Diaqua-(2,5-di-4-pyridyl-1,3,4-thia-diazole-κN)bis-(thio-cyanato-κN)nickel(II) dihydrate.

In the title mononuclear complex, [Ni(NCS)(2)(C(12)H(8)N(4)S)(2)(H(2)O)(2)]·2H(2)O, the Ni(II) atom is located on an inversion center and is octa-hedrally coordinated by four N atoms from two 2,5-di-4-pyridyl-1,3,4-thia-diazole (bpt) ligands and two thio-cyanate mol-ecules forming the equatorial plane; the axial positions are occupied by two O atoms of coordinated water mol-ecules. O-H⋯O, O-H⋯N and O-H⋯S hydrogen bonds, involving the uncoordinated water molecules, result in the formation of a sheet structure developing parallel to (021).

Related literature

For related structures, see: Ma & Yang (2008 ▶); Du et al. (2002 ▶); Dong et al. (2003 ▶); Gudbjarlson et al. (1991 ▶). For related literature, see: Su et al. (2005 ▶).

Experimental

Crystal data

[Ni(NCS)2(C12H8N4S)2(H2O)2]·2H2O

M = 727.50

Triclinic,

a = 7.0555 (11) Å

b = 8.3034 (13) Å

c = 14.849 (2) Å

α = 104.629 (2)°

β = 93.067 (2)°

γ = 112.228 (2)°

V = 768.3 (2) Å3

Z = 1

Mo Kα radiation

μ = 0.95 mm−1

T = 298 (2) K

0.26 × 0.21 × 0.17 mm

Data collection

Bruker SMART diffractometer

Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T min = 0.789, T max = 0.855

3967 measured reflections

2747 independent reflections

1810 reflections with I > 2σ(I)

R int = 0.028

Refinement

R[F 2 > 2σ(F 2)] = 0.055

wR(F 2) = 0.143

S = 1.06

2747 reflections

205 parameters

H-atom parameters constrained

Δρmax = 0.39 e Å−3

Δρmin = −0.51 e Å−3

Data collection: SMART (Bruker, 1998 ▶); cell refinement: SAINT (Bruker, 1999 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: ORTEPIII (Burnett & Johnson, 1996 ▶), ORTEP-3 for Windows (Farrugia, 1997 ▶) and CAMERON (Pearce et al., 2000 ▶); software used to prepare material for publication: SHELXL97.

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536808030444/dn2378sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808030444/dn2378Isup2.hkl

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

[Ni(NCS)2(C12H8N4S)2(H2O)2]·2H2O	Z = 1
Mr = 727.50	F(000) = 374
Triclinic, P1	Dx = 1.572 Mg m−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 7.0555 (11) Å	Cell parameters from 2721 reflections
b = 8.3034 (13) Å	θ = 1.4–25.2°
c = 14.849 (2) Å	µ = 0.96 mm−1
α = 104.629 (2)°	T = 298 K
β = 93.067 (2)°	Block, green
γ = 112.228 (2)°	0.26 × 0.21 × 0.17 mm
V = 768.3 (2) Å3

Bruker SMART diffractometer	2747 independent reflections
Radiation source: fine-focus sealed tube	1810 reflections with I > 2σ(I)
graphite	Rint = 0.028
φ and ω scans	θmax = 25.3°, θmin = 1.4°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −8→5
Tmin = 0.789, Tmax = 0.855	k = −9→9
3967 measured reflections	l = −17→17

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)] = 0.055	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.143	H-atom parameters constrained
S = 1.06	w = 1/[σ2(Fo2) + (0.0643P)2 + 0.1149P] where P = (Fo2 + 2Fc2)/3
2747 reflections	(Δ/σ)max < 0.001
205 parameters	Δρmax = 0.39 e Å−3
0 restraints	Δρmin = −0.51 e Å−3

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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	0.5000	0.5000	0.5000	0.0397 (3)
S1	−0.0367 (2)	0.2796 (2)	0.90422 (9)	0.0507 (4)
S2	0.7893 (2)	0.05582 (18)	0.46356 (10)	0.0499 (4)
N1	0.4008 (5)	0.4385 (5)	0.6282 (3)	0.0370 (9)
N2	0.3264 (6)	0.2926 (6)	0.9413 (3)	0.0507 (11)
N3	0.2307 (7)	0.2566 (6)	1.0167 (3)	0.0512 (11)
N4	−0.3536 (7)	0.1274 (6)	1.2103 (3)	0.0530 (11)
N5	0.6832 (6)	0.3540 (6)	0.4939 (3)	0.0439 (10)
O1W	0.2492 (4)	0.2685 (4)	0.4104 (2)	0.0456 (8)
H1WA	0.1300	0.2324	0.4268	0.068*
H1WB	0.2655	0.1751	0.3792	0.068*
C1	0.2114 (7)	0.4119 (6)	0.6465 (3)	0.0448 (12)
H1	0.1217	0.4267	0.6042	0.054*
C2	0.1394 (7)	0.3639 (7)	0.7239 (3)	0.0479 (13)
H2	0.0026	0.3409	0.7317	0.058*
C3	0.2717 (7)	0.3502 (6)	0.7897 (3)	0.0392 (11)
C4	0.4712 (8)	0.3790 (7)	0.7725 (3)	0.0490 (13)
H4	0.5656	0.3697	0.8149	0.059*
C5	0.5267 (7)	0.4217 (7)	0.6915 (3)	0.0454 (12)
H5	0.6606	0.4399	0.6803	0.054*
C6	0.2059 (7)	0.3069 (6)	0.8769 (3)	0.0408 (12)
C7	0.0422 (8)	0.2485 (7)	1.0080 (3)	0.0435 (12)
C8	−0.0933 (7)	0.2144 (6)	1.0799 (3)	0.0395 (11)
C9	−0.0247 (8)	0.1812 (7)	1.1595 (3)	0.0514 (13)
H9	0.1090	0.1867	1.1704	0.062*
C10	−0.1584 (8)	0.1398 (8)	1.2222 (4)	0.0573 (15)
H10	−0.1108	0.1191	1.2760	0.069*
C11	−0.4142 (8)	0.1632 (7)	1.1355 (4)	0.0516 (13)
H11	−0.5477	0.1593	1.1273	0.062*
C12	−0.2923 (7)	0.2065 (7)	1.0682 (3)	0.0459 (12)
H12	−0.3433	0.2298	1.0160	0.055*
C13	0.7270 (6)	0.2306 (7)	0.4811 (3)	0.0366 (11)
O2W	0.3283 (5)	−0.0225 (5)	0.3113 (2)	0.0604 (10)
H2WA	0.3641	−0.0509	0.3583	0.091*
H2WB	0.4342	0.0242	0.2871	0.091*

	U11	U22	U33	U12	U13	U23
Ni1	0.0396 (5)	0.0406 (5)	0.0449 (6)	0.0187 (4)	0.0124 (4)	0.0176 (4)
S1	0.0513 (8)	0.0705 (10)	0.0435 (8)	0.0301 (7)	0.0153 (6)	0.0290 (7)
S2	0.0508 (8)	0.0442 (8)	0.0686 (9)	0.0269 (6)	0.0198 (7)	0.0260 (7)
N1	0.034 (2)	0.039 (2)	0.041 (2)	0.0152 (17)	0.0086 (17)	0.0156 (18)
N2	0.046 (3)	0.065 (3)	0.045 (3)	0.022 (2)	0.013 (2)	0.024 (2)
N3	0.051 (3)	0.066 (3)	0.042 (2)	0.023 (2)	0.015 (2)	0.027 (2)
N4	0.051 (3)	0.065 (3)	0.046 (3)	0.023 (2)	0.017 (2)	0.023 (2)
N5	0.045 (2)	0.045 (2)	0.055 (3)	0.027 (2)	0.0162 (19)	0.022 (2)
O1W	0.0367 (18)	0.045 (2)	0.053 (2)	0.0146 (15)	0.0120 (15)	0.0130 (16)
C1	0.041 (3)	0.054 (3)	0.044 (3)	0.018 (2)	0.008 (2)	0.024 (3)
C2	0.037 (3)	0.058 (3)	0.048 (3)	0.014 (2)	0.010 (2)	0.024 (3)
C3	0.041 (3)	0.036 (3)	0.038 (3)	0.011 (2)	0.012 (2)	0.010 (2)
C4	0.045 (3)	0.066 (4)	0.046 (3)	0.027 (3)	0.010 (2)	0.026 (3)
C5	0.042 (3)	0.057 (3)	0.045 (3)	0.024 (2)	0.018 (2)	0.021 (3)
C6	0.044 (3)	0.039 (3)	0.037 (3)	0.014 (2)	0.009 (2)	0.012 (2)
C7	0.047 (3)	0.046 (3)	0.039 (3)	0.018 (2)	0.007 (2)	0.015 (2)
C8	0.044 (3)	0.038 (3)	0.037 (3)	0.016 (2)	0.008 (2)	0.013 (2)
C9	0.045 (3)	0.067 (4)	0.046 (3)	0.022 (3)	0.008 (2)	0.024 (3)
C10	0.056 (3)	0.076 (4)	0.043 (3)	0.024 (3)	0.013 (3)	0.026 (3)
C11	0.043 (3)	0.055 (3)	0.059 (4)	0.021 (3)	0.011 (3)	0.019 (3)
C12	0.047 (3)	0.053 (3)	0.049 (3)	0.026 (2)	0.009 (2)	0.025 (3)
C13	0.033 (3)	0.046 (3)	0.035 (3)	0.016 (2)	0.012 (2)	0.018 (2)
O2W	0.057 (2)	0.061 (2)	0.054 (2)	0.0141 (18)	0.0183 (17)	0.0132 (19)

Ni1—N5	2.072 (4)	C1—H1	0.9300
Ni1—N5i	2.072 (4)	C2—C3	1.371 (6)
Ni1—O1Wi	2.116 (3)	C2—H2	0.9300
Ni1—O1W	2.116 (3)	C3—C4	1.385 (6)
Ni1—N1	2.176 (4)	C3—C6	1.481 (6)
Ni1—N1i	2.176 (4)	C4—C5	1.374 (6)
S1—C7	1.723 (5)	C4—H4	0.9300
S1—C6	1.724 (5)	C5—H5	0.9300
S2—C13	1.635 (5)	C7—C8	1.480 (6)
N1—C1	1.325 (6)	C8—C12	1.380 (6)
N1—C5	1.328 (6)	C8—C9	1.383 (6)
N2—C6	1.304 (6)	C9—C10	1.373 (7)
N2—N3	1.376 (5)	C9—H9	0.9300
N3—C7	1.303 (6)	C10—H10	0.9300
N4—C11	1.310 (6)	C11—C12	1.382 (7)
N4—C10	1.340 (6)	C11—H11	0.9300
N5—C13	1.153 (6)	C12—H12	0.9300
O1W—H1WA	0.8510	O2W—H2WA	0.8456
O1W—H1WB	0.8497	O2W—H2WB	0.8472
C1—C2	1.371 (6)
N5—Ni1—N5i	180.000 (2)	C2—C3—C4	117.8 (4)
N5—Ni1—O1Wi	88.99 (14)	C2—C3—C6	121.6 (4)
N5i—Ni1—O1Wi	91.01 (14)	C4—C3—C6	120.5 (4)
N5—Ni1—O1W	91.01 (14)	C5—C4—C3	118.6 (4)
N5i—Ni1—O1W	88.99 (14)	C5—C4—H4	120.7
O1Wi—Ni1—O1W	180.0	C3—C4—H4	120.7
N5—Ni1—N1	91.17 (14)	N1—C5—C4	124.0 (4)
N5i—Ni1—N1	88.83 (14)	N1—C5—H5	118.0
O1Wi—Ni1—N1	86.52 (12)	C4—C5—H5	118.0
O1W—Ni1—N1	93.48 (13)	N2—C6—C3	123.7 (4)
N5—Ni1—N1i	88.83 (14)	N2—C6—S1	113.8 (3)
N5i—Ni1—N1i	91.17 (14)	C3—C6—S1	122.4 (4)
O1Wi—Ni1—N1i	93.48 (13)	N3—C7—C8	123.5 (4)
O1W—Ni1—N1i	86.52 (12)	N3—C7—S1	113.8 (3)
N1—Ni1—N1i	180.000 (1)	C8—C7—S1	122.7 (4)
C7—S1—C6	87.2 (2)	C12—C8—C9	118.1 (4)
C1—N1—C5	116.3 (4)	C12—C8—C7	121.8 (4)
C1—N1—Ni1	122.2 (3)	C9—C8—C7	119.9 (4)
C5—N1—Ni1	121.4 (3)	C10—C9—C8	118.5 (5)
C6—N2—N3	112.5 (4)	C10—C9—H9	120.7
C7—N3—N2	112.7 (4)	C8—C9—H9	120.7
C11—N4—C10	116.8 (4)	N4—C10—C9	123.8 (5)
C13—N5—Ni1	159.3 (4)	N4—C10—H10	118.1
Ni1—O1W—H1WA	120.3	C9—C10—H10	118.1
Ni1—O1W—H1WB	121.7	N4—C11—C12	124.1 (5)
H1WA—O1W—H1WB	107.7	N4—C11—H11	117.9
N1—C1—C2	124.1 (4)	C12—C11—H11	117.9
N1—C1—H1	118.0	C8—C12—C11	118.6 (4)
C2—C1—H1	118.0	C8—C12—H12	120.7
C1—C2—C3	119.1 (5)	C11—C12—H12	120.7
C1—C2—H2	120.5	N5—C13—S2	179.7 (4)
C3—C2—H2	120.5	H2WA—O2W—H2WB	109.2

D—H···A	D—H	H···A	D···A	D—H···A
O1W—H1WB···O2W	0.85	1.91	2.762 (5)	175.
O2W—H2WB···N4ii	0.85	2.00	2.833 (5)	170.
O1W—H1WA···S2iii	0.85	2.47	3.303 (3)	166.
O2W—H2WA···S2iv	0.85	2.92	3.540 (4)	132.

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1W—H1WB⋯O2W	0.85	1.91	2.762 (5)	175
O2W—H2WB⋯N4i	0.85	2.00	2.833 (5)	170
O1W—H1WA⋯S2ii	0.85	2.47	3.303 (3)	166
O2W—H2WA⋯S2iii	0.85	2.92	3.540 (4)	132

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