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metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890
Volume 65| Part 11| November 2009| Page m1485
https://doi.org/10.1107/S1600536809044821

Tetra­ethyl­ammonium dicyanidobis(ethane-1,2-di­thiol­ato)tetra-μ3-sulfido-dimolybdenum(V)dicopper(I)

Xiu-Li Youa* and Yue-Long Liua

aJiangxi Key Laboratory of Organic Chemistry, Jiangxi Science and Technology Normal University, Nanchang 330013, People's Republic of China
*Correspondence e-mail: jxstnu2008@yahoo.cn

(Received 26 September 2009; accepted 27 October 2009; online 31 October 2009)

The title compound, (C8H20N)2[Cu2Mo2(C2H4S2)2(CN)2S4], is a sulfide-bridged tetranuclear complex in which the complex anion comprises one [(edt)2Mo2S2(μ-S)2]2− unit (edt = ethanedithiol­ate) and two CuCN units joined through six Cu—μ3-S bonds, thus forming a cubane-like [Mo2S4Cu2] core. There are two independent cation–anion complex entities in the asymmetric unit. Bond distances are normal for this type of complex [ranges: Mo—S = 2.193 (2)–2.390 (2); Cu—S = 2.266 (2)–2.470 (2); Cu—C = 1.899 (7)–1.911 (9) Å]. One of the thiol­ato C atoms is disordered over two sites in a 0.52 (3):0.48 (3) ratio.

Related literature

For related structures, see: Hidai et al. (1999[Hidai, M., Ikada, T., Kuwata, S. & Mizobe, Y. (1999). Inorg. Chem. 38, 64-69.]); Lang et al. (2003[Lang, J.-P., Wei, Z.-H., Xu, Q.-F., Li, H.-X. & Chen, J.-X. (2003). J. Organomet. Chem. 87, 197-202.]); Curtis et al. (1997[Curtis, M. D., Druker, S. H., Goossen, L. & Kampf, J. W. (1997). Organometallics, 16, 231-235.]); Stiefel et al. (1985[Stiefel, E. I., Halbert, T. R. & Cohen, S. A. (1985). Organometallics, 4, 1689-1690.]); Brunner et al. (1985[Brunner, H., Janietz, N., Wachter, J., Zahn, T. & Ziegler, M. L. (1985). Angew. Chem. Int. Ed. 24, 133-135.]); Wu et al. (1990[Wu, X.-T., Zhu, N.-Y. & Zheng, Y.-F. (1990). J. Chem. Soc. Chem. Commun. pp. 780-781.]).

[Scheme 1]

Experimental

Crystal data

  • (C8H20N)2[Cu2Mo2(C2H4S2)2(CN)2S4]

  • Mr = 944.18

  • Orthorhombic, P c a 21

  • a = 12.509 (3) Å

  • b = 16.582 (3) Å

  • c = 34.976 (7) Å

  • V = 7255 (3) Å3

  • Z = 8

  • Mo Kα radiation

  • μ = 2.31 mm−1

  • T = 291 K

  • 0.20 × 0.15 × 0.06 mm
Data collection

  • Rigaku Mercury diffractometer

  • Absorption correction: multi-scan (REQAB; Jacobson, 1998[Jacobson, R. (1998). REQAB. Private communication to the Rigaku Corporation, Tokyo, Japan.]) Tmin = 0.666, Tmax = 0.870

  • 77483 measured reflections

  • 16412 independent reflections

  • 15033 reflections with I > 2σ(I)

  • Rint = 0.075
Refinement

  • R[F2 > 2σ(F2)] = 0.066

  • wR(F2) = 0.097

  • S = 1.19

  • 16412 reflections

  • 705 parameters

  • 1 restraint

  • H-atom parameters constrained

  • Δρmax = 0.58 e Å−3

  • Δρmin = −0.77 e Å−3

  • Absolute structure: Flack (1983[Flack, H. D. (1983). Acta Cryst. A39, 876-881.]), 7995 Friedel pairs

  • Flack parameter: 0.030 (16)

Data collection: CrystalClear (Rigaku/MSC, 2001[Rigaku/MSC (2001). CrystalClear. Rigaku/MSC, The Woodlands, Texas, USA.]); cell refinement: CrystalClear; data reduction: CrystalStructure (Rigaku/MSC, 2004[Rigaku/MSC (2004). CrystalStructure. Rigaku/MSC, The Woodlands, Texas, USA.]); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); software used to prepare material for publication: SHELXTL.

Supporting information

Crystal structure: contains datablocks I, global. DOI: https://doi.org/10.1107/S1600536809044821/zs2011sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536809044821/zs2011Isup2.hkl

checkCIF report


Comment top

Over the past few decades, the chemistry of the sulfido-bridged dinuclear complexes with a M2S4 core (M = Mo, W) with various transition metals has been extensively investigated. For example, the precursors [(dtc)2Mo2S2(µ-S)2] (dtc = S2CNEt2) (Hidai et al., 1999; Lang et al., 2003) and [Cpx2Mo2S2(µ-S)2] (Cpx = pentamethyl-, pentaethyl- or pentabutyl-cyclopentadienyl) (Curtis et al., 1997; Stiefel et al., 1985) and [Et4N]2[(edt)2Mo2S2(µ-S)2] (edt = ethanedithiolate) (Wu et al., 1990) were shown to react with transition metals (M) to form both the incomplete cubane-like [Mo2MS4] clusters and the complete cubane-like [Mo2M2S4] clusters. We report here the formation of a complete cubane-like [Mo2Cu2S4] compound [Et4N]2[(edt)2Mo2Cu2S2(µ-S)2(CN)2] (I) by reacting [Et4N]2[(edt)2Mo2S2(µ-S)2] with two equivalents of CuCN in MeCN solution.

The complex anion in (I) contains one [(edt)2Mo2S2(µ-S)2]2- moiety and two CuCN units which are assembled into a distorted Mo2S4Cu2 cubane-like core. (Fig. 1) The formal oxidation states for each Mo and Cu are +5 and +1, respectively. Each Mo center is coordinated by one terminal µ3-St, two bridging µ-Sb atoms and two Sedt atoms of an edt group, forming a distorted square pyramidal geometry. Each Cu atom is tetrahedrally coordinated by three µ3-S atoms and a terminal cyanide ligand. The Mo—S bond lengths vary from 2.193 (2) to 2.390 (2) Å due to the different types of coordinated S. The average Mo—Sedt bond distance [2.3794 (2) Å] is longer than the average Mo—St value [2.1957 (2) Å] and the Mo—Sb value [2.3604 (7) Å]. The Cu—St bond lengths [av. 2.410 (2) Å] are longer than the Cu—Sb values [av. 2.267 (2) Å). The Mo···Mo distances [2.8508 (11) and 2.8564 (11) Å] and the Mo···Cu distances [range: 2.7999 (13)–2.8594 (14) Å] are normal when compared with those found in other [Mo2S4] cubane-like clusters. The Cu—C bond length range is 1.899 (7)–1.911 (9) Å.

Related literature top

For related structures, see: Hidai et al. (1999); Lang et al. (2003); Curtis et al. (1997); Stiefel et al. (1985); Brunner et al. (1985); Wu et al. (1990).

Experimental top

[Et4N]2[(edt)2Mo2S2(µ-S)2] (0.76 g, 1.0 mmol), and CuCN (0.18 g 2.0 mmol) were added to 50 ml of a MeCN solution (100%). The mixture was stirred at room temperature for 6 h, the suspension gradually changing into a bright red solution. After filtering, the solution was layered with ether (30 ml), producing dark red crystals within one week.

Refinement top

The C1 atom of edt group was found to be disordered over two adjacent sites with an occupancy ratio of 0.48 (3)/0.52 (3) for C1/C1A. All non-hydrogen atoms were refined anisotropically. All the H atoms were placed in geometrically idealized positions [C—H = 0.98 Å, with Uiso(H) = 1.5Ueq(C) for methyl groups and C—H = 0.99 Å, with Uiso(H)= 1.2Ueq(C) for methylene groups] and constrained to ride on their parent atoms. The second SHELXL weighting factor is relatively high, possibly due to the disorder of this structure. The absence of 12 reflections below τ(min) from the FCF list is due to instrumental limitations.

Structure description top

?

# Following replaced by publCIF - Fri September 27 10:31:02 2008

The stucture of the title compound, (I), is shown below. Dimensions are available in the archived CIF.

For related literature, see [type here to add references to related literature].

Computing details top

Data collection: CrystalClear (Rigaku/MSC, 2001); cell refinement: CrystalClear (Rigaku/MSC, 2001); data reduction: CrystalStructure (Rigaku/MSC, 2004); 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 (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. The molecular structure of the title molecule, with the atom-numbering scheme. Displacement ellipsoids are drawn at the 35% probability level
(I) top
Crystal data top
(C8H20N)2[Cu2Mo2(C2H4S2)2(CN)2S4]F(000) = 3824
Mr = 944.18Dx = 1.729 Mg m−3
Orthorhombic, Pca21Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2c -2acCell parameters from 11016 reflections
a = 12.509 (3) Åθ = 3.0–27.5°
b = 16.582 (3) ŵ = 2.31 mm−1
c = 34.976 (7) ÅT = 291 K
V = 7255 (3) Å3Platelet, red
Z = 80.20 × 0.15 × 0.06 mm
Data collection top
Rigaku Mercury
diffractometer		16412 independent reflections
Radiation source: fine-focus sealed tube15033 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.075
ω scansθmax = 27.5°, θmin = 3.0°
Absorption correction: multi-scan
(REQAB; Jacobson, 1998)		h = −16→16
Tmin = 0.666, Tmax = 0.870k = −21→21
77483 measured reflectionsl = −44→45
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.066H-atom parameters constrained
wR(F2) = 0.097 w = 1/[σ2(Fo2) + (0.0156P)2 + 23.3405P]
where P = (Fo2 + 2Fc2)/3
S = 1.19(Δ/σ)max = 0.001
16412 reflectionsΔρmax = 0.58 e Å−3
705 parametersΔρmin = −0.77 e Å−3
1 restraintAbsolute structure: Flack (1983), 7995 Friedel pairs
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.030 (16)
Crystal data top
(C8H20N)2[Cu2Mo2(C2H4S2)2(CN)2S4]V = 7255 (3) Å3
Mr = 944.18Z = 8
Orthorhombic, Pca21Mo Kα radiation
a = 12.509 (3) ŵ = 2.31 mm−1
b = 16.582 (3) ÅT = 291 K
c = 34.976 (7) Å0.20 × 0.15 × 0.06 mm
Data collection top
Rigaku Mercury
diffractometer		16412 independent reflections
Absorption correction: multi-scan
(REQAB; Jacobson, 1998)		15033 reflections with I > 2σ(I)
Tmin = 0.666, Tmax = 0.870Rint = 0.075
77483 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.066H-atom parameters constrained
wR(F2) = 0.097 w = 1/[σ2(Fo2) + (0.0156P)2 + 23.3405P]
where P = (Fo2 + 2Fc2)/3
S = 1.19Δρmax = 0.58 e Å−3
16412 reflectionsΔρmin = −0.77 e Å−3
705 parametersAbsolute structure: Flack (1983), 7995 Friedel pairs
1 restraintAbsolute structure parameter: 0.030 (16)
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s 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 > σ(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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Mo10.02887 (5)0.33262 (4)0.102241 (18)0.02016 (14)
S10.20796 (16)0.38036 (12)0.09482 (6)0.0293 (4)
Cu1−0.17308 (8)0.27253 (6)0.08180 (3)0.0288 (2)
C10.1205 (16)0.5281 (11)0.1086 (7)0.035 (6)0.48 (3)
H1A0.10710.58080.09760.043*0.48 (3)
H1B0.14910.53590.13410.043*0.48 (3)
C1A0.0964 (18)0.5203 (14)0.0817 (12)0.072 (4)0.52 (3)
H1A10.07570.51570.05500.086*0.52 (3)
H1A20.09970.57720.08790.086*0.52 (3)
C20.1962 (8)0.4873 (6)0.0862 (4)0.072 (4)
H2A0.26550.51190.09050.086*
H2B0.17810.49530.05950.086*
C3−0.1751 (8)0.0812 (5)0.2066 (3)0.039 (2)
H3A−0.22410.07170.22770.046*
H3B−0.18770.04050.18730.046*
C4−0.0631 (8)0.0756 (5)0.2205 (2)0.040 (2)
H4A−0.04800.02040.22800.048*
H4B−0.05470.10950.24290.048*
C5−0.3065 (6)0.2843 (5)0.0560 (2)0.0266 (18)
C60.1210 (7)0.1065 (5)0.0357 (3)0.0324 (19)
C70.5228 (7)0.0099 (5)0.3221 (3)0.051 (3)
H7A0.5341−0.01600.29760.061*
H7B0.5805−0.00630.33900.061*
C80.4225 (8)−0.0173 (5)0.3380 (4)0.051 (3)
H8A0.4183−0.00150.36460.061*
H8B0.4193−0.07570.33680.061*
C90.2420 (9)0.4206 (6)0.1986 (3)0.050 (3)
H9A0.25490.47650.19180.061*
H9B0.25020.38830.17560.061*
C100.1285 (9)0.4116 (6)0.2137 (3)0.052 (3)
H10A0.07770.42090.19330.063*
H10B0.11570.45120.23360.063*
C110.4415 (7)0.3910 (5)0.3819 (3)0.034 (2)
C120.0144 (6)0.2175 (5)0.3661 (2)0.0273 (18)
C13−0.1852 (7)0.2114 (5)0.2908 (2)0.037 (2)
H13A−0.11090.21280.29760.055*
H13B−0.19230.21760.26360.055*
H13C−0.21540.16060.29840.055*
C14−0.2433 (6)0.2789 (4)0.3107 (2)0.0308 (19)
H14A−0.23190.27380.33800.037*
H14B−0.31930.27300.30600.037*
C15−0.3262 (7)0.3566 (5)0.2376 (3)0.040 (2)
H15A−0.37840.39240.24840.060*
H15B−0.34610.30180.24290.060*
H15C−0.32270.36460.21050.060*
C16−0.2177 (6)0.3739 (5)0.2552 (2)0.0278 (18)
H16A−0.19820.42900.24900.033*
H16B−0.16560.33880.24310.033*
C17−0.2684 (7)0.4297 (5)0.3609 (2)0.042 (2)
H17A−0.20320.45830.36610.063*
H17B−0.26450.37680.37190.063*
H17C−0.32750.45850.37190.063*
C18−0.2838 (6)0.4229 (4)0.3184 (3)0.0295 (18)
H18A−0.27360.47580.30710.035*
H18B−0.35710.40690.31350.035*
C19−0.0536 (7)0.4624 (5)0.3027 (3)0.043 (2)
H19A−0.10010.50040.31500.064*
H19B−0.05240.47290.27570.064*
H19C0.01740.46770.31280.064*
C20−0.0940 (6)0.3775 (5)0.3097 (2)0.0294 (19)
H20A−0.04910.34010.29570.035*
H20B−0.08630.36530.33670.035*
C210.6951 (9)−0.0144 (5)0.4246 (3)0.052 (3)
H21A0.7374−0.02560.44690.078*
H21B0.7196−0.04690.40370.078*
H21C0.6215−0.02660.42980.078*
C220.7057 (8)0.0737 (5)0.4143 (2)0.034 (2)
H22A0.65560.08570.39390.041*
H22B0.77710.08290.40440.041*
C230.8810 (7)0.1219 (7)0.4688 (3)0.053 (3)
H23A0.89420.08190.44960.080*
H23B0.92460.11090.49080.080*
H23C0.89810.17430.45890.080*
C240.7639 (6)0.1196 (5)0.4802 (2)0.0303 (19)
H24A0.75120.16110.49920.036*
H24B0.74890.06790.49210.036*
C250.4841 (8)0.1355 (7)0.4369 (3)0.054 (3)
H25A0.48240.19160.43010.081*
H25B0.41770.12080.44870.081*
H25C0.49460.10370.41430.081*
C260.5743 (6)0.1207 (6)0.4643 (2)0.035 (2)
H26A0.56850.06610.47400.042*
H26B0.56670.15720.48580.042*
C270.6721 (7)0.2845 (5)0.4563 (3)0.037 (2)
H27A0.60290.27620.46750.055*
H27B0.67230.33410.44220.055*
H27C0.72500.28710.47620.055*
C280.6976 (6)0.2159 (5)0.4300 (2)0.0262 (17)
H28A0.77050.22230.42110.031*
H28B0.65110.21970.40780.031*
C290.5600 (7)0.3799 (6)−0.0479 (3)0.047 (2)
H29A0.57400.4247−0.03130.070*
H29B0.60420.3842−0.07030.070*
H29C0.57570.3305−0.03480.070*
C300.4436 (6)0.3807 (5)−0.0597 (2)0.0307 (19)
H30A0.42830.4322−0.07160.037*
H30B0.43300.3392−0.07890.037*
C310.3698 (9)0.5160 (5)−0.0075 (3)0.052 (3)
H31A0.41610.5273−0.02870.079*
H31B0.38890.54980.01370.079*
H31C0.29710.5264−0.01470.079*
C320.3815 (7)0.4284 (5)0.0039 (3)0.034 (2)
H32A0.33120.41720.02440.041*
H32B0.45280.42040.01410.041*
C330.3522 (7)0.2128 (5)−0.0351 (3)0.037 (2)
H33A0.27890.2141−0.04320.056*
H33B0.36550.1637−0.02130.056*
H33C0.39810.2152−0.05700.056*
C340.3746 (6)0.2850 (4)−0.0091 (2)0.0244 (17)
H34A0.32620.28260.01250.029*
H34B0.44680.28010.00080.029*
C350.1619 (7)0.3618 (6)−0.0201 (3)0.045 (2)
H35A0.16810.3086−0.00960.067*
H35B0.09660.3658−0.03440.067*
H35C0.16150.40070.00020.067*
C360.2550 (6)0.3779 (5)−0.0461 (3)0.031 (2)
H36A0.24940.4327−0.05560.037*
H36B0.25000.3420−0.06790.037*
C37−0.1202 (7)0.0466 (5)0.6145 (3)0.047 (3)
H37A−0.07560.01620.59740.070*
H37B−0.19310.04390.60590.070*
H37C−0.11500.02450.63980.070*
C38−0.0843 (6)0.1329 (5)0.6149 (3)0.0309 (19)
H38A−0.13510.16380.62990.037*
H38B−0.08710.15340.58900.037*
C390.1328 (10)0.1435 (6)0.6930 (3)0.062 (3)
H39A0.19170.11910.67980.093*
H39B0.12890.12220.71850.093*
H39C0.14330.20080.69420.093*
C400.0298 (8)0.1253 (6)0.6720 (3)0.043 (2)
H40A0.01620.06780.67390.052*
H40B−0.02810.15270.68510.052*
C41−0.0107 (8)0.2948 (5)0.6483 (3)0.052 (3)
H41A−0.08520.28820.64260.078*
H41B0.01080.34900.64240.078*
H41C0.00130.28430.67490.078*
C420.0538 (7)0.2366 (5)0.6247 (3)0.039 (2)
H42A0.12890.24440.63050.047*
H42B0.04360.24960.59790.047*
C430.1006 (10)0.1032 (8)0.5660 (3)0.083 (4)
H43A0.03050.08750.55760.124*
H43B0.15290.06780.55490.124*
H43C0.11460.15760.55800.124*
C440.1067 (7)0.0981 (6)0.6093 (3)0.045 (2)
H44A0.09710.04230.61680.055*
H44B0.17790.11430.61720.055*
N1−0.3880 (6)0.2861 (5)0.0413 (2)0.042 (2)
N20.1619 (7)0.0639 (5)0.0138 (3)0.053 (2)
Mo2−0.05657 (5)0.19577 (4)0.141312 (18)0.02093 (13)
S2−0.00775 (19)0.47167 (13)0.11186 (8)0.0434 (6)
Cu20.05253 (8)0.17737 (6)0.07085 (3)0.0300 (2)
Mo30.25350 (5)0.29993 (4)0.277488 (18)0.02172 (13)
S30.03236 (18)0.10698 (13)0.18384 (6)0.0313 (5)
Cu30.37031 (8)0.32023 (6)0.34710 (3)0.0286 (2)
N30.4825 (7)0.4345 (5)0.4023 (2)0.045 (2)
N4−0.0642 (6)0.2169 (5)0.3830 (2)0.0351 (17)
Mo40.34607 (5)0.16534 (4)0.315903 (18)0.01961 (13)
S4−0.19841 (17)0.18212 (12)0.18646 (6)0.0300 (5)
Cu40.14535 (7)0.22251 (6)0.33871 (3)0.0262 (2)
N5−0.2092 (5)0.3632 (3)0.29831 (19)0.0232 (14)
S50.12491 (16)0.22166 (12)0.12619 (6)0.0256 (4)
N60.3632 (5)0.3674 (4)−0.02800 (18)0.0224 (14)
S6−0.12893 (15)0.32645 (11)0.13939 (6)0.0244 (4)
N70.6861 (5)0.1320 (4)0.44682 (19)0.0244 (14)
S7−0.02092 (15)0.29986 (12)0.04405 (6)0.0246 (4)
N80.0266 (5)0.1487 (4)0.63065 (18)0.0243 (14)
S8−0.11924 (16)0.13066 (12)0.09146 (6)0.0248 (4)
S90.30935 (19)0.02490 (13)0.31218 (8)0.0345 (5)
S100.52654 (17)0.11911 (13)0.31587 (8)0.0415 (6)
S110.1106 (2)0.31074 (13)0.23289 (7)0.0380 (5)
S120.3383 (2)0.38889 (14)0.23379 (7)0.0407 (6)
S130.43748 (16)0.27776 (12)0.29061 (6)0.0279 (4)
S140.18517 (15)0.16796 (11)0.28071 (6)0.0240 (4)
S150.19383 (16)0.36416 (11)0.32809 (6)0.0244 (4)
S160.30285 (16)0.19827 (12)0.37463 (6)0.0214 (4)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mo10.0213 (3)0.0207 (3)0.0184 (3)−0.0003 (2)−0.0018 (3)−0.0006 (3)
S10.0247 (10)0.0314 (11)0.0316 (12)−0.0062 (8)−0.0011 (8)−0.0007 (8)
Cu10.0223 (5)0.0391 (6)0.0250 (6)0.0012 (4)−0.0038 (4)−0.0004 (4)
C10.045 (12)0.024 (9)0.038 (14)−0.007 (8)0.003 (10)−0.007 (8)
C1A0.036 (5)0.049 (6)0.130 (11)−0.009 (5)0.020 (6)0.018 (6)
C20.036 (5)0.049 (6)0.130 (11)−0.009 (5)0.020 (6)0.018 (6)
C30.057 (6)0.032 (5)0.027 (5)−0.008 (4)0.008 (4)0.005 (4)
C40.074 (7)0.020 (4)0.026 (5)0.016 (4)0.000 (5)0.001 (4)
C50.025 (4)0.026 (4)0.029 (5)−0.005 (3)−0.003 (3)−0.002 (3)
C60.028 (4)0.038 (5)0.031 (5)0.007 (4)0.001 (4)−0.001 (4)
C70.039 (5)0.038 (5)0.076 (7)0.012 (4)−0.008 (5)−0.009 (5)
C80.055 (6)0.022 (4)0.077 (8)−0.002 (4)−0.026 (6)0.009 (5)
C90.092 (9)0.040 (5)0.019 (5)−0.005 (5)0.000 (5)0.004 (4)
C100.090 (9)0.034 (5)0.032 (6)0.013 (5)−0.015 (5)−0.001 (4)
C110.038 (5)0.035 (5)0.030 (5)−0.010 (4)−0.004 (4)0.000 (4)
C120.031 (5)0.032 (4)0.019 (4)0.000 (3)−0.003 (4)0.000 (3)
C130.056 (6)0.028 (4)0.027 (5)−0.001 (4)−0.009 (4)−0.006 (3)
C140.027 (4)0.028 (4)0.037 (5)−0.002 (3)0.005 (4)0.002 (4)
C150.040 (5)0.039 (5)0.040 (6)0.002 (4)−0.005 (4)0.005 (4)
C160.031 (4)0.028 (4)0.025 (4)0.001 (3)−0.004 (3)0.001 (3)
C170.050 (6)0.042 (5)0.035 (5)0.007 (4)0.006 (4)−0.005 (4)
C180.025 (4)0.018 (4)0.046 (5)0.009 (3)−0.002 (4)0.000 (3)
C190.031 (5)0.037 (5)0.060 (7)−0.005 (4)−0.012 (4)0.001 (4)
C200.030 (4)0.034 (4)0.024 (5)0.003 (3)−0.015 (3)−0.004 (3)
C210.061 (7)0.033 (5)0.063 (7)0.001 (5)−0.007 (5)−0.013 (5)
C220.046 (5)0.032 (5)0.024 (5)0.008 (4)0.003 (4)−0.008 (4)
C230.023 (5)0.083 (8)0.054 (7)0.007 (5)−0.008 (5)0.026 (6)
C240.028 (4)0.038 (5)0.025 (5)0.007 (4)−0.007 (3)0.006 (4)
C250.032 (5)0.081 (8)0.048 (7)−0.002 (5)−0.003 (5)0.005 (6)
C260.027 (5)0.051 (6)0.027 (5)−0.009 (4)0.008 (4)0.007 (4)
C270.047 (6)0.030 (5)0.033 (5)0.007 (4)0.006 (4)−0.001 (4)
C280.026 (4)0.033 (4)0.020 (4)0.002 (3)0.002 (3)0.006 (3)
C290.035 (5)0.055 (6)0.050 (6)−0.004 (5)0.005 (5)0.009 (5)
C300.035 (5)0.032 (4)0.026 (5)−0.002 (4)0.003 (4)0.007 (4)
C310.066 (7)0.037 (5)0.054 (7)−0.008 (5)0.009 (6)−0.005 (5)
C320.040 (5)0.027 (4)0.035 (5)−0.011 (4)0.007 (4)−0.005 (4)
C330.037 (5)0.032 (5)0.042 (6)0.003 (4)0.007 (4)0.001 (4)
C340.024 (4)0.018 (4)0.031 (5)−0.001 (3)−0.004 (3)0.004 (3)
C350.022 (5)0.061 (7)0.052 (7)0.004 (4)−0.004 (4)0.004 (5)
C360.026 (4)0.031 (5)0.036 (5)−0.006 (4)0.001 (4)0.007 (4)
C370.033 (5)0.031 (5)0.076 (8)0.006 (4)−0.016 (5)0.006 (5)
C380.025 (4)0.027 (4)0.041 (5)0.004 (3)0.000 (4)0.001 (4)
C390.090 (9)0.044 (6)0.053 (7)−0.007 (6)−0.037 (6)0.000 (5)
C400.062 (6)0.042 (5)0.025 (5)−0.010 (5)0.000 (4)0.008 (4)
C410.069 (7)0.018 (4)0.069 (7)0.008 (4)−0.015 (6)−0.012 (4)
C420.037 (5)0.027 (4)0.053 (6)0.001 (4)−0.006 (4)0.010 (4)
C430.080 (9)0.102 (11)0.066 (9)0.020 (8)0.028 (7)−0.025 (8)
C440.032 (5)0.046 (5)0.058 (7)0.006 (4)−0.002 (4)−0.014 (5)
N10.028 (4)0.057 (5)0.039 (5)−0.011 (4)−0.007 (4)0.005 (4)
N20.054 (5)0.058 (6)0.048 (6)0.012 (4)0.003 (4)−0.021 (4)
Mo20.0260 (3)0.0192 (3)0.0176 (3)0.0010 (3)−0.0008 (3)−0.0001 (3)
S20.0384 (13)0.0206 (10)0.0711 (19)−0.0006 (9)0.0134 (12)−0.0022 (10)
Cu20.0310 (5)0.0326 (6)0.0265 (6)0.0061 (4)−0.0012 (4)−0.0094 (4)
Mo30.0293 (3)0.0193 (3)0.0166 (3)−0.0018 (3)0.0001 (3)−0.0012 (3)
S30.0414 (13)0.0274 (11)0.0249 (11)0.0083 (9)−0.0041 (9)0.0035 (9)
Cu30.0297 (5)0.0283 (5)0.0279 (6)−0.0078 (4)−0.0011 (4)−0.0060 (4)
N30.049 (5)0.048 (5)0.038 (5)−0.021 (4)−0.003 (4)−0.011 (4)
N40.024 (4)0.049 (5)0.032 (4)−0.007 (3)0.001 (3)0.001 (3)
Mo40.0179 (3)0.0187 (3)0.0222 (3)0.0005 (2)0.0019 (3)−0.0028 (3)
S40.0363 (11)0.0308 (11)0.0229 (11)−0.0011 (9)0.0060 (9)0.0038 (8)
Cu40.0200 (5)0.0319 (5)0.0267 (6)−0.0010 (4)0.0047 (4)−0.0034 (4)
N50.021 (3)0.016 (3)0.032 (4)0.000 (2)−0.004 (3)0.001 (3)
S50.0234 (10)0.0275 (10)0.0258 (11)0.0042 (8)−0.0017 (8)−0.0004 (8)
N60.025 (3)0.022 (3)0.020 (4)0.001 (3)0.005 (3)0.002 (3)
S60.0267 (10)0.0237 (9)0.0228 (10)0.0020 (7)0.0027 (8)−0.0005 (8)
N70.019 (3)0.031 (4)0.024 (4)0.003 (3)0.002 (3)0.006 (3)
S70.0234 (10)0.0301 (10)0.0204 (10)−0.0034 (8)−0.0020 (8)0.0003 (8)
N80.027 (3)0.021 (3)0.025 (4)0.005 (3)−0.005 (3)−0.002 (3)
S80.0278 (10)0.0243 (10)0.0221 (11)−0.0035 (8)−0.0025 (8)−0.0018 (8)
S90.0337 (12)0.0209 (10)0.0490 (15)0.0017 (9)−0.0109 (11)−0.0071 (10)
S100.0223 (10)0.0362 (12)0.0659 (17)0.0057 (9)0.0059 (11)−0.0042 (11)
S110.0518 (14)0.0344 (12)0.0279 (12)0.0014 (10)−0.0148 (11)−0.0020 (9)
S120.0641 (17)0.0344 (12)0.0235 (12)−0.0103 (11)0.0046 (11)0.0048 (9)
S130.0261 (10)0.0276 (10)0.0300 (12)−0.0045 (8)0.0080 (9)0.0006 (8)
S140.0261 (10)0.0203 (9)0.0255 (11)0.0007 (7)−0.0012 (8)−0.0040 (8)
S150.0295 (10)0.0207 (9)0.0231 (10)0.0005 (8)−0.0010 (8)−0.0019 (8)
S160.0232 (10)0.0217 (10)0.0193 (10)0.0006 (8)−0.0006 (8)0.0011 (8)
Geometric parameters (Å, º) top
Mo1—Mo22.8564 (11)C15—H15A0.9600
Mo1—Cu12.8081 (14)C15—H15C0.9600
Mo1—Cu22.8143 (14)C16—H16A0.9700
Mo1—S12.390 (2)C16—H16B0.9700
Mo1—S22.375 (2)C17—H17A0.9600
Mo1—S52.352 (2)C17—H17B0.9600
Mo1—S62.365 (2)C17—H17C0.9600
Mo1—S72.197 (2)C18—H18B0.9700
Mo2—Cu12.8420 (14)C18—H18A0.9700
Mo2—Cu22.8336 (14)C19—H19C0.9600
Mo2—S32.370 (2)C19—H19A0.9600
Mo2—S42.386 (2)C19—H19B0.9600
Mo2—S52.370 (2)C20—H20A0.9700
Mo2—S62.349 (2)C20—H20B0.9700
Mo2—S82.196 (2)C29—C301.514 (12)
Mo3—Cu32.8594 (14)C31—C321.513 (12)
Mo3—Cu42.8396 (14)C33—C341.529 (11)
Mo3—S112.379 (3)C35—C361.502 (13)
Mo3—S122.374 (3)C29—H29C0.9600
Mo3—S132.375 (2)C29—H29A0.9600
Mo3—S142.352 (2)C29—H29B0.9600
Mo3—S152.196 (2)C30—H30B0.9700
Mo3—Mo42.8508 (11)C30—H30A0.9700
Mo4—Cu42.7999 (13)C31—H31A0.9600
Mo4—S92.377 (2)C31—H31C0.9600
Mo4—S102.384 (2)C31—H31B0.9600
Mo4—S132.359 (2)C32—H32B0.9700
Mo4—S142.360 (2)C32—H32A0.9700
Mo4—S162.193 (2)C33—H33B0.9600
Mo4—Cu32.8070 (14)C33—H33C0.9600
Cu1—S62.272 (2)C33—H33A0.9600
Cu1—S72.360 (2)C34—H34B0.9700
Cu1—S82.470 (2)C34—H34A0.9700
Cu1—C51.907 (7)C35—H35C0.9600
Cu2—S52.260 (2)C35—H35B0.9600
Cu2—S72.418 (2)C35—H35A0.9600
Cu2—S82.395 (2)C36—H36A0.9700
Cu2—C61.904 (9)C36—H36B0.9700
Cu3—S152.418 (2)C21—C221.511 (12)
Cu3—S162.394 (2)C23—C241.519 (12)
Cu3—C111.911 (9)C25—C261.501 (13)
Cu3—S132.260 (2)C27—C281.497 (12)
Cu4—S152.454 (2)C21—H21B0.9600
Cu4—S162.371 (2)C21—H21C0.9600
Cu4—S142.276 (2)C21—H21A0.9600
Cu4—C121.899 (7)C22—H22A0.9700
S1—C21.805 (10)C22—H22B0.9700
S2—C1A1.86 (3)C23—H23A0.9600
S2—C11.86 (2)C23—H23C0.9600
S3—C41.828 (9)C23—H23B0.9600
S4—C31.839 (9)C24—H24B0.9700
S9—C81.819 (11)C24—H24A0.9700
S10—C71.825 (9)C25—H25C0.9600
S11—C101.816 (10)C25—H25A0.9600
S12—C91.801 (11)C25—H25B0.9600
N1—C51.142 (10)C26—H26B0.9700
N2—C61.161 (13)C26—H26A0.9700
N5—C181.531 (10)C27—H27B0.9600
N5—C201.514 (10)C27—H27A0.9600
N5—C161.522 (10)C27—H27C0.9600
N5—C141.524 (9)C28—H28B0.9700
N6—C301.513 (10)C28—H28A0.9700
N6—C341.525 (9)C37—C381.500 (12)
N6—C361.504 (10)C39—C401.514 (16)
N6—C321.523 (12)C41—C421.505 (13)
N7—C261.538 (10)C43—C441.519 (15)
N7—C281.517 (10)C37—H37C0.9600
N7—C241.534 (10)C37—H37B0.9600
N7—C221.513 (10)C37—H37A0.9600
N8—C441.505 (12)C38—H38A0.9700
N8—C421.511 (11)C38—H38B0.9700
N8—C381.515 (10)C39—H39A0.9600
N8—C401.498 (12)C39—H39B0.9600
C1—C21.40 (2)C39—H39C0.9600
C1A—C21.37 (3)C40—H40B0.9700
C3—C41.486 (14)C40—H40A0.9700
N3—C111.137 (12)C41—H41A0.9600
N4—C121.147 (10)C41—H41C0.9600
C1—H1A0.9700C41—H41B0.9600
C1—H1B0.9700C42—H42A0.9700
C1A—H1A10.9700C42—H42B0.9700
C1A—H1A20.9700C43—H43C0.9600
C2—H2A0.9700C43—H43B0.9600
C3—H3A0.9700C43—H43A0.9600
C3—H3B0.9700C44—H44B0.9700
C4—H4B0.9700C44—H44A0.9700
C4—H4A0.9700C7—C81.445 (14)
C13—C141.505 (11)C9—C101.522 (16)
C15—C161.518 (12)C7—H7A0.9700
C17—C181.503 (13)C7—H7B0.9700
C19—C201.516 (12)C8—H8A0.9700
C13—H13A0.9600C8—H8B0.9700
C13—H13C0.9600C9—H9A0.9700
C13—H13B0.9600C9—H9B0.9700
C14—H14B0.9700C10—H10A0.9700
C14—H14A0.9700C10—H10B0.9700
C15—H15B0.9600
S7—Mo1—S5106.35 (8)H35A—C35—H35C109.5
S7—Mo1—S6105.17 (8)H35B—C35—H35C109.5
S5—Mo1—S6101.35 (7)C35—C36—N6115.0 (7)
S7—Mo1—S2108.46 (9)C35—C36—H36A108.5
S5—Mo1—S2143.87 (9)N6—C36—H36A108.5
S6—Mo1—S278.65 (7)C35—C36—H36B108.5
S7—Mo1—S1104.30 (8)N6—C36—H36B108.5
S5—Mo1—S179.57 (7)H36A—C36—H36B107.5
S6—Mo1—S1148.88 (8)C38—C37—H37A109.5
S2—Mo1—S182.79 (8)C38—C37—H37B109.5
S7—Mo1—Cu154.64 (6)H37A—C37—H37B109.5
S5—Mo1—Cu1105.82 (6)C38—C37—H37C109.5
S6—Mo1—Cu151.23 (5)H37A—C37—H37C109.5
S2—Mo1—Cu1101.95 (7)H37B—C37—H37C109.5
S1—Mo1—Cu1158.92 (6)C37—C38—N8116.3 (6)
S7—Mo1—Cu256.09 (6)C37—C38—H38A108.2
S5—Mo1—Cu250.92 (6)N8—C38—H38A108.2
S6—Mo1—Cu2105.22 (5)C37—C38—H38B108.2
S2—Mo1—Cu2164.52 (8)N8—C38—H38B108.2
S1—Mo1—Cu299.33 (6)H38A—C38—H38B107.4
Cu1—Mo1—Cu270.78 (3)C40—C39—H39A109.5
S7—Mo1—Mo298.09 (6)C40—C39—H39B109.5
S5—Mo1—Mo253.07 (5)H39A—C39—H39B109.5
S6—Mo1—Mo252.46 (5)C40—C39—H39C109.5
S2—Mo1—Mo2129.15 (7)H39A—C39—H39C109.5
S1—Mo1—Mo2131.74 (6)H39B—C39—H39C109.5
Cu1—Mo1—Mo260.22 (3)N8—C40—C39116.1 (8)
Cu2—Mo1—Mo259.95 (3)N8—C40—H40A108.3
C2—S1—Mo1105.5 (3)C39—C40—H40A108.3
C5—Cu1—S6126.3 (2)N8—C40—H40B108.3
C5—Cu1—S7114.9 (3)C39—C40—H40B108.3
S6—Cu1—S7102.97 (8)H40A—C40—H40B107.4
C5—Cu1—S8113.6 (2)C42—C41—H41A109.5
S6—Cu1—S8100.80 (7)C42—C41—H41B109.5
S7—Cu1—S892.26 (8)H41A—C41—H41B109.5
C5—Cu1—Mo1150.6 (2)C42—C41—H41C109.5
S6—Cu1—Mo154.27 (5)H41A—C41—H41C109.5
S7—Cu1—Mo149.37 (5)H41B—C41—H41C109.5
S8—Cu1—Mo193.32 (6)C41—C42—N8115.0 (7)
C5—Cu1—Mo2147.2 (2)C41—C42—H42A108.5
S6—Cu1—Mo253.29 (5)N8—C42—H42A108.5
S7—Cu1—Mo294.71 (6)C41—C42—H42B108.5
S8—Cu1—Mo248.20 (5)N8—C42—H42B108.5
Mo1—Cu1—Mo260.73 (3)H42A—C42—H42B107.5
C2—C1—S2111.9 (12)C44—C43—H43A109.5
C2—C1—H1A109.2C44—C43—H43B109.5
S2—C1—H1A109.2H43A—C43—H43B109.5
C2—C1—H1B109.2C44—C43—H43C109.5
S2—C1—H1B109.2H43A—C43—H43C109.5
H1A—C1—H1B107.9H43B—C43—H43C109.5
C2—C1A—S2113.5 (19)N8—C44—C43115.5 (8)
C2—C1A—H1A1108.9N8—C44—H44A108.4
S2—C1A—H1A1108.9C43—C44—H44A108.4
C2—C1A—H1A2108.9N8—C44—H44B108.4
S2—C1A—H1A2108.9C43—C44—H44B108.4
H1A1—C1A—H1A2107.7H44A—C44—H44B107.5
C1A—C2—S1119.1 (12)S8—Mo2—S6107.05 (8)
C1—C2—S1115.8 (11)S8—Mo2—S3111.13 (8)
C1A—C2—H2A131.6S6—Mo2—S3140.52 (8)
C1—C2—H2A108.3S8—Mo2—S5104.71 (8)
S1—C2—H2A108.3S6—Mo2—S5101.28 (7)
C1A—C2—H2B67.8S3—Mo2—S578.64 (8)
C1—C2—H2B108.3S8—Mo2—S4102.32 (8)
S1—C2—H2B108.3S6—Mo2—S479.63 (7)
H2A—C2—H2B107.4S3—Mo2—S482.81 (8)
C4—C3—S4109.4 (6)S5—Mo2—S4151.30 (8)
C4—C3—H3A109.8S8—Mo2—Cu255.13 (6)
S4—C3—H3A109.8S6—Mo2—Cu2105.07 (6)
C4—C3—H3B109.8S3—Mo2—Cu2104.65 (6)
S4—C3—H3B109.8S5—Mo2—Cu250.51 (6)
H3A—C3—H3B108.2S4—Mo2—Cu2157.45 (6)
C3—C4—S3111.7 (6)S8—Mo2—Cu157.01 (6)
C3—C4—H4A109.3S6—Mo2—Cu150.82 (6)
S3—C4—H4A109.3S3—Mo2—Cu1168.11 (6)
C3—C4—H4B109.3S5—Mo2—Cu1104.28 (6)
S3—C4—H4B109.3S4—Mo2—Cu198.38 (6)
H4A—C4—H4B108.0Cu2—Mo2—Cu170.01 (4)
N1—C5—Cu1175.3 (8)S8—Mo2—Mo198.29 (6)
N2—C6—Cu2179.0 (9)S6—Mo2—Mo152.96 (5)
C8—C7—S10112.2 (6)S3—Mo2—Mo1128.18 (6)
C8—C7—H7A109.2S5—Mo2—Mo152.48 (5)
S10—C7—H7A109.2S4—Mo2—Mo1132.08 (6)
C8—C7—H7B109.2Cu2—Mo2—Mo159.28 (3)
S10—C7—H7B109.2Cu1—Mo2—Mo159.05 (3)
H7A—C7—H7B107.9C1A—S2—Mo1101.8 (8)
C7—C8—S9111.5 (8)C1—S2—Mo1108.3 (6)
C7—C8—H8A109.3C6—Cu2—S5125.0 (3)
S9—C8—H8A109.3C6—Cu2—S8113.5 (3)
C7—C8—H8B109.3S5—Cu2—S8101.94 (8)
S9—C8—H8B109.3C6—Cu2—S7116.0 (3)
H8A—C8—H8B108.0S5—Cu2—S7102.20 (8)
C10—C9—S12110.9 (7)S8—Cu2—S792.72 (8)
C10—C9—H9A109.5C6—Cu2—Mo1149.7 (3)
S12—C9—H9A109.5S5—Cu2—Mo153.89 (5)
C10—C9—H9B109.5S8—Cu2—Mo194.82 (6)
S12—C9—H9B109.5S7—Cu2—Mo148.93 (5)
H9A—C9—H9B108.1C6—Cu2—Mo2147.6 (3)
C9—C10—S11109.5 (7)S5—Cu2—Mo254.05 (6)
C9—C10—H10A109.8S8—Cu2—Mo248.78 (5)
S11—C10—H10A109.8S7—Cu2—Mo293.65 (6)
C9—C10—H10B109.8Mo1—Cu2—Mo260.76 (3)
S11—C10—H10B109.8S15—Mo3—S14106.80 (8)
H10A—C10—H10B108.2S15—Mo3—S12111.67 (8)
N3—C11—Cu3178.5 (9)S14—Mo3—S12140.47 (8)
N4—C12—Cu4177.8 (8)S15—Mo3—S13104.39 (8)
C14—C13—H13A109.5S14—Mo3—S13101.47 (7)
C14—C13—H13B109.5S12—Mo3—S1377.75 (8)
H13A—C13—H13B109.5S15—Mo3—S11103.67 (8)
C14—C13—H13C109.5S14—Mo3—S1180.12 (8)
H13A—C13—H13C109.5S12—Mo3—S1182.35 (9)
H13B—C13—H13C109.5S13—Mo3—S11150.04 (8)
C13—C14—N5114.6 (6)S15—Mo3—Cu456.61 (6)
C13—C14—H14A108.6S14—Mo3—Cu450.95 (6)
N5—C14—H14A108.6S12—Mo3—Cu4168.28 (7)
C13—C14—H14B108.6S13—Mo3—Cu4104.24 (6)
N5—C14—H14B108.6S11—Mo3—Cu499.81 (7)
H14A—C14—H14B107.6S15—Mo3—Mo497.92 (6)
C16—C15—H15A109.5S14—Mo3—Mo452.89 (5)
C16—C15—H15B109.5S12—Mo3—Mo4127.47 (7)
H15A—C15—H15B109.5S13—Mo3—Mo452.71 (5)
C16—C15—H15C109.5S11—Mo3—Mo4132.31 (6)
H15A—C15—H15C109.5Cu4—Mo3—Mo458.95 (3)
H15B—C15—H15C109.5S15—Mo3—Cu355.28 (6)
C15—C16—N5116.2 (7)S14—Mo3—Cu3104.74 (6)
C15—C16—H16A108.2S12—Mo3—Cu3104.29 (7)
N5—C16—H16A108.2S13—Mo3—Cu350.10 (6)
C15—C16—H16B108.2S11—Mo3—Cu3158.95 (7)
N5—C16—H16B108.2Cu4—Mo3—Cu369.79 (3)
H16A—C16—H16B107.4Mo4—Mo3—Cu358.89 (3)
C18—C17—H17A109.5C4—S3—Mo2108.1 (3)
C18—C17—H17B109.5C11—Cu3—S13125.1 (3)
H17A—C17—H17B109.5C11—Cu3—S16115.3 (3)
C18—C17—H17C109.5S13—Cu3—S16102.68 (8)
H17A—C17—H17C109.5C11—Cu3—S15114.6 (3)
H17B—C17—H17C109.5S13—Cu3—S15101.13 (8)
C17—C18—N5115.1 (6)S16—Cu3—S1592.48 (8)
C17—C18—H18A108.5C11—Cu3—Mo4149.3 (3)
N5—C18—H18A108.5S13—Cu3—Mo454.20 (6)
C17—C18—H18B108.5S16—Cu3—Mo449.09 (6)
N5—C18—H18B108.5S15—Cu3—Mo494.02 (6)
H18A—C18—H18B107.5C11—Cu3—Mo3148.5 (3)
C20—C19—H19A109.5S13—Cu3—Mo353.76 (6)
C20—C19—H19B109.5S16—Cu3—Mo393.61 (6)
H19A—C19—H19B109.5S15—Cu3—Mo348.30 (5)
C20—C19—H19C109.5Mo4—Cu3—Mo360.40 (3)
H19A—C19—H19C109.5S16—Mo4—S13105.90 (8)
H19B—C19—H19C109.5S16—Mo4—S14105.88 (8)
N5—C20—C19114.9 (6)S13—Mo4—S14101.73 (8)
N5—C20—H20A108.6S16—Mo4—S9104.33 (9)
C19—C20—H20A108.6S13—Mo4—S9147.91 (9)
N5—C20—H20B108.6S14—Mo4—S979.90 (7)
C19—C20—H20B108.6S16—Mo4—S10108.30 (9)
H20A—C20—H20B107.5S13—Mo4—S1078.17 (8)
C22—C21—H21A109.5S14—Mo4—S10144.42 (9)
C22—C21—H21B109.5S9—Mo4—S1082.41 (8)
H21A—C21—H21B109.5S16—Mo4—Cu455.10 (6)
C22—C21—H21C109.5S13—Mo4—Cu4105.90 (6)
H21A—C21—H21C109.5S14—Mo4—Cu451.49 (6)
H21B—C21—H21C109.5S9—Mo4—Cu4100.02 (7)
C21—C22—N7115.1 (7)S10—Mo4—Cu4163.37 (8)
C21—C22—H22A108.5S16—Mo4—Cu355.57 (6)
N7—C22—H22A108.5S13—Mo4—Cu350.98 (6)
C21—C22—H22B108.5S14—Mo4—Cu3106.14 (5)
N7—C22—H22B108.5S9—Mo4—Cu3159.80 (8)
H22A—C22—H22B107.5S10—Mo4—Cu3101.08 (6)
C24—C23—H23A109.5Cu4—Mo4—Cu371.11 (3)
C24—C23—H23B109.5S16—Mo4—Mo398.41 (6)
H23A—C23—H23B109.5S13—Mo4—Mo353.24 (6)
C24—C23—H23C109.5S14—Mo4—Mo352.65 (5)
H23A—C23—H23C109.5S9—Mo4—Mo3131.50 (7)
H23B—C23—H23C109.5S10—Mo4—Mo3129.50 (7)
C23—C24—N7114.1 (7)Cu4—Mo4—Mo360.32 (3)
C23—C24—H24A108.7Cu3—Mo4—Mo360.71 (3)
N7—C24—H24A108.7C3—S4—Mo2102.9 (3)
C23—C24—H24B108.7C12—Cu4—S14128.4 (2)
N7—C24—H24B108.7C12—Cu4—S16116.2 (2)
H24A—C24—H24B107.6S14—Cu4—S16102.88 (8)
C26—C25—H25A109.5C12—Cu4—S15109.4 (2)
C26—C25—H25B109.5S14—Cu4—S15101.04 (8)
H25A—C25—H25B109.5S16—Cu4—S1592.12 (7)
C26—C25—H25C109.5C12—Cu4—Mo4154.4 (2)
H25A—C25—H25C109.5S14—Cu4—Mo454.22 (5)
H25B—C25—H25C109.5S16—Cu4—Mo449.34 (6)
C25—C26—N7114.2 (7)S15—Cu4—Mo493.41 (6)
C25—C26—H26A108.7C12—Cu4—Mo3144.2 (2)
N7—C26—H26A108.7S14—Cu4—Mo353.38 (5)
C25—C26—H26B108.7S16—Cu4—Mo394.61 (6)
N7—C26—H26B108.7S15—Cu4—Mo348.36 (5)
H26A—C26—H26B107.6Mo4—Cu4—Mo360.73 (3)
C28—C27—H27A109.5C20—N5—C14109.6 (6)
C28—C27—H27B109.5C20—N5—C16108.0 (6)
H27A—C27—H27B109.5C14—N5—C16111.6 (6)
C28—C27—H27C109.5C20—N5—C18111.0 (6)
H27A—C27—H27C109.5C14—N5—C18107.0 (6)
H27B—C27—H27C109.5C16—N5—C18109.7 (6)
C27—C28—N7115.9 (7)Cu2—S5—Mo175.19 (7)
C27—C28—H28A108.3Cu2—S5—Mo275.43 (7)
N7—C28—H28A108.3Mo1—S5—Mo274.45 (6)
C27—C28—H28B108.3C36—N6—C30105.9 (6)
N7—C28—H28B108.3C36—N6—C32111.5 (6)
H28A—C28—H28B107.4C30—N6—C32109.9 (6)
C30—C29—H29A109.5C36—N6—C34111.8 (6)
C30—C29—H29B109.5C30—N6—C34112.7 (6)
H29A—C29—H29B109.5C32—N6—C34105.2 (6)
C30—C29—H29C109.5Cu1—S6—Mo275.88 (6)
H29A—C29—H29C109.5Cu1—S6—Mo174.51 (7)
H29B—C29—H29C109.5Mo2—S6—Mo174.58 (6)
N6—C30—C29116.1 (7)C22—N7—C28106.1 (6)
N6—C30—H30A108.3C22—N7—C24112.6 (6)
C29—C30—H30A108.3C28—N7—C24111.0 (6)
N6—C30—H30B108.3C22—N7—C26111.6 (7)
C29—C30—H30B108.3C28—N7—C26110.6 (6)
H30A—C30—H30B107.4C24—N7—C26105.0 (6)
C32—C31—H31A109.5Mo1—S7—Cu175.98 (7)
C32—C31—H31B109.5Mo1—S7—Cu274.98 (7)
H31A—C31—H31B109.5Cu1—S7—Cu285.89 (7)
C32—C31—H31C109.5C40—N8—C44108.5 (7)
H31A—C31—H31C109.5C40—N8—C42112.1 (6)
H31B—C31—H31C109.5C44—N8—C42108.6 (7)
C31—C32—N6115.5 (8)C40—N8—C38109.3 (7)
C31—C32—H32A108.4C44—N8—C38109.5 (6)
N6—C32—H32A108.4C42—N8—C38108.8 (6)
C31—C32—H32B108.4Mo2—S8—Cu276.09 (7)
N6—C32—H32B108.4Mo2—S8—Cu174.79 (7)
H32A—C32—H32B107.5Cu2—S8—Cu184.00 (7)
C34—C33—H33A109.5C8—S9—Mo4101.5 (3)
C34—C33—H33B109.5C7—S10—Mo4107.1 (3)
H33A—C33—H33B109.5C10—S11—Mo3102.6 (4)
C34—C33—H33C109.5C9—S12—Mo3108.8 (3)
H33A—C33—H33C109.5Cu3—S13—Mo474.82 (7)
H33B—C33—H33C109.5Cu3—S13—Mo376.14 (7)
N6—C34—C33115.2 (7)Mo4—S13—Mo374.05 (6)
N6—C34—H34A108.5Cu4—S14—Mo375.67 (6)
C33—C34—H34A108.5Cu4—S14—Mo474.29 (7)
N6—C34—H34B108.5Mo3—S14—Mo474.47 (6)
C33—C34—H34B108.5Mo3—S15—Cu376.42 (7)
H34A—C34—H34B107.5Mo3—S15—Cu475.03 (6)
C36—C35—H35A109.5Cu3—S15—Cu484.01 (7)
C36—C35—H35B109.5Mo4—S16—Cu475.57 (7)
H35A—C35—H35B109.5Mo4—S16—Cu375.33 (7)
C36—C35—H35C109.5Cu4—S16—Cu386.36 (7)

Experimental details

Crystal data
Chemical formula(C8H20N)2[Cu2Mo2(C2H4S2)2(CN)2S4]
Mr944.18
Crystal system, space groupOrthorhombic, Pca21
Temperature (K)291
a, b, c (Å)12.509 (3), 16.582 (3), 34.976 (7)
V (Å3)7255 (3)
Z8
Radiation typeMo Kα
µ (mm−1)2.31
Crystal size (mm)0.20 × 0.15 × 0.06
Data collection
DiffractometerRigaku Mercury
Absorption correctionMulti-scan
(REQAB; Jacobson, 1998)
Tmin, Tmax0.666, 0.870
No. of measured, independent and
observed [I > 2σ(I)] reflections		77483, 16412, 15033
Rint0.075
(sin θ/λ)max (Å−1)0.649
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.066, 0.097, 1.19
No. of reflections16412
No. of parameters705
No. of restraints1
H-atom treatmentH-atom parameters constrained
w = 1/[σ2(Fo2) + (0.0156P)2 + 23.3405P]
where P = (Fo2 + 2Fc2)/3
Δρmax, Δρmin (e Å−3)0.58, −0.77
Absolute structureFlack (1983), 7995 Friedel pairs
Absolute structure parameter0.030 (16)

Computer programs: CrystalClear (Rigaku/MSC, 2001), CrystalStructure (Rigaku/MSC, 2004), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

 

Acknowledgements

The authors acknowledge Jiangxi Science and Technology Normal University for funding.

References

First citationBrunner, H., Janietz, N., Wachter, J., Zahn, T. & Ziegler, M. L. (1985). Angew. Chem. Int. Ed. 24, 133–135.  CSD CrossRef Google Scholar
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 First citationFlack, H. D. (1983). Acta Cryst. A39, 876–881.  CrossRef CAS Web of Science IUCr Journals Google Scholar
 First citationHidai, M., Ikada, T., Kuwata, S. & Mizobe, Y. (1999). Inorg. Chem. 38, 64–69.  Google Scholar
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 First citationLang, J.-P., Wei, Z.-H., Xu, Q.-F., Li, H.-X. & Chen, J.-X. (2003). J. Organomet. Chem. 87, 197–202.  Google Scholar
 First citationRigaku/MSC (2001). CrystalClear. Rigaku/MSC, The Woodlands, Texas, USA.  Google Scholar
 First citationRigaku/MSC (2004). CrystalStructure. Rigaku/MSC, The Woodlands, Texas, USA.  Google Scholar
 First citationSheldrick, G. M. (2008). Acta Cryst. A64, 112–122.  Web of Science CrossRef CAS IUCr Journals Google Scholar
 First citationStiefel, E. I., Halbert, T. R. & Cohen, S. A. (1985). Organometallics, 4, 1689–1690.  Google Scholar
 First citationWu, X.-T., Zhu, N.-Y. & Zheng, Y.-F. (1990). J. Chem. Soc. Chem. Commun. pp. 780–781.  Google Scholar

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ISSN: 2056-9890
Volume 65| Part 11| November 2009| Page m1485
https://doi.org/10.1107/S1600536809044821
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