Bis(μ(2)-4,7-dimethyl-4,7-diazadecane-1,10-dithiolato)trinickel(II) bis(perchlorate).

In the title compound, [Ni(3)(C(10)H(22)N(2)S(2))(2)](ClO(4))(2), the complex cation consists of a nickel(II) ion and two [Ni(C(10)H(22)N(2)S(2))] units with an N(2)S(2) tetra-dentate ligand, 3,3'-[1,2-ethane-diylbis(methyl-imino)]bis-(1-propane-thiol-ate). The central Ni(II) ion is located on a crystallographic inversion centre and is bound to the four S atoms of the two [Ni(C(10)H(22)N(2)S(2))] units to form a linear sulfur-bridged trimetallic moiety. The dihedral angle between the central NiS(4) plane and the terminal NiN(2)S(2) plane is 145.71 (5)°. In the [Ni(C(10)H(22)N(2)S(2))] unit, the two methyl groups on the chelating N atoms are cis to each other, and the two six-membered N,S-chelate rings adopt a chair conformation. The Ni-S bond lengths and the S-Ni-S bite angles in the central NiS(4) group are similar to those in the [Ni(C(10)H(22)N(2)S(2))] unit.

Related literature

For general background, see: Konno et al. (2000 ▶); Konno (2004 ▶); Igashira-Kamiyama & Konno (2011 ▶). For related structures, see: Grapperhaus et al. (2007 ▶); Turner et al. (1990 ▶).

Experimental

Crystal data

[Ni3(C10H22N2S2)2](ClO4)2

M = 843.83

Monoclinic,

a = 8.0253 (19) Å

b = 16.208 (4) Å

c = 12.807 (3) Å

β = 105.033 (6)°

V = 1608.8 (7) Å3

Z = 2

Mo Kα radiation

μ = 2.21 mm−1

T = 123 K

0.24 × 0.24 × 0.17 mm

Data collection

Rigaku AFC7 (Mercury CCD) diffractometer

Absorption correction: multi-scan (REQAB; Jacobson 1998 ▶) T min = 0.619, T max = 0.705

15030 measured reflections

3626 independent reflections

3391 reflections with F 2 > 2.0σ(F 2)

R int = 0.027

Refinement

R[F 2 > 2σ(F 2)] = 0.035

wR(F 2) = 0.082

S = 1.04

3626 reflections

235 parameters

H atoms treated by a mixture of independent and constrained refinement

Δρmax = 1.71 e Å−3

Δρmin = −0.70 e Å−3

Data collection: CrystalClear (Rigaku, 2007 ▶); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997 ▶); software used to prepare material for publication: WinGX (Farrugia, 1999 ▶) and publCIF (Westrip, 2010 ▶).

Crystal structure: contains datablock(s) global, I. DOI: 10.1107/S1600536812006034/fj2508sup1.cif

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536812006034/fj2508Isup2.hkl

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

[Ni3(C10H22N2S2)2](ClO4)2	F(000) = 876.00
Mr = 843.83	Dx = 1.742 Mg m−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71075 Å
Hall symbol: -P 2ybc	Cell parameters from 7222 reflections
a = 8.0253 (19) Å	θ = 4.1–27.5°
b = 16.208 (4) Å	µ = 2.21 mm−1
c = 12.807 (3) Å	T = 123 K
β = 105.033 (6)°	Prism, red
V = 1608.8 (7) Å3	0.24 × 0.24 × 0.17 mm
Z = 2

Rigaku AFC7 (Mercury CCD) diffractometer	3626 independent reflections
Radiation source: rotating anode X-ray tube	3391 reflections with F2 > 2.0σ(F2)
Graphite monochromator	Rint = 0.027
Detector resolution: 7.31 pixels mm-1	θmax = 27.5°, θmin = 4.1°
ω scans	h = −10→10
Absorption correction: multi-scan (REQAB; Jacobson, 1998)	k = −21→20
Tmin = 0.619, Tmax = 0.705	l = −13→16
15030 measured reflections

Refinement on F2	0 restraints
Least-squares matrix: full	H atoms treated by a mixture of independent and constrained refinement
R[F2 > 2σ(F2)] = 0.035	w = 1/[σ2(Fo2) + (0.0319P)2 + 3.9221P] where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.082	(Δ/σ)max = 0.002
S = 1.04	Δρmax = 1.71 e Å−3
3626 reflections	Δρmin = −0.70 e Å−3
235 parameters

Refinement. Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F2. R-factor (gt) are based on F. The threshold expression of F2 > 2.0 σ(F2) is used only for calculating R-factor (gt).

	x	y	z	Uiso*/Ueq
Ni1	0.04531 (4)	0.626726 (19)	0.82272 (2)	0.01439 (10)
Ni2	0.0000	0.5000	1.0000	0.01306 (11)
Cl1	0.28814 (8)	0.39140 (4)	0.71998 (5)	0.02463 (15)
S1	−0.16594 (8)	0.55517 (4)	0.85310 (5)	0.01655 (13)
S2	0.14612 (8)	0.61385 (4)	0.99699 (5)	0.01539 (13)
O1	0.2236 (4)	0.4191 (2)	0.8082 (2)	0.0720 (11)
O2	0.4299 (3)	0.33683 (14)	0.76150 (19)	0.0357 (5)
O3	0.1505 (3)	0.35038 (17)	0.64509 (18)	0.0431 (6)
O4	0.3425 (4)	0.46058 (19)	0.6684 (3)	0.0680 (10)
N1	−0.0478 (3)	0.63136 (14)	0.66462 (17)	0.0224 (5)
N2	0.2398 (3)	0.69848 (15)	0.80846 (18)	0.0228 (5)
C1	−0.2110 (4)	0.47418 (18)	0.7507 (2)	0.0241 (6)
C2	−0.2552 (4)	0.5093 (2)	0.6370 (2)	0.0286 (6)
C3	−0.1047 (4)	0.55199 (17)	0.6077 (2)	0.0222 (5)
C4	0.3641 (3)	0.57575 (18)	1.0035 (2)	0.0212 (5)
C5	0.4731 (4)	0.63872 (18)	0.9633 (2)	0.0225 (5)
C6	0.4124 (3)	0.65719 (17)	0.8436 (2)	0.0202 (5)
C7	0.1093 (5)	0.6568 (3)	0.6256 (3)	0.0433 (9)
C8	0.2043 (5)	0.7223 (3)	0.6932 (3)	0.0433 (9)
C9	−0.1854 (6)	0.6932 (2)	0.6355 (3)	0.0478 (10)
C10	0.2471 (4)	0.77787 (18)	0.8711 (3)	0.0356 (7)
H1A	−0.308 (5)	0.443 (2)	0.762 (3)	0.030 (9)*
H1B	−0.117 (5)	0.443 (2)	0.759 (3)	0.028 (9)*
H2A	−0.353 (4)	0.549 (2)	0.629 (3)	0.023 (8)*
H2B	−0.284 (5)	0.464 (2)	0.587 (3)	0.038 (10)*
H3A	−0.127 (5)	0.562 (2)	0.530 (3)	0.033 (9)*
H3B	−0.005 (4)	0.514 (2)	0.624 (3)	0.024 (8)*
H4A	0.413 (4)	0.562 (2)	1.076 (3)	0.027 (8)*
H4B	0.353 (4)	0.526 (2)	0.960 (3)	0.022 (8)*
H5A	0.477 (4)	0.688 (2)	1.004 (2)	0.017 (7)*
H5B	0.589 (5)	0.617 (2)	0.974 (3)	0.027 (9)*
H6A	0.498 (4)	0.6915 (19)	0.822 (2)	0.020 (7)*
H6B	0.403 (4)	0.6070 (19)	0.800 (2)	0.017 (7)*
H7A	0.1858	0.6086	0.6278	0.052*
H7B	0.0711	0.6762	0.5497	0.052*
H8A	0.1359	0.7739	0.6806	0.052*
H8B	0.3143	0.7325	0.6740	0.052*
H9A	−0.1460	0.7449	0.6735	0.072*
H9B	−0.2876	0.6732	0.6562	0.072*
H9C	−0.2146	0.7028	0.5573	0.072*
H10A	0.2703	0.7655	0.9485	0.053*
H10B	0.1364	0.8067	0.8472	0.053*
H10C	0.3393	0.8130	0.8584	0.053*

	U11	U22	U33	U12	U13	U23
Ni1	0.01653 (17)	0.01475 (17)	0.01300 (16)	0.00004 (11)	0.00584 (12)	0.00248 (11)
Ni2	0.0134 (2)	0.0146 (2)	0.0115 (2)	−0.00204 (16)	0.00396 (15)	0.00100 (15)
Cl1	0.0182 (3)	0.0289 (3)	0.0237 (3)	0.0002 (2)	−0.0003 (2)	−0.0014 (3)
S1	0.0151 (3)	0.0209 (3)	0.0145 (3)	0.0007 (2)	0.0053 (2)	0.0034 (2)
S2	0.0182 (3)	0.0161 (3)	0.0133 (3)	−0.0033 (2)	0.0064 (2)	−0.0009 (2)
O1	0.0498 (17)	0.120 (3)	0.0414 (15)	0.0461 (19)	0.0037 (13)	−0.0256 (17)
O2	0.0267 (11)	0.0350 (12)	0.0436 (13)	0.0125 (9)	0.0061 (9)	−0.0016 (10)
O3	0.0362 (13)	0.0549 (15)	0.0302 (12)	−0.0205 (12)	−0.0056 (10)	0.0011 (11)
O4	0.0394 (15)	0.0534 (17)	0.098 (2)	−0.0159 (13)	−0.0057 (15)	0.0363 (17)
N1	0.0326 (13)	0.0209 (11)	0.0140 (10)	−0.0057 (9)	0.0066 (9)	0.0031 (8)
N2	0.0195 (11)	0.0279 (12)	0.0220 (11)	0.0008 (9)	0.0071 (9)	0.0125 (9)
C1	0.0269 (15)	0.0270 (14)	0.0168 (12)	−0.0116 (12)	0.0028 (10)	0.0000 (11)
C2	0.0315 (16)	0.0348 (16)	0.0161 (12)	−0.0104 (13)	0.0001 (11)	0.0015 (12)
C3	0.0282 (14)	0.0242 (14)	0.0146 (11)	0.0002 (11)	0.0065 (10)	0.0005 (10)
C4	0.0160 (12)	0.0272 (14)	0.0194 (12)	−0.0016 (10)	0.0028 (10)	0.0074 (11)
C5	0.0178 (13)	0.0273 (14)	0.0221 (13)	−0.0043 (11)	0.0045 (10)	0.0030 (11)
C6	0.0194 (13)	0.0225 (13)	0.0210 (12)	−0.0005 (10)	0.0095 (10)	0.0016 (10)
C7	0.052 (2)	0.055 (2)	0.0265 (15)	−0.0176 (18)	0.0173 (15)	0.0042 (15)
C8	0.0329 (17)	0.068 (2)	0.0264 (15)	−0.0106 (17)	0.0029 (13)	0.0233 (16)
C9	0.076 (3)	0.0329 (18)	0.0271 (16)	0.0233 (18)	−0.0007 (16)	0.0034 (14)
C10	0.0289 (16)	0.0184 (14)	0.064 (2)	−0.0007 (12)	0.0207 (15)	0.0058 (14)

Ni1—N1	1.969 (2)	C4—H4B	0.98 (3)
Ni1—N2	1.993 (2)	C5—C6	1.513 (4)
Ni1—S1	2.1709 (8)	C5—H5A	0.95 (3)
Ni1—S2	2.1777 (8)	C5—H5B	0.97 (4)
Ni2—S1	2.1938 (7)	C6—N2	1.498 (3)
Ni2—S2	2.1921 (7)	C6—H6A	0.98 (3)
Cl1—O1	1.432 (3)	C6—H6B	0.98 (3)
Cl1—O2	1.430 (2)	C7—C8	1.454 (5)
Cl1—O3	1.425 (2)	C7—N1	1.529 (4)
Cl1—O4	1.426 (3)	C7—H7A	0.9900
C1—C2	1.518 (4)	C7—H7B	0.9900
C1—S1	1.824 (3)	C8—N2	1.481 (4)
C1—H1A	0.97 (4)	C8—H8A	0.9900
C1—H1B	0.89 (4)	C8—H8B	0.9900
C2—C3	1.520 (4)	C9—N1	1.466 (4)
C2—H2A	1.00 (3)	C9—H9A	0.9800
C2—H2B	0.97 (4)	C9—H9B	0.9800
C3—N1	1.491 (3)	C9—H9C	0.9800
C3—H3A	0.98 (4)	C10—N2	1.510 (4)
C3—H3B	0.99 (3)	C10—H10A	0.9800
C4—C5	1.519 (4)	C10—H10B	0.9800
C4—S2	1.836 (3)	C10—H10C	0.9800
C4—H4A	0.94 (3)	Ni1—Ni2	3.1518 (6)
N1—Ni1—N2	88.90 (9)	C3—C2—H2A	109.8 (19)
N1—Ni1—S1	95.68 (7)	C1—C2—H2B	108 (2)
N2—Ni1—S1	174.27 (7)	C3—C2—H2B	105 (2)
N1—Ni1—S2	176.66 (7)	H2A—C2—H2B	112 (3)
N2—Ni1—S2	93.34 (7)	N1—C3—H3A	108 (2)
S1—Ni1—S2	82.24 (3)	C2—C3—H3A	112 (2)
S1—Ni2—S2	81.39 (3)	N1—C3—H3B	107.9 (19)
S1—Ni2—S2i	98.61 (3)	C2—C3—H3B	108.7 (19)
Ni1—S1—C1	105.91 (10)	H3A—C3—H3B	104 (3)
Ni2—S1—C1	106.63 (10)	C5—C4—H4A	112 (2)
Ni1—S2—C4	100.09 (9)	S2—C4—H4A	106 (2)
Ni2—S2—C4	102.93 (9)	C5—C4—H4B	110.2 (19)
Ni1—S1—Ni2	92.46 (3)	S2—C4—H4B	107.8 (19)
Ni1—S2—Ni2	92.32 (2)	H4A—C4—H4B	109 (3)
O3—Cl1—O4	109.37 (17)	C6—C5—H5A	110.1 (18)
O3—Cl1—O2	111.38 (16)	C4—C5—H5A	108.8 (18)
O4—Cl1—O2	110.42 (16)	C6—C5—H5B	105 (2)
O3—Cl1—O1	107.56 (19)	C4—C5—H5B	109 (2)
O4—Cl1—O1	109.6 (2)	H5A—C5—H5B	110 (3)
O2—Cl1—O1	108.46 (16)	N2—C6—H6A	108.8 (18)
C2—C1—S1	111.9 (2)	C5—C6—H6A	109.7 (18)
C1—C2—C3	113.9 (2)	N2—C6—H6B	106.0 (18)
N1—C3—C2	115.7 (2)	C5—C6—H6B	111.5 (18)
C5—C4—S2	112.6 (2)	H6A—C6—H6B	105 (2)
C6—C5—C4	114.5 (2)	C8—C7—H7A	109.5
N2—C6—C5	115.0 (2)	N1—C7—H7A	109.5
C8—C7—N1	110.6 (3)	C8—C7—H7B	109.5
C7—C8—N2	109.8 (3)	N1—C7—H7B	109.5
C9—N1—C3	110.5 (2)	H7A—C7—H7B	108.1
C9—N1—C7	111.3 (3)	C7—C8—H8A	109.7
C3—N1—C7	104.3 (2)	N2—C8—H8A	109.7
C9—N1—Ni1	110.34 (19)	C7—C8—H8B	109.7
C3—N1—Ni1	117.14 (16)	N2—C8—H8B	109.7
C7—N1—Ni1	102.81 (18)	H8A—C8—H8B	108.2
C8—N2—C6	109.9 (2)	N1—C9—H9A	109.5
C8—N2—C10	106.2 (3)	N1—C9—H9B	109.5
C6—N2—C10	108.4 (2)	H9A—C9—H9B	109.5
C8—N2—Ni1	106.90 (19)	N1—C9—H9C	109.5
C6—N2—Ni1	113.38 (16)	H9A—C9—H9C	109.5
C10—N2—Ni1	111.83 (17)	H9B—C9—H9C	109.5
C2—C1—H1A	110 (2)	N2—C10—H10A	109.5
S1—C1—H1A	106 (2)	N2—C10—H10B	109.5
C2—C1—H1B	108 (2)	H10A—C10—H10B	109.5
S1—C1—H1B	109 (2)	N2—C10—H10C	109.5
H1A—C1—H1B	112 (3)	H10A—C10—H10C	109.5
C1—C2—H2A	108.7 (18)	H10B—C10—H10C	109.5
S1—C1—C2—C3	67.6 (3)	S1—Ni1—Ni2—S2i	37.83 (4)
C1—C2—C3—N1	−69.6 (3)	S2—Ni1—Ni2—S2i	180.0
S2—C4—C5—C6	−67.3 (3)	N1—Ni1—Ni2—S2	177.99 (10)
C4—C5—C6—N2	65.5 (3)	N2—Ni1—Ni2—S2	30.68 (10)
N1—C7—C8—N2	51.0 (4)	S1—Ni1—Ni2—S2	−142.17 (4)
C2—C3—N1—C9	−63.8 (3)	N1—Ni1—Ni2—S1i	140.16 (10)
C2—C3—N1—C7	176.5 (3)	N2—Ni1—Ni2—S1i	−7.16 (10)
C2—C3—N1—Ni1	63.7 (3)	S1—Ni1—Ni2—S1i	180.0
C8—C7—N1—C9	74.6 (4)	S2—Ni1—Ni2—S1i	−37.83 (4)
C8—C7—N1—C3	−166.2 (3)	N1—Ni1—Ni2—S1	−39.84 (10)
C8—C7—N1—Ni1	−43.5 (3)	N2—Ni1—Ni2—S1	172.84 (10)
C7—C8—N2—C6	92.5 (3)	S2—Ni1—Ni2—S1	142.17 (4)
C7—C8—N2—C10	−150.5 (3)	C2—C1—S1—Ni1	−57.8 (2)
C7—C8—N2—Ni1	−31.0 (4)	C2—C1—S1—Ni2	−155.3 (2)
C5—C6—N2—C8	173.2 (3)	N1—Ni1—S1—C1	43.83 (13)
C5—C6—N2—C10	57.6 (3)	S2—Ni1—S1—C1	−133.54 (11)
C5—C6—N2—Ni1	−67.2 (3)	Ni2—Ni1—S1—C1	−108.06 (11)
C9—N1—Ni1—N2	−98.6 (2)	N1—Ni1—S1—Ni2	151.89 (7)
C3—N1—Ni1—N2	133.8 (2)	S2—Ni1—S1—Ni2	−25.48 (2)
C7—N1—Ni1—N2	20.1 (2)	S2i—Ni2—S1—C1	−47.23 (10)
C9—N1—Ni1—S1	77.9 (2)	S2—Ni2—S1—C1	132.77 (10)
C3—N1—Ni1—S1	−49.7 (2)	Ni1—Ni2—S1—C1	107.41 (10)
C7—N1—Ni1—S1	−163.34 (19)	S2i—Ni2—S1—Ni1	−154.64 (2)
C9—N1—Ni1—Ni2	104.5 (2)	S2—Ni2—S1—Ni1	25.36 (2)
C3—N1—Ni1—Ni2	−23.1 (2)	C5—C4—S2—Ni1	64.9 (2)
C7—N1—Ni1—Ni2	−136.74 (18)	C5—C4—S2—Ni2	159.63 (18)
C8—N2—Ni1—N1	4.8 (2)	N2—Ni1—S2—C4	−54.60 (12)
C6—N2—Ni1—N1	−116.41 (18)	S1—Ni1—S2—C4	129.07 (10)
C10—N2—Ni1—N1	120.7 (2)	Ni2—Ni1—S2—C4	103.57 (10)
C8—N2—Ni1—S2	−177.6 (2)	N2—Ni1—S2—Ni2	−158.17 (7)
C6—N2—Ni1—S2	61.11 (17)	S1—Ni1—S2—Ni2	25.50 (2)
C10—N2—Ni1—S2	−61.82 (19)	S1i—Ni2—S2—C4	53.82 (9)
C8—N2—Ni1—Ni2	161.56 (19)	S1—Ni2—S2—C4	−126.18 (9)
C6—N2—Ni1—Ni2	40.3 (2)	Ni1—Ni2—S2—C4	−100.91 (9)
C10—N2—Ni1—Ni2	−82.6 (2)	S1i—Ni2—S2—Ni1	154.73 (2)
N1—Ni1—Ni2—S2i	−2.01 (10)	S1—Ni2—S2—Ni1	−25.27 (2)
N2—Ni1—Ni2—S2i	−149.32 (10)