Poly[bis-(acetonitrile-κN)di-μ-thio-cyanato-κN,S;κS,N-nickel(II)].

In the title compound, [Ni(NCS)(2)(CH(3)CN)(2)](n), the Ni(II) cation is coordinated by two N-bonded and two S-bonded thio-cyanate anions, as well as two acetonitrile mol-ecules in an octa-hedral NiN(4)S(2) coordination mode. The asymmetric unit comprises one nickel cation, two thio-cyanate anions and two actonitrile mol-ecules. In the crystal, the Ni(II) cations are connected by bridging thio-cyanate anions into a three-dimensional coordination network.

Related literature

For background of this work see: Boeckmann & Näther (2010 ▶); Wriedt et al. (2009a ▶,b ▶).

Experimental

Crystal data

[Ni(NCS)2(C2H3N)2]

M = 256.98

Orthorhombic,

a = 9.0666 (4) Å

b = 9.1215 (3) Å

c = 12.0696 (6) Å

V = 998.17 (7) Å3

Z = 4

Mo Kα radiation

μ = 2.32 mm−1

T = 293 K

0.11 × 0.09 × 0.06 mm

Data collection

Stoe IPDS-2 diffractometer

Absorption correction: numerical (X-SHAPE and X-RED32; Stoe & Cie, 2008) ▶ T min = 0.683, T max = 0.772

11157 measured reflections

2694 independent reflections

2479 reflections with I > 2σ(I)

R int = 0.023

Refinement

R[F 2 > 2σ(F 2)] = 0.027

wR(F 2) = 0.051

S = 1.29

2694 reflections

120 parameters

H-atom parameters constrained

Δρmax = 0.29 e Å−3

Δρmin = −0.28 e Å−3

Absolute structure: Flack (1983 ▶), 1141 Friedel pairs

Flack parameter: −0.003 (13)

Data collection: X-AREA (Stoe & Cie, 2008) ▶; cell refinement: X-AREA ▶; data reduction: X-AREA; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008) ▶; molecular graphics: XP in SHELXTL (Sheldrick, 2008 ▶) and DIAMOND (Brandenburg, 1999 ▶); software used to prepare material for publication: XCIF in SHELXTL.

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536811004132/im2264sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536811004132/im2264Isup2.hkl

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

[Ni(NCS)2(C2H3N)2]	F(000) = 520
Mr = 256.98	Dx = 1.710 Mg m−3
Orthorhombic, P212121	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2ac 2ab	Cell parameters from 11157 reflections
a = 9.0666 (4) Å	θ = 2.8–29.2°
b = 9.1215 (3) Å	µ = 2.32 mm−1
c = 12.0696 (6) Å	T = 293 K
V = 998.17 (7) Å3	Block, blue
Z = 4	0.11 × 0.09 × 0.06 mm

Stoe IPDS-2 diffractometer	2694 independent reflections
Radiation source: fine-focus sealed tube	2479 reflections with I > 2σ(I)
graphite	Rint = 0.023
ω scans	θmax = 29.2°, θmin = 2.8°
Absorption correction: numerical (X-SHAPE and X-RED32; Stoe & Cie, 2008)	h = −12→10
Tmin = 0.683, Tmax = 0.772	k = −12→12
11157 measured reflections	l = −16→16

Refinement on F2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.027	H-atom parameters constrained
wR(F2) = 0.051	w = 1/[σ2(Fo2) + (0.0221P)2] where P = (Fo2 + 2Fc2)/3
S = 1.29	(Δ/σ)max = 0.001
2694 reflections	Δρmax = 0.29 e Å−3
120 parameters	Δρmin = −0.28 e Å−3
0 restraints	Absolute structure: Flack (1983), 1127 Friedel pairs
Primary atom site location: structure-invariant direct methods	Flack parameter: −0.003 (13)

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 > 2sigma(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	−0.10172 (3)	0.83322 (3)	0.62898 (2)	0.02615 (6)
N1	−0.0070 (2)	1.0335 (2)	0.63730 (18)	0.0388 (4)
C1	0.0391 (2)	1.1504 (3)	0.64845 (15)	0.0307 (4)
S1	0.10459 (8)	1.31745 (6)	0.66142 (4)	0.03781 (12)
N2	0.0983 (2)	0.7362 (2)	0.61691 (15)	0.0356 (4)
C2	0.2172 (2)	0.6972 (2)	0.60194 (15)	0.0283 (4)
S2	0.38867 (6)	0.64753 (7)	0.58006 (4)	0.03776 (13)
N3	−0.2036 (2)	0.6293 (2)	0.62176 (17)	0.0341 (4)
C3	−0.2491 (2)	0.5139 (3)	0.6242 (2)	0.0335 (4)
C4	−0.3109 (3)	0.3669 (3)	0.6278 (3)	0.0468 (6)
H4A	−0.4134	0.3723	0.6472	0.070*
H4B	−0.2593	0.3098	0.6823	0.070*
H4C	−0.3007	0.3215	0.5565	0.070*
N4	−0.3065 (2)	0.9326 (2)	0.63801 (17)	0.0365 (4)
C5	−0.4170 (2)	0.9893 (2)	0.63197 (19)	0.0344 (4)
C6	−0.5579 (3)	1.0633 (3)	0.6230 (3)	0.0452 (5)
H6A	−0.5743	1.1215	0.6881	0.068*
H6B	−0.6351	0.9920	0.6161	0.068*
H6C	−0.5575	1.1256	0.5589	0.068*

	U11	U22	U33	U12	U13	U23
Ni1	0.02348 (10)	0.02426 (11)	0.03072 (11)	−0.00044 (11)	−0.00046 (11)	−0.00142 (9)
N1	0.0458 (11)	0.0336 (10)	0.0371 (9)	−0.0091 (8)	−0.0039 (10)	−0.0018 (9)
C1	0.0340 (9)	0.0322 (11)	0.0258 (9)	−0.0008 (9)	−0.0008 (7)	0.0003 (8)
S1	0.0523 (3)	0.0278 (3)	0.0333 (2)	−0.0104 (3)	−0.0001 (2)	0.00087 (19)
N2	0.0288 (7)	0.0434 (9)	0.0346 (9)	0.0041 (9)	0.0021 (10)	−0.0025 (7)
C2	0.0318 (9)	0.0280 (10)	0.0252 (8)	−0.0010 (8)	−0.0010 (7)	−0.0013 (7)
S2	0.0262 (2)	0.0527 (3)	0.0343 (2)	0.0089 (3)	0.0010 (2)	0.0033 (2)
N3	0.0339 (8)	0.0314 (10)	0.0369 (9)	−0.0033 (7)	0.0016 (9)	−0.0011 (9)
C3	0.0351 (9)	0.0332 (11)	0.0322 (9)	−0.0013 (8)	−0.0007 (9)	0.0025 (9)
C4	0.0585 (15)	0.0327 (12)	0.0492 (13)	−0.0105 (11)	−0.0028 (14)	−0.0001 (12)
N4	0.0334 (9)	0.0379 (10)	0.0382 (9)	0.0053 (8)	−0.0016 (9)	−0.0003 (9)
C5	0.0333 (10)	0.0368 (10)	0.0332 (9)	−0.0002 (9)	0.0007 (10)	−0.0034 (9)
C6	0.0326 (10)	0.0485 (13)	0.0547 (14)	0.0061 (10)	0.0018 (12)	−0.0008 (13)

Ni1—N1	2.0210 (19)	S2—Ni1iv	2.5305 (6)
Ni1—N2	2.0231 (18)	N3—C3	1.131 (3)
Ni1—N4	2.0685 (19)	C3—C4	1.454 (3)
Ni1—N3	2.0782 (18)	C4—H4A	0.9600
Ni1—S2i	2.5305 (6)	C4—H4B	0.9600
Ni1—S1ii	2.5341 (6)	C4—H4C	0.9600
N1—C1	1.154 (3)	N4—C5	1.130 (3)
C1—S1	1.643 (2)	C5—C6	1.449 (3)
S1—Ni1iii	2.5341 (6)	C6—H6A	0.9600
N2—C2	1.149 (3)	C6—H6B	0.9600
C2—S2	1.641 (2)	C6—H6C	0.9600
N1—Ni1—N2	91.02 (8)	N2—C2—S2	178.0 (2)
N1—Ni1—N4	89.02 (8)	C2—S2—Ni1iv	100.02 (7)
N2—Ni1—N4	178.89 (9)	C3—N3—Ni1	173.7 (2)
N1—Ni1—N3	178.69 (9)	N3—C3—C4	178.7 (3)
N2—Ni1—N3	90.23 (8)	C3—C4—H4A	109.5
N4—Ni1—N3	89.73 (8)	C3—C4—H4B	109.5
N1—Ni1—S2i	90.09 (6)	H4A—C4—H4B	109.5
N2—Ni1—S2i	89.40 (5)	C3—C4—H4C	109.5
N4—Ni1—S2i	89.50 (6)	H4A—C4—H4C	109.5
N3—Ni1—S2i	90.29 (6)	H4B—C4—H4C	109.5
N1—Ni1—S1ii	90.35 (6)	C5—N4—Ni1	173.2 (2)
N2—Ni1—S1ii	93.23 (6)	N4—C5—C6	179.2 (3)
N4—Ni1—S1ii	87.88 (6)	C5—C6—H6A	109.5
N3—Ni1—S1ii	89.22 (6)	C5—C6—H6B	109.5
S2i—Ni1—S1ii	177.34 (2)	H6A—C6—H6B	109.5
C1—N1—Ni1	174.6 (2)	C5—C6—H6C	109.5
N1—C1—S1	178.77 (19)	H6A—C6—H6C	109.5
C1—S1—Ni1iii	98.29 (7)	H6B—C6—H6C	109.5
C2—N2—Ni1	170.90 (18)