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The title compound, poly[[[mu]4-5-carb­oxy-4-carboxyl­ato-2-(pyri­din-4-yl)-1H-imidazol-1-ido]disilver(I)], [Ag2(C10H5N3O4)]n, was synthesized by reacting silver nitrate with 2-(pyridin-4-yl)-1H-imidazole-4,5-dicarb­oxy­lic acid (H3PyIDC) under hydro­thermal conditions. The asymmetric unit contains two crystallographically independent AgI cations and one unique HPyIDC2- anion. Both AgI cations are three-coordinated in distorted T-shaped coordination geometries. One AgI cation is coordinated by one N and two O atoms from two HPyIDC2- anions, while the other is bonded to one O and two N atoms from two HPyIDC2- anions. It is inter­esting to note that the HPyIDC2- group acts as a [mu]4-bridging ligand to link the AgI cations into a three-dimensional framework, which can be simplified as a diamondoid topology. The thermal stability and photoluminescent properties of the title compound have also been studied.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270113006768/sf3194sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270113006768/sf3194Isup2.hkl
Contains datablock I

CCDC reference: 950346

Comment top

Recently, 1H-imidazole-4,5-dicarboxylic acid (H3IDC), an N-heterocyclic carboxylic acid ligand, has attracted significant attention in the construction of interesting metal–organic frameworks (MOFs) due to its versatile coordination modes under hydro(solvo)thermal conditions (Fang & Zhang, 2006; Li, Zheng et al., 2012; Lu et al., 2012; Wang et al., 2010; Zhang et al., 2006; Zhao et al., 2007). Most recently, a series of functionalized H3IDC ligands have been prepared by introducing diverse substituent groups, such as methyl (Gao et al., 2011; Li, Luo et al., 2012; Song et al., 2010), ethyl (Gu et al., 2011; Li, Guo et al., 2009; Wang et al., 2008; Zhang et al., 2011) and propyl (Fan et al., 2012; Li et al., 2011; Wang et al., 2011; Zeng et al., 2011) groups, on the 2-position of the imidazole ring. Many novel MOFs with intriguing structural topologies and useful properties based on these ligands have been successfully synthesized, and it has been discovered that the different substituent groups may have different spatial effects on neighbouring carboxylate groups, which give rise to their various coordination modes.

Compared with the well studied H3IDC ligand and its 2-position aliphatic hydrocarbon-substituted derivatives, the ligand 2-(pyridin-4-yl)-1H-imidazole-4,5-dicarboxylic acid (H3PyIDC), an imidazole-4,5-dicarboxylate ligand bearing an aromatic pyridinyl group on the 2-position, remains largely unexplored (Jing et al., 2010; Li, Wu et al., 2009; Yuan et al., 2012). H3PyIDC contains the H3IDC building block and can be successively deprotonated to produce the H2PyIDC-, HPyIDC2- and PyIDC3- species under certain conditions. The additional pyridinyl group in the backbone of H3PyIDC can rotate freely about the C—C bond to meet the different coordination requirements of metal atoms, thus increasing the dimensionality of the final structures.

On the basis of the aforementioned points, we consider H3PyIDC to be an ideal multidentate organic ligand for constructing new three-dimensional MOFs. As expected, the title three-dimensional silver(I) coordination framework, poly[[µ4-5-carboxy-4-carboxylato-2-(pyridin-4-yl)-1H-imidazol-1-ido]disilver(I)], [Ag2(HPyIDC)]n, (I), was successfully synthesized by reacting silver nitrate with H3PyIDC under hydrothermal conditions. The as-synthesized sample was characterized by single-crystal X-ray diffraction, elemental analysis and IR spectroscopy. The thermal stability and photoluminescent properties of (I) have also been investigated.

Compound (I) crystallizes in the noncentrosymmetric monoclinic space group Cc, and the asymmetric unit comprises two crystallographically independent AgI cations and one unique HPyIDC2- anion. As shown in Fig. 1, atoms Ag1 and Ag2 are both three-coordinated in distorted T-shaped coordination geometries. Atom Ag1 is coordinated by one imidazole N and two carboxylate O atoms from two different HPyIDC2- anions, while atom Ag2 is bonded to one carboxylate O atom and two imidazole N atoms from two individual HPyIDC2- anions. The Ag—N bond lengths are in the range 2.130 (5)–2.169 (4) Å and the Ag—O bond distances vary from 2.151 (4) to 2.577 (4) Å, all of which are comparable with those reported for other imidazole-based dicarboxyate AgI coordination polymers (Fang & Zhang, 2006; Zhao et al., 2007). In each HPyIDC2- ligand, the dihedral angles between the planes of the carboxy and carboxylate groups and the imidazole ring are 5.7 (4) and 5.9 (5)°, respectively, while the planes of the imidazole and pyridine rings form a dihedral angle of 15.19 (21)°. Interestingly, the doubly deprotonated HPyIDC2- anion adopts an unusual µ4-κ2N1,O5:κN2:κ2N3,O4:κ2O4 coordination mode, bridging four AgI cations in bis-N,O-chelating, O-bridging and monodentate fashions. The uncoordinated carboxy/carboxylate atoms O2 and O3 form an intramolecular hydrogen bond (Table 2).

In (I), the HPyIDC2- ligand links atoms Ag1 and Ag2 via a bis-N,O-chelating mode into a dinuclear [Ag2(HPyIDC)] unit with an Ag···Ag separation of 6.4609 (11) Å. These units are further connected by Ag—O coordination bonds (Ag1—O4ii; Table 1) to produce an infinite one-dimensional chain (Fig. 2a). In the chain, the shortest Ag···Ag distance is 4.3125 (9) Å. These one-dimensional chains are bridged by the pyridine N atom of the HPyIDC2- ligand in different orientations, giving rise to the formation of a three-dimensional framework (Fig. 3). It is worth noting that the Ag2···O1iii distance (Fig. 2b) between two neighbouring one-dimensional chains is 2.886 (5) Å, which is shorter than the sum of the corresponding van der Waals radii (3.1 Å; Standard reference?), indicative of a weak interaction between atoms Ag2 and O1 (Zhao et al., 2007). To better understand the structure of (I), topology analysis is employed to describe the architecture. Both atoms Ag1 and Ag2 are bound to two µ4-HPyIDC2- ligands and thus can be denoted as linkers, while the µ4-HPyIDC2- ligand, which connects four adjacent µ4-HPyIDC2- ligands through two Ag1 and two Ag2 centres, can be regarded as a 4-connected node. As a result, the overall framework of (I) can be described as an uninodal 4-connected network with a diamondoid topology (Zhang et al., 2008).

Thermogravimetric analysis (TGA) of (I) was carried out from 303 to 1073 K at a heating rate of 10 K min-1 in air (Fig. 4). It can be seen from the TGA curve that there is no noticeable weight loss below 573 K, indicating that the three-dimensional framework of (I) is stable up to 573 K. On heating, a large weight loss occurs in the range 573–1073 K, which can be attributed to the decomposition of the framework and loss of the organic component.

The solid-state emission spectrum of (I) was investigated at room temperature (Fig. 5). When excited at 468 nm, (I) displays a strong green photoluminescence with a maximum emission band at 550 nm. In contrast, the free H3PyIDC ligand exhibits a maximum emission at 470 nm upon excitation at 380 nm (Jing et al., 2010). The significant red shift in the emission of (I) from the free-ligand emission can probably be attributed to ligand-to-metal charge transfer (LMCT) (Allendorf et al.,2009; Sun et al., 2010).

Related literature top

For related literature, see: Allendorf et al. (2009); Fan et al. (2012); Fang & Zhang (2006); Gao et al. (2011); Gu et al. (2011); Jing et al. (2010); Li et al. (2011); Li, Guo, Wang & Wang (2009); Li, Luo, Gao, Lu & Li (2012); Li, Wu, Niu, Niu & Zhang (2009); Li, Zheng, Yuan, Ablet & Jin (2012); Lu et al. (2012); Song et al. (2010); Sun et al. (2010); Wang et al. (2008, 2010, 2011); Yuan et al. (2012); Zeng et al. (2011); Zhang et al. (2006, 2008, 2011); Zhao et al. (2007).

Experimental top

A mixture of AgNO3 (24.0 mg, 0.2 mmol), H3PyIDC (46.6 mg, 0.2 mmol) and H2O (8 ml) was placed in a 25 ml Teflon reactor and heated at 443 K for 96 h under autogenous pressure. After cooling to room temperature, yellow block-shaped crystals of (I) were obtained in a yield of 35% based on Ag. Elemental analysis, calculated for C10H5Ag2N3O4: C 26.88, H 1.13, N 9.40%; found: C 26.93, H 1.09, N 9.46%. FT–IR (KBr pellet, ν, cm-1): 3425 (s), 2974 (w), 1635 (m), 1600 (w), 1568 (w), 1524 (s), 1490 (w), 1468 (w), 1402 (s), 1345 (w), 1260 (w), 1244 (w), 1187 (w), 1108 (m), 1047 (w), 980 (w), 852 (m), 814 (m), 782 (w), 735 (w), 638 (w), 546 (w).

Refinement top

H atoms bonded to C atoms were placed in calculated positions, with C—H = 0.93 Å, and refined as riding atoms, with Uiso(H) = 1.2Ueq(C). The carboxy H atom was located in the idealized position, with O—H = 0.82 Å, and refined as a riding atom, with Uiso(H) = 1.5Ueq(O).

Computing details top

Data collection: APEX2 (Bruker, 2004); cell refinement: APEX2 (Bruker, 2004); data reduction: APEX2 (Bruker, 2004); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEPIII (Burnett & Johnson, 1996) and PLATON (Spek, 2009); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. The structure of (I), showing the atom-numbering scheme. Displacement ellipsoids are drawn at the 30% probability level. All H atoms have been omitted for clarity, except for the carboxyl H atom, which is shown as a small sphere of arbitrary radius. The dashed line indicates the intramolecular hydrogen bond. [Symmetry codes: (i) x + 3/2, -y + 3/2, z + 1/2; (ii) x - 1, -y + 1, z - 1/2.]
[Figure 2] Fig. 2. (a) A perspective view of the one-dimensional chain structure of (I). (b) Weak Ag2···O1iii interactions between neighbouring one-dimensional chains. All H atoms have been omitted for clarity. Dashed lines indicate weak interactions. [Symmetry code: (iii) x - 1/2, -y + 3/2, z - 1/2.]
[Figure 3] Fig. 3. A perspective view of the three-dimensional framework of (I). All H atoms have been omitted for clarity.
[Figure 4] Fig. 4. The TGA curve for (I).
[Figure 5] Fig. 5. The emission spectrum of (I) in the solid state at room temperature.
Poly[[µ4-5-carboxy-4-carboxylato-2-(pyridin-4-yl)-1H-imidazol-1-ido]disilver(I)] top
Crystal data top
[Ag2(C10H5N3O4)]F(000) = 848
Mr = 446.91Dx = 2.734 Mg m3
Monoclinic, CcMo Kα radiation, λ = 0.71073 Å
Hall symbol: C -2ycCell parameters from 2374 reflections
a = 5.2180 (13) Åθ = 2.8–27.9°
b = 20.188 (5) ŵ = 3.62 mm1
c = 10.503 (3) ÅT = 298 K
β = 101.139 (3)°Block, yellow
V = 1085.6 (5) Å30.28 × 0.25 × 0.22 mm
Z = 4
Data collection top
Bruker APEXII CCD area-detector
diffractometer
1856 independent reflections
Radiation source: fine-focus sealed tube1780 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.034
ϕ and ω scansθmax = 26.0°, θmin = 2.0°
Absorption correction: multi-scan
(APEX2; Bruker, 2004)
h = 56
Tmin = 0.431, Tmax = 0.503k = 1924
2835 measured reflectionsl = 1212
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)] = 0.038H-atom parameters constrained
wR(F2) = 0.097 w = 1/[σ2(Fo2) + (0.0421P)2 + 4.9899P]
where P = (Fo2 + 2Fc2)/3
S = 1.11(Δ/σ)max = 0.001
1856 reflectionsΔρmax = 0.64 e Å3
173 parametersΔρmin = 1.11 e Å3
2 restraintsAbsolute structure: Flack (1983), 786 Friedel pairs
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.26 (7)
Crystal data top
[Ag2(C10H5N3O4)]V = 1085.6 (5) Å3
Mr = 446.91Z = 4
Monoclinic, CcMo Kα radiation
a = 5.2180 (13) ŵ = 3.62 mm1
b = 20.188 (5) ÅT = 298 K
c = 10.503 (3) Å0.28 × 0.25 × 0.22 mm
β = 101.139 (3)°
Data collection top
Bruker APEXII CCD area-detector
diffractometer
1856 independent reflections
Absorption correction: multi-scan
(APEX2; Bruker, 2004)
1780 reflections with I > 2σ(I)
Tmin = 0.431, Tmax = 0.503Rint = 0.034
2835 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.038H-atom parameters constrained
wR(F2) = 0.097Δρmax = 0.64 e Å3
S = 1.11Δρmin = 1.11 e Å3
1856 reflectionsAbsolute structure: Flack (1983), 786 Friedel pairs
173 parametersAbsolute structure parameter: 0.26 (7)
2 restraints
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
Ag20.42402 (8)0.58992 (2)0.24408 (5)0.03294 (11)
Ag11.30921 (5)0.77225 (2)0.59249 (4)0.03079 (11)
O40.1812 (8)0.69932 (19)0.2062 (4)0.0263 (10)
C10.8059 (12)0.8409 (3)0.4286 (6)0.0250 (14)
C20.7763 (10)0.7680 (2)0.4103 (5)0.0155 (12)
C50.8799 (10)0.6657 (2)0.4466 (5)0.0172 (12)
N20.6480 (8)0.6642 (2)0.3631 (4)0.0179 (10)
N10.9629 (9)0.7273 (2)0.4773 (4)0.0187 (11)
C30.5790 (11)0.7291 (2)0.3406 (5)0.0206 (13)
C91.2615 (12)0.6092 (3)0.5837 (7)0.0352 (17)
H91.35740.64820.58840.042*
C61.0114 (10)0.6054 (2)0.5081 (5)0.0179 (12)
O30.2580 (8)0.8066 (2)0.2463 (4)0.0297 (11)
C40.3248 (11)0.7469 (3)0.2582 (6)0.0221 (13)
N31.2451 (10)0.4951 (2)0.6445 (5)0.0322 (14)
C81.0093 (13)0.4920 (3)0.5679 (6)0.0341 (17)
H80.92180.45160.56020.041*
C101.3637 (13)0.5534 (4)0.6515 (7)0.0398 (19)
H101.52660.55700.70570.048*
C70.8893 (13)0.5451 (3)0.4997 (6)0.0338 (16)
H70.72460.54020.44780.041*
O20.6059 (9)0.8779 (2)0.3724 (5)0.0389 (13)
H20.47980.85400.34560.058*
O10.9996 (9)0.8660 (2)0.4926 (5)0.0342 (12)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ag20.0348 (2)0.01957 (18)0.0365 (2)0.00696 (19)0.01300 (18)0.00411 (19)
Ag10.01864 (18)0.0351 (2)0.0321 (2)0.00503 (19)0.01132 (16)0.0035 (2)
O40.0182 (18)0.0218 (18)0.033 (2)0.0066 (16)0.0092 (17)0.0027 (17)
C10.021 (3)0.025 (3)0.026 (3)0.000 (2)0.002 (2)0.003 (2)
C20.020 (2)0.006 (2)0.019 (2)0.0022 (18)0.000 (2)0.0031 (18)
C50.027 (3)0.007 (2)0.016 (2)0.004 (2)0.000 (2)0.0002 (18)
N20.016 (2)0.0145 (19)0.019 (2)0.0030 (17)0.0074 (17)0.0015 (17)
N10.018 (2)0.017 (2)0.019 (2)0.0006 (17)0.0003 (18)0.0026 (17)
C30.019 (3)0.016 (2)0.024 (3)0.001 (2)0.001 (2)0.002 (2)
C90.026 (3)0.019 (3)0.052 (4)0.002 (2)0.013 (3)0.009 (3)
C60.018 (3)0.013 (2)0.019 (2)0.004 (2)0.004 (2)0.004 (2)
O30.022 (2)0.023 (2)0.037 (2)0.0074 (17)0.0118 (18)0.0009 (17)
C40.015 (3)0.025 (3)0.021 (2)0.002 (2)0.009 (2)0.006 (2)
N30.030 (3)0.017 (2)0.042 (3)0.006 (2)0.013 (2)0.003 (2)
C80.035 (3)0.022 (3)0.041 (3)0.003 (3)0.003 (3)0.002 (3)
C100.023 (3)0.039 (4)0.047 (4)0.004 (3)0.018 (3)0.000 (3)
C70.031 (3)0.026 (3)0.035 (3)0.003 (3)0.017 (3)0.000 (3)
O20.031 (2)0.022 (2)0.054 (3)0.0051 (18)0.017 (2)0.006 (2)
O10.033 (2)0.022 (2)0.043 (2)0.0031 (18)0.004 (2)0.0012 (19)
Geometric parameters (Å, º) top
Ag2—N3i2.130 (5)N2—C31.367 (7)
Ag2—N22.148 (4)C3—C41.481 (7)
Ag2—O42.539 (4)C9—C101.384 (9)
Ag1—O4ii2.151 (4)C9—C61.392 (8)
Ag1—N12.169 (4)C9—H90.9300
Ag1—O12.577 (4)C6—C71.368 (8)
O4—C41.275 (7)O3—C41.254 (7)
O4—Ag1iii2.151 (4)N3—C101.324 (9)
C1—O11.212 (7)N3—C81.336 (8)
C1—O21.326 (7)N3—Ag2iv2.130 (5)
C1—C21.487 (7)C8—C71.372 (9)
C2—N11.362 (7)C8—H80.9300
C2—C31.387 (7)C10—H100.9300
C5—N11.337 (6)C7—H70.9300
C5—N21.351 (6)O2—H20.8200
C5—C61.482 (7)
N3i—Ag2—N2170.49 (18)N2—C3—C4120.7 (5)
N3i—Ag2—O4117.78 (17)C2—C3—C4131.3 (5)
N2—Ag2—O471.52 (14)C10—C9—C6118.3 (6)
O4ii—Ag1—N1170.45 (16)C10—C9—H9120.9
O4ii—Ag1—O1117.22 (14)C6—C9—H9120.9
N1—Ag1—O171.99 (15)C7—C6—C9117.4 (5)
C4—O4—Ag1iii115.4 (3)C7—C6—C5122.1 (5)
C4—O4—Ag2110.7 (3)C9—C6—C5120.5 (5)
Ag1iii—O4—Ag2133.52 (18)O3—C4—O4123.5 (5)
O1—C1—O2120.7 (5)O3—C4—C3119.5 (5)
O1—C1—C2122.8 (5)O4—C4—C3116.9 (5)
O2—C1—C2116.5 (5)C10—N3—C8116.3 (5)
N1—C2—C3108.3 (4)C10—N3—Ag2iv122.2 (4)
N1—C2—C1118.9 (5)C8—N3—Ag2iv121.5 (4)
C3—C2—C1132.6 (5)N3—C8—C7123.5 (6)
N1—C5—N2112.6 (4)N3—C8—H8118.3
N1—C5—C6123.9 (4)C7—C8—H8118.3
N2—C5—C6123.1 (4)N3—C10—C9124.4 (6)
C5—N2—C3105.3 (4)N3—C10—H10117.8
C5—N2—Ag2135.4 (3)C9—C10—H10117.8
C3—N2—Ag2118.2 (3)C6—C7—C8120.1 (6)
C5—N1—C2105.7 (4)C6—C7—H7119.9
C5—N1—Ag1136.0 (4)C8—C7—H7119.9
C2—N1—Ag1118.1 (3)C1—O2—H2109.5
N2—C3—C2108.0 (4)C1—O1—Ag1107.9 (4)
N3i—Ag2—O4—C4171.7 (4)C1—C2—C3—N2176.9 (6)
N2—Ag2—O4—C410.5 (4)N1—C2—C3—C4176.0 (6)
N3i—Ag2—O4—Ag1iii1.5 (4)C1—C2—C3—C40.3 (11)
N2—Ag2—O4—Ag1iii176.3 (3)C10—C9—C6—C74.0 (10)
O1—C1—C2—N16.2 (9)C10—C9—C6—C5172.4 (6)
O2—C1—C2—N1172.8 (5)N1—C5—C6—C7162.9 (6)
O1—C1—C2—C3178.5 (6)N2—C5—C6—C79.9 (9)
O2—C1—C2—C32.5 (10)N1—C5—C6—C913.3 (9)
N1—C5—N2—C30.5 (6)N2—C5—C6—C9173.9 (6)
C6—C5—N2—C3173.0 (5)Ag1iii—O4—C4—O30.5 (8)
N1—C5—N2—Ag2166.8 (4)Ag2—O4—C4—O3175.0 (5)
C6—C5—N2—Ag219.6 (8)Ag1iii—O4—C4—C3178.1 (4)
O4—Ag2—N2—C5178.1 (6)Ag2—O4—C4—C37.3 (6)
O4—Ag2—N2—C312.0 (4)N2—C3—C4—O3175.0 (5)
N2—C5—N1—C20.2 (6)C2—C3—C4—O31.9 (10)
C6—C5—N1—C2173.7 (5)N2—C3—C4—O42.7 (9)
N2—C5—N1—Ag1176.4 (4)C2—C3—C4—O4179.6 (6)
C6—C5—N1—Ag110.0 (9)C10—N3—C8—C70.6 (11)
C3—C2—N1—C50.9 (6)Ag2iv—N3—C8—C7178.5 (5)
C1—C2—N1—C5177.2 (5)C8—N3—C10—C91.3 (11)
C3—C2—N1—Ag1177.9 (4)Ag2iv—N3—C10—C9176.6 (6)
C1—C2—N1—Ag15.7 (7)C6—C9—C10—N33.6 (12)
O1—Ag1—N1—C5178.9 (6)C9—C6—C7—C82.3 (10)
O1—Ag1—N1—C22.9 (4)C5—C6—C7—C8174.0 (6)
C5—N2—C3—C21.1 (6)N3—C8—C7—C60.1 (11)
Ag2—N2—C3—C2168.9 (4)O2—C1—O1—Ag1175.8 (5)
C5—N2—C3—C4176.5 (5)C2—C1—O1—Ag13.2 (7)
Ag2—N2—C3—C413.6 (7)O4ii—Ag1—O1—C1177.5 (4)
N1—C2—C3—N21.2 (7)N1—Ag1—O1—C10.2 (4)
Symmetry codes: (i) x1, y+1, z1/2; (ii) x+3/2, y+3/2, z+1/2; (iii) x3/2, y+3/2, z1/2; (iv) x+1, y+1, z+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O2—H2···O30.821.702.489 (6)162

Experimental details

Crystal data
Chemical formula[Ag2(C10H5N3O4)]
Mr446.91
Crystal system, space groupMonoclinic, Cc
Temperature (K)298
a, b, c (Å)5.2180 (13), 20.188 (5), 10.503 (3)
β (°) 101.139 (3)
V3)1085.6 (5)
Z4
Radiation typeMo Kα
µ (mm1)3.62
Crystal size (mm)0.28 × 0.25 × 0.22
Data collection
DiffractometerBruker APEXII CCD area-detector
diffractometer
Absorption correctionMulti-scan
(APEX2; Bruker, 2004)
Tmin, Tmax0.431, 0.503
No. of measured, independent and
observed [I > 2σ(I)] reflections
2835, 1856, 1780
Rint0.034
(sin θ/λ)max1)0.616
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.038, 0.097, 1.11
No. of reflections1856
No. of parameters173
No. of restraints2
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.64, 1.11
Absolute structureFlack (1983), 786 Friedel pairs
Absolute structure parameter0.26 (7)

Computer programs: APEX2 (Bruker, 2004), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), ORTEPIII (Burnett & Johnson, 1996) and PLATON (Spek, 2009).

Selected geometric parameters (Å, º) top
Ag2—N3i2.130 (5)Ag1—O4ii2.151 (4)
Ag2—N22.148 (4)Ag1—N12.169 (4)
Ag2—O42.539 (4)Ag1—O12.577 (4)
N3i—Ag2—N2170.49 (18)O4ii—Ag1—N1170.45 (16)
N3i—Ag2—O4117.78 (17)O4ii—Ag1—O1117.22 (14)
N2—Ag2—O471.52 (14)N1—Ag1—O171.99 (15)
Symmetry codes: (i) x1, y+1, z1/2; (ii) x+3/2, y+3/2, z+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O2—H2···O30.821.702.489 (6)161.7
 

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