Buy article online - an online subscription or single-article purchase is required to access this article.
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
CCDC reference: 189302
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (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
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
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)]NO3 | F(000) = 752 |
Mr = 380.12 | Dx = 1.825 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 25 reflections |
a = 15.053 (1) Å | θ = 4.7–10.0° |
b = 13.703 (1) Å | µ = 1.47 mm−1 |
c = 6.772 (1) Å | T = 293 K |
β = 97.93 (1)° | Block, yellow |
V = 1383.5 (2) Å3 | 0.3 × 0.2 × 0.2 mm |
Z = 4 | |
Data collection top
Bruker P4 diffractometer | 1064 reflections with I > 2σ(I) |
Radiation source: sealed tube | Rint = 0.020 |
Graphite monochromator | θmax = 25.0°, θmin = 2.0° |
2θ/ω scans | h = −1→17 |
Absorption correction: empirical (using intensity measurements) (Sheldrick, 1990) | k = −1→16 |
Tmin = 0.709, Tmax = 0.745 | l = −8→8 |
1490 measured reflections | 3 standard reflections every 97 reflections |
1214 independent reflections | intensity decay: 8.1% |
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)] = 0.045 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.145 | H-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 parameters | Δρmax = 1.56 e Å−3 |
0 restraints | Δρmin = −1.31 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 | x | y | z | Uiso*/Ueq | Occ. (<1) |
Ag1 | 0.5000 | 0.38478 (5) | 0.2500 | 0.0543 (3) | |
N1 | 0.3562 (3) | 0.3769 (3) | 0.1504 (7) | 0.0430 (10) | |
N2 | 0.0469 (4) | 0.4089 (5) | −0.2282 (10) | 0.0664 (16) | |
C1 | 0.2970 (4) | 0.3386 (5) | 0.2564 (9) | 0.0528 (14) | |
H1A | 0.3183 | 0.3105 | 0.3788 | 0.063* | |
C2 | 0.2057 (4) | 0.3380 (5) | 0.1955 (9) | 0.0531 (14) | |
H2A | 0.1670 | 0.3108 | 0.2762 | 0.064* | |
C3 | 0.1723 (4) | 0.3785 (4) | 0.0127 (9) | 0.0450 (13) | |
C4 | 0.2341 (4) | 0.4181 (5) | −0.0979 (9) | 0.0499 (13) | |
H4A | 0.2147 | 0.4459 | −0.2216 | 0.060* | |
C5 | 0.3234 (4) | 0.4165 (4) | −0.0264 (9) | 0.0488 (13) | |
H5A | 0.3634 | 0.4440 | −0.1034 | 0.059* | |
C6 | 0.0759 (4) | 0.3805 (4) | −0.0559 (10) | 0.0500 (14) | |
H6A | 0.0359 | 0.3605 | 0.0291 | 0.060* | |
N3 | 1.0000 | 0.1528 (11) | 0.2500 | 0.087 (2) | |
O1 | 0.9721 (8) | 0.0724 (8) | 0.1412 (16) | 0.075 (3) | 0.50 |
O2 | 0.9708 (8) | 0.2349 (9) | 0.1584 (19) | 0.089 (3) | 0.50 |
O3 | 0.9417 (8) | 0.1541 (13) | 0.1121 (16) | 0.087 (2) | 0.50 |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ag1 | 0.0241 (4) | 0.0764 (5) | 0.0579 (5) | 0.000 | −0.0103 (3) | 0.000 |
N1 | 0.026 (2) | 0.050 (3) | 0.049 (3) | −0.0008 (17) | −0.0071 (19) | 0.0021 (18) |
N2 | 0.023 (3) | 0.100 (4) | 0.071 (4) | −0.006 (3) | −0.010 (2) | 0.002 (3) |
C1 | 0.038 (3) | 0.064 (4) | 0.054 (3) | −0.002 (3) | −0.004 (2) | 0.015 (3) |
C2 | 0.034 (3) | 0.068 (4) | 0.056 (3) | −0.007 (3) | −0.001 (2) | 0.019 (3) |
C3 | 0.027 (3) | 0.048 (3) | 0.056 (3) | −0.002 (2) | −0.007 (2) | 0.000 (2) |
C4 | 0.031 (3) | 0.062 (3) | 0.052 (3) | −0.003 (3) | −0.009 (2) | 0.010 (3) |
C5 | 0.030 (3) | 0.058 (3) | 0.056 (3) | −0.004 (2) | −0.005 (2) | 0.008 (3) |
C6 | 0.023 (3) | 0.060 (3) | 0.063 (4) | 0.000 (2) | −0.007 (3) | −0.001 (3) |
N3 | 0.049 (4) | 0.155 (8) | 0.058 (4) | 0.000 | 0.013 (3) | 0.000 |
O1 | 0.084 (8) | 0.067 (6) | 0.077 (6) | −0.020 (6) | 0.019 (6) | −0.012 (5) |
O2 | 0.082 (8) | 0.083 (8) | 0.105 (9) | 0.005 (7) | 0.018 (6) | 0.017 (6) |
O3 | 0.049 (4) | 0.155 (8) | 0.058 (4) | 0.000 | 0.013 (3) | 0.000 |
Geometric parameters (Å, º) top
Ag1—N1 | 2.180 (5) | C4—H4A | 0.9300 |
Ag1—N1i | 2.180 (5) | C5—H5A | 0.9300 |
N1—C1 | 1.327 (8) | C6—H6A | 0.9300 |
N1—C5 | 1.345 (8) | N3—O3 | 1.190 (12) |
N2—C6 | 1.250 (9) | N3—O3iii | 1.190 (12) |
N2—N2ii | 1.403 (11) | N3—O2iii | 1.330 (16) |
C1—C2 | 1.379 (8) | N3—O2 | 1.330 (16) |
C1—H1A | 0.9300 | N3—O1 | 1.359 (16) |
C2—C3 | 1.386 (8) | N3—O1iii | 1.359 (16) |
C2—H2A | 0.9300 | O1—O3 | 1.215 (19) |
C3—C4 | 1.383 (9) | O1—O1iii | 1.59 (2) |
C3—C6 | 1.462 (8) | O2—O3 | 1.216 (19) |
C4—C5 | 1.365 (8) | O2—O2iii | 1.42 (3) |
| | | |
N1—Ag1—N1i | 174.3 (2) | O3—N3—O2iii | 120.9 (17) |
C1—N1—C5 | 116.7 (5) | O3iii—N3—O2iii | 57.4 (10) |
C1—N1—Ag1 | 124.4 (4) | O3—N3—O2 | 57.4 (10) |
C5—N1—Ag1 | 118.8 (4) | O3iii—N3—O2 | 120.9 (17) |
C6—N2—N2ii | 114.1 (7) | O2iii—N3—O2 | 64.4 (14) |
N1—C1—C2 | 123.8 (5) | O3—N3—O1 | 56.5 (10) |
N1—C1—H1A | 118.1 | O3iii—N3—O1 | 125.2 (17) |
C2—C1—H1A | 118.1 | O2iii—N3—O1 | 174.9 (10) |
C1—C2—C3 | 119.2 (5) | O2—N3—O1 | 112.1 (8) |
C1—C2—H2A | 120.4 | O3—N3—O1iii | 125.2 (17) |
C3—C2—H2A | 120.4 | O3iii—N3—O1iii | 56.5 (10) |
C4—C3—C2 | 116.9 (5) | O2iii—N3—O1iii | 112.1 (8) |
C4—C3—C6 | 122.2 (5) | O2—N3—O1iii | 174.9 (10) |
C2—C3—C6 | 120.9 (5) | O1—N3—O1iii | 71.7 (14) |
C5—C4—C3 | 120.3 (5) | O3—O1—N3 | 54.7 (8) |
C5—C4—H4A | 119.8 | O3—O1—O1iii | 106.8 (8) |
C3—C4—H4A | 119.8 | N3—O1—O1iii | 54.1 (7) |
N1—C5—C4 | 123.0 (5) | O3—O2—N3 | 55.5 (8) |
N1—C5—H5A | 118.5 | O3—O2—O2iii | 112.5 (9) |
C4—C5—H5A | 118.5 | N3—O2—O2iii | 57.8 (7) |
N2—C6—C3 | 120.4 (6) | N3—O3—O1 | 68.8 (11) |
N2—C6—H6A | 119.8 | N3—O3—O2 | 67.1 (12) |
C3—C6—H6A | 119.8 | O1—O3—O2 | 133.1 (13) |
O3—N3—O3iii | 178 (2) | | |
Symmetry codes: (i) −x+1, y, −z+1/2; (ii) −x, y, −z−1/2; (iii) −x+2, y, −z+1/2. |
Subscribe to Acta Crystallographica Section E: Crystallographic Communications
The full text of this article is available to subscribers to the journal.
If you have already registered and are using a computer listed in your registration details, please email
support@iucr.org for assistance.