Issue contents
Download PDF of article
Download CIF
3D view
Navigation
Highlighting
Dictionary of Crystallography reference
IUPAC Gold Book reference
more ...
Download citation
FormatBIBTeX
EndNote
RefMan
Refer
Medline
CIF
SGML
Plain Text
share
Previous article
Next article
Previous article
Issue contents
Download PDF of article
Download CIF
3D view
Navigation
Highlighting
Dictionary of Crystallography reference
IUPAC Gold Book reference
more ...
Download citation
FormatBIBTeX
EndNote
RefMan
Refer
Medline
CIF
SGML
Plain Text
share
Next article

metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890
Volume 66| Part 12| December 2010| Pages m1606-m1607
https://doi.org/10.1107/S1600536810047252

Hexa­aqua­zinc(II) bis­­[tris­­(3-carb­­oxy­pyridine-2-carboxyl­ato)zincate(II)]

Mehrnaz Gharagozlou,a* Vratislav Langerb and Andya Nematic

aDepartment of Nanotechnology and Nanomaterials, Institute for Color Science and Technology, PO Box 16765-654 Tehran, Iran, bEnvironmental Inorganic Chemistry, Department of Chemical and Biological Engineering, Chalmers University of Technology, SE-412 96 Gothenburg, Sweden, and cIran Compiling Encyclopedia Foundation, Tajrish, Tehran, Iran
*Correspondence e-mail: gharagozlou@icrc.ac.ir

(Received 18 October 2010; accepted 15 November 2010; online 20 November 2010)

The title compound, [Zn(H2O)6][Zn(C7H4NO4)3]2, consists of two [Zn(py-2,3-dcH)3]− anions (py-2,3-dcH is 3-carboxy­pyridine-2-carboxylate) and one [Zn(H2O)6]2+ cation. The anion is a six-coordinate complex located on a threefold rotation axis with a slightly distorted octa­hedral geometry around Zn2+ ion. The cation is also six-coordinate with an octa­hedral geometry around the Zn atom, located at a [\overline{3}] axis. Non-covalent inter­actions such as π–π stacking [centroid–centroid distance = 3.828 (4)Å] and O—H⋯O hydrogen bonds play important roles in stabilizing the supra­molecular structure.

Related literature

For first-row transition metal complexes of pyridine-2,3-dicarb­oxy­lic acid and various bases and for Zn—O distances, see: Aghabozorg, Daneshvar et al. (2007[Aghabozorg, H., Daneshvar, S., Motyeian, E., Ghadermazi, M. & Attar Gharamaleki, J. (2007). Acta Cryst. E63, m2468-m2469.]); Aghabozorg, Sadr-khanlou et al. (2007)[Aghabozorg, H., Sadr-khanlou, E., Soleimannejad, J. & Adams, H. (2007). Acta Cryst. E63, m1769.]; Goher et al. (1993[Goher, M. A. S., Youssef, A. A., Zhou, Z.-Y. & Mak, T. C. W. (1993). Polyhedron, 12, 1871-1878.]); Kang et al. (2006[Kang, Y., Zhang, J., Li, Z.-J., Cheng, J.-K. & Yao, Y.-G. (2006). Inorg. Chim. Acta, 359, 2201-2209.]); Li et al. (2006[Li, M., Xiang, J., Yuan, L., Wu, S., Chen, S. & Sun, J. (2006). Cryst. Growth Des. 6, 2036-2040.]); Prior & Rosseinsky (2001[Prior, T. J. & Rosseinsky, M. J. (2001). Chem. Commun. pp. 495-496.]); Swiegers & Malefetse (2000[Swiegers, G. F. & Malefetse, T. J. (2000). Chem. Rev. 100, 3483-3537.]); Yin & Liu (2009[Yin, H. & Liu, S.-X. (2009). J. Mol. Struct. 918, 165-173.]). For hydrogen-bond motifs, see: Bernstein et al. (1995[Bernstein, J., Davis, R. E., Shimoni, L. & Chang, N.-L. (1995). Angew. Chem. Int. Ed. Engl. 34, 1555-1573.]).

[Scheme 1]

Experimental

Crystal data

  • [Zn(H2O)6][Zn(C7H4NO4)3]2

  • Mr = 1300.88

  • Trigonal, [P \overline 3]

  • a = 14.470 (4) Å

  • c = 6.284 (2) Å

  • V = 1139.4 (6) Å3

  • Z = 1

  • Mo Kα radiation

  • μ = 1.68 mm−1

  • T = 153 K

  • 1.20 × 0.44 × 0.42 mm
Data collection

  • Siemens SMART CCD area-detector diffractometer

  • Absorption correction: multi-scan (SADABS; Sheldrick, 2003[Sheldrick, G. M. (2003). SADABS. University of Göttingen, Germany.]) Tmin = 0.237, Tmax = 0.538

  • 10776 measured reflections

  • 1356 independent reflections

  • 1009 reflections with I > 2σ(I)

  • Rint = 0.154
Refinement

  • R[F2 > 2σ(F2)] = 0.061

  • wR(F2) = 0.158

  • S = 1.00

  • 1356 reflections

  • 133 parameters

  • 4 restraints

  • H atoms treated by a mixture of independent and constrained refinement

  • Δρmax = 0.86 e Å−3

  • Δρmin = −0.82 e Å−3

Table 1
Selected bond lengths (Å)

Zn1—O1 2.083 (4)
Zn1—N1 2.157 (5)
Zn2—O5 2.095 (5)

Table 2
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A D⋯A D—H⋯A
O3—H3⋯O2iv 0.83 (5) 1.72 (2) 2.547 (5) 169 (7)
O5—H52⋯O4 0.83 (5) 2.38 (4) 3.157 (7) 156 (7)
O5—H51⋯O4v 0.82 (6) 2.02 (3) 2.795 (6) 158 (6)
Symmetry codes: (iv) y, -x+y, -z; (v) -y, x-y, z.

Data collection: SMART (Bruker, 2003[Bruker (2003). SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2003[Bruker (2003). SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: DIAMOND (Brandenburg, 2010[Brandenburg, K. (2010). DIAMOND. Crystal Impact GbR, Bonn, Germany.]); software used to prepare material for publication: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]).

Supporting information

Crystal structure: contains datablocks I, global. DOI: https://doi.org/10.1107/S1600536810047252/om2373sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536810047252/om2373Isup2.hkl

checkCIF report


Comment top

Metal-organic coordination complexes with one-, two- or three-dimensional structures have attracted attentions for their potential applications as photoelectric materials, catalysis, carriers, sensors, etc. (Prior & Rosseinsky, 2001; Swiegers & Malefetse, 2000). From a chemical point of view, L-lysine, a base, contains two amino groups and one carboxylic acid group, these amino groups often participate in hydrogen bonding and as a general base in catalysis. There are previously reported compounds containing pyridine-2,3-dicarboxylic acid, (py-2,3-dcH2), (Goher et al., 1993; Yin & Liu 2009; Aghabozorg, Daneshvar et al., 2007, Kang et al., 2006, Li et al., 2006).

The title compound consists of two [Zn(py-2,3-dcH)3]¯ anions and one Zn(H2O)62+ cation. The anion is a six-coordinate complex located at a 3-fold crystallographic axis around Zn1 atom by three chelating (py-2,3-dcH)¯ ligands via one N and one O atom from carboxylate groups (Fig. 1). The cation is also six-coordinate with an octahedral geometry around Zn2 atom, located at a 3-bar axis. L-lysine, even it was included during the synthesis, is not part of this crystal structure and we were surprised that the product material contains Zn atoms in both form of cation and anion units. In anionic complex the three O—Zn1—N angles indicate that there is a distorted octahedral geometry around Zn1 atoms (for selected bond distances and angles see Table 1), but in cationic unit there are three O—Zn2—O angles exactly 180° as imposed by the crystallographic symmetry and good octahedral geometry environment around Zn2 atom (Table 1). The anionic Zn—O distances (Table 1) fall within the range of those found in related Zn complexes, 2.031- 2.117 Å (Aghabozorg, Daneshvar et al., 2007; Aghabozorg, Sadr-khanlou et al., 2007; Kang, et al., 2006; Li, et al., 2006;Yin, et al., 2009).

There are three principal hydrogen bonds of O—H···O type (see Table 2) forming a complicated and extensive hydrogen bonding pattern. Graph-set analysis (Bernstein et al., 1995) on the first level is indicating chains with symbols C22(20) and C22(16) for hydrogen bond with donor atoms O3 and O5, respectively, as well as ring R22(20) for hydrogen bond with O3 as a donor. On second level graph-set, most important are ring R12(6) and chains C22(14) and C22(16) between hexaaqua zinc cations, as well as rings R33(15) formed between anions and cations.

There are π-π stacking interactions between anions proved by short distance Cg4···Cg4 3.828 (4)Å [Cg4 is centroid of N1/C2—C6 ring. Symmetry code: 1 - x,1 - y,1 - z]. These π-π stacking interactions and O—H···O hydrogen bonds have important roles in stabilizing the structure. Crystal packing is depicted in Fig. 2.

Related literature top

For first-row transition metal complexes of pyridine-2,3-dicarboxylic acid and various bases and for Zn—O distances, see: Aghabozorg, Daneshvar et al. (2007); Aghabozorg, Sadr-khanlou et al. (2007); Goher et al. (1993); Kang et al. (2006); Li et al. (2006); Prior & Rosseinsky (2001); Swiegers & Malefetse (2000); Yin & Liu (2009). For hydrogen-bond motifs, see: Bernstein et al. (1995).

Experimental top

The title compound was prepared by the reaction of pyridine-2,3-dicarboxylic acid (py-2,3-dcH2) (167 mg, 1 mmol), L-Lysine (L-Lys) (164 mg, 1 mmol) and with zinc(II) nitrate hexahydrate Zn(NO3)2. 6H2O (148.7 mg, 0.5 mmol), which were dissolved in distilled water (30 ml) as solvent in 2:2:1 molar ratio. The crystals were obtained by slow evaporation of solvent at room temperature.

Refinement top

Aromatic hydrogen atoms were refined isotropically with Uiso(H) = 1.2Ueq(C) and their positions were constrained to ideal geometry using an appropriate riding model, with C—H = 0.95. The carboxylate and water H atoms were located at the difference Fourier map and refined isotropically with Uiso(H) = 1.5Ueq(O), and restrained to ideal geometry with O—H distances 0.84 (2)Å and H···H distance 1.34 (2) Å for the water molecule.

Structure description top

Metal-organic coordination complexes with one-, two- or three-dimensional structures have attracted attentions for their potential applications as photoelectric materials, catalysis, carriers, sensors, etc. (Prior & Rosseinsky, 2001; Swiegers & Malefetse, 2000). From a chemical point of view, L-lysine, a base, contains two amino groups and one carboxylic acid group, these amino groups often participate in hydrogen bonding and as a general base in catalysis. There are previously reported compounds containing pyridine-2,3-dicarboxylic acid, (py-2,3-dcH2), (Goher et al., 1993; Yin & Liu 2009; Aghabozorg, Daneshvar et al., 2007, Kang et al., 2006, Li et al., 2006).

The title compound consists of two [Zn(py-2,3-dcH)3]¯ anions and one Zn(H2O)62+ cation. The anion is a six-coordinate complex located at a 3-fold crystallographic axis around Zn1 atom by three chelating (py-2,3-dcH)¯ ligands via one N and one O atom from carboxylate groups (Fig. 1). The cation is also six-coordinate with an octahedral geometry around Zn2 atom, located at a 3-bar axis. L-lysine, even it was included during the synthesis, is not part of this crystal structure and we were surprised that the product material contains Zn atoms in both form of cation and anion units. In anionic complex the three O—Zn1—N angles indicate that there is a distorted octahedral geometry around Zn1 atoms (for selected bond distances and angles see Table 1), but in cationic unit there are three O—Zn2—O angles exactly 180° as imposed by the crystallographic symmetry and good octahedral geometry environment around Zn2 atom (Table 1). The anionic Zn—O distances (Table 1) fall within the range of those found in related Zn complexes, 2.031- 2.117 Å (Aghabozorg, Daneshvar et al., 2007; Aghabozorg, Sadr-khanlou et al., 2007; Kang, et al., 2006; Li, et al., 2006;Yin, et al., 2009).

There are three principal hydrogen bonds of O—H···O type (see Table 2) forming a complicated and extensive hydrogen bonding pattern. Graph-set analysis (Bernstein et al., 1995) on the first level is indicating chains with symbols C22(20) and C22(16) for hydrogen bond with donor atoms O3 and O5, respectively, as well as ring R22(20) for hydrogen bond with O3 as a donor. On second level graph-set, most important are ring R12(6) and chains C22(14) and C22(16) between hexaaqua zinc cations, as well as rings R33(15) formed between anions and cations.

There are π-π stacking interactions between anions proved by short distance Cg4···Cg4 3.828 (4)Å [Cg4 is centroid of N1/C2—C6 ring. Symmetry code: 1 - x,1 - y,1 - z]. These π-π stacking interactions and O—H···O hydrogen bonds have important roles in stabilizing the structure. Crystal packing is depicted in Fig. 2.

For first-row transition metal complexes of pyridine-2,3-dicarboxylic acid and various bases and for Zn—O distances, see: Aghabozorg, Daneshvar et al. (2007); Aghabozorg, Sadr-khanlou et al. (2007); Goher et al. (1993); Kang et al. (2006); Li et al. (2006); Prior & Rosseinsky (2001); Swiegers & Malefetse (2000); Yin & Liu (2009). For hydrogen-bond motifs, see: Bernstein et al. (1995).

Computing details top

Data collection: SMART (Bruker, 2003); cell refinement: SAINT (Bruker, 2003); data reduction: SAINT (Bruker, 2003); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg, 2010); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. The molecular structure of the title compound, with the displacement ellipsoids drawn at 50% probability level.
[Figure 2] Fig. 2. A view of along the a axis of the crystal packing in the title compounds. Layers perpendicular to c-directions are connected via hydrogen bonds.
Hexaaquazinc(II) bis[tris(3-carboxypyridine-2-carboxylato)zincate(II)] top
Crystal data top
[Zn(H2O)6][Zn(C7H4NO4)3]2Dx = 1.896 Mg m−3
Mr = 1300.88Mo Kα radiation, λ = 0.71073 Å
Trigonal, P3Cell parameters from 1491 reflections
Hall symbol: -P 3θ = 2.8–22.5°
a = 14.470 (4) ŵ = 1.68 mm−1
c = 6.284 (2) ÅT = 153 K
V = 1139.4 (6) Å3Block, colourless
Z = 11.20 × 0.44 × 0.42 mm
F(000) = 660
Data collection top
Siemens SMART CCD area-detector
diffractometer		1356 independent reflections
Radiation source: fine-focus sealed tube1009 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.154
ω scansθmax = 25.1°, θmin = 2.8°
Absorption correction: multi-scan
(SADABS; Sheldrick, 2003)		h = −17→17
Tmin = 0.237, Tmax = 0.538k = −17→17
10776 measured reflectionsl = −7→7
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)] = 0.061H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.158 w = 1/[σ2(Fo2) + (0.0993P)2 + 0.9035P]
where P = (Fo2 + 2Fc2)/3
S = 1.00(Δ/σ)max < 0.001
1356 reflectionsΔρmax = 0.86 e Å−3
133 parametersΔρmin = −0.82 e Å−3
4 restraintsExtinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.035 (5)
Crystal data top
[Zn(H2O)6][Zn(C7H4NO4)3]2Z = 1
Mr = 1300.88Mo Kα radiation
Trigonal, P3µ = 1.68 mm−1
a = 14.470 (4) ÅT = 153 K
c = 6.284 (2) Å1.20 × 0.44 × 0.42 mm
V = 1139.4 (6) Å3
Data collection top
Siemens SMART CCD area-detector
diffractometer		1356 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 2003)		1009 reflections with I > 2σ(I)
Tmin = 0.237, Tmax = 0.538Rint = 0.154
10776 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0614 restraints
wR(F2) = 0.158H atoms treated by a mixture of independent and constrained refinement
S = 1.00Δρmax = 0.86 e Å−3
1356 reflectionsΔρmin = −0.82 e Å−3
133 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
Zn10.33330.66670.29441 (18)0.0155 (4)
O10.2510 (3)0.5298 (3)0.1090 (6)0.0193 (9)
O20.1958 (3)0.3552 (3)0.0954 (6)0.0194 (10)
O30.3623 (3)0.2972 (3)0.1662 (6)0.0213 (10)
H30.352 (5)0.247 (4)0.086 (9)0.032*
O40.2312 (4)0.1865 (3)0.3858 (7)0.0322 (11)
N10.3482 (4)0.5491 (4)0.4789 (7)0.0161 (11)
C20.3119 (4)0.4565 (4)0.3746 (8)0.0155 (12)
C30.3237 (4)0.3729 (4)0.4533 (9)0.0167 (13)
C40.3667 (5)0.3851 (5)0.6543 (10)0.0216 (14)
H40.37250.32830.71640.026*
C50.4011 (4)0.4781 (5)0.7648 (9)0.0200 (13)
H50.42940.48630.90440.024*
C60.3935 (4)0.5601 (5)0.6677 (9)0.0183 (13)
H60.42190.62670.73910.022*
C70.2490 (4)0.4467 (4)0.1750 (9)0.0168 (13)
C80.2983 (5)0.2751 (4)0.3263 (9)0.0187 (13)
Zn20.00000.00000.00000.0226 (5)
O50.0098 (3)0.1271 (4)0.1776 (7)0.0305 (11)
H51−0.038 (3)0.109 (5)0.267 (8)0.046*
H520.069 (2)0.161 (5)0.238 (9)0.046*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Zn10.0124 (5)0.0124 (5)0.0217 (7)0.0062 (2)0.0000.000
O10.017 (2)0.016 (2)0.024 (2)0.0074 (18)−0.0023 (17)−0.0024 (17)
O20.016 (2)0.011 (2)0.031 (2)0.0056 (18)−0.0076 (17)−0.0055 (17)
O30.019 (2)0.016 (2)0.029 (3)0.0096 (19)0.0048 (19)−0.0047 (18)
O40.040 (3)0.013 (2)0.035 (3)0.007 (2)0.012 (2)0.0014 (19)
N10.012 (2)0.012 (2)0.020 (3)0.003 (2)0.0024 (19)−0.003 (2)
C20.013 (3)0.013 (3)0.018 (3)0.005 (2)0.001 (2)0.002 (2)
C30.011 (3)0.013 (3)0.025 (3)0.005 (2)0.003 (2)0.000 (2)
C40.021 (3)0.021 (3)0.027 (3)0.014 (3)0.003 (3)0.001 (3)
C50.015 (3)0.027 (3)0.021 (3)0.013 (3)−0.002 (2)−0.002 (3)
C60.014 (3)0.025 (3)0.018 (3)0.012 (3)−0.002 (2)−0.005 (2)
C70.009 (3)0.022 (3)0.022 (3)0.010 (3)0.003 (2)0.000 (3)
C80.020 (3)0.015 (3)0.026 (3)0.012 (3)−0.001 (3)0.001 (2)
Zn20.0185 (6)0.0185 (6)0.0307 (11)0.0092 (3)0.0000.000
O50.018 (2)0.029 (3)0.038 (3)0.008 (2)0.001 (2)−0.004 (2)
Geometric parameters (Å, º) top
Zn1—O12.083 (4)C3—C41.380 (8)
Zn1—N12.157 (5)C3—C81.502 (8)
O1—C71.259 (7)C4—C51.369 (8)
O2—C71.256 (7)C4—H40.9500
O3—C81.294 (7)C5—C61.386 (8)
O3—H30.83 (5)C5—H50.9500
O4—C81.217 (7)C6—H60.9500
N1—C61.327 (7)Zn2—O52.095 (5)
N1—C21.340 (7)O5—H510.82 (5)
C2—C31.393 (8)O5—H520.83 (6)
C2—C71.514 (8)
O1—Zn1—O1i91.76 (15)C5—C4—H4119.7
O1—Zn1—N1i165.35 (16)C6—C5—C4118.2 (5)
O1—Zn1—N177.62 (16)C6—C5—H5120.9
O1i—Zn1—N198.55 (15)C4—C5—H5120.9
N1i—Zn1—N193.83 (16)N1—C6—C5122.5 (5)
C7—O1—Zn1116.9 (4)N1—C6—H6118.8
C8—O3—H3117 (5)C5—C6—H6118.8
C6—N1—C2118.7 (5)O2—C7—O1125.8 (5)
C6—N1—Zn1128.6 (4)O2—C7—C2116.8 (5)
C2—N1—Zn1112.5 (3)O1—C7—C2117.3 (5)
N1—C2—C3122.5 (5)O4—C8—O3126.5 (5)
N1—C2—C7114.5 (5)O4—C8—C3121.3 (5)
C3—C2—C7122.8 (5)O3—C8—C3111.9 (5)
C4—C3—C2117.2 (5)O5—Zn2—O5ii180.0
C4—C3—C8119.2 (5)O5—Zn2—O5iii85.74 (18)
C2—C3—C8123.5 (5)Zn2—O5—H51114 (5)
C3—C4—C5120.6 (5)Zn2—O5—H52111 (5)
C3—C4—H4119.7H51—O5—H52109 (3)
O1iv—Zn1—O1—C7−172.0 (4)C7—C2—C3—C4−169.1 (5)
O1i—Zn1—O1—C796.2 (4)N1—C2—C3—C8−170.8 (5)
N1iv—Zn1—O1—C7−94.3 (4)C7—C2—C3—C814.7 (9)
N1i—Zn1—O1—C753.1 (8)C2—C3—C4—C5−3.3 (9)
N1—Zn1—O1—C7−2.2 (4)C8—C3—C4—C5173.0 (5)
O1iv—Zn1—N1—C6−132.6 (6)C3—C4—C5—C6−1.3 (9)
O1—Zn1—N1—C6−176.9 (5)C2—N1—C6—C5−2.6 (8)
O1i—Zn1—N1—C693.2 (5)Zn1—N1—C6—C5−177.4 (4)
N1iv—Zn1—N1—C6−79.0 (4)C4—C5—C6—N14.5 (9)
N1i—Zn1—N1—C615.1 (5)Zn1—O1—C7—O2173.2 (4)
O1iv—Zn1—N1—C252.4 (8)Zn1—O1—C7—C2−3.5 (6)
O1—Zn1—N1—C28.0 (4)N1—C2—C7—O2−166.2 (5)
O1i—Zn1—N1—C2−81.9 (4)C3—C2—C7—O28.7 (8)
N1iv—Zn1—N1—C2105.9 (4)N1—C2—C7—O110.8 (7)
N1i—Zn1—N1—C2−159.9 (4)C3—C2—C7—O1−174.3 (5)
C6—N1—C2—C3−2.5 (8)C4—C3—C8—O463.8 (8)
Zn1—N1—C2—C3173.1 (4)C2—C3—C8—O4−120.1 (7)
C6—N1—C2—C7172.4 (5)C4—C3—C8—O3−110.0 (6)
Zn1—N1—C2—C7−12.0 (6)C2—C3—C8—O366.1 (7)
N1—C2—C3—C45.4 (8)
Symmetry codes: (i) −y+1, x−y+1, z; (ii) −x, −y, −z; (iii) x−y, x, −z; (iv) −x+y, −x+1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O3—H3···O2v0.83 (5)1.72 (2)2.547 (5)169 (7)
O5—H52···O40.83 (5)2.38 (4)3.157 (7)156 (7)
O5—H51···O4vi0.82 (6)2.02 (3)2.795 (6)158 (6)
Symmetry codes: (v) y, −x+y, −z; (vi) −y, x−y, z.

Experimental details

Crystal data
Chemical formula[Zn(H2O)6][Zn(C7H4NO4)3]2
Mr1300.88
Crystal system, space groupTrigonal, P3
Temperature (K)153
a, c (Å)14.470 (4), 6.284 (2)
V (Å3)1139.4 (6)
Z1
Radiation typeMo Kα
µ (mm−1)1.68
Crystal size (mm)1.20 × 0.44 × 0.42
Data collection
DiffractometerSiemens SMART CCD area-detector
Absorption correctionMulti-scan
(SADABS; Sheldrick, 2003)
Tmin, Tmax0.237, 0.538
No. of measured, independent and
observed [I > 2σ(I)] reflections		10776, 1356, 1009
Rint0.154
(sin θ/λ)max (Å−1)0.597
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.061, 0.158, 1.00
No. of reflections1356
No. of parameters133
No. of restraints4
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å−3)0.86, −0.82

Computer programs: SMART (Bruker, 2003), SAINT (Bruker, 2003), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), DIAMOND (Brandenburg, 2010), SHELXTL (Sheldrick, 2008).

Selected geometric parameters (Å, º) top
Zn1—O12.083 (4)O3—C81.294 (7)
Zn1—N12.157 (5)O4—C81.217 (7)
O1—C71.259 (7)Zn2—O52.095 (5)
O2—C71.256 (7)
O1—Zn1—O1i91.76 (15)N1i—Zn1—N193.83 (16)
O1—Zn1—N1i165.35 (16)O5—Zn2—O5ii180.0
O1—Zn1—N177.62 (16)O5—Zn2—O5iii85.74 (18)
O1i—Zn1—N198.55 (15)
Symmetry codes: (i) −y+1, x−y+1, z; (ii) −x, −y, −z; (iii) x−y, x, −z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O3—H3···O2iv0.83 (5)1.72 (2)2.547 (5)169 (7)
O5—H52···O40.83 (5)2.38 (4)3.157 (7)156 (7)
O5—H51···O4v0.82 (6)2.02 (3)2.795 (6)158 (6)
Symmetry codes: (iv) y, −x+y, −z; (v) −y, x−y, z.
 

Acknowledgements

We acknowledge financial support of this work by the Nation Elite Foundation. We are also grateful to the Institute for Color Science and Technology.

References

First citationAghabozorg, H., Daneshvar, S., Motyeian, E., Ghadermazi, M. & Attar Gharamaleki, J. (2007). Acta Cryst. E63, m2468–m2469.  Web of Science CSD CrossRef IUCr Journals Google Scholar
 First citationAghabozorg, H., Sadr-khanlou, E., Soleimannejad, J. & Adams, H. (2007). Acta Cryst. E63, m1769.  Web of Science CSD CrossRef IUCr Journals Google Scholar
 First citationBernstein, J., Davis, R. E., Shimoni, L. & Chang, N.-L. (1995). Angew. Chem. Int. Ed. Engl. 34, 1555–1573.  CrossRef CAS Web of Science Google Scholar
 First citationBrandenburg, K. (2010). DIAMOND. Crystal Impact GbR, Bonn, Germany.  Google Scholar
 First citationBruker (2003). SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.  Google Scholar
 First citationGoher, M. A. S., Youssef, A. A., Zhou, Z.-Y. & Mak, T. C. W. (1993). Polyhedron, 12, 1871–1878.  CSD CrossRef CAS Web of Science Google Scholar
 First citationKang, Y., Zhang, J., Li, Z.-J., Cheng, J.-K. & Yao, Y.-G. (2006). Inorg. Chim. Acta, 359, 2201–2209.  Web of Science CrossRef CAS Google Scholar
 First citationLi, M., Xiang, J., Yuan, L., Wu, S., Chen, S. & Sun, J. (2006). Cryst. Growth Des. 6, 2036–2040.  Web of Science CSD CrossRef CAS Google Scholar
 First citationPrior, T. J. & Rosseinsky, M. J. (2001). Chem. Commun. pp. 495–496.  Web of Science CSD CrossRef Google Scholar
 First citationSheldrick, G. M. (2003). SADABS. University of Göttingen, Germany.  Google Scholar
 First citationSheldrick, G. M. (2008). Acta Cryst. A64, 112–122.  Web of Science CrossRef CAS IUCr Journals Google Scholar
 First citationSwiegers, G. F. & Malefetse, T. J. (2000). Chem. Rev. 100, 3483–3537.  Web of Science CrossRef PubMed CAS Google Scholar
 First citationYin, H. & Liu, S.-X. (2009). J. Mol. Struct. 918, 165–173.  Web of Science CSD CrossRef CAS Google Scholar

This is an open-access article distributed under the terms of the Creative Commons Attribution (CC-BY) Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890
Volume 66| Part 12| December 2010| Pages m1606-m1607
https://doi.org/10.1107/S1600536810047252
Follow Acta Cryst. E
Sign up for e-alerts
E-alerts
Follow Acta Cryst. on Twitter
Twitter
Follow us on facebook
Facebook
Sign up for RSS feeds
RSS