Tetra-aqua-bis(3,5-di-4-pyridyl-1,2,4-triazolato-κN)nickel(II) dihydrate.

The Ni(II) atom in the title compound, [Ni(C(12)H(8)N(5))(2)(H(2)O)(4)]·2H(2)O, lies on a center of inversion and is coordinated by the N atoms of two 3,5-di-4-pyridine-1,2,4-triazolate ligands and by four water O atoms in a slightly distorted octa-hedral geometry. The coordinated and uncoordinated water mol-ecules inter-act with the N-heterocycles through O-H⋯N and O-H⋯O hydrogen bonds, generating a three-dimensional supra-molecular architecture.

Related literature

For magnetic studies of transition metal complexes with 1,2,4- triazole derivatives, see: Haasnoot (2000 ▶). For 3,5-di-4-pyridine-1,2,4-triazole, see: Zhang et al. (2005 ▶, 2006 ▶). For the synthesis, see: Basu & Dutta (1964 ▶).

Experimental

Crystal data

[Ni(C12H8N5)2(H2O)4]·2H2O

M = 611.27

Monoclinic,

a = 7.3390 (15) Å

b = 15.653 (3) Å

c = 11.829 (2) Å

β = 107.20 (3)°

V = 1298.1 (5) Å3

Z = 2

Mo Kα radiation

μ = 0.81 mm−1

T = 293 K

0.43 × 0.27 × 0.21 mm

Data collection

Bruker SMART CCD area-detector diffractometer

Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T min = 0.722, T max = 0.848

10883 measured reflections

2344 independent reflections

2131 reflections with I > 2σ(I)

R int = 0.034

Refinement

R[F 2 > 2σ(F 2)] = 0.036

wR(F 2) = 0.078

S = 1.14

2344 reflections

211 parameters

H atoms treated by a mixture of independent and constrained refinement

Δρmax = 0.26 e Å−3

Δρmin = −0.34 e Å−3

Data collection: SMART (Bruker, 1998 ▶); cell refinement: SAINT (Bruker, 1999 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536809027688/hg2531sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809027688/hg2531Isup2.hkl

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

[Ni(C12H8N5)2(H2O)4]·2H2O	F(000) = 636
Mr = 611.27	Dx = 1.564 Mg m−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 467 reflections
a = 7.3390 (15) Å	θ = 1.5–25.3°
b = 15.653 (3) Å	µ = 0.81 mm−1
c = 11.829 (2) Å	T = 293 K
β = 107.20 (3)°	Block, green
V = 1298.1 (5) Å3	0.43 × 0.27 × 0.21 mm
Z = 2

Bruker SMART CCD area-detector diffractometer	2344 independent reflections
Radiation source: fine-focus sealed tube	2131 reflections with I > 2σ(I)
graphite	Rint = 0.034
φ and ω scans	θmax = 25.2°, θmin = 3.2°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −8→8
Tmin = 0.722, Tmax = 0.848	k = −18→18
10883 measured reflections	l = −14→14

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)] = 0.036	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.078	H atoms treated by a mixture of independent and constrained refinement
S = 1.14	w = 1/[σ2(Fo2) + (0.0259P)2 + 1.0454P] where P = (Fo2 + 2Fc2)/3
2344 reflections	(Δ/σ)max < 0.001
211 parameters	Δρmax = 0.26 e Å−3
0 restraints	Δρmin = −0.34 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
C1	0.4927 (3)	0.33129 (14)	0.6238 (2)	0.0265 (5)
H1C	0.5402	0.3645	0.6914	0.032*
C2	0.4672 (3)	0.24522 (14)	0.6376 (2)	0.0272 (5)
H2C	0.4983	0.2216	0.7131	0.033*
C3	0.3951 (3)	0.19348 (13)	0.53900 (19)	0.0218 (5)
C4	0.3570 (4)	0.23293 (14)	0.4292 (2)	0.0287 (5)
H4A	0.3117	0.2010	0.3603	0.034*
C5	0.3864 (4)	0.31953 (14)	0.4228 (2)	0.0283 (5)
H5A	0.3590	0.3446	0.3483	0.034*
C6	0.3545 (3)	0.10302 (13)	0.55253 (19)	0.0217 (5)
C7	0.2505 (3)	−0.02231 (13)	0.52360 (19)	0.0224 (5)
C8	0.1688 (3)	−0.10334 (14)	0.46845 (19)	0.0232 (5)
C9	0.1536 (4)	−0.17397 (16)	0.5368 (2)	0.0370 (6)
H9A	0.1892	−0.1697	0.6189	0.044*
C10	0.0858 (4)	−0.24977 (16)	0.4823 (2)	0.0411 (7)
H10A	0.0794	−0.2962	0.5301	0.049*
C11	0.0428 (4)	−0.19348 (16)	0.3005 (2)	0.0359 (6)
H11A	0.0042	−0.1995	0.2186	0.043*
C12	0.1111 (4)	−0.11487 (15)	0.3471 (2)	0.0312 (6)
H12A	0.1184	−0.0699	0.2971	0.037*
H1A	0.413 (5)	0.550 (2)	0.686 (3)	0.051 (9)*
H2A	0.149 (5)	0.527 (2)	0.358 (3)	0.051 (10)*
H3A	0.163 (5)	0.426 (2)	0.782 (3)	0.054 (10)*
H1B	0.283 (5)	0.493 (2)	0.633 (3)	0.055 (10)*
H2B	0.257 (4)	0.5122 (18)	0.292 (3)	0.048 (9)*
H3B	0.077 (5)	0.372 (2)	0.691 (3)	0.062 (10)*
N1	0.4525 (3)	0.36961 (11)	0.51811 (16)	0.0237 (4)
N2	0.3943 (3)	0.06670 (12)	0.65942 (16)	0.0279 (5)
N3	0.3259 (3)	−0.01470 (12)	0.64046 (17)	0.0290 (5)
N4	0.2645 (3)	0.04985 (11)	0.46332 (16)	0.0226 (4)
N5	0.0286 (3)	−0.26126 (13)	0.3656 (2)	0.0360 (5)
Ni1	0.5000	0.5000	0.5000	0.01983 (13)
O1	0.3476 (3)	0.53202 (12)	0.61834 (15)	0.0275 (4)
O2	0.2507 (3)	0.50476 (11)	0.35989 (15)	0.0287 (4)
O3	0.1179 (3)	0.42339 (11)	0.70636 (17)	0.0314 (4)

	U11	U22	U33	U12	U13	U23
C1	0.0368 (14)	0.0208 (12)	0.0204 (12)	−0.0048 (10)	0.0062 (10)	−0.0025 (9)
C2	0.0390 (14)	0.0215 (12)	0.0197 (12)	−0.0036 (10)	0.0066 (10)	0.0023 (9)
C3	0.0249 (12)	0.0178 (11)	0.0234 (12)	−0.0009 (9)	0.0083 (9)	−0.0001 (9)
C4	0.0434 (15)	0.0199 (12)	0.0204 (12)	−0.0063 (11)	0.0057 (10)	−0.0029 (9)
C5	0.0416 (15)	0.0216 (12)	0.0199 (12)	−0.0021 (10)	0.0062 (10)	0.0026 (9)
C6	0.0269 (12)	0.0174 (11)	0.0209 (11)	−0.0006 (9)	0.0073 (9)	0.0001 (9)
C7	0.0281 (12)	0.0162 (11)	0.0224 (11)	−0.0009 (9)	0.0068 (9)	−0.0005 (8)
C8	0.0239 (12)	0.0188 (11)	0.0254 (12)	−0.0003 (9)	0.0051 (9)	−0.0010 (9)
C9	0.0588 (18)	0.0260 (13)	0.0251 (13)	−0.0116 (12)	0.0108 (12)	0.0001 (10)
C10	0.0624 (19)	0.0225 (13)	0.0392 (16)	−0.0129 (13)	0.0161 (13)	0.0020 (11)
C11	0.0424 (15)	0.0314 (14)	0.0280 (13)	−0.0042 (11)	0.0014 (11)	−0.0060 (11)
C12	0.0400 (15)	0.0221 (12)	0.0269 (13)	−0.0029 (10)	0.0031 (11)	0.0039 (10)
N1	0.0310 (11)	0.0168 (9)	0.0223 (10)	−0.0024 (8)	0.0067 (8)	−0.0006 (7)
N2	0.0413 (12)	0.0175 (10)	0.0232 (10)	−0.0064 (9)	0.0070 (9)	0.0002 (8)
N3	0.0429 (12)	0.0189 (10)	0.0232 (10)	−0.0071 (9)	0.0067 (9)	0.0009 (8)
N4	0.0281 (10)	0.0161 (9)	0.0222 (10)	−0.0016 (8)	0.0053 (8)	0.0011 (7)
N5	0.0408 (13)	0.0244 (11)	0.0416 (13)	−0.0077 (10)	0.0102 (10)	−0.0075 (9)
Ni1	0.0263 (2)	0.0140 (2)	0.0186 (2)	−0.00180 (17)	0.00564 (16)	−0.00025 (16)
O1	0.0322 (10)	0.0267 (9)	0.0246 (9)	−0.0036 (8)	0.0101 (8)	−0.0021 (7)
O2	0.0288 (10)	0.0329 (10)	0.0228 (9)	0.0044 (8)	0.0054 (7)	−0.0001 (7)
O3	0.0420 (11)	0.0222 (9)	0.0288 (10)	−0.0034 (8)	0.0088 (8)	−0.0015 (7)

C1—N1	1.339 (3)	C10—N5	1.331 (3)
C1—C2	1.377 (3)	C10—H10A	0.9300
C1—H1C	0.9300	C11—N5	1.333 (3)
C2—C3	1.390 (3)	C11—C12	1.380 (3)
C2—H2C	0.9300	C11—H11A	0.9300
C3—C4	1.389 (3)	C12—H12A	0.9300
C3—C6	1.465 (3)	N1—Ni1	2.0921 (18)
C4—C5	1.378 (3)	N2—N3	1.364 (3)
C4—H4A	0.9300	Ni1—O2	2.0753 (19)
C5—N1	1.341 (3)	Ni1—O2i	2.0753 (19)
C5—H5A	0.9300	Ni1—N1i	2.0921 (18)
C6—N2	1.337 (3)	Ni1—O1	2.0945 (17)
C6—N4	1.353 (3)	Ni1—O1i	2.0945 (17)
C7—N3	1.334 (3)	O1—H1A	0.85 (3)
C7—N4	1.356 (3)	O1—H1B	0.82 (3)
C7—C8	1.471 (3)	O2—H2A	0.82 (3)
C8—C12	1.384 (3)	O2—H2B	0.82 (3)
C8—C9	1.393 (3)	O3—H3A	0.85 (3)
C9—C10	1.372 (3)	O3—H3B	0.86 (4)
C9—H9A	0.9300
N1—C1—C2	123.3 (2)	C11—C12—C8	119.6 (2)
N1—C1—H1C	118.3	C11—C12—H12A	120.2
C2—C1—H1C	118.3	C8—C12—H12A	120.2
C1—C2—C3	120.1 (2)	C1—N1—C5	116.65 (19)
C1—C2—H2C	119.9	C1—N1—Ni1	122.37 (14)
C3—C2—H2C	119.9	C5—N1—Ni1	120.94 (15)
C4—C3—C2	116.5 (2)	C6—N2—N3	105.95 (17)
C4—C3—C6	122.7 (2)	C7—N3—N2	105.88 (17)
C2—C3—C6	120.7 (2)	C6—N4—C7	101.41 (18)
C5—C4—C3	119.8 (2)	C10—N5—C11	115.9 (2)
C5—C4—H4A	120.1	O2—Ni1—O2i	180.0
C3—C4—H4A	120.1	O2—Ni1—N1i	90.99 (7)
N1—C5—C4	123.5 (2)	O2i—Ni1—N1i	89.01 (7)
N1—C5—H5A	118.2	O2—Ni1—N1	89.01 (7)
C4—C5—H5A	118.2	O2i—Ni1—N1	90.99 (7)
N2—C6—N4	113.30 (19)	N1i—Ni1—N1	180.0
N2—C6—C3	121.29 (19)	O2—Ni1—O1	90.36 (8)
N4—C6—C3	125.27 (19)	O2i—Ni1—O1	89.64 (8)
N3—C7—N4	113.45 (19)	N1i—Ni1—O1	88.45 (7)
N3—C7—C8	121.77 (19)	N1—Ni1—O1	91.55 (7)
N4—C7—C8	124.7 (2)	O2—Ni1—O1i	89.64 (8)
C12—C8—C9	116.5 (2)	O2i—Ni1—O1i	90.36 (8)
C12—C8—C7	122.2 (2)	N1i—Ni1—O1i	91.55 (7)
C9—C8—C7	121.3 (2)	N1—Ni1—O1i	88.45 (7)
C10—C9—C8	119.6 (2)	O1—Ni1—O1i	180.0
C10—C9—H9A	120.2	Ni1—O1—H1A	117 (2)
C8—C9—H9A	120.2	Ni1—O1—H1B	115 (2)
N5—C10—C9	124.3 (2)	H1A—O1—H1B	104 (3)
N5—C10—H10A	117.8	Ni1—O2—H2A	128 (2)
C9—C10—H10A	117.8	Ni1—O2—H2B	119 (2)
N5—C11—C12	124.1 (2)	H2A—O2—H2B	103 (3)
N5—C11—H11A	118.0	H3A—O3—H3B	106 (3)
C12—C11—H11A	118.0
N1—C1—C2—C3	−0.5 (4)	C4—C5—N1—Ni1	178.32 (19)
C1—C2—C3—C4	1.7 (3)	N4—C6—N2—N3	−0.5 (3)
C1—C2—C3—C6	−175.6 (2)	C3—C6—N2—N3	175.4 (2)
C2—C3—C4—C5	−1.7 (4)	N4—C7—N3—N2	−0.2 (3)
C6—C3—C4—C5	175.6 (2)	C8—C7—N3—N2	177.4 (2)
C3—C4—C5—N1	0.5 (4)	C6—N2—N3—C7	0.4 (2)
C4—C3—C6—N2	179.4 (2)	N2—C6—N4—C7	0.4 (3)
C2—C3—C6—N2	−3.4 (3)	C3—C6—N4—C7	−175.3 (2)
C4—C3—C6—N4	−5.2 (4)	N3—C7—N4—C6	−0.2 (3)
C2—C3—C6—N4	172.1 (2)	C8—C7—N4—C6	−177.6 (2)
N3—C7—C8—C12	−172.1 (2)	C9—C10—N5—C11	1.0 (4)
N4—C7—C8—C12	5.1 (4)	C12—C11—N5—C10	−0.2 (4)
N3—C7—C8—C9	4.9 (4)	C1—N1—Ni1—O2	−142.48 (19)
N4—C7—C8—C9	−177.8 (2)	C5—N1—Ni1—O2	40.10 (19)
C12—C8—C9—C10	0.6 (4)	C1—N1—Ni1—O2i	37.52 (19)
C7—C8—C9—C10	−176.6 (2)	C5—N1—Ni1—O2i	−139.90 (19)
C8—C9—C10—N5	−1.2 (5)	C1—N1—Ni1—N1i	139 (100)
N5—C11—C12—C8	−0.4 (4)	C5—N1—Ni1—N1i	−39 (100)
C9—C8—C12—C11	0.2 (4)	C1—N1—Ni1—O1	−52.15 (19)
C7—C8—C12—C11	177.3 (2)	C5—N1—Ni1—O1	130.43 (19)
C2—C1—N1—C5	−0.7 (4)	C1—N1—Ni1—O1i	127.85 (19)
C2—C1—N1—Ni1	−178.26 (18)	C5—N1—Ni1—O1i	−49.57 (19)
C4—C5—N1—C1	0.8 (4)

D—H···A	D—H	H···A	D···A	D—H···A
O2—H2A···O3ii	0.82 (3)	2.03 (3)	2.818 (3)	160 (3)
O3—H3A···N4iii	0.85 (3)	2.09 (3)	2.939 (3)	172 (3)
O3—H3B···N5iv	0.86 (4)	1.94 (4)	2.789 (3)	173 (3)

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O2—H2A⋯O3i	0.82 (3)	2.03 (3)	2.818 (3)	160 (3)
O3—H3A⋯N4ii	0.85 (3)	2.09 (3)	2.939 (3)	172 (3)
O3—H3B⋯N5iii	0.86 (4)	1.94 (4)	2.789 (3)	173 (3)

Symmetry codes: (i) ; (ii) ; (iii) .