Tetra-aqua-bis-[5-(3-pyrid-yl)tetra-zolido-κN]zinc(II) tetra-hydrate.

The title compound, [Zn(C(6)H(4)N(5))(2)(H(2)O)(4)]·4H(2)O, was synthesized by the hydro-thermal reaction of Zn(CH(3)COO)(2)·2H(2)O with 3-(2H-tetra-zol-5-yl)pyridine. The Zn(II) ion is located on an inversion center and is coordinated by two pyridine N atoms from two 5-(3-pyrid-yl)tetra-zolide ligands and four coordinated water mol-ecules in a slightly distorted octa-hedral geometry. The dihedral angle between the pyridine and tetra-zole rings is 9.920 (7)°. In the crystal, mol-ecules are linked into a three-dimensional network by inter-molecular O-H⋯O and O-H⋯N hydrogen bonds involving the tetra-zole group N atoms, the aqua ligands and solvent water mol-ecules.

Related literature

For background to 5-(3-pyrid­yl)tetra­zolate complexes, see: Xiong et al. (2002 ▶); Wang et al. (2005 ▶). For a related structure, see: Zhang et al. (2006 ▶). For hydrogen-bond motifs, see: Bernstein et al. (1995 ▶).

Experimental

Crystal data

[Zn(C6H4N5)2(H2O)4]·4H2O

M = 501.78

Triclinic,

a = 8.0930 (13) Å

b = 8.5836 (14) Å

c = 8.7082 (14) Å

α = 85.942 (2)°

β = 65.075 (2)°

γ = 72.369 (2)°

V = 521.69 (15) Å3

Z = 1

Mo Kα radiation

μ = 1.24 mm−1

T = 296 K

0.35 × 0.23 × 0.18 mm

Data collection

Bruker SMART CCD diffractometer

Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T min = 0.717, T max = 0.800

2640 measured reflections

1814 independent reflections

1788 reflections with I > 2σ(I)

R int = 0.018

Refinement

R[F 2 > 2σ(F 2)] = 0.026

wR(F 2) = 0.071

S = 1.00

1814 reflections

142 parameters

H-atom parameters constrained

Δρmax = 0.25 e Å−3

Δρmin = −0.48 e Å−3

Data collection: SMART (Bruker, 2007) ▶; cell refinement: SAINT (Bruker, 2007) ▶; 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 ▶) and DIAMOND (Brandenburg, 1999 ▶); software used to prepare material for publication: SHELXTL.

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536810048464/lh5162sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536810048464/lh5162Isup2.hkl

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

[Zn(C6H4N5)2(H2O)4]·4H2O	Z = 1
Mr = 501.78	F(000) = 260
Triclinic, P1	Dx = 1.597 Mg m−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 8.0930 (13) Å	Cell parameters from 2640 reflections
b = 8.5836 (14) Å	θ = 2.5–25.0°
c = 8.7082 (14) Å	µ = 1.24 mm−1
α = 85.942 (2)°	T = 296 K
β = 65.075 (2)°	Prism, colorless
γ = 72.369 (2)°	0.35 × 0.23 × 0.18 mm
V = 521.69 (15) Å3

Bruker SMART CCD diffractometer	1814 independent reflections
Radiation source: fine-focus sealed tube	1788 reflections with I > 2σ(I)
graphite	Rint = 0.018
φ and ω scans	θmax = 25.0°, θmin = 2.5°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −8→9
Tmin = 0.717, Tmax = 0.800	k = −10→9
2640 measured reflections	l = −9→10

Refinement on F2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.026	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.071	H-atom parameters constrained
S = 1.00	w = 1/[σ2(Fo2) + (0.038P)2 + 0.3832P] where P = (Fo2 + 2Fc2)/3
1814 reflections	(Δ/σ)max < 0.001
142 parameters	Δρmax = 0.25 e Å−3
0 restraints	Δρmin = −0.48 e Å−3

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
Zn1	1.0000	0.5000	0.0000	0.02415 (12)
N1	0.9006 (2)	0.5872 (2)	0.2605 (2)	0.0253 (3)
N2	1.2471 (2)	0.8188 (2)	0.3456 (2)	0.0295 (4)
N3	1.3341 (2)	0.8789 (2)	0.4176 (2)	0.0323 (4)
N4	1.2417 (3)	0.8856 (2)	0.5824 (2)	0.0316 (4)
N5	1.0910 (2)	0.8308 (2)	0.6230 (2)	0.0277 (4)
O1	1.2917 (2)	0.49525 (18)	−0.06216 (18)	0.0332 (3)
H1A	1.3635	0.4132	−0.0366	0.050*
H1B	1.3182	0.5786	−0.0438	0.050*
O2	0.9302 (2)	0.74166 (18)	−0.05239 (19)	0.0431 (4)
H2A	0.9749	0.7802	−0.1488	0.052*
H2B	0.8479	0.8183	0.0214	0.065*
O3	0.5798 (2)	0.25397 (19)	1.00465 (19)	0.0359 (3)
H3B	0.5938	0.1703	1.0616	0.054*
H3A	0.6317	0.2165	0.9019	0.054*
O4	0.6545 (2)	−0.01658 (18)	0.19326 (18)	0.0337 (3)
H4A	0.6930	0.0211	0.2554	0.051*
H4B	0.5598	−0.0480	0.2593	0.051*
C1	1.0065 (3)	0.6594 (2)	0.2951 (2)	0.0280 (4)
H1	1.1170	0.6696	0.2055	0.034*
C2	0.9644 (3)	0.7203 (2)	0.4543 (2)	0.0233 (4)
C3	0.7977 (3)	0.7081 (3)	0.5869 (2)	0.0284 (4)
H3	0.7630	0.7474	0.6965	0.034*
C4	0.6849 (3)	0.6368 (3)	0.5532 (3)	0.0332 (5)
H4	0.5716	0.6286	0.6401	0.040*
C5	0.7393 (3)	0.5773 (2)	0.3904 (2)	0.0283 (4)
H5	0.6616	0.5287	0.3700	0.034*
C6	1.0978 (3)	0.7907 (2)	0.4753 (2)	0.0234 (4)

	U11	U22	U33	U12	U13	U23
Zn1	0.02550 (18)	0.02944 (19)	0.01939 (18)	−0.01032 (13)	−0.00976 (13)	0.00137 (12)
N1	0.0254 (8)	0.0299 (8)	0.0232 (8)	−0.0103 (7)	−0.0113 (7)	0.0027 (6)
N2	0.0297 (9)	0.0378 (9)	0.0237 (8)	−0.0157 (7)	−0.0099 (7)	0.0023 (7)
N3	0.0321 (9)	0.0394 (10)	0.0304 (9)	−0.0173 (8)	−0.0134 (7)	0.0026 (7)
N4	0.0353 (9)	0.0353 (9)	0.0318 (9)	−0.0161 (8)	−0.0176 (8)	0.0031 (7)
N5	0.0331 (9)	0.0313 (9)	0.0231 (8)	−0.0147 (7)	−0.0127 (7)	0.0033 (7)
O1	0.0273 (7)	0.0398 (8)	0.0351 (8)	−0.0100 (6)	−0.0148 (6)	−0.0026 (6)
O2	0.0585 (10)	0.0300 (8)	0.0218 (7)	−0.0056 (7)	−0.0051 (7)	0.0046 (6)
O3	0.0379 (8)	0.0388 (8)	0.0276 (8)	−0.0126 (7)	−0.0099 (6)	0.0030 (6)
O4	0.0364 (8)	0.0421 (8)	0.0248 (7)	−0.0187 (7)	−0.0099 (6)	0.0004 (6)
C1	0.0277 (10)	0.0370 (11)	0.0201 (9)	−0.0155 (8)	−0.0067 (8)	0.0013 (8)
C2	0.0246 (9)	0.0236 (9)	0.0229 (9)	−0.0071 (7)	−0.0115 (7)	0.0034 (7)
C3	0.0274 (10)	0.0355 (10)	0.0202 (9)	−0.0096 (8)	−0.0076 (8)	−0.0004 (8)
C4	0.0254 (10)	0.0461 (12)	0.0258 (10)	−0.0154 (9)	−0.0055 (8)	0.0021 (9)
C5	0.0253 (10)	0.0357 (11)	0.0275 (10)	−0.0128 (8)	−0.0123 (8)	0.0033 (8)
C6	0.0260 (9)	0.0231 (9)	0.0227 (9)	−0.0086 (7)	−0.0111 (7)	0.0037 (7)

Zn1—O2i	2.0503 (15)	O2—H2A	0.8498
Zn1—O2	2.0503 (15)	O2—H2B	0.8498
Zn1—N1i	2.1662 (16)	O3—H3B	0.8499
Zn1—N1	2.1662 (16)	O3—H3A	0.8499
Zn1—O1i	2.1760 (14)	O4—H4A	0.8498
Zn1—O1	2.1760 (14)	O4—H4B	0.8498
N1—C1	1.333 (3)	C1—C2	1.381 (3)
N1—C5	1.341 (2)	C1—H1	0.9300
N2—C6	1.335 (2)	C2—C3	1.385 (3)
N2—N3	1.339 (2)	C2—C6	1.463 (3)
N3—N4	1.305 (3)	C3—C4	1.373 (3)
N4—N5	1.339 (2)	C3—H3	0.9300
N5—C6	1.329 (3)	C4—C5	1.380 (3)
O1—H1A	0.8499	C4—H4	0.9300
O1—H1B	0.8500	C5—H5	0.9300
O2i—Zn1—O2	180.0	H1A—O1—H1B	106.1
O2i—Zn1—N1i	86.61 (6)	Zn1—O2—H2A	126.3
O2—Zn1—N1i	93.39 (6)	Zn1—O2—H2B	123.6
O2i—Zn1—N1	93.39 (6)	H2A—O2—H2B	110.0
O2—Zn1—N1	86.61 (6)	H3B—O3—H3A	105.1
N1i—Zn1—N1	180.0	H4A—O4—H4B	107.1
O2i—Zn1—O1i	91.09 (7)	N1—C1—C2	124.80 (17)
O2—Zn1—O1i	88.91 (7)	N1—C1—H1	117.6
N1i—Zn1—O1i	92.52 (6)	C2—C1—H1	117.6
N1—Zn1—O1i	87.48 (6)	C1—C2—C3	117.46 (17)
O2i—Zn1—O1	88.91 (7)	C1—C2—C6	119.00 (17)
O2—Zn1—O1	91.09 (7)	C3—C2—C6	123.53 (17)
N1i—Zn1—O1	87.48 (6)	C4—C3—C2	118.58 (18)
N1—Zn1—O1	92.52 (6)	C4—C3—H3	120.7
O1i—Zn1—O1	180.00 (8)	C2—C3—H3	120.7
C1—N1—C5	116.84 (17)	C3—C4—C5	120.07 (18)
C1—N1—Zn1	117.54 (12)	C3—C4—H4	120.0
C5—N1—Zn1	125.61 (13)	C5—C4—H4	120.0
C6—N2—N3	104.97 (16)	N1—C5—C4	122.24 (18)
N4—N3—N2	109.42 (16)	N1—C5—H5	118.9
N3—N4—N5	109.47 (16)	C4—C5—H5	118.9
C6—N5—N4	105.07 (15)	N5—C6—N2	111.07 (16)
Zn1—O1—H1A	118.6	N5—C6—C2	125.41 (17)
Zn1—O1—H1B	122.1	N2—C6—C2	123.50 (17)
O2i—Zn1—N1—C1	109.54 (15)	N1—C1—C2—C6	177.49 (18)
O2—Zn1—N1—C1	−70.46 (15)	C1—C2—C3—C4	0.0 (3)
N1i—Zn1—N1—C1	−69 (100)	C6—C2—C3—C4	−178.70 (19)
O1i—Zn1—N1—C1	−159.52 (15)	C2—C3—C4—C5	0.8 (3)
O1—Zn1—N1—C1	20.48 (15)	C1—N1—C5—C4	−0.7 (3)
O2i—Zn1—N1—C5	−71.60 (16)	Zn1—N1—C5—C4	−179.59 (15)
O2—Zn1—N1—C5	108.40 (16)	C3—C4—C5—N1	−0.5 (3)
N1i—Zn1—N1—C5	110 (100)	N4—N5—C6—N2	0.0 (2)
O1i—Zn1—N1—C5	19.35 (16)	N4—N5—C6—C2	178.35 (17)
O1—Zn1—N1—C5	−160.65 (16)	N3—N2—C6—N5	−0.2 (2)
C6—N2—N3—N4	0.2 (2)	N3—N2—C6—C2	−178.53 (17)
N2—N3—N4—N5	−0.2 (2)	C1—C2—C6—N5	−169.29 (19)
N3—N4—N5—C6	0.1 (2)	C3—C2—C6—N5	9.4 (3)
C5—N1—C1—C2	1.6 (3)	C1—C2—C6—N2	8.8 (3)
Zn1—N1—C1—C2	−179.40 (15)	C3—C2—C6—N2	−172.44 (19)
N1—C1—C2—C3	−1.3 (3)

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1A···O3ii	0.85	2.02	2.848 (2)	165
O1—H1B···O3iii	0.85	1.97	2.813 (2)	171
O2—H2A···N5iv	0.85	1.89	2.733 (2)	171
O2—H2B···O4v	0.85	1.92	2.768 (2)	177
O3—H3B···O4vi	0.85	1.97	2.811 (2)	173
O3—H3A···N2iii	0.85	1.96	2.792 (2)	167
O4—H4A···N4iii	0.85	1.99	2.838 (2)	175
O4—H4B···N3vii	0.85	2.02	2.870 (2)	180

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1—H1A⋯O3i	0.85	2.02	2.848 (2)	165
O1—H1B⋯O3ii	0.85	1.97	2.813 (2)	171
O2—H2A⋯N5iii	0.85	1.89	2.733 (2)	171
O2—H2B⋯O4iv	0.85	1.92	2.768 (2)	177
O3—H3B⋯O4v	0.85	1.97	2.811 (2)	173
O3—H3A⋯N2ii	0.85	1.96	2.792 (2)	167
O4—H4A⋯N4ii	0.85	1.99	2.838 (2)	175
O4—H4B⋯N3vi	0.85	2.02	2.870 (2)	180

Symmetry codes: (i) ; (ii) ; (iii) ; (iv) ; (v) ; (vi) .