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The structure of the title complex, [Zn(NCS)2(C8H12N6)]n, exhibits a one-dimensional zigzag chain through a 1,4-bis­(1,2,4-triazol-1-yl)butane bridge, in which the ZnII atom, lying on a twofold rotation axis, is in a distorted tetra­hedral environment formed by two N atoms of the triazoles and two N atoms from two thio­cyanate ligands.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807051239/at2425sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807051239/at2425Isup2.hkl
Contains datablock I

CCDC reference: 672679

Key indicators

  • Single-crystal X-ray study
  • T = 298 K
  • Mean [sigma](C-C) = 0.004 Å
  • R factor = 0.034
  • wR factor = 0.132
  • Data-to-parameter ratio = 19.4

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT066_ALERT_1_C Predicted and Reported Transmissions Identical . ? PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for N4 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C5
Alert level G PLAT794_ALERT_5_G Check Predicted Bond Valency for Zn1 (2) 2.02
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 3 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 2 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion 1 ALERT type 5 Informative message, check

Comment top

Recently a new class of flexible ligands, [bis(1,2,4-triazol-1-yl)-alkanes], have been found to be very effective in the formation of various interesting extended structures. As bridging ligands, these 1,2,4-triazole derivatives show a great coordination diversity. Among these ligands, 1,4-bis(1,2,4-triazol-1-yl)butane(btb), with a appropriate length between two hetercyclic donors, is expected to play an important role in the construction of transition-metal supramolecular structures. To our knowledge, there are a few reports on the crystal structures of manganese(II) and cadmium(II) complexes with bridging 1,4-bis(1,2,4-triazol-1-yl)butane ligand [Li et al., 2006; Liu et al., 2006]. As part of our investigations of the coordination mode of the ligand in metal complexes incorporating 1,2,4-triazole derivatives, we here report the synthesis and crystal structure of a new polymeric Zn(II) with btb bridges.

The molecular structure of the title complex, with the atom-numbering scheme, is shown in Fig. 1. The Zn(II) atoms are surrounded by two triazoles and two NCS– ions, forming a distorted tetrahedral geometry. The Zn—N bond distances of btb [2.017 (2) Å] are slightly longer than the Zn—N from NCS [1.934 (3) Å]. The N—Zn—N angles around Zn centers range from 102.75 (8)o to 117.45 (13)o. The Zn—N—C angles are 176.8 (3)o, which deviating from 180° expected for sp hybrid orbital of the N atom. The NCS group is almost linear with a N(4)—C(5)—S(1) angle of 177.0 (3)o. The C—N distances [1.143 (4) Å] and C—S distances [1.610 (3) Å] in the SCN moiety show the normal structure of the thiocyanate in the complex.

As shown in Fig. 2, the Zn(II) ions are linked by btb ligands, building up coordination polymers to one-dimensional zigzag chain. The btb ligand adopts an anti-gauche conformation in this complex.

Related literature top

For related literature, see: Gromova et al. (2000); Li et al. (2006); Liu et al. (2006).

Experimental top

1,4-Bis(1,2,4-triazol-1-yl)butane (btb) was prepared according to literature method (Gromova et al., 2000). A 15 mL me thanol of ZnCl2(0.136 g, 1 mmol) was added to a 15 ml me thanol of KSCN (0.348 g, 2 mmol). The resulting precipitate of KCl was filtered off. A 15 ml aqueous solution of btb (0.192 g, 1 mmol) was added to the above filtrate. The reaction mixture was stirred at reflux temperature for 2 h. The colourless single crystals of the title complex were obtained by evaporating the reaction solution at room temperature for one week.

Refinement top

The H atoms were placed in a calculated positions, with C—H = 0.93 or 0.97 Å. All H atoms were included in the final cycle of refinement in riding mode, with Uiso(H) = 1.2Ueq(C,N,O).

Computing details top

Data collection: PROCESS-AUTO (Rigaku, 1998); cell refinement: PROCESS-AUTO (Rigaku, 1998); data reduction: CrystalStructure (Rigaku/MSC, 2004); program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: CRYSTALS (Watkin et al., 1996); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: CrystalStructure (Rigaku/MSC, 2004).

Figures top
[Figure 1] Fig. 1. Molecular structure showing 50% probability displacement ellipsoids.
[Figure 2] Fig. 2. The extended structure of the title complex.
catena-Poly[[bis(thiocyanato-κN)zinc(II)]-µ-1,4-bis(1,2,4-triazol-1- yl)butane] top
Crystal data top
[Zn(NCS)2(C8H12N6)]F(000) = 760.00
Mr = 373.76Dx = 1.519 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71069 Å
Hall symbol: -C 2ycCell parameters from 5666 reflections
a = 15.1950 (9) Åθ = 4.0–27.4°
b = 5.8261 (2) ŵ = 1.76 mm1
c = 18.8040 (7) ÅT = 298 K
β = 100.893 (2)°Platelet, colourless
V = 1634.68 (13) Å30.38 × 0.28 × 0.11 mm
Z = 4
Data collection top
Rigaku R-AXIS RAPID
diffractometer
1473 reflections with F2 > 2σ(F2)
Detector resolution: 10.00 pixels mm-1Rint = 0.049
ω scansθmax = 27.5°
Absorption correction: multi-scan
(ABSCOR; Higashi, 1995)
h = 1919
Tmin = 0.515, Tmax = 0.824k = 77
7229 measured reflectionsl = 2423
1867 independent reflections
Refinement top
Refinement on F2H-atom parameters constrained
R[F2 > 2σ(F2)] = 0.034 w = 1/[0.002Fo2 + σ(Fo2)]/(4Fo2)
wR(F2) = 0.132(Δ/σ)max < 0.001
S = 1.00Δρmax = 0.50 e Å3
1867 reflectionsΔρmin = 0.46 e Å3
96 parameters
Crystal data top
[Zn(NCS)2(C8H12N6)]V = 1634.68 (13) Å3
Mr = 373.76Z = 4
Monoclinic, C2/cMo Kα radiation
a = 15.1950 (9) ŵ = 1.76 mm1
b = 5.8261 (2) ÅT = 298 K
c = 18.8040 (7) Å0.38 × 0.28 × 0.11 mm
β = 100.893 (2)°
Data collection top
Rigaku R-AXIS RAPID
diffractometer
1867 independent reflections
Absorption correction: multi-scan
(ABSCOR; Higashi, 1995)
1473 reflections with F2 > 2σ(F2)
Tmin = 0.515, Tmax = 0.824Rint = 0.049
7229 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.03496 parameters
wR(F2) = 0.132H-atom parameters constrained
S = 1.00Δρmax = 0.50 e Å3
1867 reflectionsΔρmin = 0.46 e Å3
Special details top

Refinement. Refinement using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F2. R-factor (gt) are based on F. The threshold expression of F2 > 2.0 σ(F2) is used only for calculating R-factor (gt).

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Zn10.50000.23651 (6)0.75000.04427 (14)
S10.38748 (10)0.21390 (18)0.91869 (6)0.0815 (3)
N10.40464 (14)0.4526 (3)0.69942 (11)0.0434 (5)
N20.29337 (19)0.7082 (5)0.68471 (14)0.0552 (7)
N30.34510 (17)0.7371 (3)0.63403 (12)0.0423 (5)
N40.45101 (19)0.0641 (5)0.82138 (17)0.0697 (9)
C10.33192 (19)0.5365 (5)0.72290 (14)0.0514 (8)
C20.41033 (18)0.5847 (4)0.64281 (14)0.0452 (7)
C30.3238 (2)0.9165 (4)0.57881 (14)0.0525 (7)
C40.24236 (19)0.8540 (4)0.52201 (14)0.0468 (7)
C50.4231 (2)0.0470 (5)0.86203 (17)0.0560 (8)
H10.31140.47700.76270.063*
H20.45350.57160.61400.055*
H320.31181.05860.60210.061*
H310.37480.93750.55530.061*
H420.19260.82250.54620.055*
H410.22750.98330.48950.055*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Zn10.0450 (2)0.0382 (2)0.0481 (3)0.00000.0050 (2)0.0000
S10.0995 (8)0.0692 (6)0.0903 (7)0.0024 (5)0.0551 (6)0.0129 (5)
N10.0409 (11)0.0462 (11)0.0422 (11)0.0023 (9)0.0056 (9)0.0020 (9)
N20.0512 (14)0.0688 (16)0.0481 (13)0.0132 (11)0.0162 (11)0.0018 (11)
N30.0425 (12)0.0445 (12)0.0383 (11)0.0014 (9)0.0033 (9)0.0008 (9)
N40.0612 (17)0.0663 (17)0.0835 (19)0.0009 (13)0.0181 (14)0.0246 (15)
C10.0490 (16)0.0660 (18)0.0422 (13)0.0042 (13)0.0160 (11)0.0065 (13)
C20.0405 (13)0.0523 (15)0.0442 (13)0.0006 (11)0.0115 (10)0.0024 (11)
C30.0634 (18)0.0432 (14)0.0468 (14)0.0039 (13)0.0001 (12)0.0039 (12)
C40.0507 (15)0.0426 (14)0.0440 (12)0.0090 (11)0.0012 (11)0.0004 (12)
C50.0516 (17)0.0522 (16)0.0664 (18)0.0015 (13)0.0167 (13)0.0038 (15)
Geometric parameters (Å, º) top
Zn1—N12.017 (2)N3—C31.466 (3)
Zn1—N1i2.017 (2)N4—C51.143 (4)
Zn1—N41.934 (3)C3—C41.518 (3)
Zn1—N4i1.934 (3)C4—C4ii1.510 (4)
S1—C51.610 (3)C1—H10.930
N1—C11.356 (3)C2—H20.930
N1—C21.330 (3)C3—H320.970
N2—N31.356 (4)C3—H310.970
N2—C11.304 (4)C4—H420.970
N3—C21.318 (3)C4—H410.970
N1—Zn1—N1i102.75 (8)C3—C4—C4ii112.9 (2)
N1—Zn1—N4108.35 (10)S1—C5—N4177.0 (3)
N1—Zn1—N4i109.46 (10)N1—C1—H1123.0
N1i—Zn1—N4109.46 (10)N2—C1—H1123.0
N1i—Zn1—N4i108.35 (10)N1—C2—H2125.4
N4—Zn1—N4i117.45 (13)N3—C2—H2125.4
Zn1—N1—C1128.93 (18)N3—C3—H32108.9
Zn1—N1—C2126.10 (19)N3—C3—H31108.9
C1—N1—C2103.4 (2)C4—C3—H32108.9
N3—N2—C1102.9 (2)C4—C3—H31108.9
N2—N3—C2110.5 (2)H32—C3—H31109.5
N2—N3—C3120.5 (2)C3—C4—H42108.6
C2—N3—C3129.0 (2)C3—C4—H41108.6
Zn1—N4—C5176.8 (3)C4ii—C4—H42108.6
N1—C1—N2114.0 (2)C4ii—C4—H41108.6
N1—C2—N3109.2 (2)H42—C4—H41109.5
N3—C3—C4111.6 (2)
N1—Zn1—N1i—C1i93.0 (2)Zn1—N1—C1—N2166.49 (19)
N1—Zn1—N1i—C2i70.5 (2)Zn1—N1—C2—N3166.57 (17)
N1i—Zn1—N1—C193.0 (2)C1—N1—C2—N30.3 (2)
N1i—Zn1—N1—C270.5 (2)C2—N1—C1—N20.2 (3)
N4—Zn1—N1—C122.8 (2)N3—N2—C1—N10.5 (3)
N4—Zn1—N1—C2173.7 (2)C1—N2—N3—C20.7 (3)
N4i—Zn1—N1—C1152.0 (2)C1—N2—N3—C3179.6 (2)
N4i—Zn1—N1—C244.5 (2)N2—N3—C2—N10.6 (3)
N4—Zn1—N1i—C1i152.0 (2)N2—N3—C3—C473.6 (3)
N4—Zn1—N1i—C2i44.5 (2)C2—N3—C3—C4105.1 (3)
N4i—Zn1—N1i—C1i22.8 (2)C3—N3—C2—N1179.4 (2)
N4i—Zn1—N1i—C2i173.7 (2)N3—C3—C4—C4ii64.9 (3)
Symmetry codes: (i) x+1, y, z+3/2; (ii) x+1/2, y+3/2, z+1.

Experimental details

Crystal data
Chemical formula[Zn(NCS)2(C8H12N6)]
Mr373.76
Crystal system, space groupMonoclinic, C2/c
Temperature (K)298
a, b, c (Å)15.1950 (9), 5.8261 (2), 18.8040 (7)
β (°) 100.893 (2)
V3)1634.68 (13)
Z4
Radiation typeMo Kα
µ (mm1)1.76
Crystal size (mm)0.38 × 0.28 × 0.11
Data collection
DiffractometerRigaku R-AXIS RAPID
diffractometer
Absorption correctionMulti-scan
(ABSCOR; Higashi, 1995)
Tmin, Tmax0.515, 0.824
No. of measured, independent and
observed [F2 > 2σ(F2)] reflections
7229, 1867, 1473
Rint0.049
(sin θ/λ)max1)0.649
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.034, 0.132, 1.00
No. of reflections1867
No. of parameters96
No. of restraints?
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.50, 0.46

Computer programs: PROCESS-AUTO (Rigaku, 1998), CrystalStructure (Rigaku/MSC, 2004), SIR97 (Altomare et al., 1999), CRYSTALS (Watkin et al., 1996), ORTEP-3 for Windows (Farrugia, 1997).

Selected geometric parameters (Å, º) top
Zn1—N12.017 (2)N1—C11.356 (3)
Zn1—N41.934 (3)N1—C21.330 (3)
S1—C51.610 (3)N2—N31.356 (4)
N1—Zn1—N1i102.75 (8)Zn1—N1—C1128.93 (18)
N1—Zn1—N4108.35 (10)Zn1—N1—C2126.10 (19)
N1—Zn1—N4i109.46 (10)Zn1—N4—C5176.8 (3)
N4—Zn1—N4i117.45 (13)S1—C5—N4177.0 (3)
Symmetry code: (i) x+1, y, z+3/2.
 

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