Acta 351 (2003) 114ꢂ
/118
115
2. Experimental
2.2.2. [NBu4][Pd(C6F5)2{PhNC(O)NEt2}] (2)
Yield: 65 mg, 76%. Anal. Found: C, 53.3; H, 5.7; N,
5.0. Calcd. for C39H51F10N3OPd: C, 53.6; H, 5.9; N,
2.1. Materials and physical measurements
4.8%. M.p.: 223 dec. LMꢁ
cmꢀ1): 1680 n(CÄ
((CD3)2CO): d 7.18 (d, 2Ho, Jom
2Hm, Jom Jmp 7.4 Hz), 6.68 (t, 1Hp, Jmp
2.87 (m, 2H, NCH2), 2.44 (m, 2H, NCH2), 1.64 (t, 6H,
N(CH2CH3)2, JHH
7.1 Hz). 19F NMR ((CD3)2CO): d
113.6 (d, 2Fo, Jom 29.3 Hz), ꢀ113.9 (d, 2Fo, Jom
28.8 Hz), ꢀ164.9 (t, 1Fp, Jpm 18.6 Hz), ꢀ165.2 (t,
166.2 (m, 4Fm). Mass spectrum
/
125 S cm2 molꢀ1. IR (Nujol,
1
/
O), 790, 780 (PdÃ
/
C6F5). H NMR
C, H, and N analyses were performed with a Carlo
Erba model EA 1108 microanalyzer. Decomposition
temperatures were determined with a Mettler TG-50
thermobalance at a heating rate of 5 8C minꢀ1 and the
solid samples under nitrogen flow (100 mL minꢀ1).
Molar conductivities were measured in acetone solution
ꢁ
/
7.4 Hz), 6.91 (dd,
ꢁ
/
ꢁ
/
ꢁ
/
7.4 Hz),
ꢁ
/
ꢀ
/
ꢁ
/
/
ꢁ
/
/
ꢁ
/
/
(c :
/
5ꢄ
/
10ꢂ4 mol Lꢀ1) with a Crison 525 conducti-
1Fp, Jpm
ꢁ
/
19.8 Hz), ꢀ
/
meter. The NMR spectra were recorded on a Bruker AC
200E or Varian Unity 300 spectrometer, using SiMe4
and CFCl3 as the standard, respectively. In the 1H NMR
spectra of the ionic compounds, the signal of the NBu4ꢃ
cation have been omitted. IR spectra were recorded on a
(FAB)ꢀ: m/z 440 (Pd(C6F5)2).
2.2.3. [NBu4][Pd(C6F5)2{PhNC(O)NPri2}] (3)
Yield: 67 mg, 75%. Anal. Found: C, 54.3; H, 6.2; N,
4.6. Calcd. for C41H55F10N3OPd: C, 54.6; H, 6.1; N,
PerkinꢂElmer 1430 spectrophotometer using Nujol
/
4.7%. M.p.: 237 dec. LMꢁ
cmꢀ1): 1680 n(CÄ
((CD3)2CO): d 7.10 (d, 2Ho, Jom
2Hm, Jom Jmp 7.4 Hz), 6.65 (t, 1Hp, Jmp
3.34 (m, 2H, NCH), 1.52 (d, 6H, NCH(CH3)2, JHH
6.3 Hz), 1.34 (d, 6H, NCH(CH3)2, JHH
7.4 Hz). 19F
NMR ((CD3)2CO): d ꢀ113.7 (d, 2Fo, Jom 31.3 Hz),
114.2 (d, 2Fo, Jom 30.5 Hz), ꢀ165.4 (t, 1Fp, Jpm
166.7 (m,
/
112 S cm2 molꢀ1. IR (Nujol,
mulls between polyethylene sheets. Mass spectra were
recorded on a Fisons V.G. Autospec spectrometer using
the standard Csꢃ ion FAB (acceleration voltage 25 kV)
and nitrobenzyl alcohol as matrix.
1
/
O), 790, 780 (PdÃ
/
C6F5). H NMR
ꢁ
/
7.4 Hz), 6.88 (dd,
ꢁ
/
ꢁ
/
ꢁ
/
7.4 Hz),
ꢁ
/
The starting complexes [NBu4]2[{M(C6F5)2(m-OH)}2]
ꢁ
/
(MꢁPd [1a], Pt [1b]) were prepared by procedures
/
/
ꢁ
/
described elsewhere. The commercially available chemi-
cals were purchased from Aldrich Chemical Co. and
were used without further purification. Solvents were
dried by the usual methods.
ꢀ
/
ꢁ
/
/
ꢁ
/
19.8 Hz), ꢀ
/
165.7 (t, 1Fp, Jpm
ꢁ
/
19.8 Hz), ꢀ
/
4Fm). Mass spectrum (FAB)ꢀ: m/z 659 (M)
2.3. Preparation of
Et (4), Pri
2.2. Preparation of
[NBu4][Pt(C6F5)2{PhNC(O)NR2}] [Rꢁ
(5)]
/
[NBu4][Pd(C6F5)2{PhNC(O)NR2}] [Rꢁ
/
Me (1), Et
(2), Pri (3)]
To a solution of [NBu4]2[{Pt(C6F5)2(m-OH)}2] (100
mg, 0.063 mmol) in toluene (8 mL) was added the
corresponding amine (0.252 mmol) and PhNCO (27.3
mL, 0.252 mmol). The solution was boiled under reflux
for 7 h. The solvent was completely evaporated under
reduced pressure and the residue was treated with Et2O,
then the solid formed was collected by filtration and air-
dried.
To a solution of [NBu4]2[{Pd(C6F5)2(m-OH)}2] (100
mg, 0.071 mmol) in THF (6 mL) was added the
corresponding amine (0.142 mmol) and PhNCO (15.4
mL, 0.142 mmol). The mixture was stirred at room
temperature (r.t.) for 2 h. The solvent was completely
evaporated under reduced pressure and the residue was
treated with Et2O/hexane, then the solid formed was
collected by filtration and air-dried.
2.3.1. [NBu4][Pt(C6F5)2{PhNC(O)NEt2}] (4)
Yield: 68 mg, 79%. Anal. Found: C, 48.6; H, 5.3; N,
4.3. Calcd. for C39H51F10N3OPt: C, 48.7; H, 5.3; N,
2.2.1. [NBu4][Pd(C6F5)2{PhNC(O)NMe2}] (1)
Yield: 60 mg, 74%. Anal. Found: C, 52.3; H, 5.4; N,
5.1. Calcd. for C37H47F10N3OPd: C, 52.5; H, 5.6; N,
4.4%. M.p.: 217 dec. LMꢁ
cmꢀ1): 1690 n(CÄ
O), 805, 790 (PtÃ
((CD3)2CO): d 7.22 (d, 2Ho, Jom 7.6 Hz), 6.93 (dd,
2Hm, Jom Jmp 7.6 Hz), 6.72 (t, 1Hp, Jmp 7.2 Hz),
3.10 (m, 2H, NCH2), 2.62 (m, 2H, NCH2), 1.58 (t, 6H,
N(CH2CH3)2, JHH
7.1 Hz). 19F NMR ((CD3)2CO): d
117.6 (d, 2Fo, Jom 27.7 Hz, JPtFo 536.2 Hz), ꢀ118.1
(d, 2Fo, Jom 27.7 Hz, JPtFo 468.5 Hz), ꢀ167.5 (t, 1Fp,
Jpm 19.8 Hz), ꢀ166.2 (m, 1Fpꢃ4Fm). Mass spectrum
(FAB)ꢀ: m/z 529 (Pt(C6F5)2).
/
109 S cm2 molꢀ1. IR (Nujol,
C6F5). 1H NMR
5.0%. M.p.: 211 dec. LMꢁ
cmꢀ1): 1685 n(CÄ
((CD3)2CO): d 7.18 (d, 2Ho, Jom
2Hm, Jom Jmp 7.4 Hz), 6.69 (t, 1Hp, Jmp
2.58 (s, 6H, N(CH3)2). 19F NMR ((CD3)2CO): d ꢀ
(d, 2Fo, Jom 27.7 Hz), ꢀ114.9 (d, 2Fo, Jom 28.8 Hz),
164.6 (t, 1Fp, Jpm 19.2 Hz), ꢀ165.0 (t, 1Fp, Jpm
19.5 Hz), ꢀ
166.1 (m, 4Fm). Mass spectrum (FAB)ꢀ: m/
z 440 (Pd(C6F5)2).
/
112 S cm2 molꢀ1. IR (Nujol,
/
/
1
/
O), 790, 780 (PdÃ
/
C6F5). H NMR
ꢁ
/
ꢁ
/
7.4 Hz), 6.92 (dd,
7.4 Hz),
113.0
ꢁ
/
ꢁ
/
ꢁ
/
ꢁ
/
ꢁ
/
ꢁ
/
/
ꢁ
/
ꢁ
/
/
ꢁ
/
ꢀ
/
ꢁ
/
/
ꢀ
/
ꢁ
/
/
ꢁ
/
ꢁ
/
/
/
ꢁ
/
/
/

116
J. Ruiz et al. / Inorganica Chimica Acta 351 (2003) 114ꢂ118
/
2.3.2. [NBu4][Pt(C6F5)2{PhNC(O)NPri2}] (5)
Yield: 79 mg, 86%. Anal. Found: C, 49.5; H, 5.5; N,
4.1. Calcd. for C41H55F10N3OPt: C, 49.7; H, 5.6; N,
3. Results and discussion
The reaction of [NBu4]2[{M(C6F5)2(m-OH)}2] (Mꢁ
Pd, Pt) with amines R2NH in the presence of PhNCO
leads to the synthesis of the ureato(1ꢀ) complexes
[NBu4][M(C6F5)2{PhNC(O)NR2}] 1ꢂ5 (MꢁPd, Pt)
shown in Scheme 1. The complexes are air-stable, both
in the solid state and in solution. The new complexes
have been characterized by partial elemental analyses
and spectroscopic (IR and H and 19F NMR) methods.
/
4.2%. M.p.: 229 dec. LMꢁ
cmꢀ1): 1690 n(CÄ
((CD3)2CO): d 7.16 (d, 2Ho, Jom
2Hm, Jom Jmp 8.1 Hz), 6.69 (t, 1Hp, Jmp
3.54 (m, 2H, NCH), 1.52 (d, 6H, NCH(CH3)2, JHH
6.4 Hz), 1.39 (d, 6H, NCH(CH3)2, JHH
6.3 Hz). 19F
NMR ((CD3)2CO): d ꢀ117.6 (d, 2Fo, Jom 29.1 Hz,
JPtFo 554.3 Hz), ꢀ118.0 (d, 2Fo, Jom 29.1 Hz, JPtFo
516.4 Hz), ꢀ167.6 (t, 1Fp, Jpm 19.8 Hz), ꢀ168.0 (m,
1Fpꢃ
4Fm). Mass spectrum (FAB)ꢀ: m/z 748 (M).
/
121 S cm2 molꢀ1. IR (Nujol,
1
/
/
O), 805, 795 (PdÃ
/
C6F5). H NMR
/
/
ꢁ
/
8.1 Hz), 6.91 (dd,
ꢁ
/
ꢁ
/
ꢁ/8.1 Hz),
ꢁ
/
ꢁ
/
1
/
ꢁ
/
In acetone solution, these complexes behave as 1:1
electrolytes [22]. The presence of the ureato ligand is
supported by the IR spectra, which show a band at
approximately 1680 cmꢀ1 assignable to n(CÄ
The IR spectra of complexes 1ꢂ5 show also the
/
ꢁ
/
/
ꢁ
/
/
/
/
O) [11].
/
characteristic absorptions of the C6F5 group [23] at
1630, 1490, 1450, 1050, 950 cmꢀ1 and a split band at
approximately 800 cmꢀ1, derived from the so-called X-
sensitive mode in C6F5 halogen molecules, which is
characteristic of the cis-M(C6F5)2 fragment [24,25] and
2.4. Crystal structure determination of
[NBu4][Pt(C6F5)2{PhNC(O)NPri2}] (5)
Suitable crystals for the X-ray diffraction study of
compound 5 were grown from a dry CH2Cl2/hexane
solution. X-ray diffraction experiment was carried out
on an Enraf Nonius CAD4 diffractometer at r.t. The
crystallographic data are shown in Table 1. Data were
behaves like a v(MÃ
/
C) band [26]. Mass spectra (FABꢀ)
of complexes 3 and 5 clearly support the proposed
formulae showing the peaks corresponding to
[M(C6F5)2{PhNC(O)NR2}]ꢀ, with coincident experi-
mental and calculated isotopic distributions.
collected using a single crystal of dimensions 0.5ꢄ
0.3 mm. Accurate cell parameters were determined by
least-squares fitting of 25 reflections. The range of hkl
/
0.5ꢄ
/
The reaction of [NBu4]2[{M(C6F5)2(m-OH)}2] (Mꢁ
/
Pd, Pt) with amines R2NH should give the amide
was 05
/
h 5
/
11, 05
/
k 5
/
25, ꢀ
/
125
/
l512, corresponding
/
complex [NBu4]2[{M(C6F5)2(m-NR2)}2] followed by in-
to 2umax
methods [20] and refined anisotropically on F2 [21].
Hydrogen atoms were introduced in calculated posi-
ꢁ508. The structure was solved by direct
/
sertion of PhNCO into the MÃ
of the related arylamide
[NBu4]2[{M(C6F5)2(m-NHAr)}2] (Mꢁ
/
NR2 bond. The synthesis
complexes
/Pd, Pt) and their
tions. The final R factor was 0.031, RWꢁ
/
0.069 over
reactions with CS2 to yield the corresponding dithio-
carbamate complexes [M(C6F5)2(S2CNR2)]ꢀ have been
previously reported [5]. External attack by NR2ꢀ of the
coordinated heterocumulene is an alternative pathway
3472 observed reflections [I ꢀ2s(I)].
/
to the formation of 1ꢂ
It has also been reported the insertion of PhNCO into
the PtÃNHPh bond of trans-[PtH(NHPh)(PEt3)2] to
give the monodentate N,N?-diphenylureato(1ꢀ)-N
complex trans-[PtH{PhNC(O)NHPh}(PEt3)2] [11] and
/
5.
Table 1
Crystal data and summary of data collection and refinement for
/
[NBu4][Pt(C6F5)2{PhNC(O)NPri2}] (5)
/
Empirical formula
Formula weight
Crystal system
C41H55F10N3OPt
990.97
the insertion of ButNCO into MoÃ
/
N amido bonds to
yield the molibdenum complex [Mo{ButNC(O)NH-
monoclinic
P2(1)
Space group
Unit cell dimensions
But}2(NBut)2] [15], which has two chelating (N,O)
ureato(1ꢀ
complex 5 (vide infra) has revealed the presence of an
N,N?-chelating ureato(1ꢀ) ligand.
The 19F NMR spectra of complexes 1ꢂ
/) ligands. The X-ray diffraction study of
˚
a (A)
9.854(4)
21.094(6)
10.596(6)
97.14(4)
2185(2)
2
˚
b (A)
˚
c (A)
/
b (8)
/
5 are consis-
3
˚
V (A )
tent with this structure, showing the presence of two
nonequivalent freely rotating C6F5 groups, one trans to
NR2 and one trans to NPh, with two 2:2 resonances in
the o- and m-fluorine region, and two 1:1 resonances in
the p-fluorine region. As expected, the ortho-F signals of
complexes 4 and 5 are flanked by the satellites due to the
coupling to 195Pt.
Z
Dcalc (Mg mꢀ3
F (mmꢀ1
)
1.51
3.29
)
˚
l (A)
0.71073
3472
Observed reflections
Final R1, wR2 indices (all data)
Goodness-of-fit
0.041, 0.079
1.096

J. Ruiz et al. / Inorganica Chimica Acta 351 (2003) 114ꢂ
/118
117
Scheme 1.
3.1. X-ray structure of
[NBu4][Pt(C6F5)2{PhNC(O)NPri2}] (5)
Table 2
˚
Selected bond lengths [A] and angles [8] for complex 5
Bond lengths
Fig. 1 shows the X-ray structure of complex 5, with
selected bond lengths and angles listed in Table 2. The
metal is coordinated in a distorted square-planar
PtÃ
PtÃ
PtÃ
PtÃ
/
C(1)
C(7)
N(1)
N(2)
1.986(9)
2.020(9)
2.063(7)
2.158(8)
1.313(11)
1.505(11)
1.212(10)
/
/
arrangement. The main distortion is the N(1)Ã
/
PtÃ/N(2)
/
N(1)Ã
N(2)Ã
OÃ
/C(19)
bite angle, which is 64.0(3)8. This is due to the
geometrical constraint set by the ligand. The angle
between the two C6F5 rings is 87.8(4)8. The four-
/C(19)
/C(19)
Bond angles
membered metallacycle N(2)Ã
/
PtÃ
/
N(1)Ã
/
C(19) is essen-
tially planar (with no atom deviating from the least-
C(1)Ã
C(1)Ã
C(7)Ã
C(1)Ã
C(7)Ã
N(1)Ã
OÃC(19)Ã
OÃC(19)Ã
N(1)Ã
/
PtÃ
PtÃ
PtÃ
PtÃ
PtÃ
PtÃ
/
C(7)
N(1)
N(1)
N(2)
N(2)
87.8(4)
103.4(3)
168.6(3)
167.3(3)
104.9(3)
64.0(3)
/
/
˚
square plane by more than 0.030(6) A, for C(19)). The
/
/
˚
N(1) bond length (2.063(7) A) is shorter than the
/
/
PtÃ
/
/
/
˚
N(2) bond length (2.158(8) A). These values are
similar to those reported in complexes containing the
PtÃ
/
/
/
N(2)
/
/N(1)
134.1(9)
120.9(8)
104.9(7)
{Pt(C6F5)2N2} moiety such as [Pt(C6F5)2(pzÁ Á ÁHÁ Á Ápz)]
/
/N(2)
˚
(pzꢁ
(chxnꢁ
[27], [Pt(C6F5)2(tmeda)] (tmedaꢁ
/
pyrazolate) (2.091(5) A) [24], [Pt(C6F5)2(cis-chxn)]
/
C(19)ÃN(2)
/
˚
/
cyclohexane-1,2-diamine) (2.125(5), 2.106(5) A)
/
N,N,N?,N?-tetra-
˚
platinum
(phenꢁ1,10-phenantroline)
[Pt{PhNC(O)NAd}(COD)]
CODꢁ1,5-cyclo-octadiene) (1.24(5) A) [29] and [Pd2(a-
cac)2(m4-NHCONH)]2×
C6F5 distances (1.986(9) and 2.020(9) A) are
complexes
[Pd{PhNC(O)NPh}(phen)]
methylethane-1,2-diamine) (2.141(5) A) [28] and those
observed in the ureato(2ꢀ platinum complex
[Pt{PhNC(O)NAd}(COD)] (Adꢁ1-adamantyl,
CODꢁ1,5-cyclo-octadiene) (2.048(8), 2.021(8) A) [29].
The C(19)Ã
than that found in the ureato(2ꢀ
˚
A)
/
(1.238(5)
(Adꢁ
[30],
/
)
/
1-adamantyl,
/
˚
˚
/
/
˚
Et2O (1.24(3) A) [31].
˚
/
/O bond length (1.212(10) A) is shorter
˚
The PtÃ
/
/) palladium or
in the range found in the literature [1b,7].
4. Supplementary material
Crystallographic data for the structural analysis have
been deposited with the Cambridge Crystallographic
Data Centre, CCDC No. 195158 for compound 5.
Copies of this information may be obtained free of
charge from The Director, CCDC, 12 Union Road,
Cambridge, CB2 1EZ, UK (fax: ꢃ44-1223-336-033; e-
/
mail: deposit@ccdc.cam.ac.uk or www: http://
www.ccdc.cam.ac.uk).
Acknowledgements
This work was supported by the Direccio´n General de
Investigacio´n del Ministerio de Ciencia y Tecnolog´ıa
Fig. 1. An ORTEP drawing of the [(C6F5)2Pt{PhNC(O)NPri2}]ꢀ anion.

118
J. Ruiz et al. / Inorganica Chimica Acta 351 (2003) 114ꢂ118
/
[13] J.M. Boncella, L.A. Villanueva, J. Organomet. Chem. 465 (1994)
297.
(Project No. BQU2001-0979-C02-01), Spain, and the
Fundacio´n Se´neca de la Comunidad Auto´noma de la
Regio´n de Murcia (Project No. PI-72-00773-FS-01).
[14] S. Okeya, S. Koshino, M. Namie, I. Nagasawa, Y. Kushi, J.
Chem. Soc., Chem. Commun. (1995) 2123.
[15] H.-w. Lam, G. Wilkinson, B. Hussain-Bates, M.B. Hursthouse, J.
Chem. Soc., Dalton Trans. (1993) 781.
[16] F. Meyer, H. Pritzkow, J. Chem. Soc., Chem. Commun. (1998)
1555.
References
[17] F. Meyer, M. Konrad, E. Kaifer, Eur. J. Inorg. Chem. (1999)
1851.
[1] (a) G. Lo´pez, J. Ruiz, G. Garc´ıa, C. Vicente, J. Casabo´, E.
Molins, C. Miravitlles, Inorg. Chem. 30 (1991) 2605;
(b) G. Lo´pez, J. Ruiz, G. Garc´ıa, C. Vicente, J.M. Mart´ı, J.A.
Hermoso, A. Vegas, M. Mart´ınez-Ripoll, J. Chem. Soc., Dalton
Trans. (1992) 53.
[18] F. Paul, J. Fischer, P. Oschenbein, J.A. Osborn, Angew. Chem.,
Int. Ed. Engl. 32 (1993) 1638.
[19] M.B. Dinger, W. Henderson, B.K. Nicholson, A.L. Wilkins, J.
Organomet. Chem. 526 (1996) 303.
[20] G.M. Sheldrick, SHELXS-86. Program for the Solution of Crystal
[2] (a) J. Ruiz, V. Rodr´ıguez, G. Lo´pez, P.A. Chaloner, P.B.
Hitchcock, J. Organomet. Chem. 493 (1995) 77;
Structures, Univ. of Gottingen, Gottingen, Germany, 1985.
¨ ¨
[21] G.M. Sheldrick, SHELXL-93. Program for Crystal Structure
Refinement, Univ. of Gottingen, Gottingen, Germany, 1993.
(b) J. Ruiz, V. Rodr´ıguez, G. Lo´pez, P.A. Chaloner, P.B.
Hitchcock, J. Organomet. Chem. 523 (1996) 23.
¨
¨
[3] J. Ruiz, V. Rodr´ıguez, G. Lo´pez, P.A. Chaloner, P.B. Hitchcock,
Organometallics 15 (1996) 1662.
[22] W.J. Geary, Coord. Chem. Rev. 7 (1971) 81.
[23] D.A. Long, D. Steel, Spectrochim. Acta 19 (1963) 1955.
[24] G. Lo´pez, J. Ruiz, C. Vicente, J.M. Mart´ı, G. Garc´ıa, P.A.
Chaloner, P.B. Hitchcock, R.M. Harrison, Organometallics 11
(1992) 4090.
[4] J. Ruiz, M.T. Mart´ınez, C. Vicente, G. Garc´ıa, G. Lo´pez, P.A.
Chaloner, P.B. Hitchcock, Organometallics 12 (1993) 4321.
[5] J. Ruiz, V. Rodr´ıguez, G. Lo´pez, J. Casabo´, E. Molins, C.
Miravitlles, Organometallics 18 (1999) 1177.
[25] E. Alonso, J. Fornie´s, C. Fortuno, M. Toma´s, J. Chem. Soc.,
˜
Dalton Trans. (1995) 3777.
[6] J. Ruiz, V. Rodr´ıguez, N. Cutillas, M. Pardo, J. Pe´rez, G. Lo´pez,
P.A. Chaloner, P.B. Hitchcock, Organometallics 20 (2001) 1973.
[7] J. Ruiz, V. Rodr´ıguez, C. Vicente, J.M. Mart´ı, G. Lo´pez, J. Pe´rez,
Inorg. Chem. 40 (2001) 5354.
[26] E. Maslowski, Vibrational Spectra of Organometallic Com-
pounds, Wiley, New York, 1977, p. 437.
[27] C. Cullinane, G.B. Deacon, P.R. Drago, T.W. Hambley, K.T.
Nelson, L.K. Webster, J. Inorg. Biochem. 89 (2002) 293.
[28] G.B. Deacon, K.T. Nelson, E.R.T. Tiekink, Acta Crystallogr.
C47 (1991) 1819.
[8] G. Lo´pez, J. Ruiz, G. Garc´ıa, C. Vicente, J.M. Mart´ı, V.
Rodr´ıguez, J. Organomet. Chem. 436 (1992) 121.
[9] B.F. Hoskins, C.J. McKenzie, I.A.S. MacDonald, R. Robson, J.
Chem. Soc., Dalton Trans. (1993) 781.
[29] M.B. Dinger, W. Henderson, B.K. Nicholson, A.L. Wilkins, J.
Organomet. Chem. 526 (1996) 303.
[10] M. Konrad, F. Meyer, A. Jacobi, P. Kircher, P. Rutsch, L.
Zsolnai, Inorg. Chem. 38 (1999) 4459.
[30] F. Paul, J. Fischer, P. Ochsenbein, J.A. Osborn, Angew. Chem.,
Int. Ed. Engl. 32 (1993) 1638.
[11] R.L. Cowan, W.C. Trogler, J. Am. Chem. Soc. 111 (1989) 4750.
[12] A.L. Seligson, R.L. Cowan, W.C. Trogler, Inorg. Chem. 30 (1991)
3371.
[31] S. Okeya, S. Koshino, M. Namie, I. Nagasawa, Y. Kushi, J.
Chem. Soc., Chem. Commun. (1995) 2123.