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Acta Cryst. (2008). E64, m545-m546    [ doi:10.1107/S1600536808006673 ]

6-(2-Chlorobenzylamino)purinium tetrachlorido(dimethyl sulfoxide-[kappa]O)(nitrosyl-[kappa]N)ruthenate(III) monohydrate

Z. Trávnícek, M. Matiková-Malarová and K. Stepánková

Abstract top

The asymmetric unit of the title complex salt, (C12H11ClN5)[RuCl4(NO)(C2H6OS)]·H2O, contains a 6-(2-chlorobenzylamino)purinium cation, a tetrachlorido(dimethyl sulfoxide)nitrosylruthenate(III) anion and one solvent water molecule. The RuIII atom is octahedrally coordinated by four Cl atoms in the equatorial plane, and by a dimethyl sulfoxide O atom and a nitrosyl N atom in axial positions. The cation is an N3-protonated N7 tautomer. Intermolecular N-H...N hydrogen bonds connect two cations into centrosymmetric dimers, with an N...N distance of 2.821 (4) Å. The crystal structure also involves N-H...O, N-H...Cl and O-H...Cl hydrogen bonds.

Comment top

As a part of our systematic study of Ru(III) complexes involving substituted 6-benzylaminopurines, we have prepared the title complex salt, (I), Fig. 1. The structure comprises a 6-(2-chlorobenzylamino)purin-3-ium cation, a [tetrachloro(dimethyl sulfoxide-κO)(nitrosyl-κN)]ruthenate(III) anion and one water molecule of crystallization. The cation exists as the N3-protonated N7 tautomer and contains three different aromatic rings: benzene, pyrimidine (A) and imidazole (B). The A and B rings are nearly co-planar forming a dihedral angle of 1.49 (1)°, while the angle between the benzene ring and purine skeleton (rings A + B) is 85.95 (7)°. The bond lengths and angles in the cation of (I) are similar to those found for 6-(3-chlorobenzylamino)purinium chloride (Maloň et al., 2001), 6-(4-chlorobenzylamino)purinium perchlorate (Maloň et al., 2002), 6-(4-methoxybenzylamino)purinium chloride (Trávníček et al., 2004), 6-(3-methoxybenzylamino)purinium chloride monohydrate (Trávníček et al., 2005), 6-(3-bromobenzylamino)purinium chloride (Trávníček et al., 2006) and 6-(4-hydroxybenzylamino)purinium chloride (Trávníček et al., 2007). Suprisingly, only nine Ru complexes having a RuCl4NO coordination geometry have been structurally characterized up to now and deposited in the CSD (Cambridge Structural Database, Version 5.29; Allen, 2002). Moreover, the title complex salt represents only the second X-ray structure determined involving a Ru(NO-κN)Cl4(DMSO-κO) moiety.

The geometry about the RuIII atom can be described as a distorted octahedron, as can be seen from the following angles: Cl2-Ru1-Cl4 (174.92 (3)°), Cl3-Ru1-Cl5 (172.39 (3)°), and O1-Ru1-N2 (178.16 (12)°). The N-bonded nitrosyl group occupies a position trans to the O-coordinated dimethyl sulfoxide (DMSO). The Ru–Cl, Ru–N and Ru–O bond lengths of 2.3585 (9)-2.3798 (8), 1.703 (3), and 2.042 (2) Å, respectively, are close to those found for [(DMSO)2H][trans-RuCl4(NO)(DMSO-κO)] (2.356 (2)-2.373 (2), 1.712 (5), and 2.029 (3) Å, respectively) (Serli et al., 2002).

The O—H···Cl, N—H···Cl, N–H···O and N—H···N hydrogen bonds in (I) contribute to the stabilization of the secondary structure (Table 1, Figs. 2 and 3). Non-bonding interactions of the type C17···C11xi (3.3914 (5) Å), C17···Cl6xi (3.3825 (4) Å), C17—H17A···O3xii (C···O = 3.4419 (5) Å), C16—H16C···Cl3vii (C···Cl = 3.5709 (6) Å) are also present [symmetry codes: xi: 1-x, 0.5+y, 0.5-z; xii: 1.5-x, 0.5+y, z; vii: -0.5+x, y, 0.5-z]. The periodic alternation of anionic and cationic layers in the ac plane can be seen from Fig. 3.

Related literature top

For related structures of 6-benzylaminopurine derivatives, see: Maloň et al. (2001, 2002); Trávníček et al. (2004, 2005, 2007); Trávníček & Matiková-Maľarová (2006). For the structure of a related Ru complex, see: Serli et al. (2002). For a description of the Cambridge Structural Database, see: Allen (2002).

Experimental top

The title complex salt, (I), was prepared by mixing of an ethanolic suspension (2 ml) of 6-(2-chlorobenzylamino)purine and an ethanolic solution (3 ml) of [(DMSO)2H][RuCl4NO(DMSO-κO)] (DMSO = dimethyl sulfoxide) in a molar ratio of 2:1. The reaction mixture was stirred at room temperature for 5 min. After this time, a violet solution formed which was left to stand at room temperature. Violet crystals, suitable for single-crystal X-ray analysis, were deposited after slow evaporation of the solvent over a period of two days.

Refinement top

All H atoms were located in difference maps and refined using a riding model, with C–H distances of 0.95 and 0.99 Å, N–H distances of 0.88 Å, and with Uiso(H) values of 1.2Ueq(C,N). The O–H atoms were refined freely, see Table 1 for distances. The highest unassigned difference Fourier peak of 1.25 e Å-3 is located 0.84 Å from the Ru1 atom.

Computing details top

Data collection: CrysAlis CCD (Oxford Diffraction, 2007); cell refinement: CrysAlis RED (Oxford Diffraction, 2007); data reduction: CrysAlis RED (Oxford Diffraction, 2007); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg, 2006); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. The molecular structure of (I), showing the non-H atoms as 50% probability displacement ellipsoids.
[Figure 2] Fig. 2. Hydrogen bonding interactions of the type O—H···Cl, N—H···Cl, N–H···O and N—H···N (dashed lines) operating in the crystal structure of (I). Symmetry codes: (i) 1 - x, -y, 1 - z; (ii) 1.5 - x, 1 - y, 1/2 + z; (v) 1.5 - x, 1 - y, -1/2 + z; (vi) 1/2 + x, 1 + y, 0.5 - z; (vii) -1/2 + x, y, 0.5 - z; (viii) 2 - x, 1 - y, 1 - z.
[Figure 3] Fig. 3. Part of the crystal structure of (I), showing the formation of non-bonding C–H···Cl, C–H···O, C···Cl and C···C (dashed lines) interactions. Symmetry codes: (vii) -1/2 + x, y, 0.5 - z; (ix) 1 - x, -1/2 + y, 0.5 - z; (x) 1.5 - x, -1/2 + y, z; (xi) 1 - x, 1/2 + y, 0.5 - z; (xii) 1.5 - x, 1/2 + y, z.
6-(2-Chlorobenzylamino)purinium tetrachlorido(dimethyl sulfoxide-κO)(nitrosyl-κN)ruthenate(III) monohydrate top
Crystal data top
(C12H11ClN5)[RuCl4(NO)(C2H6OS)]·H2OF000 = 2512
Mr = 629.73Dx = 1.844 Mg m−3
Orthorhombic, PbcaMo Kα radiation
λ = 0.71073 Å
Hall symbol: -P 2ac 2abCell parameters from 29289 reflections
a = 15.6229 (5) Åθ = 2.6–31.9º
b = 12.8014 (4) ŵ = 1.40 mm−1
c = 22.6866 (16) ÅT = 120 (2) K
V = 4537.2 (4) Å3Prism, violet
Z = 80.40 × 0.30 × 0.25 mm
Data collection top
Oxford Diffraction Xcalibur2
diffractometer with CCD detector		3984 independent reflections
Radiation source: Enhance (Mo) X-ray Source3588 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.018
Detector resolution: 8.3611 pixels mm-1θmax = 25.0º
T = 120(2) Kθmin = 2.6º
rotation method ω scansh = −18→15
Absorption correction: multi-scan
(CrysAlis RED; Oxford Diffraction, 2007)		k = −13→15
Tmin = 0.604, Tmax = 0.721l = −26→26
36172 measured reflections
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 atoms treated by a mixture of
independent and constrained refinement
wR(F2) = 0.079  w = 1/[σ2(Fo2) + (0.0366P)2 + 10.7079P]
where P = (Fo2 + 2Fc2)/3
S = 1.09(Δ/σ)max < 0.001
3984 reflectionsΔρmax = 1.25 e Å−3
279 parametersΔρmin = −0.58 e Å−3
2 restraintsExtinction correction: none
Primary atom site location: structure-invariant direct methods
Crystal data top
(C12H11ClN5)[RuCl4(NO)(C2H6OS)]·H2OV = 4537.2 (4) Å3
Mr = 629.73Z = 8
Orthorhombic, PbcaMo Kα
a = 15.6229 (5) ŵ = 1.40 mm−1
b = 12.8014 (4) ÅT = 120 (2) K
c = 22.6866 (16) Å0.40 × 0.30 × 0.25 mm
Data collection top
Oxford Diffraction Xcalibur2
diffractometer with CCD detector		3984 independent reflections
Absorption correction: multi-scan
(CrysAlis RED; Oxford Diffraction, 2007)		3588 reflections with I > 2σ(I)
Tmin = 0.604, Tmax = 0.721Rint = 0.018
36172 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0312 restraints
wR(F2) = 0.079H atoms treated by a mixture of
independent and constrained refinement
S = 1.09  w = 1/[σ2(Fo2) + (0.0366P)2 + 10.7079P]
where P = (Fo2 + 2Fc2)/3
3984 reflectionsΔρmax = 1.25 e Å−3
279 parametersΔρmin = −0.58 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
Ru10.616687 (16)0.769508 (19)0.208516 (10)0.01845 (9)
S10.47079 (7)0.93802 (7)0.19053 (4)0.0406 (3)
N10.57623 (16)0.3182 (2)0.47999 (11)0.0210 (6)
O10.52917 (14)0.85527 (17)0.16242 (10)0.0250 (5)
Cl20.67103 (5)0.72294 (6)0.11452 (3)0.02083 (17)
C20.5321 (2)0.2412 (2)0.45576 (14)0.0225 (7)
H2A0.50520.25460.41900.027*
N20.68824 (19)0.6944 (2)0.24609 (12)0.0285 (6)
O20.7319 (2)0.6425 (2)0.27444 (12)0.0498 (8)
O30.87301 (19)0.6670 (2)0.18872 (13)0.0445 (7)
Cl30.70383 (5)0.92198 (7)0.20765 (4)0.0304 (2)
N30.52234 (16)0.1460 (2)0.47885 (11)0.0199 (5)
H3A0.49030.09860.46150.024*
Cl40.55053 (6)0.81931 (7)0.29846 (3)0.0326 (2)
C40.56383 (19)0.1251 (2)0.53017 (13)0.0183 (6)
Cl50.51797 (6)0.63075 (7)0.20103 (4)0.0317 (2)
C50.61254 (19)0.2011 (2)0.55736 (14)0.0198 (6)
Cl60.63017 (6)0.69071 (6)0.46836 (4)0.0329 (2)
C60.61565 (18)0.3025 (2)0.53287 (14)0.0189 (6)
N60.65345 (17)0.3834 (2)0.55878 (12)0.0224 (6)
H6A0.68130.37240.59190.027*
N70.64498 (18)0.1527 (2)0.60684 (12)0.0237 (6)
H7A0.67880.18090.63350.028*
C80.6151 (2)0.0543 (3)0.60655 (15)0.0237 (7)
H8A0.62870.00440.63610.028*
N90.56465 (17)0.0337 (2)0.56098 (12)0.0219 (6)
C90.6513 (2)0.4892 (2)0.53527 (14)0.0239 (7)
H9A0.66350.53890.56760.029*
H9B0.59280.50400.52070.029*
C100.7143 (2)0.5083 (2)0.48574 (14)0.0210 (7)
C110.7108 (2)0.6004 (2)0.45299 (14)0.0247 (7)
C120.7666 (2)0.6214 (3)0.40738 (15)0.0306 (8)
H12A0.76360.68590.38680.037*
C130.8268 (2)0.5472 (3)0.39215 (16)0.0358 (9)
H13A0.86480.55970.36020.043*
C140.8317 (2)0.4551 (3)0.42324 (17)0.0357 (9)
H14A0.87320.40410.41260.043*
C150.7766 (2)0.4362 (3)0.47003 (15)0.0281 (7)
H15A0.78150.37290.49160.034*
C160.3684 (3)0.8778 (5)0.1860 (3)0.094 (2)
H16A0.36640.81770.21280.142*
H16B0.35830.85420.14550.142*
H16C0.32420.92820.19730.142*
C170.4570 (3)1.0279 (3)0.13257 (18)0.0391 (9)
H17A0.51081.06540.12570.059*
H17B0.41211.07800.14310.059*
H17C0.44050.99050.09670.059*
H3W0.860 (3)0.606 (2)0.2071 (18)0.050*
H3V0.9236 (18)0.687 (3)0.2050 (18)0.050*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ru10.02301 (15)0.01753 (15)0.01482 (14)−0.00037 (10)−0.00315 (10)−0.00055 (9)
S10.0678 (7)0.0305 (5)0.0233 (4)0.0244 (5)0.0070 (4)−0.0014 (4)
N10.0198 (14)0.0203 (14)0.0229 (14)−0.0022 (11)−0.0009 (11)0.0034 (11)
O10.0259 (12)0.0285 (12)0.0207 (11)0.0062 (10)−0.0028 (9)−0.0053 (10)
Cl20.0188 (4)0.0246 (4)0.0191 (4)0.0011 (3)−0.0003 (3)−0.0024 (3)
C20.0215 (16)0.0227 (16)0.0232 (17)−0.0017 (13)−0.0035 (13)0.0038 (13)
N20.0396 (17)0.0275 (15)0.0183 (13)0.0064 (14)−0.0060 (13)−0.0014 (12)
O20.062 (2)0.0545 (18)0.0328 (15)0.0269 (16)−0.0130 (14)0.0043 (13)
O30.0407 (16)0.0503 (18)0.0424 (17)−0.0016 (14)−0.0104 (13)0.0060 (14)
Cl30.0320 (5)0.0241 (4)0.0350 (5)−0.0075 (3)−0.0039 (4)−0.0059 (3)
N30.0186 (13)0.0181 (13)0.0229 (14)−0.0032 (11)−0.0041 (11)−0.0002 (11)
Cl40.0444 (5)0.0349 (5)0.0186 (4)0.0014 (4)0.0033 (4)−0.0049 (3)
C40.0161 (15)0.0169 (15)0.0218 (16)−0.0008 (12)0.0021 (12)−0.0004 (12)
Cl50.0378 (5)0.0261 (4)0.0312 (5)−0.0117 (4)0.0078 (4)−0.0043 (3)
C50.0185 (15)0.0197 (15)0.0212 (15)−0.0019 (13)−0.0024 (12)0.0025 (13)
Cl60.0488 (5)0.0182 (4)0.0316 (4)0.0042 (4)0.0020 (4)−0.0021 (3)
C60.0148 (15)0.0189 (15)0.0231 (16)−0.0004 (12)0.0029 (12)0.0012 (13)
N60.0259 (14)0.0175 (13)0.0238 (14)−0.0049 (11)−0.0042 (11)0.0023 (11)
N70.0257 (14)0.0228 (14)0.0225 (14)−0.0066 (12)−0.0072 (11)0.0039 (11)
C80.0257 (17)0.0198 (16)0.0257 (17)−0.0049 (13)−0.0057 (14)0.0059 (13)
N90.0230 (14)0.0187 (13)0.0240 (14)−0.0026 (11)−0.0022 (11)0.0041 (11)
C90.0279 (17)0.0184 (16)0.0255 (17)−0.0014 (13)0.0023 (14)−0.0007 (13)
C100.0222 (16)0.0188 (15)0.0220 (16)−0.0056 (13)−0.0043 (13)−0.0021 (13)
C110.0289 (18)0.0214 (16)0.0238 (17)−0.0051 (14)−0.0048 (14)−0.0046 (13)
C120.037 (2)0.0308 (19)0.0239 (17)−0.0133 (16)−0.0009 (15)0.0044 (14)
C130.0263 (19)0.053 (2)0.0280 (19)−0.0101 (17)0.0050 (15)0.0023 (17)
C140.0235 (18)0.045 (2)0.038 (2)0.0023 (16)0.0033 (16)−0.0018 (18)
C150.0237 (17)0.0291 (18)0.0317 (18)−0.0014 (14)−0.0010 (14)0.0026 (15)
C160.050 (3)0.075 (4)0.158 (6)0.028 (3)0.062 (4)0.052 (4)
C170.045 (2)0.031 (2)0.041 (2)0.0084 (17)0.0006 (18)0.0047 (17)
Geometric parameters (Å, °) top
Ru1—N21.703 (3)N6—H6A0.8800
Ru1—O12.042 (2)N7—C81.344 (4)
Ru1—Cl52.3585 (9)N7—H7A0.8800
Ru1—Cl22.3713 (8)C8—N91.326 (4)
Ru1—Cl42.3746 (8)C8—H8A0.9500
Ru1—Cl32.3798 (8)C9—C101.514 (4)
S1—O11.536 (2)C9—H9A0.9900
S1—C171.761 (4)C9—H9B0.9900
S1—C161.778 (6)C10—C151.388 (5)
N1—C21.323 (4)C10—C111.394 (5)
N1—C61.363 (4)C11—C121.379 (5)
C2—N31.335 (4)C12—C131.382 (5)
C2—H2A0.9500C12—H12A0.9500
N2—O21.149 (4)C13—C141.376 (5)
O3—H3W0.904 (19)C13—H13A0.9500
O3—H3V0.909 (19)C14—C151.388 (5)
N3—C41.359 (4)C14—H14A0.9500
N3—H3A0.8800C15—H15A0.9500
C4—N91.363 (4)C16—H16A0.9800
C4—C51.380 (4)C16—H16B0.9800
C5—N71.379 (4)C16—H16C0.9800
C5—C61.412 (5)C17—H17A0.9800
Cl6—C111.745 (3)C17—H17B0.9800
C6—N61.329 (4)C17—H17C0.9800
N6—C91.457 (4)
N2—Ru1—O1178.16 (12)C5—N7—H7A126.6
N2—Ru1—Cl592.30 (10)N9—C8—N7113.4 (3)
O1—Ru1—Cl586.00 (7)N9—C8—H8A123.3
N2—Ru1—Cl294.19 (10)N7—C8—H8A123.3
O1—Ru1—Cl285.09 (6)C8—N9—C4103.6 (3)
Cl5—Ru1—Cl288.86 (3)N6—C9—C10114.0 (3)
N2—Ru1—Cl490.41 (10)N6—C9—H9A108.7
O1—Ru1—Cl490.24 (7)C10—C9—H9A108.7
Cl5—Ru1—Cl488.82 (3)N6—C9—H9B108.7
Cl2—Ru1—Cl4174.92 (3)C10—C9—H9B108.7
N2—Ru1—Cl395.26 (10)H9A—C9—H9B107.6
O1—Ru1—Cl386.44 (7)C15—C10—C11116.9 (3)
Cl5—Ru1—Cl3172.39 (3)C15—C10—C9122.6 (3)
Cl2—Ru1—Cl389.65 (3)C11—C10—C9120.5 (3)
Cl4—Ru1—Cl392.06 (3)C12—C11—C10122.7 (3)
O1—S1—C17102.31 (16)C12—C11—Cl6118.4 (3)
O1—S1—C16102.2 (2)C10—C11—Cl6118.8 (3)
C17—S1—C1697.5 (3)C11—C12—C13118.9 (3)
C2—N1—C6119.4 (3)C11—C12—H12A120.5
S1—O1—Ru1123.75 (13)C13—C12—H12A120.5
N1—C2—N3125.2 (3)C14—C13—C12120.0 (3)
N1—C2—H2A117.4C14—C13—H13A120.0
N3—C2—H2A117.4C12—C13—H13A120.0
O2—N2—Ru1175.0 (3)C13—C14—C15120.4 (4)
H3W—O3—H3V104 (4)C13—C14—H14A119.8
C2—N3—C4117.4 (3)C15—C14—H14A119.8
C2—N3—H3A121.3C14—C15—C10121.1 (3)
C4—N3—H3A121.3C14—C15—H15A119.5
N3—C4—N9127.7 (3)C10—C15—H15A119.5
N3—C4—C5120.5 (3)S1—C16—H16A109.5
N9—C4—C5111.8 (3)S1—C16—H16B109.5
N7—C5—C4104.5 (3)H16A—C16—H16B109.5
N7—C5—C6136.1 (3)S1—C16—H16C109.5
C4—C5—C6119.4 (3)H16A—C16—H16C109.5
N6—C6—N1118.4 (3)H16B—C16—H16C109.5
N6—C6—C5123.9 (3)S1—C17—H17A109.5
N1—C6—C5117.8 (3)S1—C17—H17B109.5
C6—N6—C9123.5 (3)H17A—C17—H17B109.5
C6—N6—H6A118.2S1—C17—H17C109.5
C9—N6—H6A118.2H17A—C17—H17C109.5
C8—N7—C5106.8 (3)H17B—C17—H17C109.5
C8—N7—H7A126.6
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
N3—H3A···N9i0.881.972.821 (4)164
N6—H6A···O3ii0.882.413.046 (4)130
N6—H6A···Cl2ii0.882.663.312 (3)132
N7—H7A···O3ii0.882.452.976 (4)119
N7—H7A···Cl2ii0.882.683.290 (3)127
N7—H7A···Cl3ii0.882.823.424 (3)128
O3—H3W···Cl3iii0.904 (19)2.56 (3)3.386 (3)152 (4)
O3—H3V···Cl4iv0.909 (19)2.61 (3)3.402 (3)146 (4)
O3—H3V···Cl5iv0.909 (19)2.69 (3)3.406 (3)136 (4)
Symmetry codes: (i) −x+1, −y, −z+1; (ii) −x+3/2, −y+1, z+1/2; (iii) −x+3/2, y−1/2, z; (iv) x+1/2, y, −z+1/2.
Table 1
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
N3—H3A···N9i0.881.972.821 (4)164
N6—H6A···O3ii0.882.413.046 (4)130
N6—H6A···Cl2ii0.882.663.312 (3)132
N7—H7A···O3ii0.882.452.976 (4)119
N7—H7A···Cl2ii0.882.683.290 (3)127
N7—H7A···Cl3ii0.882.823.424 (3)128
O3—H3W···Cl3iii0.904 (19)2.56 (3)3.386 (3)152 (4)
O3—H3V···Cl4iv0.909 (19)2.61 (3)3.402 (3)146 (4)
O3—H3V···Cl5iv0.909 (19)2.69 (3)3.406 (3)136 (4)
Symmetry codes: (i) −x+1, −y, −z+1; (ii) −x+3/2, −y+1, z+1/2; (iii) −x+3/2, y−1/2, z; (iv) x+1/2, y, −z+1/2.
Acknowledgements top

Financial support of this work by the Ministry of Education, Youth and Sport of the Czech Republic (MSM6198959218) and the Grant Agency of the Czech Republic (GAČR 203/08/P436) is gratefully acknowledged.

references
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