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The crystal structure of the title compound, K[Ag(CN)2]·C12H24O6, conventionally denoted K(18-crown-6)Ag(CN)2, where 18-crown-6 is 1,4,7,10,13,16-hexa­oxa­cyclo­octa­decane, is characterized by closely packed linear chains formed by the coordination of the nitrile N atoms of the [Ag(CN)2]- anions to the K+ cations. The K atoms lie on centers of inversion and are additionally bound to the six O atoms of the crown ether.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270103014318/fr1429sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270103014318/fr1429Isup2.hkl
Contains datablock I

CCDC reference: 219552

Comment top

The coordination chemistry of crown ethers has been studied extensively over the past thirty five years (Izatt et al., 1995), and recently, much attention has been given to the structural aspects of their complexation (Steed, 2001; Belsky & Bulychev, 1999). To a lesser extent, these macrocycles have also been studied as molecular building blocks for solid-state structures with novel electronic and magnetic properties (Akutagawa et al., 2002; Nishihara et al., 2002). We are interested in building molecular solids of various dimensionalities, namely one-dimensional chains, two-dimensional sheets and three-dimensional networks. The K(18-crown-6)+ cation has the potential to act as a building block for one-dimensional chains, because additional coordination to the K+ cation can occur both above and below the macrocyclic plane. We have recently investigated the use of the linear Ag(CN)2 anion as a bidentate pseudohalide capable of forming polymeric structures, and we have shown that KMn[Ag(CN)2]3 forms a triply interpenetrating three-dimensional network (Geiser & Schlueter, 2003). The K(18-crown-6)+ cation should be capable of linking linear Ag(CN)2 anions into infinite one-dimensional chains.

The KAg(CN)2 salt, without the addition of crown ether, is characterized by layers of potassium cations separated by layers of linear Ag(CN)2 anions (Hoard, 1933). The synthesis and infrared spectroscopic characterization of K(18-crown-6) A g(CN)2 was first reported by Poladyan et al. (1984), but no structural characterization has been reported until now. The crystal structures of the related Cs(18-crown-6) A g(CN)2 and Rb(18-crown-6) A g(CN)2 salts have been published recently (Manskaya et al., 1998). The Cs(18-crown-6) A g(CN)2 structure is characterized by zigzag chains of Cs(18-crown-6)+ cations, which are coupled into two-dimensional layers through the coordination of the nitrile N atoms of the Ag(CN)2 anions to Cs+ cations in adjacent chains. Rb(18-crown-6) A g(CN)2 forms zigzag chains that are regularly broken, because the Ag(CN)2 anion is too short for the formation of a continuous chain. In both cases, the cavity of 18-crown-6 is too small to accommodate these alkali metal cations, forcing them to lie significantly out of the molecular plane and preventing the formation of linear chains of cofacially joined macrocycles. In this communication, we report that the potassium analog K(18-crown-6) A g(CN)2, (I), forms a third distinct structural type characterized by the cofacial joining of macrocyclic K(18-crown-6)+ cations by bidentate anionic Ag(CN)2 linkers to form a linear chain structure. This structure is related to that recently reported for K(18-crown-6)AuCl2 (Hossain et al., 2003) and that of K(18-crown-6)CuI2 (Rath & Holt, 1986). However, in these salts the K—Cl and K—I bonds are considerably weaker than the K—N bond observed in (I), resulting in Au—Cl—K and Cu—I—K angles of 90.52° and 92.3°, respectively.

In the present structure, each K atom is coordinated to the nitrile N atoms of two Ag(CN)2 anions, one above and one below the macrocyclic ring (Fig. 1), leading to the formation of a chain structure (–Ag—K1—Ag—K2—Ag-) that runs along the [201] direction (Fig. 2). These chains are essentially linear, with K—N—C angles of 176.1 (2) and 175.6 (2)°. Along the chain, the macrocyclic planes are alternately tilted 4.36 (7)° with respect to one another, and the Ag atoms are alternately separated by 11.9687 (6) and 12.0049 (6) Å. The Ag—K distances are 5.9844 (3) and 6.0024 (3) Å, and the K—K separations are therefore 11.9867 (5) Å. The chains are approximately hexagonally packed, with interchain Ag···Ag interactions ranging from 8.1150 (3) to 8.2914 (5) Å.

Ignoring the crown ether groups, the chain packing derives from an idealized rhombohedral prototype (a b c 8.2 Å, α β γ 98°; space group R-3 m). The trigonal axis corresponds to the chain direction. This high-symmetry lattice is distorted, leading to a monoclinic intermediate structure (a = 10.719 Å, b = 12.219 Å, c = 8.241 Å, β = 102.79°, space group C2/m) whose symmetry is further broken by the mutual orientation of the crown ether rings with concomitant doubling of the c axis. Because of the presence of this hypersymmetry (K at 0, 1/2, 0 and 0, 1/2, 0; Ag near 1/2, 1/2, 1/4) a large number of reflections are weak; only those with both l = 2n and h + 2 l = 2n are strong.

The Ag(CN)2 anion in (I) is essentially linear, with an C—Ag—C angle of 179.80 (8)°, and Ag—C—N angles of 179.0 (3)° and 179.5 (2)°. The bond distances are also similar to those previously reported in K2Na[Ag(CN)2]3 (Zabel et al., 1989) and Na[Ag(CN)2] (Range et al., 1989). The nitrile N atoms of the anion are coordinated to one K atom each, with K—N bond lengths of 2.860 (2) and 2.856 (2) Å. The K atoms are eight-coordinate, including the six K—O bonds to the crown ether, which range from 2.793 (1) to 2.828 (1) Å. The K atoms lie on inversion centers and are thus entirely in the plane of the six coordinating O atoms. Around the periphery of the macrocycle, the O atoms lie alternately above and below this plane. The O atoms in the crown ether associated with atom K1 lie above or below the molecular plane by 0.1950 (8) to 0.1968 (8) Å, while those associated with atom K2 deviate from their molecular plane by 0.1964 (9) to 0.1991 (9) Å. Both the 18-crown-6 macrocycles in (I) are largely ordered. The C—C bond lengths range from 1.487 (3) to 1.501 (3) Å, while the C—O bond lengths are between 1.407 (3) and 1.421 (3) Å, and the geometry of the K(18-crown-6)+ cation in all respects is consistent with previously reported results (e.g. Dunitz et al., 1974).

Experimental top

Potassium dicyanoargentate(I) (Aldrich, 1.194 g, 6 mmol) was dissolved in water (15 ml) and combined with an ethanolic solution (10 ml) containing 18-crown-6 (Aldrich, 2.378 g, 9 mmol). In a futile attempt to make a ternary salt, this mixture was then added to a solution of tetrapropylammonium bromide (Aldrich, 0.532 mg, 2 mmol) in ethanol (10 ml). This colorless solution was layered on top of an aquous solution (10 ml) containing manganese(II) nitrate hydrate (Aldrich, 358 mg, 2 mmol). The solution was allowed to evaporate slowly at room temperature. After one month, clear colorless block-like crystals of (I) were collected from the concentrated solution by gravity filtration. Decomposition began near 525 K as the colorless crystals began to darken.

Refinement top

H atoms were placed geometrically at a C—H distance of 0.97 Å and refined as riding. The Uiso values were constrained to be 1.2Ueq of their respective methylene C atom.

Computing details top

Data collection: SMART (Siemens, 1995); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT (Bruker, 2001); program(s) used to solve structure: SHELXTL (Sheldrick, 2001); program(s) used to refine structure: SHELXTL (Sheldrick, 2001); molecular graphics: SHELXTL (Sheldrick, 2001); software used to prepare material for publication: SHELXTL (Sheldrick, 2001).

Figures top
[Figure 1] Fig. 1. The atomic numbering scheme of (I), illustrating a dumbbell-like fragment of the linear cofacially joined macrocyclic chain. Displacement ellipsoids are drawn at the 50% probablility level.
[Figure 2] Fig. 2. The chain structure of (I), which runs along the [201] direction. Displacement ellipsoids are drawn at the 20% probablility level and H atoms have been omitted for clarity.
Potassium 1,4,7,10,13,16-hexaoxacyclooctadecane dicyanoargentate(I) top
Crystal data top
K[Ag(CN)2](C12H24O6)F(000) = 944
Mr = 463.32Dx = 1.462 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 2038 reflections
a = 10.7189 (5) Åθ = 2.5–30.5°
b = 12.2191 (5) ŵ = 1.18 mm1
c = 16.4816 (7) ÅT = 298 K
β = 102.795 (2)°Block, colorless
V = 2105.08 (16) Å30.50 × 0.44 × 0.40 mm
Z = 4
Data collection top
Siemens SMART CCD area-detector
diffractometer
6428 independent reflections
Radiation source: fine-focus sealed tube3178 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.031
area detector ω scansθmax = 30.5°, θmin = 2.1°
Absorption correction: integration
(Sheldrick, 2001)
h = 1515
Tmin = 0.604, Tmax = 0.694k = 1717
26868 measured reflectionsl = 2323
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)] = 0.026H-atom parameters constrained
wR(F2) = 0.086 w = 1/[σ2(Fo2) + (0.0272P)2 + 0.5054P]
where P = (Fo2 + 2Fc2)/3
S = 1.03(Δ/σ)max = 0.049
6428 reflectionsΔρmax = 0.28 e Å3
221 parametersΔρmin = 0.19 e Å3
0 restraintsExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0173 (4)
Crystal data top
K[Ag(CN)2](C12H24O6)V = 2105.08 (16) Å3
Mr = 463.32Z = 4
Monoclinic, P21/nMo Kα radiation
a = 10.7189 (5) ŵ = 1.18 mm1
b = 12.2191 (5) ÅT = 298 K
c = 16.4816 (7) Å0.50 × 0.44 × 0.40 mm
β = 102.795 (2)°
Data collection top
Siemens SMART CCD area-detector
diffractometer
6428 independent reflections
Absorption correction: integration
(Sheldrick, 2001)
3178 reflections with I > 2σ(I)
Tmin = 0.604, Tmax = 0.694Rint = 0.031
26868 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0260 restraints
wR(F2) = 0.086H-atom parameters constrained
S = 1.03Δρmax = 0.28 e Å3
6428 reflectionsΔρmin = 0.19 e Å3
221 parameters
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
K10.00000.50000.00000.04561 (12)
O10.11468 (14)0.38682 (12)0.11319 (9)0.0617 (4)
O20.11733 (13)0.62026 (11)0.10878 (8)0.0575 (4)
O30.04538 (14)0.72577 (11)0.02010 (9)0.0639 (4)
C10.2034 (2)0.4524 (2)0.14310 (15)0.0687 (6)
H1A0.23270.41410.18700.082*
H1B0.27690.46750.09840.082*
C20.1397 (3)0.5573 (2)0.17600 (14)0.0725 (7)
H2A0.19390.59760.20540.087*
H2B0.05920.54200.21470.087*
C30.0517 (2)0.71923 (18)0.13454 (14)0.0667 (6)
H3A0.03230.70340.16870.080*
H3B0.09880.76170.16750.080*
C40.0387 (2)0.78289 (18)0.05996 (14)0.0660 (6)
H4A0.12160.79120.02230.079*
H4B0.00490.85520.07640.079*
C50.1664 (2)0.28454 (19)0.08307 (17)0.0798 (7)
H5A0.24130.29540.03850.096*
H5B0.19230.24430.12730.096*
C60.0677 (3)0.22123 (19)0.05174 (16)0.0792 (7)
H6A0.01090.21780.09420.095*
H6B0.09750.14710.03820.095*
K21.00000.50000.50000.04676 (13)
O40.87844 (14)0.68677 (11)0.54243 (9)0.0610 (4)
O50.88938 (15)0.49569 (11)0.63909 (10)0.0642 (4)
O60.96197 (14)0.29703 (12)0.57341 (9)0.0652 (4)
C70.9274 (2)0.78738 (18)0.51938 (17)0.0750 (7)
H7A1.00990.80250.55570.090*
H7B0.86960.84670.52480.090*
C80.8588 (3)0.6873 (2)0.62403 (15)0.0764 (7)
H8A0.80240.74710.63070.092*
H8B0.93980.69760.66340.092*
C90.8005 (3)0.5808 (2)0.64055 (16)0.0782 (7)
H9A0.77820.58310.69440.094*
H9B0.72300.56770.59850.094*
C100.8448 (3)0.3918 (2)0.65819 (18)0.0887 (8)
H10A0.76740.37270.61780.106*
H10B0.82540.39330.71290.106*
C110.9475 (3)0.3091 (2)0.65616 (16)0.0869 (8)
H11A1.02760.33300.69150.104*
H11B0.92450.23930.67690.104*
C121.0591 (3)0.22063 (19)0.56826 (17)0.0800 (7)
H12A1.03740.14950.58740.096*
H12B1.13950.24390.60360.096*
Ag10.500367 (13)0.499637 (13)0.248517 (9)0.05610 (8)
C210.6722 (2)0.49601 (17)0.33232 (14)0.0588 (5)
N210.7650 (2)0.49337 (17)0.37783 (14)0.0831 (7)
C220.3267 (2)0.50320 (18)0.16431 (16)0.0654 (6)
N220.2365 (2)0.50640 (19)0.12121 (16)0.0963 (9)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
K10.0440 (3)0.0476 (3)0.0451 (3)0.0003 (3)0.0093 (2)0.0015 (3)
O10.0656 (9)0.0552 (9)0.0705 (10)0.0025 (7)0.0283 (8)0.0018 (7)
O20.0695 (9)0.0543 (8)0.0508 (8)0.0003 (7)0.0181 (7)0.0009 (6)
O30.0741 (10)0.0518 (8)0.0729 (10)0.0065 (7)0.0317 (8)0.0022 (7)
C10.0751 (16)0.0659 (14)0.0757 (16)0.0006 (13)0.0394 (13)0.0033 (12)
C20.103 (2)0.0656 (15)0.0579 (14)0.0013 (13)0.0366 (14)0.0002 (12)
C30.0828 (16)0.0579 (13)0.0626 (14)0.0033 (12)0.0230 (12)0.0114 (11)
C40.0729 (15)0.0504 (12)0.0797 (16)0.0047 (11)0.0277 (12)0.0015 (11)
C50.0930 (18)0.0609 (15)0.100 (2)0.0138 (13)0.0533 (16)0.0062 (13)
C60.108 (2)0.0495 (13)0.0936 (19)0.0028 (13)0.0521 (16)0.0066 (12)
K20.0444 (3)0.0488 (3)0.0455 (3)0.0039 (3)0.0066 (2)0.0038 (3)
O40.0704 (10)0.0538 (8)0.0602 (9)0.0060 (7)0.0178 (7)0.0017 (7)
O50.0704 (10)0.0610 (9)0.0660 (9)0.0056 (7)0.0252 (8)0.0072 (7)
O60.0708 (10)0.0587 (9)0.0703 (10)0.0040 (7)0.0244 (8)0.0040 (8)
C70.0849 (18)0.0506 (13)0.0956 (19)0.0047 (12)0.0332 (15)0.0010 (12)
C80.0980 (19)0.0673 (16)0.0694 (16)0.0134 (14)0.0302 (14)0.0050 (12)
C90.0825 (17)0.0835 (18)0.0790 (17)0.0190 (14)0.0405 (14)0.0073 (13)
C100.112 (2)0.0759 (18)0.096 (2)0.0054 (16)0.0616 (18)0.0045 (15)
C110.129 (2)0.0616 (15)0.0810 (18)0.0075 (15)0.0457 (17)0.0199 (13)
C120.098 (2)0.0578 (14)0.0926 (19)0.0149 (13)0.0392 (16)0.0210 (13)
Ag10.04966 (10)0.06099 (11)0.05425 (11)0.00154 (7)0.00420 (7)0.00099 (7)
C210.0578 (13)0.0603 (12)0.0574 (12)0.0024 (11)0.0109 (10)0.0008 (11)
N210.0660 (14)0.0974 (19)0.0774 (16)0.0071 (12)0.0024 (12)0.0021 (12)
C220.0622 (14)0.0683 (14)0.0640 (13)0.0026 (12)0.0100 (11)0.0084 (12)
N220.0753 (17)0.112 (2)0.0894 (19)0.0184 (14)0.0088 (14)0.0071 (14)
Geometric parameters (Å, º) top
K1—O32.8081 (14)K2—O62.8283 (14)
K1—O12.8142 (14)K2—N212.856 (2)
K1—O22.8203 (13)O4—C81.407 (3)
K1—N222.860 (2)O4—C71.421 (3)
O1—C51.412 (3)O5—C91.414 (3)
O1—C11.413 (2)O5—C101.416 (3)
O2—C21.412 (2)O6—C111.414 (3)
O2—C31.416 (2)O6—C121.415 (3)
O3—C41.411 (2)C7—C12ii1.487 (3)
O3—C6i1.416 (2)C7—H7A0.9700
C1—C21.497 (3)C7—H7B0.9700
C1—H1A0.9700C8—C91.494 (3)
C1—H1B0.9700C8—H8A0.9700
C2—H2A0.9700C8—H8B0.9700
C2—H2B0.9700C9—H9A0.9700
C3—C41.487 (3)C9—H9B0.9700
C3—H3A0.9700C10—C111.501 (3)
C3—H3B0.9700C10—H10A0.9700
C4—H4A0.9700C10—H10B0.9700
C4—H4B0.9700C11—H11A0.9700
C5—C61.492 (3)C11—H11B0.9700
C5—H5A0.9700C12—H12A0.9700
C5—H5B0.9700C12—H12B0.9700
C6—H6A0.9700Ag1—C212.043 (2)
C6—H6B0.9700Ag1—C222.061 (3)
K2—O42.7926 (13)C21—N211.106 (3)
K2—O52.8050 (15)C22—N221.066 (3)
O3—K1—O1i60.38 (4)O4—K2—N2179.18 (5)
O3—K1—O260.21 (4)O5—K2—N2196.27 (6)
O1—K1—O260.85 (4)O6—K2—N2195.08 (5)
O3—K1—N2299.16 (6)C8—O4—C7113.21 (18)
O1—K1—N2291.54 (6)C8—O4—K2114.82 (12)
O2—K1—N2288.78 (6)C7—O4—K2114.82 (12)
C5—O1—C1112.48 (17)C9—O5—C10113.20 (19)
C5—O1—K1113.39 (12)C9—O5—K2114.09 (13)
C1—O1—K1112.27 (12)C10—O5—K2115.03 (13)
C2—O2—C3112.90 (16)C11—O6—C12111.45 (19)
C2—O2—K1113.08 (12)C11—O6—K2112.23 (13)
C3—O2—K1111.94 (12)C12—O6—K2112.04 (12)
C4—O3—C6i114.00 (17)O4—C7—C12ii108.91 (19)
C4—O3—K1115.40 (12)O4—C7—H7A109.9
C6i—O3—K1114.06 (13)C12ii—C7—H7A109.9
O1—C1—C2108.91 (19)O4—C7—H7B109.9
O1—C1—H1A109.9C12ii—C7—H7B109.9
C2—C1—H1A109.9H7A—C7—H7B108.3
O1—C1—H1B109.9O4—C8—C9109.1 (2)
C2—C1—H1B109.9O4—C8—H8A109.9
H1A—C1—H1B108.3C9—C8—H8A109.9
O2—C2—C1108.98 (18)O4—C8—H8B109.9
O2—C2—H2A109.9C9—C8—H8B109.9
C1—C2—H2A109.9H8A—C8—H8B108.3
O2—C2—H2B109.9O5—C9—C8109.1 (2)
C1—C2—H2B109.9O5—C9—H9A109.9
H2A—C2—H2B108.3C8—C9—H9A109.9
O2—C3—C4109.28 (18)O5—C9—H9B109.9
O2—C3—H3A109.8C8—C9—H9B109.9
C4—C3—H3A109.8H9A—C9—H9B108.3
O2—C3—H3B109.8O5—C10—C11108.3 (2)
C4—C3—H3B109.8O5—C10—H10A110.0
H3A—C3—H3B108.3C11—C10—H10A110.0
O3—C4—C3108.21 (18)O5—C10—H10B110.0
O3—C4—H4A110.1C11—C10—H10B110.0
C3—C4—H4A110.1H10A—C10—H10B108.4
O3—C4—H4B110.1O6—C11—C10109.2 (2)
C3—C4—H4B110.1O6—C11—H11A109.8
H4A—C4—H4B108.4C10—C11—H11A109.8
O1—C5—C6109.1 (2)O6—C11—H11B109.8
O1—C5—H5A109.9C10—C11—H11B109.8
C6—C5—H5A109.9H11A—C11—H11B108.3
O1—C5—H5B109.9O6—C12—C7ii109.5 (2)
C6—C5—H5B109.9O6—C12—H12A109.8
H5A—C5—H5B108.3C7ii—C12—H12A109.8
O3i—C6—C5108.5 (2)O6—C12—H12B109.8
O3i—C6—H6A110.0C7ii—C12—H12B109.8
C5—C6—H6A110.0H12A—C12—H12B108.2
O3i—C6—H6B110.0C21—Ag1—C22179.80 (8)
C5—C6—H6B110.0N21—C21—Ag1179.5 (2)
H6A—C6—H6B108.4C21—N21—K2176.1 (2)
O4—K2—O560.37 (4)N22—C22—Ag1179.0 (3)
O4—K2—O6119.34 (4)C22—N22—K1175.6 (2)
O5—K2—O660.45 (4)
O3—K1—O1—C5162.04 (14)O6—K2—O4—C831.13 (16)
O2—K1—O1—C5148.35 (16)N21—K2—O4—C8120.90 (16)
N22—K1—O1—C560.60 (16)O5—K2—O4—C7151.03 (16)
O3—K1—O1—C133.19 (15)O6—K2—O4—C7164.95 (14)
O2—K1—O1—C119.49 (14)N21—K2—O4—C7105.28 (15)
N22—K1—O1—C168.25 (15)O4—K2—O5—C917.47 (15)
O3—K1—O2—C2150.13 (15)O6—K2—O5—C9148.58 (17)
O1—K1—O2—C216.15 (14)N21—K2—O5—C956.28 (16)
N22—K1—O2—C2108.59 (15)O4—K2—O5—C10150.72 (18)
O3—K1—O2—C321.25 (13)O6—K2—O5—C1015.33 (16)
O1—K1—O2—C3145.04 (14)N21—K2—O5—C1076.97 (18)
N22—K1—O2—C3122.52 (14)O4—K2—O6—C1134.02 (16)
O1—K1—O3—C427.74 (15)O5—K2—O6—C1120.11 (15)
O2—K1—O3—C413.96 (13)N21—K2—O6—C11114.45 (16)
N22—K1—O3—C469.32 (15)O4—K2—O6—C12160.29 (15)
O1—K1—O3—C6i162.57 (14)O5—K2—O6—C12146.38 (17)
O2—K1—O3—C6i148.79 (16)N21—K2—O6—C12119.28 (16)
N22—K1—O3—C6i65.52 (16)C8—O4—C7—C12ii178.33 (19)
C5—O1—C1—C2178.3 (2)K2—O4—C7—C12ii47.1 (2)
K1—O1—C1—C252.3 (2)C7—O4—C8—C9176.8 (2)
C3—O2—C2—C1177.25 (19)K2—O4—C8—C948.7 (2)
K1—O2—C2—C148.9 (2)C10—O5—C9—C8177.1 (2)
O1—C1—C2—O269.4 (3)K2—O5—C9—C848.8 (2)
C2—O2—C3—C4176.90 (19)O4—C8—C9—O565.5 (3)
K1—O2—C3—C454.1 (2)C9—O5—C10—C11179.0 (2)
C6i—O3—C4—C3179.1 (2)K2—O5—C10—C1147.3 (3)
K1—O3—C4—C346.0 (2)C12—O6—C11—C10179.3 (2)
O2—C3—C4—O367.8 (2)K2—O6—C11—C1052.7 (2)
C1—O1—C5—C6179.2 (2)O5—C10—C11—O667.8 (3)
K1—O1—C5—C650.5 (2)C11—O6—C12—C7ii178.8 (2)
O1—C5—C6—O3i67.7 (3)K2—O6—C12—C7ii52.1 (2)
O5—K2—O4—C817.20 (14)
Symmetry codes: (i) x, y+1, z; (ii) x+2, y+1, z+1.

Experimental details

Crystal data
Chemical formulaK[Ag(CN)2](C12H24O6)
Mr463.32
Crystal system, space groupMonoclinic, P21/n
Temperature (K)298
a, b, c (Å)10.7189 (5), 12.2191 (5), 16.4816 (7)
β (°) 102.795 (2)
V3)2105.08 (16)
Z4
Radiation typeMo Kα
µ (mm1)1.18
Crystal size (mm)0.50 × 0.44 × 0.40
Data collection
DiffractometerSiemens SMART CCD area-detector
diffractometer
Absorption correctionIntegration
(Sheldrick, 2001)
Tmin, Tmax0.604, 0.694
No. of measured, independent and
observed [I > 2σ(I)] reflections
26868, 6428, 3178
Rint0.031
(sin θ/λ)max1)0.714
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.026, 0.086, 1.03
No. of reflections6428
No. of parameters221
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.28, 0.19

Computer programs: SMART (Siemens, 1995), SAINT (Bruker, 2001), SHELXTL (Sheldrick, 2001).

Selected geometric parameters (Å, º) top
K1—O32.8081 (14)K2—O62.8283 (14)
K1—O12.8142 (14)K2—N212.856 (2)
K1—O22.8203 (13)Ag1—C212.043 (2)
K1—N222.860 (2)Ag1—C222.061 (3)
K2—O42.7926 (13)C21—N211.106 (3)
K2—O52.8050 (15)C22—N221.066 (3)
O3—K1—N2299.16 (6)C21—Ag1—C22179.80 (8)
O1—K1—N2291.54 (6)N21—C21—Ag1179.5 (2)
O2—K1—N2288.78 (6)C21—N21—K2176.1 (2)
O4—K2—N2179.18 (5)N22—C22—Ag1179.0 (3)
O5—K2—N2196.27 (6)C22—N22—K1175.6 (2)
O6—K2—N2195.08 (5)
 

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