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accesscatena-Poly[[bis[2-(1H-1,2,4-triazol-1-yl-κN4)pyrazine]cadmium(II)]-di-μ-thiocyanato-κ2S:N;κ2N:S]
aDepartment of Chemistry and Chemical Engineering, Institute of Materials Chemistry, Binzhou University, Binzhou 256603, People's Republic of China, and bDepartment of Chemistry, Shandong Normal University, Jinan 250014, People's Republic of China
*Correspondence e-mail: honglizhang1968@yahoo.cn
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].
![[Scheme 1]](bt2992scheme1.gif)
Experimental
Crystal data
|
Data collection: SMART (Bruker, 1997![[Bruker (1997). SMART, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]](../../../../../../logos/arrows/e_arr.gif "Bruker (1997). SMART, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.")
); cell SAINT (Bruker, 1997); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL.
Supporting information
contains datablocks I, global. DOI: 10.1107/S1600536809027135/bt2992sup1.cif
Structure factors: contains datablock I. DOI: 10.1107/S1600536809027135/bt2992Isup2.hkl
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.
All H atoms were placed in calculated positions and refined as riding with C—H = 0.93 Å and Uiso(H) = 1.2Ueq(C).
Data collection: SMART (Bruker, 1997); cell SAINT (Bruker, 1997); data reduction: SAINT (Bruker, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).
![[Figure 1]](./bt2992fig1thm.gif) | 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] |
![[Figure 2]](./bt2992fig2thm.gif) | Fig. 2. Packing diagram of the title compound. |
| [Cd(NCS)2(C6H5N5)2] | F(000) = 1032 |
| Mr = 522.86 | Dx = 1.800 Mg m−3 |
| Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
| Hall symbol: -C 2yc | Cell parameters from 4306 reflections |
| a = 25.818 (4) Å | θ = 2.9–28.3° |
| b = 7.4077 (10) Å | µ = 1.38 mm−1 |
| c = 11.0276 (15) Å | T = 298 K |
| β = 113.843 (2)° | Block, colourless |
| V = 1929.1 (5) Å3 | 0.41 × 0.21 × 0.20 mm |
| Z = 4 |
| Bruker SMART APEX CCD diffractometer | 2085 independent reflections |
| Radiation source: fine-focus sealed tube | 2005 reflections with I > 2σ(I) |
| Graphite monochromator | Rint = 0.022 |
| ϕ and ω scans | θmax = 27.0°, θmin = 1.7° |
| Absorption correction: multi-scan (SADABS; Bruker, 1997) | h = −32→23 |
| Tmin = 0.602, Tmax = 0.770 | k = −7→9 |
| 5381 measured reflections | l = −10→13 |
| Refinement on F2 | Secondary atom site location: difference Fourier map |
| Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
| R[F2 > 2σ(F2)] = 0.022 | H-atom parameters constrained |
| wR(F2) = 0.058 | w = 1/[σ2(Fo2) + (0.0298P)2 + 1.3229P] where P = (Fo2 + 2Fc2)/3 |
| S = 1.10 | (Δ/σ)max = 0.002 |
| 2085 reflections | Δρmax = 0.35 e Å−3 |
| 133 parameters | Δρmin = −0.47 e Å−3 |
| 0 restraints | Extinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
| Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0082 (3) |
| [Cd(NCS)2(C6H5N5)2] | V = 1929.1 (5) Å3 |
| Mr = 522.86 | Z = 4 |
| Monoclinic, C2/c | Mo Kα radiation |
| a = 25.818 (4) Å | µ = 1.38 mm−1 |
| b = 7.4077 (10) Å | T = 298 K |
| c = 11.0276 (15) Å | 0.41 × 0.21 × 0.20 mm |
| β = 113.843 (2)° |
| Bruker SMART APEX CCD diffractometer | 2085 independent reflections |
| Absorption correction: multi-scan (SADABS; Bruker, 1997) | 2005 reflections with I > 2σ(I) |
| Tmin = 0.602, Tmax = 0.770 | Rint = 0.022 |
| 5381 measured reflections |
| R[F2 > 2σ(F2)] = 0.022 | 0 restraints |
| wR(F2) = 0.058 | H-atom parameters constrained |
| S = 1.10 | Δρmax = 0.35 e Å−3 |
| 2085 reflections | Δρmin = −0.47 e Å−3 |
| 133 parameters |
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. |
| x | y | z | Uiso*/Ueq | ||
| C1 | 0.43493 (9) | 0.3626 (3) | 0.9002 (2) | 0.0392 (5) | |
| H1 | 0.4636 | 0.3440 | 0.9838 | 0.047* | |
| C2 | 0.39121 (9) | 0.3614 (3) | 0.6932 (2) | 0.0382 (4) | |
| H2 | 0.3808 | 0.3457 | 0.6027 | 0.046* | |
| C3 | 0.56274 (8) | −0.1295 (3) | 0.5829 (2) | 0.0334 (4) | |
| C4 | 0.30256 (8) | 0.5013 (3) | 0.68395 (18) | 0.0322 (4) | |
| C5 | 0.27688 (11) | 0.5921 (3) | 0.7544 (2) | 0.0455 (5) | |
| H5 | 0.2974 | 0.6177 | 0.8437 | 0.055* | |
| C6 | 0.22301 (10) | 0.5174 (4) | 0.4984 (2) | 0.0493 (5) | |
| H6 | 0.2029 | 0.4949 | 0.4084 | 0.059* | |
| C7 | 0.19638 (11) | 0.6044 (3) | 0.5671 (3) | 0.0505 (6) | |
| H7 | 0.1586 | 0.6371 | 0.5226 | 0.061* | |
| Cd1 | 0.5000 | 0.10030 (3) | 0.7500 | 0.03107 (10) | |
| N1 | 0.43983 (7) | 0.3119 (2) | 0.78646 (17) | 0.0391 (4) | |
| N2 | 0.55550 (9) | −0.1113 (3) | 0.47410 (19) | 0.0455 (5) | |
| N3 | 0.35900 (7) | 0.4377 (2) | 0.74783 (16) | 0.0317 (3) | |
| N4 | 0.38687 (8) | 0.4394 (2) | 0.88241 (17) | 0.0377 (4) | |
| N5 | 0.27701 (8) | 0.4642 (3) | 0.55708 (17) | 0.0422 (4) | |
| N6 | 0.22297 (9) | 0.6433 (3) | 0.6954 (2) | 0.0535 (5) | |
| S1 | 0.57240 (3) | −0.15916 (10) | 0.73782 (5) | 0.05367 (18) |
| U11 | U22 | U33 | U12 | U13 | U23 | |
| C1 | 0.0367 (11) | 0.0455 (11) | 0.0340 (10) | −0.0001 (9) | 0.0129 (9) | −0.0018 (9) |
| C2 | 0.0371 (11) | 0.0444 (11) | 0.0356 (10) | 0.0028 (9) | 0.0172 (9) | −0.0052 (8) |
| C3 | 0.0287 (9) | 0.0379 (10) | 0.0307 (10) | 0.0051 (7) | 0.0089 (8) | −0.0017 (7) |
| C4 | 0.0329 (9) | 0.0331 (9) | 0.0335 (10) | 0.0004 (7) | 0.0162 (8) | 0.0008 (7) |
| C5 | 0.0460 (13) | 0.0563 (14) | 0.0358 (11) | 0.0117 (10) | 0.0181 (10) | −0.0034 (9) |
| C6 | 0.0409 (12) | 0.0649 (15) | 0.0373 (11) | 0.0040 (11) | 0.0106 (9) | −0.0060 (10) |
| C7 | 0.0370 (12) | 0.0666 (16) | 0.0452 (14) | 0.0126 (10) | 0.0138 (11) | 0.0007 (10) |
| Cd1 | 0.03018 (13) | 0.03752 (14) | 0.02687 (13) | 0.000 | 0.01294 (9) | 0.000 |
| N1 | 0.0349 (9) | 0.0439 (10) | 0.0404 (9) | 0.0014 (7) | 0.0171 (7) | −0.0046 (8) |
| N2 | 0.0428 (10) | 0.0607 (12) | 0.0319 (10) | 0.0058 (8) | 0.0141 (8) | 0.0017 (8) |
| N3 | 0.0321 (8) | 0.0356 (8) | 0.0300 (8) | −0.0009 (6) | 0.0153 (7) | −0.0026 (6) |
| N4 | 0.0367 (9) | 0.0465 (9) | 0.0302 (9) | 0.0006 (7) | 0.0138 (7) | −0.0024 (7) |
| N5 | 0.0369 (9) | 0.0549 (10) | 0.0349 (9) | 0.0035 (8) | 0.0146 (7) | −0.0061 (8) |
| N6 | 0.0476 (11) | 0.0696 (13) | 0.0450 (11) | 0.0190 (10) | 0.0204 (9) | −0.0017 (10) |
| S1 | 0.0699 (4) | 0.0614 (4) | 0.0296 (3) | 0.0323 (3) | 0.0201 (3) | 0.0093 (2) |
| C1—N4 | 1.306 (3) | C6—N5 | 1.337 (3) |
| C1—N1 | 1.363 (3) | C6—C7 | 1.372 (3) |
| C1—H1 | 0.9300 | C6—H6 | 0.9300 |
| C2—N1 | 1.313 (3) | C7—N6 | 1.331 (3) |
| C2—N3 | 1.334 (3) | C7—H7 | 0.9300 |
| C2—H2 | 0.9300 | Cd1—N2i | 2.3031 (19) |
| C3—N2 | 1.145 (3) | Cd1—N2ii | 2.3031 (19) |
| C3—S1 | 1.639 (2) | Cd1—N1iii | 2.3528 (18) |
| C4—N5 | 1.312 (3) | Cd1—N1 | 2.3528 (17) |
| C4—C5 | 1.383 (3) | Cd1—S1iii | 2.7220 (6) |
| C4—N3 | 1.418 (2) | Cd1—S1 | 2.7220 (6) |
| C5—N6 | 1.331 (3) | N2—Cd1ii | 2.3031 (19) |
| C5—H5 | 0.9300 | N3—N4 | 1.363 (2) |
| N4—C1—N1 | 114.71 (19) | N2ii—Cd1—N1 | 89.56 (7) |
| N4—C1—H1 | 122.6 | N1iii—Cd1—N1 | 96.47 (9) |
| N1—C1—H1 | 122.6 | N2i—Cd1—S1iii | 96.54 (5) |
| N1—C2—N3 | 109.75 (19) | N2ii—Cd1—S1iii | 86.34 (5) |
| N1—C2—H2 | 125.1 | N1iii—Cd1—S1iii | 173.10 (5) |
| N3—C2—H2 | 125.1 | N1—Cd1—S1iii | 87.01 (5) |
| N2—C3—S1 | 178.9 (2) | N2i—Cd1—S1 | 86.34 (5) |
| N5—C4—C5 | 123.5 (2) | N2ii—Cd1—S1 | 96.54 (5) |
| N5—C4—N3 | 115.64 (17) | N1iii—Cd1—S1 | 87.01 (5) |
| C5—C4—N3 | 120.82 (18) | N1—Cd1—S1 | 173.10 (5) |
| N6—C5—C4 | 120.5 (2) | S1iii—Cd1—S1 | 90.16 (4) |
| N6—C5—H5 | 119.7 | C2—N1—C1 | 103.22 (18) |
| C4—C5—H5 | 119.7 | C2—N1—Cd1 | 122.72 (14) |
| N5—C6—C7 | 121.9 (2) | C1—N1—Cd1 | 130.85 (14) |
| N5—C6—H6 | 119.1 | C3—N2—Cd1ii | 153.59 (19) |
| C7—C6—H6 | 119.1 | C2—N3—N4 | 110.16 (17) |
| N6—C7—C6 | 122.0 (2) | C2—N3—C4 | 128.28 (17) |
| N6—C7—H7 | 119.0 | N4—N3—C4 | 121.46 (16) |
| C6—C7—H7 | 119.0 | C1—N4—N3 | 102.16 (16) |
| N2i—Cd1—N2ii | 175.94 (10) | C4—N5—C6 | 115.50 (19) |
| N2i—Cd1—N1iii | 89.56 (7) | C7—N6—C5 | 116.5 (2) |
| N2ii—Cd1—N1iii | 87.73 (7) | C3—S1—Cd1 | 97.98 (7) |
| N2i—Cd1—N1 | 87.73 (7) |
| Symmetry codes: (i) x, −y, z+1/2; (ii) −x+1, −y, −z+1; (iii) −x+1, y, −z+3/2. |
Experimental details
| Crystal data | |
| Chemical formula | [Cd(NCS)2(C6H5N5)2] |
| Mr | 522.86 |
| Crystal system, space group | Monoclinic, C2/c |
| Temperature (K) | 298 |
| a, b, c (Å) | 25.818 (4), 7.4077 (10), 11.0276 (15) |
| β (°) | 113.843 (2) |
| V (Å3) | 1929.1 (5) |
| Z | 4 |
| Radiation type | Mo Kα |
| µ (mm−1) | 1.38 |
| Crystal size (mm) | 0.41 × 0.21 × 0.20 |
| Data collection | |
| Diffractometer | Bruker SMART APEX CCD diffractometer |
| Absorption correction | Multi-scan (SADABS; Bruker, 1997) |
| Tmin, Tmax | 0.602, 0.770 |
| No. of measured, independent and observed [I > 2σ(I)] reflections | 5381, 2085, 2005 |
| Rint | 0.022 |
| (sin θ/λ)max (Å−1) | 0.639 |
| Refinement | |
| R[F2 > 2σ(F2)], wR(F2), S | 0.022, 0.058, 1.10 |
| No. of reflections | 2085 |
| No. of parameters | 133 |
| H-atom treatment | H-atom parameters constrained |
| Δρmax, Δρmin (e Å−3) | 0.35, −0.47 |
Computer programs: SMART (Bruker, 1997), SAINT (Bruker, 1997), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).
Acknowledgements
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).
References
Bruker (1997). SMART, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Yang, L. Y. & Shi, J. M. (2008). Acta Cryst. E64, m1387. Web of Science CSD CrossRef IUCr Journals Google Scholar
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| CRYSTALLOGRAPHIC COMMUNICATIONS |
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.