Ni(II)-piperidinedithiocarbamate complexes with bidentate phosphorus-donor ligands

Article abstract of DOI:10.1016/S0277-5387(00)00449-6

Nickel(II) piperidinedithiocarbamate complexes of the composition [Ni(pipdtc)(P-P)]X and [Ni₂(pipdtc)₂(NCS)₂(dpph)] (X = NCS, ClO₄, I; P-P = 1,2-bis(diphenylphosphino)ethane (dppe), 1,4-bis(diphenylphosphino)butane (dppb), 1,6-bis(diphenylphosphino)hexane (dpph), 1,4-bis(diphenylphosphino)ferrocene (dppf); pip=C₅H₁₀; dtc=S₂CN^-) have been synthesized. The compounds have been characterized by elemental analyses, IR, electron and ¹H, ¹³C{¹H} and ³¹P{¹H} NMR spectroscopies, thermal analysis, magneto-chemical and conductivity measurements. A single-crystal X-ray analysis of the [Ni(pipdtc)(dppf)]ClO₄ complex proved four-coordinated nickel in a deformed square-planar arrangement with a S₂P₂ donor set. (C) 2000 Elsevier Science Ltd.

Full text of DOI:10.1016/S0277-5387(00)00449-6

www.elsevier.nl/locate/poly
Polyhedron 19 (2000) 1713–1717
Ni(II)-piperidinedithiocarbamate complexes with bidentate
phosphorus-donor ligands
Richard Pastorek a, Zdeneˇk Tra´vn´ıcˇek a,*, Jarom´ır Marek b, Dalibor Dastych b,
a
&
Zdeneˇk Sindela´rˇ
a Department of Inorganic and Physical Chemistry, Palacky´ Uni6ersity, Krˇ´ızˇko6ske´ho 10, 771 47 Olomouc, Czech Republic
b Department of Inorganic Chemistry, Masaryk Uni6ersity, Kotla´rˇska´ 2, 611 37 Brno, Czech Republic
Received 10 January 2000; accepted 7 June 2000
Abstract
Nickel(II) piperidinedithiocarbamate complexes of the composition [Ni(pipdtc)(P-P)]X and [Ni2(pipdtc)2(NCS)2(dpph)] (X=
NCS, ClO4, I; P-P=1,2-bis(diphenylphosphino)ethane (dppe), 1,4-bis(diphenylphosphino)butane (dppb), 1,6-bis(diphenylphos-
phino)hexane (dpph), 1,4-bis(diphenylphosphino)ferrocene (dppf); pip=C5H10; dtc=S2CN−) have been synthesized. The
compounds have been characterized by elemental analyses, IR, electron and 1H, 13C{1H} and 31P{1H} NMR spectroscopies,
thermal analysis, magneto-chemical and conductivity measurements. A single-crystal X-ray analysis of the [Ni(pipdtc)(dppf)]ClO4
complex proved four-coordinated nickel in a deformed square-planar arrangement with a S2P2 donor set. © 2000 Elsevier Science
Ltd. All rights reserved.
Keywords: Nickel(II) piperidinedithiocarbamate complexes; Synthesis; X-ray structure
carbamates with bidentate phosphorus donor ligands in
the coordination sphere. The aim of the present work
1. Introduction
was to study the influence of ligands used on structure
To date, no nickel(II) piperidinedithiocarbamate
and physico-chemical properties of the synthesized
complexes with bidentate P-P donor ligands in the
complexes.
coordination sphere have been prepared. Only diamag-
netic complexes with triphenylphosphine (PPh3) as a
monodentate phosphorus donor ligand of composition
[Ni(pipdtc)(PPh3)2]ClO4 [1] and [NiX(pipdtc)(PPh3)]
2. Experimental
(X=Cl, Br, I, NCS) [1–3] have been synthesized. In
both above complexes it was found that the central
2.1. Materials
nickel atom is four-coordinated in a distorted square-
planar arrangement of donor atoms with a NiS2P2, and
NiS2PX chromophore, respectively. This fact was
proved by single-crystal X-ray analysis of the [Ni(p-
ipdtc)(PPh3)2]ClO4·PPh3·H2O complex [4] in the case of
the NiS2P2 chromophore.
Nitromethane, acetone, 1,2-bis(diphenylphosphino)-
ethane (dppe), 1,4-bis(diphenylphosphino)butane
(dppb), 1,6-bis(diphenylphosphino)hexane (dpph) and
1,4-bis(diphenylphosphino)ferrocene (dppf) were sup-
plied by Fluka Co. All other reagents were obtained
from Lachema Co. and were of p.a. purity.
In the framework of systematic study of dithiocarba-
mates at our department we focused attention to prepa-
ration and study of nickel(II) piperidinedithio-
2.2. Syntheses
Caution! Perchlorate salts of metal complexes with
organic ligands are potentially explosive. Only a small
amount of the material should be prepared and it
should be handled with care.
* Corresponding author. Tel.: +420-68-563-4361; fax: +420-68-
522-5737.
E-mail address: trav@risc.upol.cz (Z. Tra´vn´ıcˇek).
0277-5387/00/$ - see front matter © 2000 Elsevier Science Ltd. All rights reserved.
PII: S0277-5387(00)00449-6

1714
R. Pastorek et al. / Polyhedron 19 (2000) 1713–1717
1
2.2.1. Preparation of [Ni(pipdtc)(P-P)]X (P-P=dppe,
dppb, dpph, dppf; X=ClO4, NCS, I)
Fine pulverized NiX2·nH2O (1 mmol, i.e. 0.21 g
2.2.1.5. NMR data for 5. H NMR: l aromatic region:
7.2–7.8(m), methylene region: 4.91(m), 3.68(s), 3.19(s),
2.47(unres.), 2.17(s), 1.96(s), 1.73(s), 1.64(s), 1.50(s),
1.40(s), 1.28(s), 1.05(s), 0.89(t); 13C{1H} NMR: l aro-
matic region: 132.9(unres.), 132.05(s), 131.4(unres.),
131.2(s), 129.0(unres.), methylene region: 48.01(s),
48.5(s), 31.5(s), 30.0(unres.), 25.8(s), 25.4(unres.),
25.3(s), 23.8(s), 22.5(s), 14.0(s); 31P{1H} NMR: l
25.0(s).
Ni(NCS)2·2H2O, 0.37
g
Ni(ClO4)2·6H2O, 0.42
g
NiI2·6H2O) and P-P ligand (1 mmol, i.e. 0.40 g dppe,
0.43 g dppb, 0.46 g dpph, 0.56 g dppf) was added to a
suspension of fine pulverized [Ni(pipdtc)2] [5] (1 mmol,
0.39 g) in 50 cm3 of absolute EtOH. The mixture was
intensively stirred under reflux for 5–6 h till the reac-
tion components were dissolved and then filtered. The
solid formed after standing for 3 days at room temper-
ature (r.t.) in all cases (except of 1). It was filtered off,
washed with Et2O and dried under an IR lamp at 40°C.
A volume of the reaction solution of complex 1 was
reduced to 1/5 and then an excess of water was added
to it. The solid substance was obtained by freezing out
of the above mixture to −25°C. It was separated by
filtration, washed with water and dried under an IR
lamp at 40°C. (Yields: 0.52 g (75%) for 1, 0.57 g (80%)
for 2, 0.56 g (78%) for 3, 0.61 g (82%) for 4, 0.64 g
(79%) for 5, 0.63 g (76%) for 7, 0.71 g (81%) for 8, 0.70
g (78%) for 9).
1
2.2.1.6. NMR data for 7. H NMR: l aromatic region:
7.70(s), 7.51(s), methylene region: 5.08(s), 4.53(s),
3.64(s), 2.13(s), 1.81(s), 1.65(s), 1.28(s), 0.90(t); 13C{1H}
NMR: l aromatic region: 133.8(s), 132.4(s), 131.6(s),
131.5(s), 131.3(s), 131.2(2×s), 128.7(s), 128.2(s),
128.1(s), methylene region: 47.9(s), 31.4(s), 25.3(s),
23.9(s), 22.4(s), 13.9(s); 31P{1H} NMR: l 29.4(s).
1
2.2.1.7. NMR data for 8. H NMR: l aromatic region:
7.79(s), 7.59(s), 7.50(s), methylene region: 4.59(s),
4.41(s), 3.63(s), 2.18(s), 1.93(s), 1.74(s), 1.61(s), 1.25(t);
13C{1H} NMR: l 196.4(s), aromatic region: 134.0(t),
132.0(s), 129.7(s), 129.0(t), 128.7(s), methine region:
76.0(t), 74.6(t), 71.8(s), 71.0(s), methylene region:
48.2(s), 25.5(s), 23.7(s); 31P{1H} NMR: l 32.7(s).
1
2.2.1.1. NMR data for 1. H NMR: l aromatic region:
7.40–7.90 (m), methylene region: 3.81(t), 3.70(t),
3.48(s), 2.77(d), 2.58(s), 2.55(s), 2.52(s), 2.16(s), 1.78(m),
1.68(m), 1.52(m), 1.27(m), 0.88(t); 13C{1H} NMR: l
199.1(s), aromatic region: 133.1(t), 132.8(t), 132.3(s),
129.6(t), 127.6(s), 127.0(s), methylene region: 48.2(s),
47.5(2 x s), 31.4(s), 26.3(t), 25.5(s), 25.3(s), 25.2(s),
23.9(s), 23.8(s); 31P{1H} NMR: l 63.0(m).
1
2.2.1.8. NMR data for 9. H NMR: l aromatic region:
8.79(s), 7.80(s), 7.62(s), 7.53(s), 7.28(s), 7.00(s), 6.85(s),
6.64(s), methylene region: 4.91(s), 4.60(s), 4.43(s),
3.73(s), 3.52(s), 3.34(s), 3.27(s), 2.53(s), 2.19(s), 2.08(s),
1.67(s); 13C{1H} NMR: l aromatic region: 134.4(t),
133.7(s), 133.6(s), 132.8(unres.), 132.0(s), 130.2(s),
130.0(s), 129.6(s), 129.0(t), 127.9(s), 127.8(s), methine
region: 76.00(s), 74.5(s), methylene region: 48.3(s),
47.5(s), 25.5(s), 25.3(s), 25.2(s), 24.1(s), 23.8(s); 31P{1H}
NMR: l 32.6(s).
1
2.2.1.2. NMR data for 2. H NMR: l aromatic region:
7.74(s), 7.56(s), methylene region: 3.80(s), 2.66(d),
1.97(s), 1.76(s), 1.68(s); 13C{1H} NMR: l 198.8(s), aro-
matic region: 132.7(t), 132.3(s), 129.6(t), 127.4(s),
126.8(s), methylene region: 48.2(s), 26.19(t), 25.5(s),
23.7(s); 31P{1H} NMR: l 62.8(m).
2.2.2. Preparation of [Ni2(pipdtc)2(NCS)2(dpph)]·2H2O
(6)
Fine pulverized Ni(NCS)2·2H2O (1 mmol, 0.21 g) and
dpph (1 mmol, 0.46 g) was added to a suspension of
fine pulverized [Ni(pipdtc)2] (1 mmol, 0.39 g) in 50 cm3
of absolute EtOH. The solid formed during intensive
stirring of the reaction mixture under reflux (6 h). The
substance was dissolved in CH2Cl2 and then filtered.
Red microcrystals formed after standing of solution for
3 days at r.t. They were filtered off, washed with Et2O
and dried under an IR lamp at 40°C. (Yield: 0.75 g
(72%)).
1
2.2.1.3. NMR data for 3. H NMR: l aromatic region:
7.74(s), 7.46(s), methylene region: 3.70(s), 3.54(s),
2.30(s), 2.06(s), 2.06(s), 1.68(s), 1.62(s); 13C{1H} NMR:
l 201.2(s), aromatic region: 133.1(d), 130.9(s), 129.1(s),
128.8(d), 128.5(s), methylene region: 47.9(unres.),
26.3(s), 26.1(s), 25.4(s), 24.9(s), 24.0(s); 31P{1H} NMR:
l 20.7(s).
1
1
2.2.1.4. NMR data for 4. H NMR: l aromatic region:
NMR data for 6: H NMR: l aromatic region: 7.53
7.2–7.9(m), methylene region: 3.73(q), 3.63(t), 3.28(s),
(s), 7.42 (m), methylene region: 3.57 (s), 2.78 (s), 2.40
(s), 2.00 (s), 1.66 (s), 1.53 (s), 1.16 (t); 13C{1H} NMR: l
198.4 (s), aromatic region: 132.7 (s), 131.0 (s), 130.5 (s),
130.4 (s), 129.6 (s), 128.8 (s), 128.4 (unres.), 128.2 (s),
methylene region: 57.7 (s), 47.7 (s), 25.7 (unres.), 25.15
(s), 24.3 (s), 23.5 (s), 18.2 (s); 31P{1H} NMR: l 25.4 (s).
2.52(s), 2.13(t), 1.72(m), 1.61(m), 1.25(t); 13C{1H}
NMR:
l 197.8(unres.), aromatic region: 133.0(t),
131.7(s), 129.4(s), 129.2(t), 128.8(s), methylene region:
48.1(s), 26.1(t), 25.4(s), 24.0(t), 23.8(s); 31P{1H} NMR:
l 30.0(s).

R. Pastorek et al. / Polyhedron 19 (2000) 1713–1717
1715
2.3. Physical measurements
tions of diffractometer axis (ƒ, s and q) were chosen in
sequence for covering of practically full 2–50° 2q hemi-
sphere. A total of 1800 frames were recorded. The
exposure time was 20 s for each 0.33° rotation step. The
cell parameters were retrieved from all frames using
KM4 software and refined on all strong reflections.
Data reduction was processed by 3D profile analysing
software KM4RED, which corrects intensities for Lorentz
and polarization effects too.
The content of nickel was determined by the chelato-
metric titration on murexid as an indicator. Chlorine
and bromine were determined by the Scho¨niger method
[6]. The elemental analyses (C, H, N, S) were performed
on an EA 1108 instrument (FISONS). The r.t. magnetic
susceptibilities of all complexes were measured by the
Faraday method. Co[Hg(NCS)4] was used as a cali-
brant. Diamagnetic corrections were made with Pascal’s
constants [7]. Conductivities were measured with an
OK 102/1 conductivity meter (Radelkis, Budapest) at
25°C. Diffuse-reflectance electronic absorption spectra
(45 000–11 000 cm−1) were carried out on a Specord
Crystal data and structure refinement: C40H38ClFe-
NNiO4P2S2: monoclinic, P21/n, a=10.056(2), b=
,
15.813(2), c=24.000(3) A, i=101.70(2)°, V=
3
3737.1(10)A , Z=4, DX-ray=1.551 g cm−3, v=1.205
,
mm−1, F(000)=1800, GOF=1.018, extinction coeffi-
cient=0.00083(13), 632 parameters, R1(obs.)=0.0617,
M40 (Carl Zeiss, Jena). IR spectra (4000–400 cm−1
)
were recorded on a Specord M80 (Carl Zeiss, Jena)
using Nujol mulls. 1H, 13C{1H} and 31P{1H} NMR
spectra of the complexes were recorded in CDCl3 on a
Bruker AVANCE DRX 300 or 500 instruments. Chem-
wR2(obs.)=0.1220, R1(all)=0.0761, wR2(all)=0.1341,
−3
DFmax=0.612 e A−3, DFmin= −0.788 e A
.
,
,
The structure was solved by the direct methods using
the program SHELXS-97 [8]. The structure was refined
anisotropically by the full-matrix least-squares proce-
dure on F2 with weight: w=1/[|2(F2o)+(0.0250P)2+
27.0000P], where P=(F2o+2Fc2)/3, using the
SHELXL-97 program [9]. All H-atoms were found from
differential Fourier maps and all their parameters were
left free for refinement. The O(1), O(2) and O(3) atoms
of perchlorate anion are disordered and their positions
and Ueq-factors were refined using a combination of
FVAR and EADP instructions. Additional calculations
were made using PARST95 [10].
1
ical shifts of H and 13C spectra were given upfield with
respect to SiMe4, chemical shifts of 31P spectra were
given upfield with respect to 85% aqueous solution of
H3PO4.
2.4. Crystal structure determination of 8
Single crystals of 8 were obtained direct from reac-
tion mixture. A crystal of size 0.80×0.20×0.20 mm
was used for data collection. All geometric and inten-
sity data were collected on a s-axis four-circle diffrac-
tometer KUMA KM-4CCD equipped with
a
OXFORD Cryostream cooler at temperature 150 K. A
total of 23 686 reflections (of which 6 482 [Rint=0.0831]
were unique) in the range 7.28B2qB50.00° were col-
lected at 150(2) K with monochromatic Mo Ka radia-
3. Results and discussion
Composition and analytical data for the complexes
are listed in Table 1. The results of physico-chemical
studies are summarized in Table 2. All the [Ni(p-
ipdtc)(P-P)]X complexes are diamagnetic and behave as
electrolytes of the 1:1 type [11]. An ionic binding of the
ClO4 and NCS anions is also supported by IR spec-
,
tion (u=0.71073 A, V=55 kV, I=30 mA) and 0.7
mm collimator. A distance of 50 mm between the
crystal and CCD detector was chosen. All rotations
were performed around omega axis perpendicular to
the direction of the X-ray beam. Six different orienta-
Table 1
The results of elemental analyses
Compound
Found (Calc.) (%)
Ni
C
H
N
S
X a
1
2
3
4
5
6
7
8
9
[Ni(pipdtc)(dppe)](NCS)·H2O
[Ni(pipdtc)(dppe)]ClO4
8.5(8.8)
8.2(8.1)
8.1(9.0)
7.9(7.6)
7.2(7.1)
11.2(10.8)
7.1(7.0)
6.7(6.7)
6.5(7.0)
57.1(56.6)
53.6(53.2)
58.3(58.0)
1.9(1.8)
53.4(53.0)
50.6(50.1)
59.2(58.8)
55.1(54.5)
53.4(53.6)
5.2(4.9)
4.8(5.2)
5.6(5.6)
54.8(54.7)
5.7(5.5)
5.4(5.1)
4.6(4.4)
4.4(4.4)
4.2(4.2)
4.0(3.9)
2.0(1.7)
3.9(4.2)
5.1(4.9)
1.7(1.6)
5.4(5.1)
3.4(3.4)
1.6(1.5)
1.6(1.6)
13.9(13.5)
9.0(8.7)
13.3(12.7)
8.6(8.1)
5.0(4.6)
[Ni(pipdtc)(dppb)](NCS)·H2O
[Ni(pipdtc)(dppb)]ClO4
[Ni(pipdtc)(dpph)]ClO4·2H2O
[Ni2(pipdtc)2(NCS)2(dpph)]·2H2O
[Ni(pipdtc)(dppf)](NCS)
[Ni(pipdtc)(dppf)]ClO4
4.8(4.2)
4.4(3.9)
7.9(8.0)
18.4(17.8)
11.6(11.0)
7.4(6.5)
4.1(4.4)
14.1(13.5)
[Ni(pipdtc)(dppf)]I
7.1(6.4)
a X=Cl, I

1716
R. Pastorek et al. / Polyhedron 19 (2000) 1713–1717
troscopy. Strong maxima at 1085 cm−1 [w3(ClO4)], 620
cm−1 [w4(ClO4)] were found in the IR spectra of the
[Ni(pipdtc)(P-P)]ClO4 complexes (2, 4, 5, 8) which can
characterize an ionic nature of the perchlorate anion
[12]. Maximum at 2050 cm−1 may be connected with
the w(CꢀN) vibration of the ionic binding NCS group
[13].
The binuclear complex [Ni2(pipdtc)2(NCS)2(dpph)]·
2H2O (6) is also diamagnetic. Maxima observed in the
IR spectrum of this complex at 2092 and 842 cm−1 can
be attributable to the w(CꢀN) and w(CꢁS) vibrations.
The presence of these maxima indicates that the NCS
group is coordinated to nickel through the N atom [13].
An assumption of square-planar geometry around
the central atom in both types of the above complexes
(1–9) may be also supported by electronic absorption
spectra. Medium strong maxima found in the 18 800–
21 600 cm−1 region in the electronic spectra of all
1
complexes can be attributed to the A1g“1B1g electron
transition [14]. The maxima above 30 000 cm−1 are
assignable to intraligand transitions in the S2CN group
[15,16]. In the IR spectra of all the complexes charac-
teristic maxima at 1536–1510 cm−1 [w(CꢁN)] and 998–
988 cm−1 [w(CꢁS)] were observed for dithiocarbamate
ligands [13,15].
The thermal decompositions of the hydrated com-
plexes (1, 3, 6) begin at 60°C. The dehydratation is
accompanied by endo-effects on DTA-curves (see Table
2). Further thermal decompositions of 1, 3 and 6
proceed without formation of thermally stable interme-
diates. Thermal decays of 7 and 9 begin at 190 and
180°C, respectively. The next process of decomposition
also proceeds without formation of thermally stable
intermediates. The decomposition of the complexes
containing the perchlorate anion (5) were not per-
formed owing to their possible explosivity.
The structure of [Ni(pipdtc)(dppf)]ClO4 (8) was de-
termined by a single-crystal X-ray analysis. Selected
bond lengths and angles are listed in Table 3. The
complex [Ni(pipdtc)(dppf)]+ cation is shown in Fig. 1.
As excepted, X-ray structure analysis proved that the
nickel(II) atom is four-coordinated by two sulfur atoms
from pipdtc and by two phosphorus atoms from dppf
in distorted square-planar arrangement. The NiS2P2
chromophore is nearly planar even if the group of
atoms deviates significantly from planarity [S((d/s)2=
2758.04, 2=5.99 at 95% probability level for 3 degrees
of freedom]. A degree of the distortion is also apparent
from displacements of the Ni(1), S(1), S(2), P(1) and
P(2) atoms from a least-squares plane fitted through the
above atoms [10]. The deviations are as follows: Ni(1)
−0.0153(5), S(1) 0.030(12), S(2) 0.0345(12), P(1)
,
0.0352(12) and P(2) 0.096(2) A. An increase of p-elec-
tron density over the S2CN− moiety was also proved.
This delocalization of electron density is obvious from
,
shortening of the CꢁS [1.733(5) and 1.727(4) A] and

R. Pastorek et al. / Polyhedron 19 (2000) 1713–1717
1717
As expected, the 31P{1H} NMR spectra measured for
selected complexes exhibit one signal at 63.0 ppm (1),
62.8 ppm (2), 20.7 (3), 30.0 ppm (4), 25.0 ppm (5), 25.4
ppm (6), 29.4 ppm (7), 32.7 ppm (8), and 32.6 ppm (9),
respectively, corresponding to one kind of phosphorus
atoms in the molecule.
Table 3
,
Selected bond lengths (A) and angles (°) for [Ni(pipdtc)(dppf)]ClO4
(8)
Ni(1)ꢁS(2)
Ni(1)ꢁP(2)
Ni(1)ꢁS(1)
Ni(1)ꢁP(1)
Fe(1)ꢁC(36)
Fe(1)ꢁC(37)
Fe(1)ꢁC(32)
Fe(1)ꢁC(40)
Fe(1)ꢁC(33)
Fe(1)ꢁC(31)
Fe(1)ꢁC(35)
Fe(1)ꢁC(34)
Fe(1)ꢁC(38)
Fe(1)ꢁC(39)
S(1)ꢁC(1)
2.2161(13)
2.2164(13)
2.2260(13)
2.2279(13)
2.014(5)
2.028(5)
2.036(5)
2.037(5)
2.040(5)
2.040(5)
2.042(5)
2.053(6)
2.067(6)
2.068(6)
1.733(5)
1.727(4)
1.307(6)
1.477(6)
1.480(6)
1.518(7)
1.524(7)
1.518(7)
1.530(7)
S(2)ꢁNi(1)ꢁP(2)
S(2)ꢁNi(1)ꢁS(1)
P(2)ꢁNi(1)ꢁS(1)
S(2)ꢁNi(1)ꢁP(1)
P(2)ꢁNi(1)ꢁP(1)
S(1)ꢁNi(1)ꢁP(1)
C(1)ꢁS(1)ꢁNi(1)
C(1)ꢁS(2)ꢁNi(1)
C(1)ꢁN(1)ꢁC(6)
C(1)ꢁN(1)ꢁC(2)
C(6)ꢁN(1)ꢁC(2)
N(1)ꢁC(1)ꢁS(2)
N(1)ꢁC(1)ꢁS(1)
S(2)ꢁC(1)ꢁS(1)
N(1)ꢁC(2)ꢁC(3)
C(2)ꢁC(3)ꢁC(4)
C(5)ꢁC(4)ꢁC(3)
C(4)ꢁC(5)ꢁC(6)
N(1)ꢁC(6)ꢁC(5)
91.78(5)
78.75(5)
170.48(5)
168.78(5)
99.11(5)
90.32(5)
85.62(16)
86.08(16)
122.0(4)
122.5(4)
113.8(4)
126.1(4)
124.8(3)
109.1(3)
108.5(4)
110.3(4)
112.3(4)
111.3(4)
108.5(4)
4. Supplementary material
Supplementary data have been deposited with the
Cambridge Crystallographic Data Centre under deposi-
tion number 137218. Copies of this information may be
obtained free of charge from The Director, CCDC, 12
Union Road, Cambridge, CB2 1EZ, UK (fax: +44-
1223-336-033; e-mail: deposit@ccdc.cam.ac.uk or www:
http://www.ccdc.cam.ac.uk).
S(2)ꢁC(1)
N(1)ꢁC(1)
N(1)ꢁC(6)
N(1)ꢁC(2)
C(2)ꢁC(3)
C(3)ꢁC(4)
C(4)ꢁC(5)
C(5)ꢁC(6)
Acknowledgements
&
We are grateful to the FRVS (Project No. 31702007/
1999) for financial support.
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,
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,
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