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Acta Crystallogr Sect E Struct Rep Online. 2009 November 1; 65(Pt 11): m1485.
Published online 2009 October 31. doi:  10.1107/S1600536809044821
PMCID: PMC2971270

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

Abstract

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 [triangle]); Lang et al. (2003 [triangle]); Curtis et al. (1997 [triangle]); Stiefel et al. (1985 [triangle]); Brunner et al. (1985 [triangle]); Wu et al. (1990 [triangle]).

An external file that holds a picture, illustration, etc.
Object name is e-65-m1485-scheme1.jpg

Experimental

Crystal data

  • (C8H20N)2[Cu2Mo2(C2H4S2)2(CN)2S4]
  • M r = 944.18
  • Orthorhombic, An external file that holds a picture, illustration, etc.
Object name is e-65-m1485-efi1.jpg
  • 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 [triangle]) T min = 0.666, T max = 0.870
  • 77483 measured reflections
  • 16412 independent reflections
  • 15033 reflections with I > 2σ(I)
  • R int = 0.075

Refinement

  • R[F 2 > 2σ(F 2)] = 0.066
  • wR(F 2) = 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 [triangle]), 7995 Friedel pairs
  • Flack parameter: 0.030 (16)

Data collection: CrystalClear (Rigaku/MSC, 2001 [triangle]); cell refinement: CrystalClear; data reduction: CrystalStructure (Rigaku/MSC, 2004 [triangle]); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 [triangle]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 [triangle]); molecular graphics: SHELXTL (Sheldrick, 2008 [triangle]); software used to prepare material for publication: SHELXTL.

Supplementary Material

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

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809044821/zs2011Isup2.hkl

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

Acknowledgments

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

supplementary crystallographic information

Comment

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.

Experimental

[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

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.

Figures

Fig. 1.
The molecular structure of the title molecule, with the atom-numbering scheme. Displacement ellipsoids are drawn at the 35% probability level

Crystal data

(C8H20N)2[Cu2Mo2(C2H4S2)2(CN)2S4]F(000) = 3824
Mr = 944.18Dx = 1.729 Mg m3
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 mm1
c = 34.976 (7) ÅT = 291 K
V = 7255 (3) Å3Platelet, red
Z = 80.20 × 0.15 × 0.06 mm

Data collection

Rigaku Mercury diffractometer16412 independent reflections
Radiation source: fine-focus sealed tube15033 reflections with I > 2σ(I)
graphiteRint = 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

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) = 0.097w = 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 Å3
705 parametersΔρmin = −0.77 e Å3
1 restraintAbsolute structure: Flack (1983), 7995 Friedel pairs
Primary atom site location: structure-invariant direct methodsFlack parameter: 0.030 (16)

Special details

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)

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)

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, °)

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)

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: ZS2011).

References

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