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Acta Crystallogr Sect E Struct Rep Online. 2010 January 1; 66(Pt 1): m93.
Published online 2009 December 24. doi:  10.1107/S1600536809053525
PMCID: PMC2980228

Poly[bis­(μ2-pyrazine-2-carboxyl­ato)-κ3 N 1,O:O′;κ3 N 1,O:O-cadmium(II)]

Abstract

In the structure of the title compound, [Cd(C5H3N2O2)2]n, the CdII ion is six-coordinated by two N atoms and four O atoms from three different pyrazine-2-carboxyl­ate ligands. One N atom and one O atom of the carboxyl­ate group in the ligand coordinate to the metal center, forming a five-membered chelate ring. The carboxyl­ate anion adopts two types of bridging modes, viz. μ2-O and synanti. Two CdII ions form a centrosymmetric dimer via a μ2-O bridge, and the dimers are linked through the synanti carboxyl­ate functional group, forming a two-dimensional polymeric structure extending along (100).

Related literature

The title compound is isostructural with the Mn(II) complex, see: Cai et al. (2002 [triangle]); Devereux et al. (2002 [triangle]); Liang et al. (2002 [triangle]). For a homologous Cd(II) complex with a picolinate ligand, see: Deloume & Loiseleur (1974 [triangle]).

An external file that holds a picture, illustration, etc.
Object name is e-66-00m93-scheme1.jpg

Experimental

Crystal data

  • [Cd(C5H3N2O2)2]
  • M r = 358.59
  • Monoclinic, An external file that holds a picture, illustration, etc.
Object name is e-66-00m93-efi4.jpg
  • a = 10.304 (2) Å
  • b = 11.044 (2) Å
  • c = 10.274 (2) Å
  • β = 107.89 (3)°
  • V = 1112.7 (4) Å3
  • Z = 4
  • Mo Kα radiation
  • μ = 1.98 mm−1
  • T = 293 K
  • 0.18 × 0.13 × 0.12 mm

Data collection

  • Rigaku R-AXIS RAPID-S diffractometer
  • 11295 measured reflections
  • 2550 independent reflections
  • 1943 reflections with I > 2σ(I)
  • R int = 0.069

Refinement

  • R[F 2 > 2σ(F 2)] = 0.048
  • wR(F 2) = 0.065
  • S = 1.16
  • 2550 reflections
  • 172 parameters
  • H-atom parameters constrained
  • Δρmax = 0.80 e Å−3
  • Δρmin = −0.64 e Å−3

Data collection: RAPID-AUTO (Rigaku, 1998 [triangle]); cell refinement: RAPID-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2002 [triangle]); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 [triangle]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 [triangle]); molecular graphics: SHELXTL (Sheldrick, 2008 [triangle]); software used to prepare material for publication: SHELXL97.

Supplementary Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536809053525/bh2262sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809053525/bh2262Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Acknowledgments

The project was supported by the Research Program of Natural Science at the Universities of Inner Mongolia Autonomous Region (No. NG09168).

supplementary crystallographic information

Comment

Pyrazine-2-carboxylate is a suitable multidentate bridging ligand to build coordination polymers and several novel structural coordination polymers containing derivatives of pyrazinecarboxylate have been obtained. Here, we report the reaction of pyrazine-2-carboxylate with a CdII salt, which afforded a two-dimensional CdII coordination polymer. The compound is isostructural with the MnII complex (Cai et al., 2002; Devereux et al., 2002; Liang et al., 2002). An isostructural Cd(II) complex including picolinate in place of pyrazine-2-carboxylate has also been X-ray characterized (Deloume & Loiseleur, 1974).

In the structure of the title compound, each CdII ion is six-coordinated by two N atoms and four O atoms from three different pyrazine-2-carboxylate ligands (Fig. 1). One N atom and one O atom of the neighboring carboxylate of the ligand coordinate to the center CdII ion forming a five-member chelate ring. The carboxylate of the ligand adopts two types of bridging mode: µ2-O and synanti. The second N atom is not involved in bonding, so the complex is also isostructural with the Cd(II) complex with picolinate (Deloume & Loiseleur, 1974). CdII ion form a dimer via an µ2-O bridge, and these dimers are linked through synanti carboxy O atoms, to form a two-dimensional structure.

Experimental

A mixture of cadmium(II) nitrate (1 mmol), pyrazine-2-carboxylate (0.5 mmol), NaOH (1 mmol), tetrazolate (0.5 mmol) and water (10 ml) was sealed in a 23 ml Teflon-lined reactor, heated to 433 K at 10.8 K/h and kept at this temperature for three days, finally cooled to 303 K at 5.4 K/h (yield 20%).

Refinement

Hydrogen atoms were included in calculated positions and treated as riding on their parent C atoms with C—H = 0.93 Å and Uiso(H) = 1.2Ueq(C).

Figures

Fig. 1.
A view of the title compound showing the coordination of Cd atom with the atom-labelling scheme. Ellipsoids are drawn at the 30% probability level. H atoms have been omitted for clarity. [Symmetry codes: (i) x, -y + 3/2, z + 1/2; (ii) -x, -y + 1, -z; ...

Crystal data

[Cd(C5H3N2O2)2]F(000) = 696
Mr = 358.59Dx = 2.141 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 9922 reflections
a = 10.304 (2) Åθ = 3.1–27.5°
b = 11.044 (2) ŵ = 1.98 mm1
c = 10.274 (2) ÅT = 293 K
β = 107.89 (3)°Block, colourless
V = 1112.7 (4) Å30.18 × 0.13 × 0.12 mm
Z = 4

Data collection

Rigaku R-AXIS RAPID-S diffractometer1943 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.069
graphiteθmax = 27.5°, θmin = 3.1°
ω scansh = −13→13
11295 measured reflectionsk = −14→14
2550 independent reflectionsl = −13→13

Refinement

Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.048Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.065H-atom parameters constrained
S = 1.16w = 1/[σ2(Fo2) + (0.0199P)2 + 0.0187P] where P = (Fo2 + 2Fc2)/3
2550 reflections(Δ/σ)max = 0.001
172 parametersΔρmax = 0.80 e Å3
0 restraintsΔρmin = −0.64 e Å3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2)

xyzUiso*/Ueq
C10.3232 (4)0.6168 (3)0.1469 (4)0.0246 (9)
C20.4605 (4)0.6443 (4)0.1809 (4)0.0373 (10)
H20.51480.60040.14020.045*
C30.4363 (5)0.7903 (4)0.3276 (4)0.0398 (12)
H30.47280.85070.39150.048*
C40.2983 (5)0.7643 (4)0.2953 (4)0.0377 (11)
H40.24460.80770.33700.045*
C50.2594 (4)0.5175 (4)0.0442 (4)0.0283 (10)
C6−0.1395 (4)0.8772 (4)−0.0343 (4)0.0294 (10)
C7−0.2299 (5)0.9723 (4)−0.0745 (5)0.0415 (12)
H7−0.22291.0226−0.14460.050*
C8−0.3322 (5)0.9200 (4)0.0826 (5)0.0412 (12)
H8−0.39910.93150.12500.049*
C9−0.2419 (4)0.8262 (4)0.1254 (4)0.0376 (12)
H9−0.24840.77700.19670.045*
C10−0.0370 (4)0.8481 (4)−0.1094 (4)0.0303 (10)
Cd10.00719 (3)0.63837 (3)0.10693 (3)0.02760 (11)
N10.2415 (3)0.6773 (3)0.2048 (3)0.0294 (8)
N20.5188 (4)0.7323 (4)0.2710 (4)0.0438 (10)
N3−0.1448 (3)0.8035 (3)0.0671 (3)0.0298 (8)
N4−0.3279 (4)0.9948 (4)−0.0163 (4)0.0473 (11)
O10.1363 (3)0.4919 (2)0.0364 (3)0.0345 (7)
O20.3285 (3)0.4700 (3)−0.0196 (3)0.0416 (8)
O30.0344 (3)0.7562 (3)−0.0752 (3)0.0396 (8)
O4−0.0375 (3)0.9214 (3)−0.2042 (3)0.0411 (8)

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
C10.023 (2)0.027 (2)0.024 (2)0.0016 (18)0.0073 (17)0.0029 (18)
C20.032 (2)0.039 (3)0.044 (3)0.001 (2)0.016 (2)0.001 (2)
C30.042 (3)0.044 (3)0.033 (3)−0.009 (2)0.010 (2)−0.011 (2)
C40.036 (3)0.042 (3)0.038 (3)−0.008 (2)0.015 (2)−0.011 (2)
C50.026 (2)0.027 (2)0.030 (3)0.005 (2)0.006 (2)0.003 (2)
C60.028 (2)0.032 (3)0.028 (2)−0.003 (2)0.0085 (18)−0.003 (2)
C70.043 (3)0.040 (3)0.042 (3)0.008 (2)0.013 (2)0.011 (2)
C80.034 (3)0.053 (3)0.040 (3)0.005 (2)0.017 (2)−0.007 (3)
C90.039 (3)0.042 (3)0.035 (3)0.004 (2)0.017 (2)−0.003 (2)
C100.026 (2)0.039 (3)0.025 (2)−0.013 (2)0.0066 (19)−0.006 (2)
Cd10.02236 (16)0.02999 (17)0.03203 (18)0.00188 (16)0.01067 (12)−0.00474 (17)
N10.029 (2)0.029 (2)0.029 (2)0.0000 (16)0.0077 (17)−0.0018 (16)
N20.035 (2)0.052 (2)0.045 (2)−0.008 (2)0.013 (2)−0.004 (2)
N30.026 (2)0.034 (2)0.032 (2)0.0025 (16)0.0122 (17)−0.0026 (17)
N40.039 (2)0.048 (3)0.057 (3)0.015 (2)0.016 (2)0.000 (2)
O10.0240 (16)0.0357 (17)0.045 (2)−0.0046 (14)0.0130 (14)−0.0159 (15)
O20.0314 (18)0.049 (2)0.049 (2)0.0041 (15)0.0189 (16)−0.0136 (16)
O30.0391 (19)0.040 (2)0.0485 (19)0.0050 (15)0.0268 (16)0.0049 (16)
O40.048 (2)0.0451 (19)0.0348 (18)−0.0053 (16)0.0193 (16)0.0032 (16)

Geometric parameters (Å, °)

C1—N11.348 (5)C7—H70.9300
C1—C21.383 (5)C8—N41.321 (6)
C1—C51.523 (5)C8—C91.372 (6)
C2—N21.350 (5)C8—H80.9300
C2—H20.9300C9—N31.339 (5)
C3—N21.332 (5)C9—H90.9300
C3—C41.388 (6)C10—O31.240 (5)
C3—H30.9300C10—O41.265 (5)
C4—N11.341 (5)Cd1—O4i2.227 (3)
C4—H40.9300Cd1—O1ii2.256 (3)
C5—O21.224 (4)Cd1—O12.346 (3)
C5—O11.277 (4)Cd1—N12.352 (3)
C6—N31.336 (5)Cd1—N32.356 (3)
C6—C71.380 (5)Cd1—O32.366 (3)
C6—C101.522 (5)O1—Cd1ii2.256 (3)
C7—N41.346 (5)O4—Cd1iii2.227 (3)
N1—C1—C2120.6 (4)O4—C10—C6114.6 (4)
N1—C1—C5117.8 (3)O4i—Cd1—O1ii96.34 (11)
C2—C1—C5121.6 (4)O4i—Cd1—O1110.68 (11)
N2—C2—C1122.5 (4)O1ii—Cd1—O171.28 (11)
N2—C2—H2118.8O4i—Cd1—N198.14 (11)
C1—C2—H2118.8O1ii—Cd1—N1140.96 (11)
N2—C3—C4122.7 (4)O1—Cd1—N169.70 (10)
N2—C3—H3118.6O4i—Cd1—N394.39 (11)
C4—C3—H3118.6O1ii—Cd1—N396.46 (11)
N1—C4—C3120.7 (4)O1—Cd1—N3152.84 (11)
N1—C4—H4119.6N1—Cd1—N3118.22 (11)
C3—C4—H4119.6O4i—Cd1—O3163.44 (10)
O2—C5—O1126.9 (4)O1ii—Cd1—O392.72 (11)
O2—C5—C1118.7 (4)O1—Cd1—O385.35 (10)
O1—C5—C1114.3 (4)N1—Cd1—O383.22 (11)
N3—C6—C7120.8 (4)N3—Cd1—O370.77 (11)
N3—C6—C10117.8 (4)C4—N1—C1117.6 (4)
C7—C6—C10121.2 (4)C4—N1—Cd1126.8 (3)
N4—C7—C6122.5 (4)C1—N1—Cd1114.8 (2)
N4—C7—H7118.8C3—N2—C2115.9 (4)
C6—C7—H7118.8C6—N3—C9116.7 (4)
N4—C8—C9122.7 (4)C6—N3—Cd1115.1 (3)
N4—C8—H8118.7C9—N3—Cd1128.0 (3)
C9—C8—H8118.7C8—N4—C7115.7 (4)
N3—C9—C8121.6 (4)C5—O1—Cd1ii128.4 (3)
N3—C9—H9119.2C5—O1—Cd1118.3 (3)
C8—C9—H9119.2Cd1ii—O1—Cd1108.72 (11)
O3—C10—O4127.1 (4)C10—O3—Cd1118.1 (3)
O3—C10—C6118.2 (4)C10—O4—Cd1iii121.9 (3)
N1—C1—C2—N2−0.7 (6)C8—C9—N3—Cd1−173.5 (3)
C5—C1—C2—N2179.6 (4)O4i—Cd1—N3—C6172.6 (3)
N2—C3—C4—N10.6 (7)O1ii—Cd1—N3—C6−90.5 (3)
N1—C1—C5—O2172.7 (4)O1—Cd1—N3—C6−29.6 (4)
C2—C1—C5—O2−7.6 (6)N1—Cd1—N3—C670.9 (3)
N1—C1—C5—O1−8.3 (5)O3—Cd1—N3—C60.2 (3)
C2—C1—C5—O1171.4 (4)O4i—Cd1—N3—C9−13.4 (3)
N3—C6—C7—N4−0.9 (7)O1ii—Cd1—N3—C983.5 (3)
C10—C6—C7—N4175.2 (4)O1—Cd1—N3—C9144.4 (3)
N4—C8—C9—N3−1.2 (7)N1—Cd1—N3—C9−115.0 (3)
N3—C6—C10—O31.6 (6)O3—Cd1—N3—C9174.2 (4)
C7—C6—C10—O3−174.6 (4)C9—C8—N4—C70.9 (7)
N3—C6—C10—O4179.9 (3)C6—C7—N4—C80.1 (7)
C7—C6—C10—O43.7 (6)O2—C5—O1—Cd1ii−5.3 (6)
C3—C4—N1—C10.0 (6)C1—C5—O1—Cd1ii175.9 (2)
C3—C4—N1—Cd1−169.2 (3)O2—C5—O1—Cd1−158.4 (3)
C2—C1—N1—C40.1 (6)C1—C5—O1—Cd122.8 (4)
C5—C1—N1—C4179.8 (3)O4i—Cd1—O1—C5−112.2 (3)
C2—C1—N1—Cd1170.6 (3)O1ii—Cd1—O1—C5158.0 (4)
C5—C1—N1—Cd1−9.7 (4)N1—Cd1—O1—C5−20.9 (3)
O4i—Cd1—N1—C4−66.6 (3)N3—Cd1—O1—C591.6 (3)
O1ii—Cd1—N1—C4−177.3 (3)O3—Cd1—O1—C563.6 (3)
O1—Cd1—N1—C4−175.7 (4)O4i—Cd1—O1—Cd1ii89.81 (14)
N3—Cd1—N1—C432.9 (4)O1ii—Cd1—O1—Cd1ii0.0
O3—Cd1—N1—C496.7 (3)N1—Cd1—O1—Cd1ii−178.94 (15)
O4i—Cd1—N1—C1124.0 (3)N3—Cd1—O1—Cd1ii−66.4 (3)
O1ii—Cd1—N1—C113.3 (4)O3—Cd1—O1—Cd1ii−94.46 (13)
O1—Cd1—N1—C114.9 (3)O4—C10—O3—Cd1−179.5 (3)
N3—Cd1—N1—C1−136.6 (3)C6—C10—O3—Cd1−1.5 (5)
O3—Cd1—N1—C1−72.7 (3)O4i—Cd1—O3—C10−26.6 (5)
C4—C3—N2—C2−1.1 (7)O1ii—Cd1—O3—C1096.6 (3)
C1—C2—N2—C31.2 (6)O1—Cd1—O3—C10167.6 (3)
C7—C6—N3—C90.6 (6)N1—Cd1—O3—C10−122.3 (3)
C10—C6—N3—C9−175.6 (3)N3—Cd1—O3—C100.7 (3)
C7—C6—N3—Cd1175.3 (3)O3—C10—O4—Cd1iii31.3 (5)
C10—C6—N3—Cd1−0.9 (4)C6—C10—O4—Cd1iii−146.8 (3)
C8—C9—N3—C60.4 (6)

Symmetry codes: (i) x, −y+3/2, z+1/2; (ii) −x, −y+1, −z; (iii) x, −y+3/2, z−1/2.

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: BH2262).

References

  • Cai, C.-X., Tian, Y.-Q., Ren, X.-M., Li, Y.-Z., You, X.-Z. & Li, S. (2002). Transition Met. Chem.27, 924–927.
  • Deloume, J.-P. & Loiseleur, H. (1974). Acta Cryst. B30, 607–609.
  • Devereux, M., McCann, M., Leon, V., McKee, V. & Ball, R. J. (2002). Polyhedron, 21, 1063–1071.
  • Liang, Y.-C., Hong, M.-C., Liu, J.-C. & Cao, R. (2002). Inorg. Chim. Acta, 328, 152–158.
  • Rigaku (1998). RAPID-AUTO Rigaku Corporation, Tokyo, Japan.
  • Rigaku/MSC (2002). CrystalStructure Rigaku/MSC Inc., The Woodlands, Texas, USA.
  • Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. [PubMed]

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