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Acta Cryst. (2007). E63, m2973-m2974    [ doi:10.1107/S1600536807054815 ]

Chlorido{1-[2-(ethylsulfonyl)phenyldiazenyl]-4-methoxy-2-naphthyl-[kappa]3C,N,O}palladium(II) sesquihydrate

S. S. Chhetri, A. N. Biswas, P. Das, A. Saha and P. Bandyopadhyay

Abstract top

In the title compound, [Pd(C9H17N2O3S)Cl]·1.5H2O, the Pd atom is tetracoordinated by a naphthyl C, a diazene N, a Cl and a sulfonyl O atom in an approximate square-planar geometry; the asymmetric unit also contains 1.5 molecules of water, one molecule lying on a twofold rotation axis. A hydrophilic environment wrapping the polar portion of the compound is created by an array of water molecules. The crystal packing is stabilized by an intermolecular C-H...O interaction and eight intermolecular [pi]-[pi] interactions; the centroid-centroid distances range from 3.647 (2)-3.8098 (18) Å, with perpendicular interplanar distances between 3.169 and 3.590 Å.

Comment top

Cyclopalladated compounds find numerous applications (Dupont et al., 2005) in organic synthesis, catalysis, photochemistry and metallomesogen chemistry. Although a number of cyclometallated complexes of palladium (Dupont et al., 2005 & Neogi et al., 2006) have been reported in literature, the chemistry of cyclopalladates having sulfonyl ligand framework is not explored much. Against this background, we report here the crystal structure of (I).

The molecular structure of the title compound, (I), is shown in Fig. 1, with the atom numbering scheme. The palladium atom along with donor set of four atoms lie in a plane. Selected bond lengths and bond angles are listed in Table 1. The packing arrangement of (I) is shown in Fig. 2. The N=N bond length is typical of other cyclopalladated azoarenes (Neogi et al., 2006). A hydrophilic environment wrapping the polar portion of the compound is being created by an array of water molecules. Intramolecular C–H···Cl and C–H···O interactions are also present in (I) (Table 2, Fig. 3). The crystal packing is stabilized by a intermolecular C18–H18A···O3i [Symmetry codes: (i) −x + 1/2, −y + 5/2, −z + 2.] interaction (Table 2, Fig. 3) and eight intermolecular π–π interactions (Bagchi et al., 2007); the Cg3-Cg3ii, Cg3-Cg4ii, Cg3—Cg5iii, Cg4—Cg3ii, Cg4—Cg5iii, Cg5—Cg3iii, Cg5—Cg4iii and Cg5—Cg5ii [Symmetry codes: (ii) −x, y, 1/2 − z; (iii) −x, −y, -z·Cg3, Cg4 and Cg5 are the centroids of C1—C10, C5—C9 and C11—C16 rings respectively.] distances are 3.647 (2), 3.6495 (18), 3.8098 (18), 3.6495 (18), 3.740 (2), 3.8098 (18), 3.740 (2) and 3.850 (3) Å (Fig. 4); the corresponding perpendicular distances are 3.396, 3.402, 3.169, 3.464, 3.590, 3.462, 3.434 and 3.480 Å respectively.

Related literature top

For related literature, see: Bagchi et al. (2007); Dupont et al. (2005); Neogi et al. (2006); Ersanlı, Albayrak, Odabaşoğlu & Kazak (2005); Ghedini et al. (1991); Lanfredi et al. (1984).

Experimental top

The title compound was synthesized by reacting 1-[2-(ethylsulfonyl)phenyldiazenyl]-4-methoxynaphthalene with disodiumtetrachloropalladate in aqueous ethanol medium at room temperature. The product was purified by chromatography. Crystals suitable for X-ray crystallography was obtained by slow diffusion of dichloromethane solution into hexane.

Refinement top

The O-bound H atom was located in a difference Fourier map and its isotropic displacement parameter were freely refined after fixing the coordinates. C-bound H atoms were included at calculated positions as riding atoms with C–H distances of 0.93 Å for aromatic, 0.96 Å for CH3 and 0.97 Å for CH2 H atoms, with Uiso (H) =1.2Ueq (C) (1.5Ueq for methyl groups).

Computing details top

Data collection: SMART (Bruker, 1998); cell refinement: SAINT (Bruker, 2000); data reduction: SAINT (Bruker, 2000); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1997); software used to prepare material for publication: SHELXTL (Bruker, 1997).

Figures top
[Figure 1] Fig. 1. The asymmetric unit of (I), with displacement ellipsoids drawn at the 50% probability level. Solvent molecules are omited for clarity.
[Figure 2] Fig. 2. The molecular arrangement of (I) in the ac plane.
[Figure 3] Fig. 3. A representation of the intramolecular C—H···O, C—H···Cl (dotted lines), intermolecular C—H···O (dashed lines) interactions of (I) [symmetry code: (i) −x + 1/2, −y + 5/2, −z + 2.]. Solvent molecules are omited for clarity.
[Figure 4] Fig. 4. The inter molecular π—π interaction for (I), indicated by the dotted line. [Symmetry codes: (ii) −x, y, 1/2 − z; (iii) −x, −y, -z. Cg3, Cg4 and Cg5 are the centroids of C1—C10, C5—C9 and C11—C16 rings, respectively.]
Chlorido{1-[2-(ethylsulfonyl)phenyldiazenyl]-4-methoxy-2-naphthyl- κ3C,N,O}palladium(II) sesquihydrate top
Crystal data top
[Pd(C9H17N2O3S)Cl]·1.5H2OF000 = 2104
Mr = 522.31Dx = 1.729 Mg m−3
Monoclinic, C2/cMo Kα radiation
λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 3904 reflections
a = 21.1870 (18) Åθ = 1.7–25.9º
b = 17.1097 (14) ŵ = 1.19 mm−1
c = 13.4827 (11) ÅT = 295 (2) K
β = 124.8240 (10)ºNeedle, pink
V = 4012.2 (6) Å30.38 × 0.26 × 0.19 mm
Z = 8
Data collection top
Bruker SMART APEX CCD area detector
diffractometer		3904 independent reflections
Radiation source: fine-focus sealed tube3503 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.020
T = 298(2) Kθmax = 25.9º
phi and ω scansθmin = 1.7º
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)		h = −26→26
Tmin = 0.694, Tmax = 0.799k = −20→20
12258 measured reflectionsl = −16→16
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.031H-atom parameters constrained
wR(F2) = 0.083  w = 1/[σ2(Fo2) + (0.0445P)2 + 5.4842P]
where P = (Fo2 + 2Fc2)/3
S = 1.08(Δ/σ)max = 0.001
3904 reflectionsΔρmax = 1.07 e Å−3
262 parametersΔρmin = −0.68 e Å−3
Primary atom site location: structure-invariant direct methodsExtinction correction: none
Crystal data top
[Pd(C9H17N2O3S)Cl]·1.5H2OV = 4012.2 (6) Å3
Mr = 522.31Z = 8
Monoclinic, C2/cMo Kα
a = 21.1870 (18) ŵ = 1.19 mm−1
b = 17.1097 (14) ÅT = 295 (2) K
c = 13.4827 (11) Å0.38 × 0.26 × 0.19 mm
β = 124.8240 (10)º
Data collection top
Bruker SMART APEX CCD area detector
diffractometer		3904 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)		3503 reflections with I > 2σ(I)
Tmin = 0.694, Tmax = 0.799Rint = 0.020
12258 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.031262 parameters
wR(F2) = 0.083H-atom parameters constrained
S = 1.08Δρmax = 1.07 e Å−3
3904 reflectionsΔρmin = −0.68 e Å−3
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
Pd10.167430 (12)0.985070 (13)0.74687 (2)0.03443 (9)
C20.09189 (15)0.90245 (17)0.6922 (2)0.0331 (6)
S10.22366 (4)1.14847 (5)0.85771 (7)0.04165 (19)
Cl10.27025 (5)0.90451 (5)0.81104 (9)0.0582 (2)
N10.00874 (14)1.01220 (14)0.6375 (2)0.0354 (5)
O20.24220 (12)1.08601 (13)0.8039 (2)0.0455 (5)
O30.27501 (13)1.21410 (14)0.9014 (2)0.0571 (6)
C30.10189 (16)0.82172 (18)0.6998 (3)0.0379 (6)
H30.15070.80060.73550.046*
C10.01766 (15)0.93370 (17)0.6381 (2)0.0330 (6)
N20.07265 (13)1.04999 (14)0.6875 (2)0.0347 (5)
C9−0.03752 (16)0.80271 (17)0.5939 (2)0.0354 (6)
C10−0.04846 (16)0.88408 (18)0.5863 (2)0.0345 (6)
O10.04360 (12)0.69462 (13)0.6603 (2)0.0477 (5)
C110.06450 (17)1.13260 (17)0.6846 (3)0.0362 (6)
C40.03909 (16)0.77313 (17)0.6542 (3)0.0370 (6)
C8−0.12377 (16)0.91331 (19)0.5259 (3)0.0422 (7)
H8−0.13180.96700.52060.051*
C180.22294 (19)1.1079 (2)0.9776 (3)0.0491 (8)
H18A0.21871.14951.02240.059*
H18B0.17851.07400.94500.059*
C5−0.10186 (17)0.7528 (2)0.5393 (3)0.0429 (7)
H5−0.09500.69890.54320.051*
C120.12879 (17)1.18202 (18)0.7525 (3)0.0400 (7)
C16−0.00722 (18)1.16709 (19)0.6124 (3)0.0419 (7)
H16−0.05061.13570.56750.050*
C6−0.17412 (17)0.7830 (2)0.4809 (3)0.0492 (8)
H6−0.21640.74970.44450.059*
C7−0.18495 (18)0.8641 (2)0.4754 (3)0.0506 (8)
H7−0.23440.88440.43690.061*
C170.1169 (2)0.6590 (2)0.7179 (4)0.0663 (11)
H17A0.14090.67510.67860.099*
H17B0.11120.60320.71290.099*
H17C0.14840.67450.80120.099*
C130.1196 (2)1.26272 (19)0.7420 (3)0.0505 (8)
H130.16241.29500.78500.061*
C15−0.0153 (2)1.2474 (2)0.6061 (3)0.0494 (8)
H15−0.06421.26940.55890.059*
C140.0481 (2)1.2949 (2)0.6691 (3)0.0549 (9)
H140.04241.34900.66210.066*
C190.2955 (2)1.0614 (3)1.0621 (4)0.0700 (11)
H19A0.29481.01451.02230.105*
H19B0.29811.04791.13350.105*
H19C0.33951.09221.08400.105*
O40.4461 (4)1.0023 (4)1.0164 (7)0.180 (3)
O50.00000.5318 (7)0.75000.221 (5)
H5A−0.01500.56800.68401.0 (3)*
H4B0.48400.99701.00000.150*
H4A0.42800.94801.01000.37 (9)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pd10.02794 (13)0.03781 (15)0.03805 (15)−0.00271 (8)0.01914 (11)−0.00357 (9)
C20.0302 (13)0.0405 (15)0.0278 (13)−0.0038 (11)0.0162 (11)−0.0027 (11)
S10.0362 (4)0.0378 (4)0.0512 (4)−0.0080 (3)0.0251 (4)−0.0050 (3)
Cl10.0369 (4)0.0491 (5)0.0855 (6)0.0040 (3)0.0331 (4)−0.0021 (4)
N10.0319 (12)0.0433 (14)0.0316 (12)−0.0012 (10)0.0185 (11)−0.0021 (10)
O20.0379 (11)0.0475 (13)0.0556 (13)−0.0094 (9)0.0295 (11)−0.0069 (10)
O30.0456 (13)0.0448 (13)0.0768 (17)−0.0139 (10)0.0326 (13)−0.0100 (12)
C30.0291 (14)0.0435 (16)0.0364 (15)−0.0001 (12)0.0158 (12)−0.0026 (12)
C10.0307 (13)0.0403 (16)0.0291 (14)−0.0028 (12)0.0177 (12)−0.0037 (11)
N20.0313 (12)0.0391 (13)0.0345 (12)−0.0007 (10)0.0193 (10)−0.0010 (10)
C90.0327 (14)0.0425 (16)0.0321 (14)−0.0028 (12)0.0191 (12)−0.0032 (12)
C100.0304 (13)0.0448 (16)0.0275 (13)−0.0021 (12)0.0161 (11)−0.0051 (12)
O10.0374 (11)0.0386 (12)0.0606 (14)0.0006 (9)0.0242 (11)−0.0002 (10)
C110.0405 (15)0.0392 (16)0.0358 (15)0.0003 (12)0.0259 (13)−0.0016 (12)
C40.0349 (14)0.0399 (16)0.0341 (15)−0.0012 (12)0.0185 (13)−0.0025 (12)
C80.0329 (15)0.0470 (18)0.0415 (16)0.0034 (13)0.0181 (13)−0.0056 (13)
C180.0490 (18)0.0493 (19)0.0474 (19)−0.0071 (15)0.0266 (16)−0.0062 (15)
C50.0373 (15)0.0453 (18)0.0444 (17)−0.0080 (13)0.0223 (14)−0.0081 (14)
C120.0395 (15)0.0385 (16)0.0462 (17)−0.0020 (13)0.0269 (14)0.0002 (13)
C160.0420 (16)0.0467 (18)0.0387 (16)0.0039 (13)0.0240 (14)0.0023 (13)
C60.0330 (16)0.058 (2)0.0501 (19)−0.0119 (14)0.0200 (15)−0.0139 (16)
C70.0279 (15)0.063 (2)0.0506 (19)−0.0002 (14)0.0161 (14)−0.0092 (16)
C170.0419 (19)0.045 (2)0.097 (3)0.0077 (16)0.031 (2)0.006 (2)
C130.0541 (19)0.0381 (17)0.061 (2)−0.0064 (15)0.0336 (18)−0.0025 (15)
C150.0516 (19)0.052 (2)0.0458 (18)0.0125 (16)0.0286 (16)0.0072 (15)
C140.069 (2)0.0399 (18)0.061 (2)0.0086 (17)0.040 (2)0.0069 (16)
C190.076 (3)0.066 (3)0.054 (2)0.008 (2)0.029 (2)0.0016 (19)
O40.146 (5)0.171 (6)0.165 (6)−0.029 (4)0.054 (5)0.013 (4)
O50.143 (7)0.224 (10)0.341 (15)0.0000.166 (10)0.000
Geometric parameters (Å, °) top
Pd1—C21.938 (3)C18—C191.514 (5)
Pd1—N22.018 (2)C18—H18A0.9700
Pd1—O22.166 (2)C18—H18B0.9700
Pd1—Cl12.2895 (8)C5—C61.362 (4)
C2—C31.392 (4)C5—H50.9300
C2—C11.408 (4)C12—C131.390 (5)
S1—O31.435 (2)C16—C151.381 (5)
S1—O21.466 (2)C16—H160.9300
S1—C181.768 (3)C6—C71.402 (5)
S1—C121.768 (3)C6—H60.9300
N1—N21.290 (3)C7—H70.9300
N1—C11.356 (4)C17—H17A0.9600
C3—C41.380 (4)C17—H17B0.9600
C3—H30.9300C17—H17C0.9600
C1—C101.433 (4)C13—C141.365 (5)
N2—C111.422 (4)C13—H130.9300
C9—C101.405 (4)C15—C141.374 (5)
C9—C51.408 (4)C15—H150.9300
C9—C41.430 (4)C14—H140.9300
C10—C81.405 (4)C19—H19A0.9600
O1—C41.346 (4)C19—H19B0.9600
O1—C171.418 (4)C19—H19C0.9600
C11—C161.384 (4)O4—H4B0.9500
C11—C121.409 (4)O4—H4A0.9900
C8—C71.358 (4)O5—H5A0.9800
C8—H80.9300
C2—Pd1—N280.32 (11)C19—C18—H18A109.4
C2—Pd1—O2173.86 (10)S1—C18—H18A109.4
N2—Pd1—O293.58 (9)C19—C18—H18B109.4
C2—Pd1—Cl196.06 (9)S1—C18—H18B109.4
N2—Pd1—Cl1176.38 (7)H18A—C18—H18B108.0
O2—Pd1—Cl190.04 (6)C6—C5—C9120.3 (3)
C3—C2—C1119.5 (2)C6—C5—H5119.8
C3—C2—Pd1129.6 (2)C9—C5—H5119.8
C1—C2—Pd1110.8 (2)C13—C12—C11120.2 (3)
O3—S1—O2114.78 (14)C13—C12—S1115.7 (2)
O3—S1—C18109.40 (16)C11—C12—S1124.1 (2)
O2—S1—C18108.13 (15)C15—C16—C11121.0 (3)
O3—S1—C12108.86 (15)C15—C16—H16119.5
O2—S1—C12110.03 (14)C11—C16—H16119.5
C18—S1—C12105.20 (15)C5—C6—C7120.2 (3)
N2—N1—C1113.1 (2)C5—C6—H6119.9
S1—O2—Pd1114.10 (11)C7—C6—H6119.9
C4—C3—C2119.8 (3)C8—C7—C6120.4 (3)
C4—C3—H3120.1C8—C7—H7119.8
C2—C3—H3120.1C6—C7—H7119.8
N1—C1—C2119.3 (2)O1—C17—H17A109.5
N1—C1—C10119.3 (2)O1—C17—H17B109.5
C2—C1—C10121.3 (3)H17A—C17—H17B109.5
N1—N2—C11114.2 (2)O1—C17—H17C109.5
N1—N2—Pd1116.19 (19)H17A—C17—H17C109.5
C11—N2—Pd1129.48 (19)H17B—C17—H17C109.5
C10—C9—C5119.5 (3)C14—C13—C12120.5 (3)
C10—C9—C4118.6 (3)C14—C13—H13119.7
C5—C9—C4121.9 (3)C12—C13—H13119.7
C9—C10—C8118.7 (3)C14—C15—C16120.5 (3)
C9—C10—C1118.5 (2)C14—C15—H15119.7
C8—C10—C1122.8 (3)C16—C15—H15119.7
C4—O1—C17118.7 (2)C13—C14—C15119.8 (3)
C16—C11—C12117.8 (3)C13—C14—H14120.1
C16—C11—N2120.7 (3)C15—C14—H14120.1
C12—C11—N2121.4 (3)C18—C19—H19A109.5
O1—C4—C3123.9 (3)C18—C19—H19B109.5
O1—C4—C9113.9 (2)H19A—C19—H19B109.5
C3—C4—C9122.2 (3)C18—C19—H19C109.5
C7—C8—C10120.8 (3)H19A—C19—H19C109.5
C7—C8—H8119.6H19B—C19—H19C109.5
C10—C8—H8119.6H4B—O4—H4A103.0
C19—C18—S1111.0 (3)
N2—Pd1—C2—C3−176.2 (3)C17—O1—C4—C30.7 (5)
Cl1—Pd1—C2—C33.6 (3)C17—O1—C4—C9179.8 (3)
N2—Pd1—C2—C13.79 (18)C2—C3—C4—O1−178.2 (3)
Cl1—Pd1—C2—C1−176.32 (18)C2—C3—C4—C92.7 (4)
O3—S1—O2—Pd1177.03 (14)C10—C9—C4—O1177.8 (2)
C18—S1—O2—Pd154.61 (17)C5—C9—C4—O1−4.2 (4)
C12—S1—O2—Pd1−59.78 (17)C10—C9—C4—C3−3.1 (4)
N2—Pd1—O2—S138.00 (15)C5—C9—C4—C3175.0 (3)
Cl1—Pd1—O2—S1−141.84 (13)C9—C10—C8—C7−0.3 (4)
C1—C2—C3—C40.1 (4)C1—C10—C8—C7178.3 (3)
Pd1—C2—C3—C4−179.9 (2)O3—S1—C18—C19−75.3 (3)
N2—N1—C1—C21.0 (4)O2—S1—C18—C1950.3 (3)
N2—N1—C1—C10179.6 (2)C12—S1—C18—C19167.9 (3)
C3—C2—C1—N1176.1 (2)C10—C9—C5—C6−0.9 (4)
Pd1—C2—C1—N1−4.0 (3)C4—C9—C5—C6−178.9 (3)
C3—C2—C1—C10−2.5 (4)C16—C11—C12—C13−2.7 (4)
Pd1—C2—C1—C10177.5 (2)N2—C11—C12—C13176.0 (3)
C1—N1—N2—C11178.1 (2)C16—C11—C12—S1175.1 (2)
C1—N1—N2—Pd12.4 (3)N2—C11—C12—S1−6.2 (4)
C2—Pd1—N2—N1−3.68 (19)O3—S1—C12—C13−7.3 (3)
O2—Pd1—N2—N1176.99 (19)O2—S1—C12—C13−133.9 (2)
C2—Pd1—N2—C11−178.6 (2)C18—S1—C12—C13109.8 (3)
O2—Pd1—N2—C112.1 (2)O3—S1—C12—C11174.8 (2)
C5—C9—C10—C81.2 (4)O2—S1—C12—C1148.2 (3)
C4—C9—C10—C8179.3 (3)C18—S1—C12—C11−68.1 (3)
C5—C9—C10—C1−177.4 (3)C12—C11—C16—C150.8 (4)
C4—C9—C10—C10.6 (4)N2—C11—C16—C15−177.9 (3)
N1—C1—C10—C9−176.4 (2)C9—C5—C6—C7−0.5 (5)
C2—C1—C10—C92.1 (4)C10—C8—C7—C6−1.0 (5)
N1—C1—C10—C84.9 (4)C5—C6—C7—C81.4 (5)
C2—C1—C10—C8−176.6 (3)C11—C12—C13—C142.1 (5)
N1—N2—C11—C16−12.3 (4)S1—C12—C13—C14−175.8 (3)
Pd1—N2—C11—C16162.7 (2)C11—C16—C15—C141.8 (5)
N1—N2—C11—C12169.0 (3)C12—C13—C14—C150.4 (5)
Pd1—N2—C11—C12−16.0 (4)C16—C15—C14—C13−2.4 (5)
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
C3—H3···Cl10.932.773.297 (4)117
C13—H13···O30.932.412.841 (5)108
C18—H18A···O3i0.972.523.443 (4)158
Symmetry codes: (i) −x+1/2, −y+5/2, −z+2.
Table 1
Selected geometric parameters (Å, °) top
Pd1—C21.938 (3)Pd1—O22.166 (2)
Pd1—N22.018 (2)Pd1—Cl12.2895 (8)
C2—Pd1—N280.32 (11)C2—Pd1—Cl196.06 (9)
N2—Pd1—O293.58 (9)O2—Pd1—Cl190.04 (6)
Table 2
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
C3—H3···Cl10.932.773.297 (4)117
C13—H13···O30.932.412.841 (5)108
C18—H18A···O3i0.972.523.443 (4)158
Symmetry codes: (i) −x+1/2, −y+5/2, −z+2.
Acknowledgements top

Financial support (SR/S1/IC-08/2007) from the DST, Government of India, is gratefully acknowledged. We thank the CSIR (India) for the award of a fellowship (PD) and the UGC (New Delhi) for the Special Assistance Programme to our Department. We also thank Professor S. Pal, School of Chemistry, University of Hyderabad, India, for the X-ray data collection.

references
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