Hexa-kis-(dimethyl sulfoxide-κO)nickel(II) bis-(2,2-dicyano-ethene-1,1-dithiol-ato-κS,S')nickelate(II).

The reaction of NiCl(2)·6H(2)O with sodium 2,2-dicyano-ethene-1,1-dithiol-ate [Na(2)(i-mnt)] in dimethyl sulfoxide produces the title complex, [Ni(C(2)H(6)OS)(6)][Ni(C(4)N(2)S(2))(2)]. There is half each of an [Ni(C(2)H(6)OS)(6)](2-) complex anion and an [Ni{(CH(3))(2)SO}(6)](2+) complex cation in the asymmetric unit. The i-mnt ligand coordinates in a bidentate manner to the Ni atom in the anion through the two chelating S atoms in an approximate square-planar geometry. The Ni atom in the complex cation has an octahedral coordination environment with six dimethyl sulfoxide mol-ecules as ligands.

Related literature

For related structures, see Gao et al. (2004 ▶, 2005 ▶); Yu et al. (2005 ▶); Chen & Yu (2005 ▶).

Experimental

Crystal data

[Ni(C2H6OS)6][Ni(C4N2S2)2]

M = 866.55

Monoclinic,

a = 8.3368 (10) Å

b = 12.6763 (17) Å

c = 18.710 (2) Å

β = 102.466 (2)°

V = 1930.6 (4) Å3

Z = 2

Mo Kα radiation

μ = 1.55 mm−1

T = 298 K

0.50 × 0.48 × 0.05 mm

Data collection

Bruker SMART CCD area-detector diffractometer

Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T min = 0.511, T max = 0.921

9458 measured reflections

3379 independent reflections

2328 reflections with I > 2σ(I)

R int = 0.054

Refinement

R[F 2 > 2σ(F 2)] = 0.038

wR(F 2) = 0.095

S = 1.06

3379 reflections

199 parameters

H-atom parameters constrained

Δρmax = 0.30 e Å−3

Δρmin = −0.35 e Å−3

Data collection: SMART (Bruker, 2007 ▶); cell refinement: SAINT (Bruker, 2007 ▶); 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 datablock(s) I, global. DOI: 10.1107/S1600536811053827/vm2141sup1.cif

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536811053827/vm2141Isup2.hkl

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

C12H36NiO6S62+·C8N4NiS42−	F(000) = 896
Mr = 866.55	Dx = 1.491 Mg m−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 2760 reflections
a = 8.3368 (10) Å	θ = 2.5–24.3°
b = 12.6763 (17) Å	µ = 1.55 mm−1
c = 18.710 (2) Å	T = 298 K
β = 102.466 (2)°	Needle, green
V = 1930.6 (4) Å3	0.50 × 0.48 × 0.05 mm
Z = 2

Bruker SMART CCD area-detector diffractometer	3379 independent reflections
Radiation source: fine-focus sealed tube	2328 reflections with I > 2σ(I)
graphite	Rint = 0.054
phi and ω scans	θmax = 25.0°, θmin = 2.0°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −9→9
Tmin = 0.511, Tmax = 0.921	k = −12→15
9458 measured reflections	l = −22→18

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)] = 0.038	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.095	H-atom parameters constrained
S = 1.06	w = 1/[σ2(Fo2) + (0.0275P)2 + 1.0073P] where P = (Fo2 + 2Fc2)/3
3379 reflections	(Δ/σ)max = 0.001
199 parameters	Δρmax = 0.30 e Å−3
0 restraints	Δρmin = −0.35 e Å−3

	x	y	z	Uiso*/Ueq
Ni1	0.5000	0.5000	0.5000	0.02973 (18)
Ni2	1.0000	0.0000	0.5000	0.0415 (2)
N1	0.7064 (6)	0.2565 (4)	0.2505 (2)	0.0863 (15)
N2	1.1494 (6)	0.0945 (4)	0.2174 (2)	0.0751 (13)
O1	0.4945 (3)	0.64165 (18)	0.44513 (13)	0.0367 (6)
O2	0.7372 (3)	0.47506 (19)	0.48840 (15)	0.0440 (7)
O3	0.4122 (3)	0.41769 (19)	0.40520 (13)	0.0436 (7)
S1	0.62727 (13)	0.72370 (8)	0.46849 (5)	0.0412 (3)
S2	0.78272 (12)	0.36249 (8)	0.47193 (5)	0.0385 (3)
S3	0.32535 (13)	0.47016 (8)	0.33476 (5)	0.0391 (3)
S4	0.81754 (14)	0.08901 (9)	0.41999 (6)	0.0489 (3)
S5	1.10676 (15)	−0.00988 (9)	0.40228 (6)	0.0533 (3)
C1	0.5310 (7)	0.8291 (4)	0.5044 (3)	0.095 (2)
H1A	0.4416	0.8553	0.4675	0.142*
H1B	0.6092	0.8846	0.5198	0.142*
H1C	0.4898	0.8047	0.5456	0.142*
C2	0.6505 (7)	0.7821 (4)	0.3864 (2)	0.0732 (16)
H2A	0.6983	0.7320	0.3586	0.110*
H2B	0.7208	0.8426	0.3971	0.110*
H2C	0.5449	0.8036	0.3586	0.110*
C3	0.9350 (5)	0.3786 (3)	0.4198 (2)	0.0503 (11)
H3A	0.8874	0.4120	0.3741	0.075*
H3B	0.9777	0.3108	0.4106	0.075*
H3C	1.0224	0.4216	0.4465	0.075*
C4	0.9093 (6)	0.3174 (4)	0.5552 (2)	0.0585 (13)
H4A	0.9998	0.3651	0.5701	0.088*
H4B	0.9504	0.2484	0.5480	0.088*
H4C	0.8462	0.3144	0.5924	0.088*
C5	0.2206 (6)	0.3635 (4)	0.2835 (2)	0.0676 (14)
H5A	0.2961	0.3066	0.2827	0.101*
H5B	0.1756	0.3863	0.2343	0.101*
H5C	0.1334	0.3399	0.3057	0.101*
C6	0.4776 (6)	0.4904 (4)	0.2835 (2)	0.0600 (13)
H6A	0.5526	0.5440	0.3065	0.090*
H6B	0.4265	0.5123	0.2348	0.090*
H6C	0.5365	0.4258	0.2813	0.090*
C7	0.9525 (5)	0.0750 (3)	0.3630 (2)	0.0409 (10)
C8	0.9395 (5)	0.1255 (3)	0.2967 (2)	0.0427 (10)
C9	0.8105 (6)	0.1979 (4)	0.2706 (2)	0.0526 (12)
C10	1.0561 (6)	0.1086 (3)	0.2528 (2)	0.0522 (12)

	U11	U22	U33	U12	U13	U23
Ni1	0.0336 (4)	0.0269 (4)	0.0290 (4)	0.0013 (3)	0.0074 (3)	−0.0017 (3)
Ni2	0.0476 (5)	0.0370 (4)	0.0408 (4)	0.0016 (4)	0.0116 (3)	−0.0019 (3)
N1	0.092 (4)	0.077 (3)	0.076 (3)	0.030 (3)	−0.011 (3)	−0.008 (2)
N2	0.080 (3)	0.093 (3)	0.058 (3)	0.006 (3)	0.029 (2)	0.002 (2)
O1	0.0380 (16)	0.0297 (14)	0.0415 (14)	−0.0024 (12)	0.0067 (12)	0.0023 (12)
O2	0.0373 (17)	0.0336 (16)	0.0633 (18)	−0.0007 (12)	0.0155 (14)	−0.0079 (13)
O3	0.061 (2)	0.0358 (15)	0.0309 (14)	−0.0010 (14)	0.0039 (13)	−0.0047 (12)
S1	0.0402 (7)	0.0377 (6)	0.0461 (6)	−0.0039 (5)	0.0104 (5)	0.0007 (5)
S2	0.0339 (6)	0.0327 (6)	0.0497 (6)	0.0002 (4)	0.0104 (5)	−0.0077 (5)
S3	0.0409 (6)	0.0434 (6)	0.0325 (5)	0.0031 (5)	0.0071 (4)	−0.0050 (4)
S4	0.0502 (8)	0.0503 (7)	0.0486 (6)	0.0102 (5)	0.0157 (5)	−0.0005 (5)
S5	0.0537 (8)	0.0614 (8)	0.0473 (6)	0.0163 (6)	0.0161 (5)	0.0049 (6)
C1	0.094 (5)	0.053 (3)	0.155 (6)	−0.023 (3)	0.067 (4)	−0.048 (4)
C2	0.086 (4)	0.072 (3)	0.063 (3)	−0.032 (3)	0.018 (3)	0.015 (3)
C3	0.045 (3)	0.048 (3)	0.063 (3)	−0.003 (2)	0.022 (2)	−0.011 (2)
C4	0.067 (3)	0.049 (3)	0.056 (3)	0.014 (2)	0.004 (2)	0.000 (2)
C5	0.077 (4)	0.074 (3)	0.049 (3)	−0.025 (3)	0.008 (2)	−0.017 (3)
C6	0.062 (3)	0.064 (3)	0.061 (3)	−0.005 (3)	0.030 (3)	0.006 (2)
C7	0.045 (3)	0.035 (2)	0.041 (2)	−0.0014 (19)	0.0061 (19)	−0.0096 (18)
C8	0.045 (3)	0.042 (3)	0.041 (2)	0.002 (2)	0.008 (2)	−0.0053 (19)
C9	0.066 (3)	0.049 (3)	0.040 (2)	−0.003 (3)	0.005 (2)	−0.010 (2)
C10	0.065 (4)	0.051 (3)	0.040 (3)	−0.002 (2)	0.008 (2)	0.001 (2)

Ni1—O3	2.052 (2)	S5—C7	1.716 (4)
Ni1—O3i	2.052 (2)	C1—H1A	0.9600
Ni1—O2i	2.060 (3)	C1—H1B	0.9600
Ni1—O2	2.060 (3)	C1—H1C	0.9600
Ni1—O1	2.064 (2)	C2—H2A	0.9600
Ni1—O1i	2.064 (2)	C2—H2B	0.9600
Ni2—S4	2.2010 (11)	C2—H2C	0.9600
Ni2—S4ii	2.2010 (11)	C3—H3A	0.9600
Ni2—S5ii	2.2030 (11)	C3—H3B	0.9600
Ni2—S5	2.2030 (11)	C3—H3C	0.9600
N1—C9	1.142 (6)	C4—H4A	0.9600
N2—C10	1.139 (5)	C4—H4B	0.9600
O1—S1	1.513 (3)	C4—H4C	0.9600
O2—S2	1.525 (3)	C5—H5A	0.9600
O3—S3	1.514 (3)	C5—H5B	0.9600
S1—C2	1.752 (4)	C5—H5C	0.9600
S1—C1	1.765 (5)	C6—H6A	0.9600
S2—C3	1.772 (4)	C6—H6B	0.9600
S2—C4	1.777 (4)	C6—H6C	0.9600
S3—C6	1.767 (4)	C7—C8	1.378 (5)
S3—C5	1.775 (4)	C8—C9	1.418 (6)
S4—C7	1.719 (4)	C8—C10	1.418 (6)
O3—Ni1—O3i	180.000 (1)	H1B—C1—H1C	109.5
O3—Ni1—O2i	89.86 (11)	S1—C2—H2A	109.5
O3i—Ni1—O2i	90.14 (11)	S1—C2—H2B	109.5
O3—Ni1—O2	90.14 (11)	H2A—C2—H2B	109.5
O3i—Ni1—O2	89.86 (11)	S1—C2—H2C	109.5
O2i—Ni1—O2	180.00 (15)	H2A—C2—H2C	109.5
O3—Ni1—O1	92.69 (9)	H2B—C2—H2C	109.5
O3i—Ni1—O1	87.31 (9)	S2—C3—H3A	109.5
O2i—Ni1—O1	90.01 (10)	S2—C3—H3B	109.5
O2—Ni1—O1	89.99 (10)	H3A—C3—H3B	109.5
O3—Ni1—O1i	87.31 (9)	S2—C3—H3C	109.5
O3i—Ni1—O1i	92.69 (9)	H3A—C3—H3C	109.5
O2i—Ni1—O1i	89.99 (10)	H3B—C3—H3C	109.5
O2—Ni1—O1i	90.01 (10)	S2—C4—H4A	109.5
O1—Ni1—O1i	180.0	S2—C4—H4B	109.5
S4—Ni2—S4ii	180.00 (5)	H4A—C4—H4B	109.5
S4—Ni2—S5ii	101.04 (4)	S2—C4—H4C	109.5
S4ii—Ni2—S5ii	78.96 (4)	H4A—C4—H4C	109.5
S4—Ni2—S5	78.96 (4)	H4B—C4—H4C	109.5
S4ii—Ni2—S5	101.04 (4)	S3—C5—H5A	109.5
S5ii—Ni2—S5	180.0	S3—C5—H5B	109.5
S1—O1—Ni1	121.20 (14)	H5A—C5—H5B	109.5
S2—O2—Ni1	116.83 (15)	S3—C5—H5C	109.5
S3—O3—Ni1	122.93 (15)	H5A—C5—H5C	109.5
O1—S1—C2	104.45 (19)	H5B—C5—H5C	109.5
O1—S1—C1	105.4 (2)	S3—C6—H6A	109.5
C2—S1—C1	99.2 (3)	S3—C6—H6B	109.5
O2—S2—C3	104.06 (18)	H6A—C6—H6B	109.5
O2—S2—C4	104.50 (18)	S3—C6—H6C	109.5
C3—S2—C4	99.1 (2)	H6A—C6—H6C	109.5
O3—S3—C6	105.8 (2)	H6B—C6—H6C	109.5
O3—S3—C5	102.88 (19)	C8—C7—S5	125.7 (3)
C6—S3—C5	98.3 (2)	C8—C7—S4	125.1 (3)
C7—S4—Ni2	85.42 (14)	S5—C7—S4	109.2 (2)
C7—S5—Ni2	85.44 (14)	C7—C8—C9	121.2 (4)
S1—C1—H1A	109.5	C7—C8—C10	121.3 (4)
S1—C1—H1B	109.5	C9—C8—C10	117.5 (4)
H1A—C1—H1B	109.5	N1—C9—C8	179.0 (5)
S1—C1—H1C	109.5	N2—C10—C8	179.7 (6)
H1A—C1—H1C	109.5
O3—Ni1—O1—S1	−142.43 (17)	Ni1—O3—S3—C5	−161.4 (2)
O3i—Ni1—O1—S1	37.57 (17)	S4ii—Ni2—S4—C7	−120 (100)
O2i—Ni1—O1—S1	127.71 (17)	S5ii—Ni2—S4—C7	173.58 (13)
O2—Ni1—O1—S1	−52.29 (17)	S5—Ni2—S4—C7	−6.42 (13)
O1i—Ni1—O1—S1	−139 (100)	S4—Ni2—S5—C7	6.44 (13)
O3—Ni1—O2—S2	−48.30 (17)	S4ii—Ni2—S5—C7	−173.56 (13)
O3i—Ni1—O2—S2	131.70 (17)	S5ii—Ni2—S5—C7	112 (14)
O2i—Ni1—O2—S2	13 (48)	Ni2—S5—C7—C8	170.5 (3)
O1—Ni1—O2—S2	−140.99 (17)	Ni2—S5—C7—S4	−8.58 (17)
O1i—Ni1—O2—S2	39.01 (17)	Ni2—S4—C7—C8	−170.5 (3)
O3i—Ni1—O3—S3	−178 (100)	Ni2—S4—C7—S5	8.59 (18)
O2i—Ni1—O3—S3	71.7 (2)	S5—C7—C8—C9	−177.2 (3)
O2—Ni1—O3—S3	−108.3 (2)	S4—C7—C8—C9	1.7 (6)
O1—Ni1—O3—S3	−18.3 (2)	S5—C7—C8—C10	1.6 (6)
O1i—Ni1—O3—S3	161.7 (2)	S4—C7—C8—C10	−179.4 (3)
Ni1—O1—S1—C2	145.1 (2)	C7—C8—C9—N1	26 (32)
Ni1—O1—S1—C1	−110.9 (3)	C10—C8—C9—N1	−153 (32)
Ni1—O2—S2—C3	149.93 (19)	C7—C8—C10—N2	79 (100)
Ni1—O2—S2—C4	−106.6 (2)	C9—C8—C10—N2	−102 (100)
Ni1—O3—S3—C6	95.9 (2)

Ni1—O3	2.052 (2)
Ni1—O2	2.060 (3)
Ni1—O1	2.064 (2)
Ni2—S4	2.2010 (11)
Ni2—S5	2.2030 (11)

O3—Ni1—O2	90.14 (11)
S4—Ni2—S5	78.96 (4)