Literature DB >> 22346869

Diaqua-bis-[5-(pyrazin-2-yl)-3-(pyridin-4-yl)-1H-1,2,4-triazol-1-ido-κN]zinc.

Bo Li1, Peng-Wen Liu, Jing Chen.   

Abstract

The title mononuclear complex, [Zn(C(11)n class="Species">H(7)N(6))(2)(H(2)O)(2)], is composed of one Zn(II) ion, two deprotonated ppt ligands [Hppt = 5-(pyrazin-2-yl)-3-(pyridin-4-yl)-1H-1,2,4-triazole] and two coordinating water mol-ecules. The asymmetric unit consists of one half-mol-ecule that is completed by application of a centre of symmetry. The Zn(II) atom is six-coordinated in an octa-hedral environment, surrounded by two O atoms in the axial positions and four N atoms in the equatorial plane. Adjacent mononuclear units are further linked via O-H⋯N hydrogen-bonding inter-actions, forming a two-dimensional network along (100).

Entities:  

Year:  2012        PMID： 22346869      PMCID： PMC3274922          DOI： 10.1107/S1600536812002061

Source DB:  PubMed          Journal:  Acta Crystallogr Sect E Struct Rep Online        ISSN： 1600-5368


Related literature

For the use of multidentate ligands containing N-n class="Species">donor heterocyclic groups in the preparation of metal complexes, see: Du et al. (2006 ▶); Li et al. (2010 ▶, 2011 ▶); Wang et al. (2012 ▶). For crystal structures based on the 5-(pyrazin-2-yl)-3-(pyridin-4-yl)-1H-1,2,4-triazole ligand, see: Liu et al. (2009 ▶).

Experimental

Crystal data

[Zn(C11n class="Species">H7N6)2(H2O)2] M = 547.85 Monoclinic, a = 10.568 (10) Å b = 12.574 (11) Å c = 9.373 (8) Å β = 114.483 (14)° V = 1133.5 (17) Å3 Z = 2 Mo Kα radiation μ = 1.13 mm−1 T = 296 K 0.28 × 0.22 × 0.20 mm

Data collection

Bruker SMART CCD area-detector diffractometer Absorption correction: multi-scan (SADABS; Bruker, 1996 ▶) T min = 0.742, T max = 0.805 5516 measured reflections 1995 independent reflections 1476 reflections with I > 2σ(I) R int = 0.032

Refinement

R[F 2 > 2σ(F 2)] = 0.035 wR(F 2) = 0.100 S = 1.13 1995 reflections 170 parameters H-atom parameters constrained Δρmax = 0.78 e Å−3 Δρmin = −1.16 e Å−3 Data collection: SMART (Bruker, 2007 ▶); cell refinement: SAINT (Bruker, 2007 ▶); data reduction: SAIn class="Chemical">NT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: DIAMOND (Brandenburg, 1999 ▶); software used to prepare material for publication: SHELXTL (Sheldrick, 2008 ▶). Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536812002061/vm2152sup1.cif Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536812002061/vm2152Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Zn(C11H7N6)2(H2O)2]F(000) = 560
Mr = 547.85Dx = 1.605 Mg m−3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 2124 reflections
a = 10.568 (10) Åθ = 2.1–27.2°
b = 12.574 (11) ŵ = 1.13 mm−1
c = 9.373 (8) ÅT = 296 K
β = 114.483 (14)°Block, colourless
V = 1133.5 (17) Å30.28 × 0.22 × 0.20 mm
Z = 2
Bruker SMART CCD area-detector diffractometer1995 independent reflections
Radiation source: fine-focus sealed tube1476 reflections with I > 2σ(I)
graphiteRint = 0.032
phi and ω scansθmax = 25.0°, θmin = 2.1°
Absorption correction: multi-scan (SADABS; Bruker, 1996)h = −9→12
Tmin = 0.742, Tmax = 0.805k = −12→14
5516 measured reflectionsl = −11→8
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.035H-atom parameters constrained
wR(F2) = 0.100w = 1/[σ2(Fo2) + (0.0319P)2 + 1.4706P] where P = (Fo2 + 2Fc2)/3
S = 1.13(Δ/σ)max < 0.001
1995 reflectionsΔρmax = 0.78 e Å−3
170 parametersΔρmin = −1.16 e Å−3
0 restraintsExtinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0049 (8)
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.
xyzUiso*/Ueq
Zn11.00000.00001.00000.0345 (2)
O10.8507 (3)0.03619 (18)1.1088 (3)0.0401 (7)
H1A0.8598−0.00731.18190.060*
H1B0.83820.10111.12520.060*
N11.0865 (3)0.1612 (2)1.0734 (3)0.0289 (7)
N21.1330 (4)0.3772 (2)1.1491 (3)0.0373 (8)
N30.8842 (3)0.0902 (2)0.8093 (3)0.0315 (7)
N40.7855 (3)0.0703 (2)0.6615 (3)0.0339 (8)
N50.8335 (3)0.2478 (2)0.6850 (3)0.0279 (7)
N60.4516 (4)0.1950 (3)0.1161 (4)0.0556 (10)
C11.1805 (4)0.1930 (3)1.2132 (4)0.0335 (9)
H11.23120.14241.28720.040*
C21.2040 (4)0.3003 (3)1.2501 (4)0.0370 (9)
H21.27120.31961.34810.044*
C31.0395 (4)0.3452 (3)1.0079 (4)0.0346 (10)
H30.98980.39630.93420.042*
C41.0145 (4)0.2375 (3)0.9682 (3)0.0270 (8)
C50.9116 (4)0.1956 (2)0.8199 (3)0.0269 (8)
C60.7575 (4)0.1661 (2)0.5912 (4)0.0286 (8)
C70.6541 (4)0.1783 (3)0.4281 (4)0.0325 (9)
C80.6080 (4)0.2768 (3)0.3576 (4)0.0385 (10)
H80.64210.33940.41310.046*
C90.5105 (5)0.2796 (3)0.2035 (4)0.0462 (11)
H90.48400.34610.15730.055*
C100.4974 (6)0.1014 (4)0.1848 (5)0.0703 (16)
H100.46030.04030.12640.084*
C110.5966 (5)0.0888 (3)0.3376 (4)0.0611 (14)
H110.62410.02120.37880.073*
U11U22U33U12U13U23
Zn10.0508 (4)0.0163 (3)0.0241 (3)0.0012 (3)0.0031 (3)0.0024 (2)
O10.064 (2)0.0205 (12)0.0351 (13)0.0068 (12)0.0202 (13)0.0035 (10)
N10.037 (2)0.0235 (15)0.0227 (14)0.0021 (13)0.0087 (13)−0.0003 (11)
N20.048 (2)0.0283 (16)0.0275 (15)−0.0072 (14)0.0081 (14)−0.0059 (12)
N30.044 (2)0.0180 (15)0.0244 (14)−0.0005 (13)0.0063 (13)0.0009 (11)
N40.046 (2)0.0230 (15)0.0229 (14)−0.0020 (14)0.0039 (13)0.0004 (11)
N50.0378 (19)0.0204 (14)0.0219 (13)0.0003 (13)0.0089 (13)0.0017 (11)
N60.058 (3)0.067 (3)0.0285 (17)−0.003 (2)0.0046 (16)0.0041 (17)
C10.037 (2)0.033 (2)0.0236 (17)0.0025 (17)0.0055 (16)0.0005 (14)
C20.044 (3)0.036 (2)0.0243 (16)−0.0060 (18)0.0069 (16)−0.0065 (15)
C30.050 (3)0.0229 (18)0.0250 (16)−0.0016 (16)0.0094 (18)0.0020 (14)
C40.039 (2)0.0207 (17)0.0214 (16)0.0010 (15)0.0123 (15)0.0009 (12)
C50.039 (2)0.0180 (16)0.0228 (16)0.0014 (15)0.0116 (15)0.0009 (13)
C60.037 (2)0.0223 (17)0.0244 (16)−0.0002 (15)0.0103 (15)0.0013 (13)
C70.042 (2)0.0292 (19)0.0235 (16)−0.0015 (17)0.0115 (16)0.0006 (14)
C80.047 (3)0.033 (2)0.0306 (18)0.0029 (18)0.0116 (18)0.0024 (15)
C90.047 (3)0.052 (3)0.034 (2)0.009 (2)0.0109 (19)0.0141 (18)
C100.090 (4)0.054 (3)0.036 (2)−0.018 (3)−0.005 (2)−0.008 (2)
C110.088 (4)0.034 (2)0.037 (2)−0.009 (2)0.001 (2)0.0009 (18)
Zn1—N32.040 (3)N6—C91.329 (5)
Zn1—N3i2.040 (3)N6—C101.332 (6)
Zn1—N1i2.212 (3)C1—C21.390 (5)
Zn1—N12.212 (3)C1—H10.9300
Zn1—O12.252 (3)C2—H20.9300
Zn1—O1i2.252 (3)C3—C41.401 (5)
O1—H1A0.8501C3—H30.9300
O1—H1B0.8502C4—C51.463 (5)
N1—C11.336 (4)C6—C71.474 (5)
N1—C41.361 (4)C7—C111.388 (5)
N2—C21.343 (5)C7—C81.393 (5)
N2—C31.343 (4)C8—C91.385 (5)
N3—C51.352 (4)C8—H80.9300
N3—N41.368 (4)C9—H90.9300
N4—C61.346 (4)C10—C111.390 (6)
N5—C51.359 (4)C10—H100.9300
N5—C61.375 (4)C11—H110.9300
N3—Zn1—N3i180.00 (12)N2—C2—C1122.2 (3)
N3—Zn1—N1i102.48 (11)N2—C2—H2118.9
N3i—Zn1—N1i77.52 (11)C1—C2—H2118.9
N3—Zn1—N177.52 (11)N2—C3—C4122.1 (3)
N3i—Zn1—N1102.48 (11)N2—C3—H3118.9
N1i—Zn1—N1180.0C4—C3—H3118.9
N3—Zn1—O190.35 (12)N1—C4—C3120.1 (3)
N3i—Zn1—O189.65 (12)N1—C4—C5114.0 (3)
N1i—Zn1—O192.83 (11)C3—C4—C5125.8 (3)
N1—Zn1—O187.17 (11)N3—C5—N5112.2 (3)
N3—Zn1—O1i89.65 (12)N3—C5—C4118.4 (3)
N3i—Zn1—O1i90.35 (12)N5—C5—C4129.5 (3)
N1i—Zn1—O1i87.17 (11)N4—C6—N5113.9 (3)
N1—Zn1—O1i92.83 (11)N4—C6—C7121.3 (3)
O1—Zn1—O1i180.0N5—C6—C7124.8 (3)
Zn1—O1—H1A111.6C11—C7—C8116.9 (3)
Zn1—O1—H1B117.7C11—C7—C6119.9 (3)
H1A—O1—H1B116.5C8—C7—C6123.2 (3)
C1—N1—C4117.7 (3)C9—C8—C7118.7 (3)
C1—N1—Zn1128.5 (2)C9—C8—H8120.7
C4—N1—Zn1112.7 (2)C7—C8—H8120.7
C2—N2—C3116.6 (3)N6—C9—C8125.4 (4)
C5—N3—N4107.7 (3)N6—C9—H9117.3
C5—N3—Zn1116.6 (2)C8—C9—H9117.3
N4—N3—Zn1135.6 (2)N6—C10—C11124.5 (4)
C6—N4—N3104.6 (3)N6—C10—H10117.7
C5—N5—C6101.6 (3)C11—C10—H10117.7
C9—N6—C10115.2 (3)C7—C11—C10119.3 (4)
N1—C1—C2121.3 (3)C7—C11—H11120.3
N1—C1—H1119.4C10—C11—H11120.3
C2—C1—H1119.4
N3—Zn1—N1—C1173.8 (3)N2—C3—C4—C5177.7 (4)
N3i—Zn1—N1—C1−6.2 (3)N4—N3—C5—N50.8 (4)
O1—Zn1—N1—C182.8 (3)Zn1—N3—C5—N5177.4 (2)
O1i—Zn1—N1—C1−97.2 (3)N4—N3—C5—C4179.8 (3)
N3—Zn1—N1—C46.1 (2)Zn1—N3—C5—C4−3.6 (4)
N3i—Zn1—N1—C4−173.9 (2)C6—N5—C5—N3−0.5 (4)
O1—Zn1—N1—C4−84.9 (2)C6—N5—C5—C4−179.4 (4)
O1i—Zn1—N1—C495.1 (2)N1—C4—C5—N39.0 (5)
N1i—Zn1—N3—C5178.8 (3)C3—C4—C5—N3−169.2 (4)
N1—Zn1—N3—C5−1.2 (3)N1—C4—C5—N5−172.2 (3)
O1—Zn1—N3—C585.8 (3)C3—C4—C5—N59.6 (6)
O1i—Zn1—N3—C5−94.2 (3)N3—N4—C6—N50.4 (4)
N1i—Zn1—N3—N4−5.9 (4)N3—N4—C6—C7−179.8 (3)
N1—Zn1—N3—N4174.1 (4)C5—N5—C6—N40.0 (4)
O1—Zn1—N3—N4−98.8 (4)C5—N5—C6—C7−179.8 (3)
O1i—Zn1—N3—N481.2 (4)N4—C6—C7—C11−8.2 (6)
C5—N3—N4—C6−0.7 (4)N5—C6—C7—C11171.6 (4)
Zn1—N3—N4—C6−176.3 (3)N4—C6—C7—C8171.0 (4)
C4—N1—C1—C20.1 (5)N5—C6—C7—C8−9.2 (6)
Zn1—N1—C1—C2−167.1 (3)C11—C7—C8—C9−0.8 (6)
C3—N2—C2—C1−1.5 (6)C6—C7—C8—C9180.0 (4)
N1—C1—C2—N20.8 (6)C10—N6—C9—C8−2.9 (7)
C2—N2—C3—C41.3 (6)C7—C8—C9—N62.6 (7)
C1—N1—C4—C3−0.3 (5)C9—N6—C10—C111.5 (8)
Zn1—N1—C4—C3168.9 (3)C8—C7—C11—C10−0.4 (7)
C1—N1—C4—C5−178.6 (3)C6—C7—C11—C10178.9 (5)
Zn1—N1—C4—C5−9.5 (4)N6—C10—C11—C70.0 (9)
N2—C3—C4—N1−0.4 (6)
D—H···AD—HH···AD···AD—H···A
O1—H1B···N5ii0.851.992.833 (4)173
O1—H1A···N2iii0.852.132.975 (4)175
Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯AD⋯AD—H⋯A
O1—H1B⋯N5i0.851.992.833 (4)173
O1—H1A⋯N2ii0.852.132.975 (4)175

Symmetry codes: (i) ; (ii) .

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