Bis(3-acetyl-pyridine-κN)bis-(methanol-κO)bis-(thio-cyanato-κN)nickel(II).

In the crystal structure of the title compound, [Ni(NCS)(2)(C(7)H(7)NO)(2)(CH(3)OH)(2)], the Ni(2+) cations are coordinated by two thio-cyanate anions, two 3-acetyl-pyridine ligands and two methanol mol-ecules within slightly distorted NiN(4)O(2) octa-hedra. The asymmetric unit consists of one Ni(2+) cation, which is located on a center of inversion, as well as one thio-cyanate anion, one 3-acetyl-pyridine ligand and one methanol mol-ecule in general positions. The discrete complexes are linked by two pairs of O-H⋯O hydrogen bonds between the hy-droxy H atom and the acetyl O atom into chains along the b axis.

Related literature

For general background information including details on thermal decomposition reactions and magnetic properties of the precursor and μ-1,3 bridging compounds, see: Näther & Greve (2003 ▶); Boeckmann & Näther (2010 ▶, 2011 ▶); Wöhlert et al. (2011 ▶). For a description of the Cambridge Structural Database, see: Allen (2002 ▶).

Experimental

Crystal data

[Ni(NCS)2(C7H7NO)(CH4O)2]

M = 481.23

Monoclinic,

a = 7.7088 (7) Å

b = 14.6893 (9) Å

c = 9.6887 (8) Å

β = 96.782 (10)°

V = 1089.44 (15) Å3

Z = 2

Mo Kα radiation

μ = 1.11 mm−1

T = 180 K

0.19 × 0.14 × 0.11 mm

Data collection

Stoe IPDS-1 diffractometer

Absorption correction: numerical (X-SHAPE and X-RED32; Stoe & Cie, 2008 ▶) T min = 0.826, T max = 0.881

9642 measured reflections

2555 independent reflections

2041 reflections with I > 2σ(I)

R int = 0.060

Refinement

R[F 2 > 2σ(F 2)] = 0.039

wR(F 2) = 0.101

S = 0.99

2555 reflections

134 parameters

H-atom parameters constrained

Δρmax = 0.41 e Å−3

Δρmin = −0.66 e Å−3

Data collection: X-AREA (Stoe & Cie, 2008 ▶); cell refinement: X-AREA; data reduction: X-RED32 (Stoe & Cie, 2008 ▶); 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 ▶); software used to prepare material for publication: publCIF (Westrip, 2010 ▶).

Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536812008860/jj2122sup1.cif

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536812008860/jj2122Isup2.hkl

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

[Ni(NCS)2(C7H7NO)(CH4O)2]	F(000) = 500
Mr = 481.23	Dx = 1.467 Mg m−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 9642 reflections
a = 7.7088 (7) Å	θ = 2.5–28.0°
b = 14.6893 (9) Å	µ = 1.11 mm−1
c = 9.6887 (8) Å	T = 180 K
β = 96.782 (10)°	Block, blue
V = 1089.44 (15) Å3	0.19 × 0.14 × 0.11 mm
Z = 2

Stoe IPDS-1 diffractometer	2555 independent reflections
Radiation source: fine-focus sealed tube	2041 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.060
φ scans	θmax = 28.0°, θmin = 2.5°
Absorption correction: numerical (X-SHAPE and X-RED32; Stoe & Cie, 2008)	h = −10→10
Tmin = 0.826, Tmax = 0.881	k = −19→18
9642 measured reflections	l = −12→12

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)] = 0.039	H-atom parameters constrained
wR(F2) = 0.101	w = 1/[σ2(Fo2) + (0.0688P)2] where P = (Fo2 + 2Fc2)/3
S = 0.99	(Δ/σ)max < 0.001
2555 reflections	Δρmax = 0.41 e Å−3
134 parameters	Δρmin = −0.66 e Å−3
0 restraints	Extinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.028 (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 > 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	0.5000	0.5000	0.5000	0.01655 (14)
N1	0.6742 (2)	0.59365 (12)	0.5873 (2)	0.0254 (4)
C1	0.7710 (3)	0.62982 (13)	0.6700 (2)	0.0205 (4)
S1	0.90677 (8)	0.68081 (4)	0.78668 (7)	0.03342 (18)
N11	0.6038 (2)	0.51317 (11)	0.30841 (19)	0.0195 (4)
O11	0.6251 (2)	0.28548 (11)	0.0710 (2)	0.0333 (4)
C11	0.6169 (3)	0.43931 (14)	0.2295 (2)	0.0203 (4)
H11	0.5778	0.3827	0.2619	0.024*
C12	0.6841 (3)	0.44086 (14)	0.1032 (2)	0.0199 (4)
C13	0.7383 (3)	0.52410 (16)	0.0541 (2)	0.0248 (5)
H13	0.7830	0.5280	−0.0330	0.030*
C14	0.7256 (3)	0.60105 (15)	0.1351 (3)	0.0265 (5)
H14	0.7621	0.6586	0.1044	0.032*
C15	0.6593 (3)	0.59317 (14)	0.2609 (2)	0.0228 (4)
H15	0.6525	0.6462	0.3162	0.027*
C16	0.6908 (3)	0.35298 (15)	0.0263 (2)	0.0249 (5)
C17	0.7795 (4)	0.3502 (2)	−0.1025 (3)	0.0365 (6)
H17A	0.7727	0.2884	−0.1408	0.055*
H17B	0.9023	0.3677	−0.0800	0.055*
H17C	0.7217	0.3927	−0.1711	0.055*
O21	0.3202 (2)	0.60443 (10)	0.44475 (18)	0.0242 (3)
H1O	0.3466	0.6599	0.4452	0.036*
C21	0.1344 (3)	0.59987 (17)	0.4463 (3)	0.0311 (5)
H21A	0.0818	0.6583	0.4156	0.047*
H21B	0.1085	0.5868	0.5409	0.047*
H21C	0.0862	0.5515	0.3835	0.047*

	U11	U22	U33	U12	U13	U23
Ni1	0.0195 (2)	0.01456 (19)	0.0153 (2)	−0.00132 (13)	0.00091 (13)	−0.00197 (13)
N1	0.0268 (9)	0.0240 (9)	0.0251 (11)	−0.0070 (7)	0.0017 (8)	−0.0042 (7)
C1	0.0229 (10)	0.0166 (9)	0.0223 (11)	−0.0008 (7)	0.0047 (8)	0.0015 (7)
S1	0.0345 (3)	0.0316 (3)	0.0306 (3)	−0.0083 (2)	−0.0113 (2)	−0.0015 (2)
N11	0.0215 (9)	0.0202 (8)	0.0167 (9)	0.0005 (6)	0.0018 (7)	0.0007 (6)
O11	0.0400 (10)	0.0245 (8)	0.0364 (10)	0.0004 (7)	0.0085 (8)	−0.0078 (7)
C11	0.0229 (10)	0.0192 (9)	0.0183 (11)	0.0000 (7)	0.0004 (8)	−0.0006 (8)
C12	0.0190 (9)	0.0224 (10)	0.0176 (10)	0.0017 (7)	−0.0003 (7)	−0.0003 (8)
C13	0.0238 (11)	0.0308 (11)	0.0202 (11)	−0.0013 (8)	0.0040 (8)	0.0046 (9)
C14	0.0285 (11)	0.0226 (10)	0.0285 (12)	−0.0024 (8)	0.0035 (9)	0.0050 (9)
C15	0.0239 (10)	0.0192 (10)	0.0249 (12)	−0.0024 (8)	0.0010 (8)	−0.0003 (8)
C16	0.0244 (10)	0.0274 (11)	0.0218 (11)	0.0039 (8)	−0.0013 (8)	−0.0046 (8)
C17	0.0398 (13)	0.0476 (15)	0.0224 (13)	0.0060 (11)	0.0044 (10)	−0.0088 (11)
O21	0.0221 (7)	0.0184 (7)	0.0318 (9)	0.0034 (5)	0.0019 (6)	0.0038 (6)
C21	0.0231 (11)	0.0335 (12)	0.0368 (14)	0.0041 (9)	0.0046 (9)	0.0042 (10)

Ni1—N1i	2.0357 (18)	C13—C14	1.386 (3)
Ni1—N1	2.0357 (18)	C13—H13	0.9500
Ni1—O21i	2.0943 (14)	C14—C15	1.380 (3)
Ni1—O21	2.0943 (14)	C14—H14	0.9500
Ni1—N11	2.1154 (19)	C15—H15	0.9500
Ni1—N11i	2.1154 (19)	C16—C17	1.493 (4)
N1—C1	1.157 (3)	C17—H17A	0.9800
C1—S1	1.629 (2)	C17—H17B	0.9800
N11—C11	1.338 (3)	C17—H17C	0.9800
N11—C15	1.350 (3)	O21—C21	1.435 (3)
O11—C16	1.216 (3)	O21—H1O	0.8399
C11—C12	1.384 (3)	C21—H21A	0.9800
C11—H11	0.9500	C21—H21B	0.9800
C12—C13	1.394 (3)	C21—H21C	0.9800
C12—C16	1.494 (3)
N1i—Ni1—N1	180.00 (13)	C14—C13—H13	120.7
N1i—Ni1—O21i	89.75 (7)	C12—C13—H13	120.7
N1—Ni1—O21i	90.25 (7)	C15—C14—C13	119.3 (2)
N1i—Ni1—O21	90.25 (7)	C15—C14—H14	120.3
N1—Ni1—O21	89.75 (7)	C13—C14—H14	120.3
O21i—Ni1—O21	180.00 (9)	N11—C15—C14	122.6 (2)
N1i—Ni1—N11	89.80 (7)	N11—C15—H15	118.7
N1—Ni1—N11	90.20 (7)	C14—C15—H15	118.7
O21i—Ni1—N11	89.06 (7)	O11—C16—C17	121.8 (2)
O21—Ni1—N11	90.94 (7)	O11—C16—C12	119.1 (2)
N1i—Ni1—N11i	90.20 (7)	C17—C16—C12	119.1 (2)
N1—Ni1—N11i	89.80 (7)	C16—C17—H17A	109.5
O21i—Ni1—N11i	90.94 (7)	C16—C17—H17B	109.5
O21—Ni1—N11i	89.06 (7)	H17A—C17—H17B	109.5
N11—Ni1—N11i	180.0	C16—C17—H17C	109.5
C1—N1—Ni1	159.66 (19)	H17A—C17—H17C	109.5
N1—C1—S1	179.8 (2)	H17B—C17—H17C	109.5
C11—N11—C15	117.6 (2)	C21—O21—Ni1	126.46 (13)
C11—N11—Ni1	119.28 (14)	C21—O21—H1O	106.7
C15—N11—Ni1	123.16 (15)	Ni1—O21—H1O	123.8
N11—C11—C12	123.58 (19)	O21—C21—H21A	109.5
N11—C11—H11	118.2	O21—C21—H21B	109.5
C12—C11—H11	118.2	H21A—C21—H21B	109.5
C11—C12—C13	118.3 (2)	O21—C21—H21C	109.5
C11—C12—C16	117.70 (19)	H21A—C21—H21C	109.5
C13—C12—C16	124.0 (2)	H21B—C21—H21C	109.5
C14—C13—C12	118.6 (2)

D—H···A	D—H	H···A	D···A	D—H···A
O21—H1O···O11ii	0.84	1.87	2.700 (2)	172

Table 1

Selected geometric parameters (Å, °)

Ni1—N1	2.0357 (18)
Ni1—O21	2.0943 (14)
Ni1—N11	2.1154 (19)

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O21—H1O⋯O11ii	0.84	1.87	2.700 (2)	172

Symmetry code: (ii) .