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Acta Cryst. (2007). E63, m2219    [ doi:10.1107/S1600536807035726 ]

catena-Poly[[(18-crown-6)potassium(I)]-[mu]-chlorido-silver(I)-[mu]-chlorido]

X.-M. Song, X.-Q. Huang, J.-M. Dou and D.-C. Li

Abstract top

The title complex, [AgKCl2(C12H24O6)]n, has been synthesized by reaction of 18-crown-6 with KCl and AgNO3. [K(18-crown-6)]+ cations and [AgCl2]- anions form one-dimensional chains through K...Cl interactions of length 3.2568 (14) Å. Both the K+ and the AgI ions lie on centres of inversion.

Comment top

Much interest has been focused on crown ethers and their metal cations because they can act as modules to form novel polymeric structures (Desai et al., 2001; Bastos et al., 2000). The title complex consists of [K(18-crown-6)]+ cations linked by [AgCl2]- anions (Figure 1).

The AgI atom lies on a centre of inversion and is coordinated in a linear manner by by two Cl atoms with an Ag—Cl bond length of 2.3114 (10) Å. In the [K(18-crown-6)]+ cation, K+ lies on a centre of inversion and is coordinated by six O atoms, with K+ lying approximately in the plane of the crown ether. The K—O bond lengths vary from 2.783 (2) to 2.830 (2) Å. The cations and anions are linked via K—Cl interactions of length 3.2568 (14) Å, forming one-dimensional chains along the b axis (Figure 2).

Related literature top

For other examples of structures incorporating [AgCl2]- anions, see: Exarchos et al. (1998); Gerisch et al. (1997). For polymeric structures incorporating crown ethers, see: Desai et al. (2001); Bastos et al. (2000).

Experimental top

KCl (0.2238 g, 3.0 mmol) and AgNO3 (0.2548 g,1.5 mmol) in 15 ml e thanol were refluxed for 4 h, then 18-crown-6 (0.421 g, 1.5 mmol) was added slowly and the mixture was refluxed for a further 4 h. After cooling to room temperature, the mixture was filtered and the resulting solid was recrystallized from ether. Elemental analysis: calculated C 29.89, H 4.98%; found: C 30.02, H 4.99.

Refinement top

H atoms were positioned geometrically and refined using a riding model with C—H = 0.97 Å and Uiso(H) = 1.2Ueq(C).

Computing details top

Data collection: SMART (Siemens, 1996); cell refinement: SAINT (Siemens, 1996); data reduction: SAINT; 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.

Figures top
[Figure 1] Fig. 1. Molecular structure of the title compound showing displacement ellipsoids at the 30% probability level. H atoms are omitted. Symmetry code (A): 1 - x, 1 - y, 1 - z.
[Figure 2] Fig. 2. One-dimensional chain running along the b-axis.
catena-Poly[[(18-crown-6)potassium(I)]-µ-chlorido-silver(I)-µ-chlorido] top
Crystal data top
[AgKCl2(C12H24O6)]F(000) = 488
Mr = 482.18Dx = 1.657 Mg m−3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 2464 reflections
a = 8.691 (4) Åθ = 2.9–26.1°
b = 8.244 (4) ŵ = 1.56 mm−1
c = 13.833 (6) ÅT = 298 K
β = 102.764 (6)°Block, colourless
V = 966.6 (8) Å30.56 × 0.34 × 0.30 mm
Z = 2
Data collection top
Bruker SMART CCD
diffractometer		1699 independent reflections
Radiation source: fine-focus sealed tube1308 reflections with I > 2σ(I)
graphiteRint = 0.020
φ and ω scansθmax = 25.0°, θmin = 2.5°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)		h = −6→10
Tmin = 0.457, Tmax = 0.627k = −9→9
4877 measured reflectionsl = −15→16
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.027Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.079H-atom parameters constrained
S = 1.03 w = 1/[σ2(Fo2) + (0.0449P)2 + 0.1659P]
where P = (Fo2 + 2Fc2)/3
1699 reflections(Δ/σ)max < 0.001
103 parametersΔρmax = 0.20 e Å−3
0 restraintsΔρmin = −0.37 e Å−3
Crystal data top
[AgKCl2(C12H24O6)]V = 966.6 (8) Å3
Mr = 482.18Z = 2
Monoclinic, P21/nMo Kα radiation
a = 8.691 (4) ŵ = 1.56 mm−1
b = 8.244 (4) ÅT = 298 K
c = 13.833 (6) Å0.56 × 0.34 × 0.30 mm
β = 102.764 (6)°
Data collection top
Bruker SMART CCD
diffractometer		1699 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)		1308 reflections with I > 2σ(I)
Tmin = 0.457, Tmax = 0.627Rint = 0.020
4877 measured reflectionsθmax = 25.0°
Refinement top
R[F2 > 2σ(F2)] = 0.027H-atom parameters constrained
wR(F2) = 0.079Δρmax = 0.20 e Å−3
S = 1.03Δρmin = −0.37 e Å−3
1699 reflectionsAbsolute structure: ?
103 parametersFlack parameter: ?
0 restraintsRogers parameter: ?
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
Cl10.68538 (10)0.17256 (10)0.45904 (7)0.0811 (3)
Ag10.50000.00000.50000.06429 (16)
K10.50000.50000.50000.0469 (2)
O10.5045 (3)0.5512 (2)0.29837 (13)0.0602 (5)
O20.7752 (2)0.6133 (2)0.45167 (15)0.0629 (5)
O30.7445 (2)0.6290 (2)0.64818 (13)0.0624 (5)
C10.4100 (4)0.4327 (4)0.2368 (2)0.0764 (10)
H1A0.45700.32610.25100.092*
H1B0.40530.45730.16770.092*
C20.6609 (4)0.5529 (4)0.2855 (2)0.0704 (9)
H2A0.66170.58100.21760.084*
H2B0.70740.44610.29920.084*
C30.7541 (4)0.6736 (4)0.3540 (2)0.0722 (9)
H3A0.85570.69050.33750.087*
H3B0.69880.77650.34830.087*
C40.8766 (4)0.7074 (4)0.5233 (3)0.0775 (10)
H4A0.83370.81580.52510.093*
H4B0.97920.71620.50700.093*
C50.8922 (3)0.6288 (4)0.6205 (3)0.0782 (10)
H5A0.92860.51810.61720.094*
H5B0.96950.68650.66980.094*
C60.7508 (4)0.5672 (5)0.7444 (2)0.0775 (10)
H6A0.81980.63390.79320.093*
H6B0.79250.45760.74950.093*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cl10.0670 (5)0.0692 (5)0.1129 (7)0.0011 (4)0.0325 (5)0.0147 (4)
Ag10.0596 (2)0.0636 (2)0.0702 (2)−0.00286 (15)0.01553 (17)0.00199 (15)
K10.0389 (4)0.0580 (5)0.0438 (4)−0.0085 (3)0.0093 (3)−0.0009 (3)
O10.0699 (13)0.0619 (11)0.0505 (11)0.0093 (10)0.0171 (10)0.0017 (9)
O20.0523 (11)0.0603 (12)0.0785 (13)−0.0153 (10)0.0193 (10)0.0032 (10)
O30.0484 (11)0.0703 (12)0.0614 (12)0.0053 (9)−0.0029 (9)−0.0083 (9)
C10.110 (3)0.0723 (19)0.0434 (16)0.006 (2)0.0098 (18)−0.0033 (15)
C20.089 (2)0.0700 (18)0.0629 (19)0.0200 (19)0.0393 (18)0.0167 (16)
C30.0593 (18)0.0677 (19)0.102 (3)0.0081 (16)0.0450 (19)0.0265 (18)
C40.0480 (17)0.068 (2)0.121 (3)−0.0186 (16)0.0290 (19)−0.019 (2)
C50.0355 (15)0.086 (2)0.104 (3)−0.0010 (15)−0.0050 (16)−0.032 (2)
C60.083 (3)0.073 (2)0.063 (2)0.0062 (18)−0.0147 (18)−0.0048 (15)
Geometric parameters (Å, °) top
Cl1—Ag12.3117 (11)C1—C6ii1.477 (4)
Cl1—K13.2568 (14)C1—H1A0.970
Ag1—Cl1i2.3117 (11)C1—H1B0.970
K1—O22.783 (2)C2—C31.484 (4)
K1—O2ii2.783 (2)C2—H2A0.970
K1—O3ii2.8145 (19)C2—H2B0.970
K1—O32.8145 (19)C3—H3A0.970
K1—O1ii2.830 (2)C3—H3B0.970
K1—O12.830 (2)C4—C51.471 (5)
K1—Cl1ii3.2568 (14)C4—H4A0.970
O1—C21.409 (4)C4—H4B0.970
O1—C11.430 (4)C5—H5A0.970
O2—C41.405 (4)C5—H5B0.970
O2—C31.413 (3)C6—C1ii1.477 (4)
O3—C61.415 (3)C6—H6A0.970
O3—C51.419 (3)C6—H6B0.970
Ag1—Cl1—K193.96 (4)C5—O3—K1112.68 (16)
Cl1i—Ag1—Cl1180.0O1—C1—C6ii109.6 (3)
O2—K1—O2ii180.0O1—C1—H1A109.7
O2—K1—O3ii120.16 (6)C6ii—C1—H1A109.7
O2ii—K1—O3ii59.84 (6)O1—C1—H1B109.7
O2—K1—O359.84 (6)C6ii—C1—H1B109.7
O2ii—K1—O3120.16 (6)H1A—C1—H1B108.2
O3ii—K1—O3180.0O1—C2—C3109.4 (2)
O2—K1—O1ii119.12 (6)O1—C2—H2A109.8
O2ii—K1—O1ii60.88 (6)C3—C2—H2A109.8
O3ii—K1—O1ii119.26 (6)O1—C2—H2B109.8
O3—K1—O1ii60.74 (6)C3—C2—H2B109.8
O2—K1—O160.88 (6)H2A—C2—H2B108.2
O2ii—K1—O1119.12 (6)O2—C3—C2108.2 (2)
O3ii—K1—O160.74 (6)O2—C3—H3A110.1
O3—K1—O1119.26 (6)C2—C3—H3A110.1
O1ii—K1—O1180.0O2—C3—H3B110.1
O2—K1—Cl1ii104.35 (5)C2—C3—H3B110.1
O2ii—K1—Cl1ii75.65 (5)H3A—C3—H3B108.4
O3ii—K1—Cl1ii96.71 (5)O2—C4—C5108.6 (3)
O3—K1—Cl1ii83.29 (5)O2—C4—H4A110.0
O1ii—K1—Cl1ii80.62 (4)C5—C4—H4A110.0
O1—K1—Cl1ii99.38 (4)O2—C4—H4B110.0
O2—K1—Cl175.65 (5)C5—C4—H4B110.0
O2ii—K1—Cl1104.35 (5)H4A—C4—H4B108.4
O3ii—K1—Cl183.29 (5)O3—C5—C4109.9 (3)
O3—K1—Cl196.71 (5)O3—C5—H5A109.7
O1ii—K1—Cl199.38 (4)C4—C5—H5A109.7
O1—K1—Cl180.62 (4)O3—C5—H5B109.7
Cl1ii—K1—Cl1180.0C4—C5—H5B109.7
C2—O1—C1112.0 (2)H5A—C5—H5B108.2
C2—O1—K1110.46 (17)O3—C6—C1ii108.9 (3)
C1—O1—K1110.70 (17)O3—C6—H6A109.9
C4—O2—C3114.2 (2)C1ii—C6—H6A109.9
C4—O2—K1116.99 (17)O3—C6—H6B109.9
C3—O2—K1114.25 (16)C1ii—C6—H6B109.9
C6—O3—C5113.9 (3)H6A—C6—H6B108.3
C6—O3—K1114.53 (18)
Ag1—Cl1—K1—O2176.84 (5)Cl1ii—K1—O2—C3−77.49 (18)
Ag1—Cl1—K1—O2ii−3.16 (5)Cl1—K1—O2—C3102.51 (18)
Ag1—Cl1—K1—O3ii−59.64 (5)O2—K1—O3—C6−152.6 (2)
Ag1—Cl1—K1—O3120.36 (5)O2ii—K1—O3—C627.4 (2)
Ag1—Cl1—K1—O1ii59.01 (5)O1ii—K1—O3—C613.5 (2)
Ag1—Cl1—K1—O1−120.99 (5)O1—K1—O3—C6−166.5 (2)
O2—K1—O1—C220.34 (18)Cl1ii—K1—O3—C696.4 (2)
O2ii—K1—O1—C2−159.66 (18)Cl1—K1—O3—C6−83.6 (2)
O3ii—K1—O1—C2−145.9 (2)O2—K1—O3—C5−20.37 (19)
O3—K1—O1—C234.1 (2)O2ii—K1—O3—C5159.63 (19)
Cl1ii—K1—O1—C2121.62 (18)O1ii—K1—O3—C5145.7 (2)
Cl1—K1—O1—C2−58.38 (18)O1—K1—O3—C5−34.3 (2)
O2—K1—O1—C1145.0 (2)Cl1ii—K1—O3—C5−131.3 (2)
O2ii—K1—O1—C1−35.0 (2)Cl1—K1—O3—C548.7 (2)
O3ii—K1—O1—C1−21.23 (18)C2—O1—C1—C6ii178.3 (3)
O3—K1—O1—C1158.77 (18)K1—O1—C1—C6ii54.5 (3)
Cl1ii—K1—O1—C1−113.71 (19)C1—O1—C2—C3−177.8 (2)
Cl1—K1—O1—C166.29 (19)K1—O1—C2—C3−53.9 (3)
O3ii—K1—O2—C4166.4 (2)C4—O2—C3—C2173.3 (2)
O3—K1—O2—C4−13.6 (2)K1—O2—C3—C2−48.3 (3)
O1ii—K1—O2—C4−27.5 (2)O1—C2—C3—O270.3 (3)
O1—K1—O2—C4152.5 (2)C3—O2—C4—C5−178.1 (2)
Cl1ii—K1—O2—C459.7 (2)K1—O2—C4—C544.7 (3)
Cl1—K1—O2—C4−120.3 (2)C6—O3—C5—C4−175.2 (3)
O3ii—K1—O2—C329.3 (2)K1—O3—C5—C452.2 (3)
O3—K1—O2—C3−150.7 (2)O2—C4—C5—O3−64.7 (3)
O1ii—K1—O2—C3−164.62 (17)C5—O3—C6—C1ii−177.8 (3)
O1—K1—O2—C315.38 (17)K1—O3—C6—C1ii−46.1 (3)
Symmetry codes: (i) −x+1, −y, −z+1; (ii) −x+1, −y+1, −z+1.
Acknowledgements top

The authors acknowledge the support of the National Natural Science Foundation of Liaocheng University (No. X051040).

references
References top

Bastos, M. B. R., Moreira, J. C. & Farias, P. A. M. (2000). Anal. Chim. Acta, 408, 83–88.

Bruker (1997). SHELXTL. Version 5.10. Bruker AXS Inc., Madison, Wisconsin, USA.

Desai, S. B., Desai, P. B. & Desai, K. R. (2001). Heterocycl. Commun. 1, 83–90.

Exarchos, G., Nyburg, S. C. & Robinson, S. D. (1998). Polyhedron, 17, 1257–1266.

Gerisch, M., Heinemann, F. W., Markgraf, U. & Steinborn, D. (1997). Z. Anorg. Allg. Chem. 623, 1651–1656.

Sheldrick (1996). SADABS. University of Göttingen, Germany.

Sheldrick, G. M. (1997). SHELXL97 and SHELXS97. University of Göttingen, Germany.

Siemens (1996). SMART and SAINT. Versions 4.0. Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA.