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Acta Crystallogr Sect E Struct Rep Online. 2009 August 1; 65(Pt 8): m935.
Published online 2009 July 18. doi:  10.1107/S1600536809027135
PMCID: PMC2977348

catena-Poly[[bis­[2-(1H-1,2,4-triazol-1-yl-κN 4)pyrazine]cadmium(II)]-di-μ-thio­cyanato-κ2 S:N2 N:S]

Abstract

The title compound, [Cd(NCS)2(C6H5N5)2]n, is a coordination polymer with the CdII centre located on a twofold rotation axis. The CdII centre assumes a distorted octa­hedral geometry. The thio­cyanate anions function as bridging ligands between the CdII centres, leading to a chain-like arrangement expanding along [001].

Related literature

For a related structure, see: Yang & Shi (2008 [triangle]).

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Object name is e-65-0m935-scheme1.jpg

Experimental

Crystal data

  • [Cd(NCS)2(C6H5N5)2]
  • M r = 522.86
  • Monoclinic, An external file that holds a picture, illustration, etc.
Object name is e-65-0m935-efi3.jpg
  • a = 25.818 (4) Å
  • b = 7.4077 (10) Å
  • c = 11.0276 (15) Å
  • β = 113.843 (2)°
  • V = 1929.1 (5) Å3
  • Z = 4
  • Mo Kα radiation
  • μ = 1.38 mm−1
  • T = 298 K
  • 0.41 × 0.21 × 0.20 mm

Data collection

  • Bruker SMART APEX CCD diffractometer
  • Absorption correction: multi-scan (SADABS; Bruker, 1997 [triangle]) T min = 0.602, T max = 0.770
  • 5381 measured reflections
  • 2085 independent reflections
  • 2005 reflections with I > 2σ(I)
  • R int = 0.022

Refinement

  • R[F 2 > 2σ(F 2)] = 0.022
  • wR(F 2) = 0.058
  • S = 1.10
  • 2085 reflections
  • 133 parameters
  • H-atom parameters constrained
  • Δρmax = 0.35 e Å−3
  • Δρmin = −0.47 e Å−3

Data collection: SMART (Bruker, 1997 [triangle]); cell refinement: SAINT (Bruker, 1997 [triangle]); data reduction: SAINT; 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: SHELXTL.

Supplementary Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536809027135/bt2992sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809027135/bt2992Isup2.hkl

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

Acknowledgments

The authors thank the Project of Scientific Studies Development of Shandong Provincial Education Department (grant No. J08LC51) and the Natural Science Foundation of Shandong Province (grant No. Y2007B26).

supplementary crystallographic information

Comment

2-(1H-1,2,4-triazol-1-yl)pyrazine is similar to 2-(pyrazol-1-yl)pyrazine (Yang & Shi, 2008) and therefore it should act as a brdiging ligand. We are interested in synthesizing complexes with mixed bridging ligands and selected thiocyanato and 2-(1H-1,2,4-triazol-1-yl)pyrazine as ligands. However, 2-(1H-1,2,4-triazol-1-yl)pyrazine only functions as a terminal ligand.

The coordination geometry of the Cd centres is shown in Fig. 1. The Cd atom is in a distorted octahedral CdN4S2 coordination geometry. In the crystal each CdII ion is surrounded by two other symmetry-related CdII ions with separation with 5.7105 (7) Å and the adjacent CdII ions were bridged by two thiocyanato anions and it forms a one-dimensional chain along the c axis. 2-(1H-1,2,4-triazol-1-yl)pyrazine only acts as a monodentate ligand.

Experimental

6 ml methanol solution of 2-(1H-1,2,4-triazol-1-yl)pyrazine (0.0345 g, 0.191 mmol), 5 ml C d(ClO4)2.6H2O (0.0809 g, 0.193 mmol) H2O solution and 5 ml NaSCN (0.0315 g, 0.389 mmol) H2O solution were mixed together and stirred for a few minutes. The colorless single crystals were obtained after the filtrate had been allowed to stand at room temperature for two weeks.

Refinement

All H atoms were placed in calculated positions and refined as riding with C—H = 0.93 Å and Uiso(H) = 1.2Ueq(C).

Figures

Fig. 1.
Coordination around the Cd atom with the atom-numbering scheme. Displacement ellipsoids are drawn at the 30% probability level. [Symmetry codes: (i) -x + 1, -y, -z + 1 (ii) -x + 1, y, -z + 3/2 (iii) x, -y, z + 1/2 (iv) -x + 1, -y, -z + 2]
Fig. 2.
Packing diagram of the title compound.

Crystal data

[Cd(NCS)2(C6H5N5)2]F(000) = 1032
Mr = 522.86Dx = 1.800 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 4306 reflections
a = 25.818 (4) Åθ = 2.9–28.3°
b = 7.4077 (10) ŵ = 1.38 mm1
c = 11.0276 (15) ÅT = 298 K
β = 113.843 (2)°Block, colourless
V = 1929.1 (5) Å30.41 × 0.21 × 0.20 mm
Z = 4

Data collection

Bruker SMART APEX CCD diffractometer2085 independent reflections
Radiation source: fine-focus sealed tube2005 reflections with I > 2σ(I)
graphiteRint = 0.022
[var phi] and ω scansθmax = 27.0°, θmin = 1.7°
Absorption correction: multi-scan (SADABS; Bruker, 1997)h = −32→23
Tmin = 0.602, Tmax = 0.770k = −7→9
5381 measured reflectionsl = −10→13

Refinement

Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.022H-atom parameters constrained
wR(F2) = 0.058w = 1/[σ2(Fo2) + (0.0298P)2 + 1.3229P] where P = (Fo2 + 2Fc2)/3
S = 1.10(Δ/σ)max = 0.002
2085 reflectionsΔρmax = 0.35 e Å3
133 parametersΔρmin = −0.47 e Å3
0 restraintsExtinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0082 (3)

Special details

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)

xyzUiso*/Ueq
C10.43493 (9)0.3626 (3)0.9002 (2)0.0392 (5)
H10.46360.34400.98380.047*
C20.39121 (9)0.3614 (3)0.6932 (2)0.0382 (4)
H20.38080.34570.60270.046*
C30.56274 (8)−0.1295 (3)0.5829 (2)0.0334 (4)
C40.30256 (8)0.5013 (3)0.68395 (18)0.0322 (4)
C50.27688 (11)0.5921 (3)0.7544 (2)0.0455 (5)
H50.29740.61770.84370.055*
C60.22301 (10)0.5174 (4)0.4984 (2)0.0493 (5)
H60.20290.49490.40840.059*
C70.19638 (11)0.6044 (3)0.5671 (3)0.0505 (6)
H70.15860.63710.52260.061*
Cd10.50000.10030 (3)0.75000.03107 (10)
N10.43983 (7)0.3119 (2)0.78646 (17)0.0391 (4)
N20.55550 (9)−0.1113 (3)0.47410 (19)0.0455 (5)
N30.35900 (7)0.4377 (2)0.74783 (16)0.0317 (3)
N40.38687 (8)0.4394 (2)0.88241 (17)0.0377 (4)
N50.27701 (8)0.4642 (3)0.55708 (17)0.0422 (4)
N60.22297 (9)0.6433 (3)0.6954 (2)0.0535 (5)
S10.57240 (3)−0.15916 (10)0.73782 (5)0.05367 (18)

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
C10.0367 (11)0.0455 (11)0.0340 (10)−0.0001 (9)0.0129 (9)−0.0018 (9)
C20.0371 (11)0.0444 (11)0.0356 (10)0.0028 (9)0.0172 (9)−0.0052 (8)
C30.0287 (9)0.0379 (10)0.0307 (10)0.0051 (7)0.0089 (8)−0.0017 (7)
C40.0329 (9)0.0331 (9)0.0335 (10)0.0004 (7)0.0162 (8)0.0008 (7)
C50.0460 (13)0.0563 (14)0.0358 (11)0.0117 (10)0.0181 (10)−0.0034 (9)
C60.0409 (12)0.0649 (15)0.0373 (11)0.0040 (11)0.0106 (9)−0.0060 (10)
C70.0370 (12)0.0666 (16)0.0452 (14)0.0126 (10)0.0138 (11)0.0007 (10)
Cd10.03018 (13)0.03752 (14)0.02687 (13)0.0000.01294 (9)0.000
N10.0349 (9)0.0439 (10)0.0404 (9)0.0014 (7)0.0171 (7)−0.0046 (8)
N20.0428 (10)0.0607 (12)0.0319 (10)0.0058 (8)0.0141 (8)0.0017 (8)
N30.0321 (8)0.0356 (8)0.0300 (8)−0.0009 (6)0.0153 (7)−0.0026 (6)
N40.0367 (9)0.0465 (9)0.0302 (9)0.0006 (7)0.0138 (7)−0.0024 (7)
N50.0369 (9)0.0549 (10)0.0349 (9)0.0035 (8)0.0146 (7)−0.0061 (8)
N60.0476 (11)0.0696 (13)0.0450 (11)0.0190 (10)0.0204 (9)−0.0017 (10)
S10.0699 (4)0.0614 (4)0.0296 (3)0.0323 (3)0.0201 (3)0.0093 (2)

Geometric parameters (Å, °)

C1—N41.306 (3)C6—N51.337 (3)
C1—N11.363 (3)C6—C71.372 (3)
C1—H10.9300C6—H60.9300
C2—N11.313 (3)C7—N61.331 (3)
C2—N31.334 (3)C7—H70.9300
C2—H20.9300Cd1—N2i2.3031 (19)
C3—N21.145 (3)Cd1—N2ii2.3031 (19)
C3—S11.639 (2)Cd1—N1iii2.3528 (18)
C4—N51.312 (3)Cd1—N12.3528 (17)
C4—C51.383 (3)Cd1—S1iii2.7220 (6)
C4—N31.418 (2)Cd1—S12.7220 (6)
C5—N61.331 (3)N2—Cd1ii2.3031 (19)
C5—H50.9300N3—N41.363 (2)
N4—C1—N1114.71 (19)N2ii—Cd1—N189.56 (7)
N4—C1—H1122.6N1iii—Cd1—N196.47 (9)
N1—C1—H1122.6N2i—Cd1—S1iii96.54 (5)
N1—C2—N3109.75 (19)N2ii—Cd1—S1iii86.34 (5)
N1—C2—H2125.1N1iii—Cd1—S1iii173.10 (5)
N3—C2—H2125.1N1—Cd1—S1iii87.01 (5)
N2—C3—S1178.9 (2)N2i—Cd1—S186.34 (5)
N5—C4—C5123.5 (2)N2ii—Cd1—S196.54 (5)
N5—C4—N3115.64 (17)N1iii—Cd1—S187.01 (5)
C5—C4—N3120.82 (18)N1—Cd1—S1173.10 (5)
N6—C5—C4120.5 (2)S1iii—Cd1—S190.16 (4)
N6—C5—H5119.7C2—N1—C1103.22 (18)
C4—C5—H5119.7C2—N1—Cd1122.72 (14)
N5—C6—C7121.9 (2)C1—N1—Cd1130.85 (14)
N5—C6—H6119.1C3—N2—Cd1ii153.59 (19)
C7—C6—H6119.1C2—N3—N4110.16 (17)
N6—C7—C6122.0 (2)C2—N3—C4128.28 (17)
N6—C7—H7119.0N4—N3—C4121.46 (16)
C6—C7—H7119.0C1—N4—N3102.16 (16)
N2i—Cd1—N2ii175.94 (10)C4—N5—C6115.50 (19)
N2i—Cd1—N1iii89.56 (7)C7—N6—C5116.5 (2)
N2ii—Cd1—N1iii87.73 (7)C3—S1—Cd197.98 (7)
N2i—Cd1—N187.73 (7)

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

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: BT2992).

References

  • Bruker (1997). SMART, SAINT and SADABS Bruker AXS Inc., Madison, Wisconsin, USA.
  • Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. [PubMed]
  • Yang, L. Y. & Shi, J. M. (2008). Acta Cryst. E64, m1387. [PMC free article] [PubMed]

Articles from Acta Crystallographica Section E: Structure Reports Online are provided here courtesy of International Union of Crystallography