Bis(cyanato-κN)tetra-kis-(2,6-dimethyl-pyrazine-κN(4))nickel(II).

Reaction of nickel(II) chloride with sodium cyanate and 2,6-di-methyl-pyrazine leads to single crystals of the title com-pound, [Ni(NCO)(2)(C(6)H(8)N(2))(4)]. The nickel(II) cation is located about a centre of inversion and is octa-hedrally coordinated by two cyanate anions and four 2,6-dimethyl-pyrazine ligands, forming discrete complexes.

Related literature

For the background to this work relating to complexes with thio­cyanato and seleno­cyanato and N-donor ligands, see: Boeckmann & Näther (2010 ▶); Wriedt et al. (2009 ▶); Boeckmann et al. (2010 ▶).

Experimental

Crystal data

[Ni(NCO)2(C6H8N2)4]

M = 575.33

Monoclinic,

a = 24.932 (2) Å

b = 8.4963 (3) Å

c = 18.1748 (13) Å

β = 133.148 (7)°

V = 2808.9 (3) Å3

Z = 4

Mo Kα radiation

μ = 0.73 mm−1

T = 293 K

0.07 × 0.04 × 0.03 mm

Data collection

Stoe IPDS-2 diffractometer

Absorption correction: numerical (X-SHAPE and X-RED32; Stoe & Cie 2008 ▶) T min = 0.888, T max = 0.969

8293 measured reflections

3341 independent reflections

2516 reflections with I > 2σ(I)

R int = 0.047

Refinement

R[F 2 > 2σ(F 2)] = 0.039

wR(F 2) = 0.102

S = 1.01

3341 reflections

182 parameters

H-atom parameters constrained

Δρmax = 0.30 e Å−3

Δρmin = −0.40 e Å−3

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, 2011 ▶); software used to prepare material for publication: XCIF in SHELXTL.

Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536812027985/zl2488sup1.cif

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536812027985/zl2488Isup2.hkl

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

[Ni(NCO)2(C6H8N2)4]	F(000) = 1208
Mr = 575.33	Dx = 1.360 Mg m−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2yc	Cell parameters from 8293 reflections
a = 24.932 (2) Å	θ = 2.7–28.0°
b = 8.4963 (3) Å	µ = 0.73 mm−1
c = 18.1748 (13) Å	T = 293 K
β = 133.148 (7)°	Block, green
V = 2808.9 (3) Å3	0.07 × 0.04 × 0.03 mm
Z = 4

Stoe IPDS-2 diffractometer	3341 independent reflections
Radiation source: fine-focus sealed tube	2516 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.047
ω scan	θmax = 28.0°, θmin = 2.7°
Absorption correction: numerical (X-SHAPE and X-RED32; Stoe & Cie 2008)	h = −25→32
Tmin = 0.888, Tmax = 0.969	k = −11→10
8293 measured reflections	l = −23→21

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)] = 0.039	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.102	H-atom parameters constrained
S = 1.01	w = 1/[σ2(Fo2) + (0.0632P)2] where P = (Fo2 + 2Fc2)/3
3341 reflections	(Δ/σ)max < 0.001
182 parameters	Δρmax = 0.30 e Å−3
0 restraints	Δρmin = −0.40 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 > 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	0.7500	0.7500	0.5000	0.01887 (11)
N20	0.64456 (8)	0.8103 (2)	0.34913 (11)	0.0212 (3)
N10	0.79329 (8)	0.6983 (2)	0.43337 (11)	0.0231 (4)
C1	0.68822 (10)	0.4093 (3)	0.46580 (14)	0.0255 (4)
N1	0.71677 (9)	0.5219 (2)	0.47971 (13)	0.0275 (4)
N21	0.50923 (9)	0.8818 (2)	0.15700 (13)	0.0270 (4)
C10	0.82299 (10)	0.5593 (3)	0.44444 (15)	0.0261 (4)
H10	0.8239	0.4804	0.4807	0.031*
C23	0.62225 (10)	0.9586 (2)	0.31901 (15)	0.0237 (4)
H23	0.6526	1.0401	0.3631	0.028*
N11	0.85370 (10)	0.6399 (3)	0.35157 (14)	0.0364 (5)
C22	0.55452 (10)	0.9952 (3)	0.22309 (15)	0.0251 (4)
C20	0.59907 (10)	0.6966 (3)	0.28228 (14)	0.0239 (4)
H20	0.6130	0.5918	0.3002	0.029*
O1	0.65623 (11)	0.2844 (2)	0.45025 (18)	0.0568 (6)
C11	0.85283 (11)	0.5294 (3)	0.40292 (15)	0.0312 (5)
C13	0.79369 (10)	0.8085 (3)	0.38110 (14)	0.0267 (4)
H13	0.7725	0.9060	0.3708	0.032*
C12	0.82493 (11)	0.7812 (3)	0.34183 (16)	0.0330 (5)
C14	0.88376 (15)	0.3709 (3)	0.4124 (2)	0.0454 (6)
H14A	0.8580	0.3295	0.3464	0.068*
H14B	0.8780	0.3006	0.4479	0.068*
H14C	0.9350	0.3812	0.4490	0.068*
C15	0.82941 (15)	0.9083 (4)	0.2884 (2)	0.0526 (8)
H15A	0.8799	0.9357	0.3276	0.079*
H15B	0.8029	0.9994	0.2800	0.079*
H15C	0.8082	0.8707	0.2234	0.079*
C21	0.53149 (10)	0.7326 (3)	0.18668 (14)	0.0272 (4)
C25	0.53126 (11)	1.1627 (3)	0.19022 (17)	0.0341 (5)
H25A	0.5382	1.1915	0.1461	0.051*
H25B	0.5604	1.2302	0.2483	0.051*
H25C	0.4803	1.1738	0.1552	0.051*
C24	0.48127 (12)	0.6054 (3)	0.11260 (18)	0.0405 (6)
H24A	0.4342	0.6160	0.0917	0.061*
H24B	0.5019	0.5045	0.1437	0.061*
H24C	0.4756	0.6143	0.0549	0.061*

	U11	U22	U33	U12	U13	U23
Ni1	0.01411 (16)	0.02221 (18)	0.01902 (17)	−0.00050 (14)	0.01083 (13)	0.00029 (14)
N20	0.0161 (7)	0.0272 (8)	0.0213 (7)	0.0021 (6)	0.0131 (6)	0.0022 (6)
N10	0.0158 (7)	0.0312 (9)	0.0196 (7)	−0.0012 (6)	0.0111 (6)	−0.0006 (6)
C1	0.0202 (9)	0.0288 (11)	0.0239 (9)	0.0043 (8)	0.0137 (8)	−0.0008 (8)
N1	0.0210 (8)	0.0326 (10)	0.0254 (8)	0.0028 (7)	0.0145 (7)	0.0032 (7)
N21	0.0194 (7)	0.0364 (10)	0.0244 (8)	0.0039 (7)	0.0147 (7)	0.0044 (7)
C10	0.0234 (9)	0.0324 (11)	0.0243 (9)	0.0031 (8)	0.0171 (8)	0.0017 (8)
C23	0.0181 (8)	0.0290 (10)	0.0244 (9)	0.0022 (7)	0.0146 (8)	0.0021 (8)
N11	0.0289 (9)	0.0556 (13)	0.0335 (9)	0.0103 (8)	0.0248 (8)	0.0102 (9)
C22	0.0179 (8)	0.0344 (11)	0.0270 (9)	0.0061 (8)	0.0169 (8)	0.0062 (8)
C20	0.0180 (8)	0.0299 (10)	0.0200 (9)	0.0013 (7)	0.0116 (8)	0.0001 (7)
O1	0.0535 (11)	0.0307 (10)	0.0848 (15)	−0.0174 (8)	0.0467 (12)	−0.0082 (9)
C11	0.0245 (10)	0.0445 (13)	0.0267 (10)	0.0061 (9)	0.0183 (9)	0.0020 (9)
C13	0.0204 (9)	0.0361 (11)	0.0240 (9)	0.0012 (8)	0.0153 (8)	0.0037 (8)
C12	0.0230 (9)	0.0498 (15)	0.0281 (10)	0.0058 (8)	0.0183 (8)	0.0114 (9)
C14	0.0521 (14)	0.0546 (16)	0.0491 (14)	0.0189 (12)	0.0422 (13)	0.0102 (12)
C15	0.0500 (14)	0.0681 (19)	0.0591 (17)	0.0181 (14)	0.0449 (14)	0.0293 (15)
C21	0.0192 (8)	0.0378 (13)	0.0218 (9)	0.0020 (8)	0.0129 (8)	0.0004 (8)
C25	0.0263 (10)	0.0380 (13)	0.0365 (11)	0.0115 (9)	0.0210 (9)	0.0139 (9)
C24	0.0270 (10)	0.0422 (14)	0.0292 (10)	−0.0009 (10)	0.0102 (9)	−0.0066 (10)

Ni1—N1i	2.0396 (19)	C22—C25	1.498 (3)
Ni1—N1	2.0396 (19)	C20—C21	1.395 (3)
Ni1—N10	2.1475 (17)	C20—H20	0.9300
Ni1—N10i	2.1475 (17)	C11—C14	1.502 (3)
Ni1—N20	2.1983 (15)	C13—C12	1.389 (3)
Ni1—N20i	2.1983 (15)	C13—H13	0.9300
N20—C23	1.335 (3)	C12—C15	1.507 (3)
N20—C20	1.345 (3)	C14—H14A	0.9600
N10—C10	1.334 (3)	C14—H14B	0.9600
N10—C13	1.339 (3)	C14—H14C	0.9600
C1—N1	1.113 (3)	C15—H15A	0.9600
C1—O1	1.238 (3)	C15—H15B	0.9600
N21—C22	1.339 (3)	C15—H15C	0.9600
N21—C21	1.341 (3)	C21—C24	1.497 (3)
C10—C11	1.398 (3)	C25—H25A	0.9600
C10—H10	0.9300	C25—H25B	0.9600
C23—C22	1.400 (3)	C25—H25C	0.9600
C23—H23	0.9300	C24—H24A	0.9600
N11—C11	1.334 (3)	C24—H24B	0.9600
N11—C12	1.347 (3)	C24—H24C	0.9600
N1i—Ni1—N1	180.00 (13)	N11—C11—C10	121.2 (2)
N1i—Ni1—N10	89.86 (7)	N11—C11—C14	117.3 (2)
N1—Ni1—N10	90.14 (7)	C10—C11—C14	121.5 (2)
N1i—Ni1—N10i	90.14 (7)	N10—C13—C12	121.8 (2)
N1—Ni1—N10i	89.86 (7)	N10—C13—H13	119.1
N10—Ni1—N10i	180.000	C12—C13—H13	119.1
N1i—Ni1—N20	89.74 (7)	N11—C12—C13	121.1 (2)
N1—Ni1—N20	90.26 (7)	N11—C12—C15	117.1 (2)
N10—Ni1—N20	88.72 (6)	C13—C12—C15	121.7 (2)
N10i—Ni1—N20	91.28 (6)	C11—C14—H14A	109.5
N1i—Ni1—N20i	90.26 (7)	C11—C14—H14B	109.5
N1—Ni1—N20i	89.74 (7)	H14A—C14—H14B	109.5
N10—Ni1—N20i	91.28 (6)	C11—C14—H14C	109.5
N10i—Ni1—N20i	88.72 (6)	H14A—C14—H14C	109.5
N20—Ni1—N20i	180.000	H14B—C14—H14C	109.5
C23—N20—C20	116.73 (16)	C12—C15—H15A	109.5
C23—N20—Ni1	122.62 (13)	C12—C15—H15B	109.5
C20—N20—Ni1	120.64 (14)	H15A—C15—H15B	109.5
C10—N10—C13	116.95 (19)	C12—C15—H15C	109.5
C10—N10—Ni1	122.49 (14)	H15A—C15—H15C	109.5
C13—N10—Ni1	120.51 (15)	H15B—C15—H15C	109.5
N1—C1—O1	179.7 (2)	N21—C21—C20	121.5 (2)
C1—N1—Ni1	167.16 (17)	N21—C21—C24	117.32 (18)
C22—N21—C21	117.19 (17)	C20—C21—C24	121.1 (2)
N10—C10—C11	121.7 (2)	C22—C25—H25A	109.5
N10—C10—H10	119.2	C22—C25—H25B	109.5
C11—C10—H10	119.2	H25A—C25—H25B	109.5
N20—C23—C22	122.01 (19)	C22—C25—H25C	109.5
N20—C23—H23	119.0	H25A—C25—H25C	109.5
C22—C23—H23	119.0	H25B—C25—H25C	109.5
C11—N11—C12	117.2 (2)	C21—C24—H24A	109.5
N21—C22—C23	121.1 (2)	C21—C24—H24B	109.5
N21—C22—C25	117.86 (17)	H24A—C24—H24B	109.5
C23—C22—C25	121.1 (2)	C21—C24—H24C	109.5
N20—C20—C21	121.5 (2)	H24A—C24—H24C	109.5
N20—C20—H20	119.3	H24B—C24—H24C	109.5
C21—C20—H20	119.3

Table 1

Selected bond lengths (Å)

Ni1—N1	2.0396 (19)
Ni1—N10	2.1475 (17)
Ni1—N20	2.1983 (15)