Tetra-aqua-bis[3-(3-pyrid-yl)-5-(4-pyrid-yl)-1,2,4-triazolido]nickel(II) dihydrate.

In the title compound, [Ni(C(12)H(8)N(5))(2)(H(2)O)(4)]·2H(2)O, the Ni(II) atom is coordinated by the two N atoms [Ni-N = 2.094 (3) Å] and four O atoms [Ni-O = 2.063 (3)-2.083 (2) Å] in a distorted octa-hedral geometry. The mol-ecule is centrosymmetric and the Ni(II) atom is located on an inversion center. Inter-molecular O-H⋯N and O-H⋯O hydrogen bonds link the complex into a three-dimensional supra-molecular framework.

Related literature

For hydrogen-bond inter­actions in biological systems, see: Deisenhofer & Michel (1989 ▶). For supra­molecular assembly through hydrogen bonds, see: Beatty (2003 ▶); Li et al. (2006 ▶); Russell & Ward (1996 ▶). For related structures, see: Liu et al. (2008 ▶); Liu & Zhang (2009 ▶); Rarig et al. (2001 ▶).

Experimental

Crystal data

[Ni(C12H8N5)2(H2O)4]·2H2O

M = 611.25

Triclinic,

a = 8.2240 (16) Å

b = 9.1990 (18) Å

c = 9.3850 (19) Å

α = 90.70 (3)°

β = 104.96 (3)°

γ = 96.47 (3)°

V = 680.9 (2) Å3

Z = 1

Mo Kα radiation

μ = 0.77 mm−1

T = 293 K

0.20 × 0.12 × 0.08 mm

Data collection

Bruker SMART CCD area-detector diffractometer

Absorption correction: multi-scan (SADABS; Bruker, 1998 ▶)’ T min = 0.866, T max = 0.943

4042 measured reflections

2437 independent reflections

2258 reflections with I > 2σ(I)

R int = 0.040

Refinement

R[F 2 > 2σ(F 2)] = 0.052

wR(F 2) = 0.150

S = 0.99

2437 reflections

211 parameters

9 restraints

H atoms treated by a mixture of independent and constrained refinement

Δρmax = 0.55 e Å−3

Δρmin = −0.85 e Å−3

Data collection: SMART (Bruker, 1998 ▶); cell refinement: SAINT (Bruker, 1998 ▶); 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.

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536809047102/bg2306sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809047102/bg2306Isup2.hkl

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

[Ni(C12H8N5)2(H2O)4]·2H2O	Z = 1
Mr = 611.25	F(000) = 318
Triclinic, P1	Dx = 1.491 Mg m−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 8.2240 (16) Å	Cell parameters from 2567 reflections
b = 9.1990 (18) Å	θ = 1.5–25.3°
c = 9.3850 (19) Å	µ = 0.77 mm−1
α = 90.70 (3)°	T = 293 K
β = 104.96 (3)°	Block, green
γ = 96.47 (3)°	0.20 × 0.12 × 0.08 mm
V = 680.9 (2) Å3

Bruker SMART CCD area-detector diffractometer	2437 independent reflections
Radiation source: fine-focus sealed tube	2258 reflections with I > 2σ(I)
graphite	Rint = 0.040
φ and ω scans	θmax = 25.2°, θmin = 3.1°
Absorption correction: multi-scan (SADABS; Bruker, 1998)'	h = −9→9
Tmin = 0.866, Tmax = 0.943	k = −9→11
4042 measured reflections	l = −11→11

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)] = 0.052	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.150	H atoms treated by a mixture of independent and constrained refinement
S = 0.99	w = 1/[σ2(Fo2) + (0.0912P)2 + 0.8P] where P = (Fo2 + 2Fc2)/3
2437 reflections	(Δ/σ)max < 0.001
211 parameters	Δρmax = 0.55 e Å−3
9 restraints	Δρmin = −0.85 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
Ni1	0.0000	0.5000	0.5000	0.0217 (2)
C1	0.2767 (4)	0.3042 (4)	0.6004 (4)	0.0291 (7)
H1	0.3256	0.3814	0.6683	0.035*
C2	0.3637 (5)	0.1847 (4)	0.5989 (4)	0.0347 (8)
H2	0.4679	0.1806	0.6663	0.042*
C3	0.2938 (4)	0.0712 (4)	0.4959 (4)	0.0299 (8)
H3	0.3508	−0.0100	0.4928	0.036*
C4	0.1385 (4)	0.0799 (3)	0.3976 (3)	0.0211 (6)
C5	0.0578 (4)	0.2022 (3)	0.4086 (3)	0.0235 (7)
H5A	−0.0480	0.2078	0.3440	0.028*
C6	0.0580 (4)	−0.0361 (3)	0.2837 (3)	0.0214 (6)
C7	−0.1047 (4)	−0.1550 (3)	0.1011 (3)	0.0231 (7)
C8	−0.2408 (4)	−0.2007 (4)	−0.0305 (4)	0.0270 (7)
C9	−0.2480 (5)	−0.3324 (4)	−0.1091 (4)	0.0382 (9)
H9A	−0.1643	−0.3938	−0.0785	0.046*
C10	−0.3798 (6)	−0.3703 (5)	−0.2319 (5)	0.0480 (11)
H10A	−0.3804	−0.4570	−0.2841	0.058*
C11	−0.4989 (5)	−0.1649 (5)	−0.2061 (4)	0.0428 (10)
H11A	−0.5863	−0.1074	−0.2379	0.051*
C12	−0.3699 (5)	−0.1149 (4)	−0.0848 (4)	0.0363 (8)
H12A	−0.3689	−0.0242	−0.0395	0.044*
N1	0.1255 (4)	0.3132 (3)	0.5083 (3)	0.0253 (6)
N2	−0.0797 (3)	−0.0233 (3)	0.1726 (3)	0.0243 (6)
N3	0.1159 (4)	−0.1651 (3)	0.2840 (3)	0.0263 (6)
N4	0.0088 (4)	−0.2439 (3)	0.1640 (3)	0.0276 (6)
N5	−0.5067 (4)	−0.2906 (4)	−0.2810 (4)	0.0442 (9)
O1	0.2181 (3)	0.6258 (3)	0.4839 (3)	0.0321 (6)
O2	0.0796 (4)	0.5155 (3)	0.7297 (3)	0.0353 (6)
O3	0.8076 (4)	0.2539 (3)	0.0662 (3)	0.0405 (7)
H1A	0.302 (4)	0.650 (5)	0.555 (3)	0.059 (15)*
H2A	0.122 (5)	0.580 (3)	0.796 (4)	0.043 (12)*
H3A	0.850 (8)	0.182 (5)	0.103 (6)	0.12 (3)*
H1B	0.210 (5)	0.695 (3)	0.427 (4)	0.043 (12)*
H2B	0.051 (6)	0.440 (3)	0.771 (4)	0.049 (13)*
H3B	0.836 (7)	0.274 (5)	−0.009 (4)	0.069 (17)*

	U11	U22	U33	U12	U13	U23
Ni1	0.0260 (4)	0.0160 (3)	0.0190 (3)	0.0037 (2)	−0.0020 (2)	−0.0023 (2)
C1	0.0293 (18)	0.0210 (17)	0.0308 (18)	0.0002 (13)	−0.0018 (15)	−0.0049 (13)
C2	0.0247 (18)	0.031 (2)	0.040 (2)	0.0061 (14)	−0.0065 (15)	−0.0046 (15)
C3	0.0285 (18)	0.0260 (18)	0.0344 (19)	0.0079 (14)	0.0048 (15)	−0.0010 (14)
C4	0.0249 (16)	0.0183 (16)	0.0203 (15)	0.0011 (12)	0.0068 (13)	0.0007 (12)
C5	0.0241 (17)	0.0199 (16)	0.0223 (16)	0.0026 (12)	−0.0016 (13)	−0.0007 (12)
C6	0.0260 (16)	0.0171 (15)	0.0211 (15)	0.0023 (12)	0.0062 (13)	0.0001 (12)
C7	0.0277 (17)	0.0209 (16)	0.0197 (16)	0.0004 (12)	0.0054 (13)	0.0008 (12)
C8	0.0285 (18)	0.0289 (18)	0.0218 (16)	−0.0021 (14)	0.0057 (14)	0.0005 (13)
C9	0.038 (2)	0.032 (2)	0.036 (2)	0.0010 (16)	−0.0030 (17)	−0.0087 (16)
C10	0.049 (3)	0.051 (3)	0.035 (2)	−0.005 (2)	0.0004 (19)	−0.0144 (18)
C11	0.031 (2)	0.052 (3)	0.039 (2)	−0.0002 (17)	−0.0001 (17)	0.0073 (18)
C12	0.033 (2)	0.038 (2)	0.034 (2)	0.0034 (16)	0.0022 (16)	−0.0022 (16)
N1	0.0311 (15)	0.0184 (14)	0.0242 (14)	0.0033 (11)	0.0031 (12)	−0.0016 (11)
N2	0.0275 (15)	0.0193 (14)	0.0239 (14)	0.0022 (11)	0.0030 (12)	−0.0017 (11)
N3	0.0363 (16)	0.0175 (14)	0.0217 (14)	0.0035 (11)	0.0015 (12)	−0.0013 (10)
N4	0.0356 (16)	0.0224 (15)	0.0203 (14)	0.0040 (12)	−0.0009 (12)	−0.0031 (11)
N5	0.0390 (19)	0.054 (2)	0.0289 (17)	−0.0109 (16)	−0.0033 (14)	0.0008 (15)
O1	0.0298 (13)	0.0263 (13)	0.0320 (14)	0.0000 (10)	−0.0057 (11)	0.0068 (11)
O2	0.0554 (17)	0.0220 (14)	0.0216 (12)	−0.0001 (12)	−0.0001 (12)	0.0005 (10)
O3	0.0514 (18)	0.0363 (16)	0.0345 (15)	0.0052 (13)	0.0128 (14)	−0.0034 (12)

Ni1—O1i	2.063 (3)	C7—N2	1.347 (4)
Ni1—O1	2.063 (3)	C7—C8	1.456 (5)
Ni1—O2	2.083 (2)	C8—C12	1.389 (5)
Ni1—O2i	2.083 (2)	C8—C9	1.398 (5)
Ni1—N1	2.094 (3)	C9—C10	1.373 (6)
Ni1—N1i	2.094 (3)	C9—H9A	0.9300
C1—N1	1.330 (4)	C10—N5	1.331 (6)
C1—C2	1.379 (5)	C10—H10A	0.9300
C1—H1	0.9300	C11—N5	1.333 (5)
C2—C3	1.381 (5)	C11—C12	1.373 (5)
C2—H2	0.9300	C11—H11A	0.9300
C3—C4	1.380 (5)	C12—H12A	0.9300
C3—H3	0.9300	N3—N4	1.376 (4)
C4—C5	1.385 (4)	O1—H1A	0.836 (19)
C4—C6	1.472 (4)	O1—H1B	0.830 (18)
C5—N1	1.345 (4)	O2—H2A	0.828 (18)
C5—H5A	0.9300	O2—H2B	0.836 (19)
C6—N3	1.327 (4)	O3—H3A	0.82 (5)
C6—N2	1.344 (4)	O3—H3B	0.81 (4)
C7—N4	1.337 (4)
O1i—Ni1—O1	180.00 (15)	N4—C7—N2	113.1 (3)
O1i—Ni1—O2	88.62 (11)	N4—C7—C8	121.9 (3)
O1—Ni1—O2	91.38 (11)	N2—C7—C8	125.0 (3)
O1i—Ni1—O2i	91.38 (11)	C12—C8—C9	116.5 (3)
O1—Ni1—O2i	88.62 (11)	C12—C8—C7	121.6 (3)
O2—Ni1—O2i	180.0	C9—C8—C7	121.9 (3)
O1i—Ni1—N1	90.86 (11)	C10—C9—C8	119.4 (4)
O1—Ni1—N1	89.14 (11)	C10—C9—H9A	120.3
O2—Ni1—N1	87.82 (11)	C8—C9—H9A	120.3
O2i—Ni1—N1	92.18 (11)	N5—C10—C9	124.1 (4)
O1i—Ni1—N1i	89.14 (11)	N5—C10—H10A	118.0
O1—Ni1—N1i	90.86 (11)	C9—C10—H10A	118.0
O2—Ni1—N1i	92.18 (11)	N5—C11—C12	124.1 (4)
O2i—Ni1—N1i	87.82 (11)	N5—C11—H11A	117.9
N1—Ni1—N1i	180.000 (1)	C12—C11—H11A	117.9
N1—C1—C2	122.5 (3)	C11—C12—C8	119.5 (4)
N1—C1—H1	118.7	C11—C12—H12A	120.2
C2—C1—H1	118.7	C8—C12—H12A	120.2
C1—C2—C3	119.1 (3)	C1—N1—C5	118.1 (3)
C1—C2—H2	120.5	C1—N1—Ni1	122.7 (2)
C3—C2—H2	120.5	C5—N1—Ni1	118.9 (2)
C4—C3—C2	119.2 (3)	C6—N2—C7	101.9 (3)
C4—C3—H3	120.4	C6—N3—N4	105.3 (3)
C2—C3—H3	120.4	C7—N4—N3	105.8 (3)
C3—C4—C5	118.1 (3)	C10—N5—C11	116.3 (3)
C3—C4—C6	122.0 (3)	Ni1—O1—H1A	125 (3)
C5—C4—C6	119.9 (3)	Ni1—O1—H1B	119 (3)
N1—C5—C4	122.9 (3)	H1A—O1—H1B	107 (3)
N1—C5—H5A	118.5	Ni1—O2—H2A	138 (3)
C4—C5—H5A	118.5	Ni1—O2—H2B	114 (3)
N3—C6—N2	114.0 (3)	H2A—O2—H2B	107 (3)
N3—C6—C4	121.9 (3)	H3A—O3—H3B	111 (3)
N2—C6—C4	124.1 (3)
N1—C1—C2—C3	1.6 (6)	C4—C5—N1—C1	−0.1 (5)
C1—C2—C3—C4	−0.3 (5)	C4—C5—N1—Ni1	174.5 (2)
C2—C3—C4—C5	−1.0 (5)	O1i—Ni1—N1—C1	−129.6 (3)
C2—C3—C4—C6	179.1 (3)	O1—Ni1—N1—C1	50.4 (3)
C3—C4—C5—N1	1.3 (5)	O2—Ni1—N1—C1	−41.0 (3)
C6—C4—C5—N1	−178.8 (3)	O2i—Ni1—N1—C1	139.0 (3)
C3—C4—C6—N3	11.2 (5)	O1i—Ni1—N1—C5	56.0 (2)
C5—C4—C6—N3	−168.7 (3)	O1—Ni1—N1—C5	−124.0 (2)
C3—C4—C6—N2	−169.8 (3)	O2—Ni1—N1—C5	144.6 (2)
C5—C4—C6—N2	10.3 (5)	O2i—Ni1—N1—C5	−35.4 (2)
N4—C7—C8—C12	172.1 (3)	N3—C6—N2—C7	−0.4 (4)
N2—C7—C8—C12	−7.2 (5)	C4—C6—N2—C7	−179.4 (3)
N4—C7—C8—C9	−8.3 (5)	N4—C7—N2—C6	0.5 (4)
N2—C7—C8—C9	172.4 (3)	C8—C7—N2—C6	179.8 (3)
C12—C8—C9—C10	−0.7 (6)	N2—C6—N3—N4	0.1 (4)
C7—C8—C9—C10	179.7 (4)	C4—C6—N3—N4	179.2 (3)
C8—C9—C10—N5	−1.7 (7)	N2—C7—N4—N3	−0.5 (4)
N5—C11—C12—C8	−2.7 (6)	C8—C7—N4—N3	−179.8 (3)
C9—C8—C12—C11	2.8 (5)	C6—N3—N4—C7	0.2 (3)
C7—C8—C12—C11	−177.6 (3)	C9—C10—N5—C11	2.0 (6)
C2—C1—N1—C5	−1.3 (5)	C12—C11—N5—C10	0.2 (6)
C2—C1—N1—Ni1	−175.7 (3)

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1A···N5ii	0.83 (2)	1.92 (3)	2.751 (4)	179 (3)
O1—H1B···N3iii	0.83 (3)	1.95 (3)	2.750 (4)	162 (3)
O2—H2A···O3iv	0.83 (3)	1.93 (3)	2.751 (4)	171 (3)
O2—H2B···N4v	0.84 (3)	1.96 (3)	2.791 (4)	169 (3)
O3—H3A···N2vi	0.82 (5)	2.10 (5)	2.911 (4)	170 (3)
O3—H3B···N4vii	0.82 (4)	2.20 (5)	2.944 (4)	151 (3)

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1—H1A⋯N5i	0.83 (2)	1.92 (3)	2.751 (4)	179 (3)
O1—H1B⋯N3ii	0.83 (3)	1.95 (3)	2.750 (4)	162 (3)
O2—H2A⋯O3iii	0.83 (3)	1.93 (3)	2.751 (4)	171 (3)
O2—H2B⋯N4iv	0.84 (3)	1.96 (3)	2.791 (4)	169 (3)
O3—H3A⋯N2v	0.82 (5)	2.10 (5)	2.911 (4)	170 (3)
O3—H3B⋯N4vi	0.82 (4)	2.20 (5)	2.944 (4)	151 (3)

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