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The bipyridyl-base ligand 1,4-bis(4-pyridyl)-2,3-di­aza-1,3-buta­diene (L) has been used in the synthesis of a new organomet­allic polymer. The reaction between AgNO3 and L afforded a one-dimensional chain structure of the cation of the title compound, {[Ag(C12N4H10)]NO3}n. The AgI ion lies on a twofold axis and is in a linear environment with respect to the two terminal N atoms of pyridyl rings. Weak interactions between H and nitrate O atoms, and between the Ag and nitrate O atoms, generate a three-dimensional framework.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802008681/ob6132sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536802008681/ob6132Isup2.hkl
Contains datablock I

CCDC reference: 189302

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.009 Å
  • Disorder in solvent or counterion
  • R factor = 0.045
  • wR factor = 0.145
  • Data-to-parameter ratio = 11.7

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


Yellow Alert Alert Level C:
PLAT_302 Alert C Anion/Solvent Disorder ....................... 43.00 Perc.
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
1 Alert Level C = Please check

Computing details top

Data collection: XSCANS (Bruker, 1997); cell refinement: XSCANS; data reduction: SHELXTL (Bruker, 1997); program(s) used to solve structure: SHELXTL; program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

catena-Poly[[[1,4-bis(4-pyridyl)-2,3-diaza-1,3-butadiene]silver(I)] nitrate] top
Crystal data top
[Ag(C12H10N4)]NO3F(000) = 752
Mr = 380.12Dx = 1.825 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 25 reflections
a = 15.053 (1) Åθ = 4.7–10.0°
b = 13.703 (1) ŵ = 1.47 mm1
c = 6.772 (1) ÅT = 293 K
β = 97.93 (1)°Block, yellow
V = 1383.5 (2) Å30.3 × 0.2 × 0.2 mm
Z = 4
Data collection top
Bruker P4
diffractometer
1064 reflections with I > 2σ(I)
Radiation source: sealed tubeRint = 0.020
Graphite monochromatorθmax = 25.0°, θmin = 2.0°
2θ/ω scansh = 117
Absorption correction: empirical (using intensity measurements)
(Sheldrick, 1990)
k = 116
Tmin = 0.709, Tmax = 0.745l = 88
1490 measured reflections3 standard reflections every 97 reflections
1214 independent reflections intensity decay: 8.1%
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)] = 0.045Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.145H-atom parameters constrained
S = 1.07 w = 1/[σ2(Fo2) + (0.1P)2 + 1.99P]
where P = (Fo2 + 2Fc2)/3
1214 reflections(Δ/σ)max < 0.001
104 parametersΔρmax = 1.56 e Å3
0 restraintsΔρmin = 1.31 e Å3
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*/UeqOcc. (<1)
Ag10.50000.38478 (5)0.25000.0543 (3)
N10.3562 (3)0.3769 (3)0.1504 (7)0.0430 (10)
N20.0469 (4)0.4089 (5)0.2282 (10)0.0664 (16)
C10.2970 (4)0.3386 (5)0.2564 (9)0.0528 (14)
H1A0.31830.31050.37880.063*
C20.2057 (4)0.3380 (5)0.1955 (9)0.0531 (14)
H2A0.16700.31080.27620.064*
C30.1723 (4)0.3785 (4)0.0127 (9)0.0450 (13)
C40.2341 (4)0.4181 (5)0.0979 (9)0.0499 (13)
H4A0.21470.44590.22160.060*
C50.3234 (4)0.4165 (4)0.0264 (9)0.0488 (13)
H5A0.36340.44400.10340.059*
C60.0759 (4)0.3805 (4)0.0559 (10)0.0500 (14)
H6A0.03590.36050.02910.060*
N31.00000.1528 (11)0.25000.087 (2)
O10.9721 (8)0.0724 (8)0.1412 (16)0.075 (3)0.50
O20.9708 (8)0.2349 (9)0.1584 (19)0.089 (3)0.50
O30.9417 (8)0.1541 (13)0.1121 (16)0.087 (2)0.50
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ag10.0241 (4)0.0764 (5)0.0579 (5)0.0000.0103 (3)0.000
N10.026 (2)0.050 (3)0.049 (3)0.0008 (17)0.0071 (19)0.0021 (18)
N20.023 (3)0.100 (4)0.071 (4)0.006 (3)0.010 (2)0.002 (3)
C10.038 (3)0.064 (4)0.054 (3)0.002 (3)0.004 (2)0.015 (3)
C20.034 (3)0.068 (4)0.056 (3)0.007 (3)0.001 (2)0.019 (3)
C30.027 (3)0.048 (3)0.056 (3)0.002 (2)0.007 (2)0.000 (2)
C40.031 (3)0.062 (3)0.052 (3)0.003 (3)0.009 (2)0.010 (3)
C50.030 (3)0.058 (3)0.056 (3)0.004 (2)0.005 (2)0.008 (3)
C60.023 (3)0.060 (3)0.063 (4)0.000 (2)0.007 (3)0.001 (3)
N30.049 (4)0.155 (8)0.058 (4)0.0000.013 (3)0.000
O10.084 (8)0.067 (6)0.077 (6)0.020 (6)0.019 (6)0.012 (5)
O20.082 (8)0.083 (8)0.105 (9)0.005 (7)0.018 (6)0.017 (6)
O30.049 (4)0.155 (8)0.058 (4)0.0000.013 (3)0.000
Geometric parameters (Å, º) top
Ag1—N12.180 (5)C4—H4A0.9300
Ag1—N1i2.180 (5)C5—H5A0.9300
N1—C11.327 (8)C6—H6A0.9300
N1—C51.345 (8)N3—O31.190 (12)
N2—C61.250 (9)N3—O3iii1.190 (12)
N2—N2ii1.403 (11)N3—O2iii1.330 (16)
C1—C21.379 (8)N3—O21.330 (16)
C1—H1A0.9300N3—O11.359 (16)
C2—C31.386 (8)N3—O1iii1.359 (16)
C2—H2A0.9300O1—O31.215 (19)
C3—C41.383 (9)O1—O1iii1.59 (2)
C3—C61.462 (8)O2—O31.216 (19)
C4—C51.365 (8)O2—O2iii1.42 (3)
N1—Ag1—N1i174.3 (2)O3—N3—O2iii120.9 (17)
C1—N1—C5116.7 (5)O3iii—N3—O2iii57.4 (10)
C1—N1—Ag1124.4 (4)O3—N3—O257.4 (10)
C5—N1—Ag1118.8 (4)O3iii—N3—O2120.9 (17)
C6—N2—N2ii114.1 (7)O2iii—N3—O264.4 (14)
N1—C1—C2123.8 (5)O3—N3—O156.5 (10)
N1—C1—H1A118.1O3iii—N3—O1125.2 (17)
C2—C1—H1A118.1O2iii—N3—O1174.9 (10)
C1—C2—C3119.2 (5)O2—N3—O1112.1 (8)
C1—C2—H2A120.4O3—N3—O1iii125.2 (17)
C3—C2—H2A120.4O3iii—N3—O1iii56.5 (10)
C4—C3—C2116.9 (5)O2iii—N3—O1iii112.1 (8)
C4—C3—C6122.2 (5)O2—N3—O1iii174.9 (10)
C2—C3—C6120.9 (5)O1—N3—O1iii71.7 (14)
C5—C4—C3120.3 (5)O3—O1—N354.7 (8)
C5—C4—H4A119.8O3—O1—O1iii106.8 (8)
C3—C4—H4A119.8N3—O1—O1iii54.1 (7)
N1—C5—C4123.0 (5)O3—O2—N355.5 (8)
N1—C5—H5A118.5O3—O2—O2iii112.5 (9)
C4—C5—H5A118.5N3—O2—O2iii57.8 (7)
N2—C6—C3120.4 (6)N3—O3—O168.8 (11)
N2—C6—H6A119.8N3—O3—O267.1 (12)
C3—C6—H6A119.8O1—O3—O2133.1 (13)
O3—N3—O3iii178 (2)
Symmetry codes: (i) x+1, y, z+1/2; (ii) x, y, z1/2; (iii) x+2, y, z+1/2.
 

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