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The structure of the title compound, [Cu(C
6H
7N)
2{Ag(CN)
2}
2]
n, is made up of neutral zigzag chains of [–NC–Ag–CN–Cu(4-Mepy)
2{Ag(CN)
2}–NC–Ag–CN–] (4-Mepy is 4-methylpyridine). Neighbouring chains are linked by weak argentophilic interactions, with Ag
Ag distances of 3.2322 (12) Å. The Cu atom, which lies on a twofold rotation axis, is pentacoordinated by one monodentate Ag(CN)
2− anion [Cu—N 1.985 (3) Å], the atoms of which lie on the same rotation axis, and by bridging dicyanoargentate anions [2 × Cu—N 2.0827 (19) Å], with Ag atoms on inversion centres. The coordination polyhedron is completed by two 4-Mepy molecules [2 × Cu—N 2.038 (2) Å], which occupy the axial positions of a distorted trigonal bipyramid.
Supporting information
CCDC reference: 184472
Data collection: EXPOSE in IPDS (Stoe & Cie, 1999); cell refinement: CELL in IPDS; data reduction: INTEGRATE in IPDS; program(s) used to solve structure: SHELXS86 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 1999); software used to prepare material for publication: SHELXL97.
Poly[[bis(4-methylpyridine-
κN)copper(II)]-bis-µ-[[dicyanoargentate(I)-
κ2N:
N']]
top
Crystal data top
[Ag2Cu(CN)4(C6H7N)2] | F(000) = 1100 |
Mr = 569.61 | Dx = 1.982 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
a = 11.752 (3) Å | Cell parameters from 6639 reflections |
b = 17.795 (3) Å | θ = 1.7–26.1° |
c = 9.594 (3) Å | µ = 3.15 mm−1 |
β = 107.95 (3)° | T = 220 K |
V = 1908.7 (8) Å3 | Prism, pale blue |
Z = 4 | 0.18 × 0.12 × 0.05 mm |
Data collection top
Stoe IPDS diffractometer | 1835 independent reflections |
Radiation source: fine-focus sealed tube | 1591 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.033 |
φ scans | θmax = 25.8°, θmin = 2.1° |
Absorption correction: numerical Please provide reference | h = −14→14 |
Tmin = 0.674, Tmax = 0.859 | k = −21→21 |
6594 measured reflections | l = −11→11 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.019 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.049 | H-atom parameters constrained |
S = 1.01 | w = 1/[σ2(Fo2) + (0.031P)2 + 0.277P] where P = (Fo2 + 2Fc2)/3 |
1835 reflections | (Δ/σ)max = 0.001 |
119 parameters | Δρmax = 0.27 e Å−3 |
0 restraints | Δρmin = −0.52 e Å−3 |
Special details top
Experimental. _diffrn_measurement_method D = 70 mm, φ 0–199.5°, Δφ 1.5°, 5 min/rec |
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 | x | y | z | Uiso*/Ueq | |
Ag2 | 0.5000 | 0.714195 (14) | 0.2500 | 0.02997 (9) | |
Cu1 | 0.5000 | 0.42233 (2) | 0.2500 | 0.01632 (10) | |
Ag1 | 0.7500 | 0.2500 | 0.0000 | 0.03079 (9) | |
N1 | 0.60216 (17) | 0.35189 (11) | 0.1625 (2) | 0.0232 (4) | |
C1 | 0.6558 (2) | 0.31594 (13) | 0.1054 (3) | 0.0243 (5) | |
N2 | 0.5000 | 0.53387 (17) | 0.2500 | 0.0248 (6) | |
C2 | 0.5000 | 0.59826 (19) | 0.2500 | 0.0248 (7) | |
N3 | 0.5000 | 0.89354 (18) | 0.2500 | 0.0526 (11) | |
C3 | 0.5000 | 0.8297 (2) | 0.2500 | 0.0365 (9) | |
N10 | 0.36819 (17) | 0.42009 (10) | 0.0536 (2) | 0.0206 (4) | |
C11 | 0.3307 (2) | 0.35279 (13) | −0.0070 (3) | 0.0256 (5) | |
H11 | 0.3654 | 0.3096 | 0.0429 | 0.031* | |
C12 | 0.2437 (2) | 0.34528 (15) | −0.1389 (3) | 0.0297 (6) | |
H12 | 0.2204 | 0.2976 | −0.1767 | 0.036* | |
C13 | 0.1897 (2) | 0.40831 (16) | −0.2169 (3) | 0.0291 (6) | |
C14 | 0.2285 (2) | 0.47735 (15) | −0.1537 (3) | 0.0320 (6) | |
H14 | 0.1947 | 0.5213 | −0.2010 | 0.038* | |
C15 | 0.3165 (2) | 0.48088 (14) | −0.0213 (3) | 0.0281 (5) | |
H15 | 0.3416 | 0.5280 | 0.0184 | 0.034* | |
C16 | 0.0963 (2) | 0.40301 (19) | −0.3636 (3) | 0.0437 (7) | |
H16A | 0.0519 | 0.3573 | −0.3690 | 0.052* | |
H16B | 0.1341 | 0.4033 | −0.4392 | 0.052* | |
H16C | 0.0430 | 0.4451 | −0.3766 | 0.052* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ag2 | 0.03663 (16) | 0.01458 (13) | 0.03291 (17) | 0.000 | 0.00222 (11) | 0.000 |
Cu1 | 0.02032 (19) | 0.01236 (18) | 0.0166 (2) | 0.000 | 0.00621 (15) | 0.000 |
Ag1 | 0.03842 (16) | 0.03343 (16) | 0.02601 (16) | 0.01822 (11) | 0.01801 (12) | 0.00097 (12) |
N1 | 0.0261 (10) | 0.0250 (10) | 0.0204 (10) | 0.0061 (8) | 0.0099 (8) | −0.0003 (9) |
C1 | 0.0269 (12) | 0.0275 (13) | 0.0184 (12) | 0.0066 (10) | 0.0069 (10) | 0.0026 (10) |
N2 | 0.0309 (14) | 0.0209 (15) | 0.0202 (14) | 0.000 | 0.0045 (11) | 0.000 |
C2 | 0.0310 (18) | 0.0185 (18) | 0.0232 (19) | 0.000 | 0.0057 (14) | 0.000 |
N3 | 0.060 (2) | 0.0199 (18) | 0.057 (3) | 0.000 | −0.0131 (19) | 0.000 |
C3 | 0.037 (2) | 0.0231 (19) | 0.036 (2) | 0.000 | −0.0076 (16) | 0.000 |
N10 | 0.0235 (9) | 0.0193 (9) | 0.0194 (10) | −0.0008 (7) | 0.0072 (8) | −0.0009 (8) |
C11 | 0.0329 (13) | 0.0198 (11) | 0.0243 (13) | −0.0032 (9) | 0.0090 (10) | 0.0009 (10) |
C12 | 0.0327 (13) | 0.0295 (13) | 0.0263 (14) | −0.0099 (10) | 0.0083 (11) | −0.0068 (11) |
C13 | 0.0213 (12) | 0.0431 (15) | 0.0236 (14) | −0.0008 (10) | 0.0078 (10) | −0.0024 (11) |
C14 | 0.0313 (12) | 0.0303 (14) | 0.0300 (14) | 0.0075 (10) | 0.0029 (10) | 0.0036 (11) |
C15 | 0.0298 (12) | 0.0222 (12) | 0.0283 (13) | 0.0036 (9) | 0.0029 (10) | −0.0006 (10) |
C16 | 0.0353 (15) | 0.061 (2) | 0.0279 (16) | −0.0008 (13) | 0.0004 (12) | −0.0023 (14) |
Geometric parameters (Å, º) top
Ag2—C3 | 2.055 (4) | N3—C3 | 1.137 (5) |
Ag2—C2 | 2.063 (3) | N10—C15 | 1.337 (3) |
Ag2—Ag1i | 3.2322 (13) | N10—C11 | 1.345 (3) |
Ag2—Ag1ii | 3.2322 (13) | C11—C12 | 1.367 (4) |
Cu1—N2 | 1.985 (3) | C11—H11 | 0.9300 |
Cu1—N10 | 2.038 (2) | C12—C13 | 1.388 (4) |
Cu1—N10iii | 2.038 (2) | C12—H12 | 0.9300 |
Cu1—N1iii | 2.0827 (19) | C13—C14 | 1.384 (4) |
Cu1—N1 | 2.0827 (19) | C13—C16 | 1.497 (4) |
Ag1—C1iv | 2.077 (2) | C14—C15 | 1.370 (4) |
Ag1—C1 | 2.077 (2) | C14—H14 | 0.9300 |
Ag1—Ag2v | 3.2322 (12) | C15—H15 | 0.9300 |
Ag1—Ag2vi | 3.2322 (12) | C16—H16A | 0.9600 |
N1—C1 | 1.149 (3) | C16—H16B | 0.9600 |
N2—C2 | 1.146 (5) | C16—H16C | 0.9600 |
| | | |
C3—Ag2—C2 | 180.0 | N3—C3—Ag2 | 180.0 |
C3—Ag2—Ag1i | 78.631 (6) | C15—N10—C11 | 117.0 (2) |
C2—Ag2—Ag1i | 101.369 (6) | C15—N10—Cu1 | 124.86 (16) |
C3—Ag2—Ag1ii | 78.631 (6) | C11—N10—Cu1 | 118.13 (16) |
C2—Ag2—Ag1ii | 101.369 (6) | N10—C11—C12 | 122.6 (2) |
Ag1i—Ag2—Ag1ii | 157.262 (13) | N10—C11—H11 | 118.7 |
N2—Cu1—N10 | 91.12 (5) | C12—C11—H11 | 118.7 |
N2—Cu1—N10iii | 91.12 (5) | C11—C12—C13 | 120.5 (2) |
N10—Cu1—N10iii | 177.76 (11) | C11—C12—H12 | 119.8 |
N2—Cu1—N1iii | 127.00 (6) | C13—C12—H12 | 119.8 |
N10—Cu1—N1iii | 89.57 (8) | C14—C13—C12 | 116.6 (2) |
N10iii—Cu1—N1iii | 89.09 (8) | C14—C13—C16 | 121.0 (3) |
N2—Cu1—N1 | 127.00 (6) | C12—C13—C16 | 122.4 (3) |
N10—Cu1—N1 | 89.09 (8) | C15—C14—C13 | 120.0 (2) |
N10iii—Cu1—N1 | 89.57 (8) | C15—C14—H14 | 120.0 |
N1iii—Cu1—N1 | 106.00 (11) | C13—C14—H14 | 120.0 |
C1iv—Ag1—C1 | 180.0 | N10—C15—C14 | 123.3 (2) |
C1iv—Ag1—Ag2v | 75.58 (7) | N10—C15—H15 | 118.3 |
C1—Ag1—Ag2v | 104.42 (7) | C14—C15—H15 | 118.3 |
C1iv—Ag1—Ag2vi | 104.42 (7) | C13—C16—H16A | 109.5 |
C1—Ag1—Ag2vi | 75.58 (7) | C13—C16—H16B | 109.5 |
Ag2v—Ag1—Ag2vi | 180.0 | H16A—C16—H16B | 109.5 |
C1—N1—Cu1 | 175.2 (2) | C13—C16—H16C | 109.5 |
N1—C1—Ag1 | 179.0 (2) | H16A—C16—H16C | 109.5 |
C2—N2—Cu1 | 180.0 | H16B—C16—H16C | 109.5 |
N2—C2—Ag2 | 180.0 | | |
Symmetry codes: (i) −x+3/2, y+1/2, −z+1/2; (ii) x−1/2, y+1/2, z; (iii) −x+1, y, −z+1/2; (iv) −x+3/2, −y+1/2, −z; (v) x+1/2, y−1/2, z; (vi) −x+1, −y+1, −z. |
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