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Acta Crystallogr Sect E Struct Rep Online. 2008 December 1; 64(Pt 12): m1546.
Published online 2008 November 13. doi:  10.1107/S1600536808036532
PMCID: PMC2959934

Tris(tetra­methyl­ammonium) tetra-μ2-sulfido-tetra­sulfidocopper(I)dimolyb­denum(VI) N,N-dimethyl­formamide solvate

Abstract

The title compound, (C4H12N)3[CuMo2S8]·C3H7NO, was obtained from the self-assembly of tetra­thio­molybdate, tetra­methyl­ammonium nitrate and cuprous sulfide in dimethyl­formamide (DMF). The asymmetric unit contains three (NMe4)+ cations, one [Mo2S8Cu]3− anion and one DMF solvent mol­ecule, and no obvious inter­actions are observed between these species. The trinuclear anion can be viewed as fused [MoS4Cu] units sharing a copper center. The geometric parameters of the trivalent anion are comparable to those reported for other related salts including isomorphous anions, namely (NEt4)2(PPh4)[Mo2S8Cu] (a) and (Ph3P=N=PPh3)2(NEt4)[W2S8Cu]·2CH3CN (b). However, the Mo—Cu—Mo angle is found to be 160.24 (3)° for the title salt, while this angle is 162.97 (2)° in (a) and the W—Cu—W angle is 170.3 (2)° in (b), indicating that the largest deviation from linearity is in the title compound.

Related literature

For related MoVI/CuI and WVI/CuI complexes, see: Niu et al. (2002 [triangle]); Maiti et al. (2004 [triangle]); Müller et al. (1989 [triangle]).

An external file that holds a picture, illustration, etc.
Object name is e-64-m1546-scheme1.jpg

Experimental

Crystal data

  • (C4H12N)3[CuMo2S8]·C3H7NO
  • M r = 807.43
  • Monoclinic, An external file that holds a picture, illustration, etc.
Object name is e-64-m1546-efi1.jpg
  • a = 9.4380 (19) Å
  • b = 20.336 (4) Å
  • c = 17.718 (4) Å
  • β = 98.60 (3)°
  • V = 3362.4 (12) Å3
  • Z = 4
  • Mo Kα radiation
  • μ = 1.87 mm−1
  • T = 293 (2) K
  • 0.40 × 0.30 × 0.25 mm

Data collection

  • Bruker APEX CCD area-detector diffractometer
  • Absorption correction: multi-scan (SADABS; Bruker, 1998 [triangle]) T min = 0.527, T max = 0.618
  • 17155 measured reflections
  • 6625 independent reflections
  • 5061 reflections with I > 2σ(I)
  • R int = 0.039

Refinement

  • R[F 2 > 2σ(F 2)] = 0.042
  • wR(F 2) = 0.136
  • S = 1.05
  • 6625 reflections
  • 274 parameters
  • H-atom parameters constrained
  • Δρmax = 0.93 e Å−3
  • Δρmin = −0.85 e Å−3

Data collection: SMART (Bruker, 1998 [triangle]); cell refinement: SAINT (Bruker, 1998 [triangle]); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2008 [triangle]); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Supplementary Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536808036532/bh2199sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808036532/bh2199Isup2.hkl

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

Acknowledgments

Financial support from NUIST is acknowledged.

supplementary crystallographic information

Comment

The title compound, (NMe4)3[Mo2S8Cu].C3H7ON, was obtained from the self-assembly of tetrathiomolybdate, tetramethylammonium nitrate and cuprous sulfide in N,N-dimethylformamide (DMF). The asymmetric unit contains three tetramethylammonium cations, one [Mo2S8Cu]3- anion and one DMF solvent molecule, with no obvious interactions observed among these species. The trinuclear anion can be viewed as fused by two binuclear units [MoS4Cu]- through one shared copper. The two binuclear units are perpendicular to each other, as found in other linear trinuclear clusters, such as {MoS4Cu2[PPh2(py)]4} (py = pyridyl) (Niu et al., 2002). However, in the latter, [MoS4]2- is a tetradentate ligand, while in the former, it serves as a bidentate ligand. In the title cluster, one Mo center is close to retain the original tetrahedral configuration of free [MoS4]2-, with six S—Mo—S bond angles varying from 108.88 (6) to 111.20 (6)°. The other Mo center distorts slightly more, the corresponding angles ranging from 107.24 (6) to 111.79 (6)°. The geometric parameters of the trivalent anion are comparable to those reported for the compounds bis(tetraethylammonium) tetraphenylphosphonium bis(di-µ2-sulfido-dithioxomolybdenum)copper (a) (Maiti et al., 2004) and bis[bis(triphenylphosphine)iminium] tetraethylammonium bis(di-µ2-sulfido-dithioxotungsten)copper acetonitrile disolvate (b) (Müller et al., 1989), except a notable difference among the Mo—Cu—Mo angles: 160.24 (3)° for the title compound, 162.97 (2)° for (a), while W—Cu—W angle is 170.3 (2)° in (b), indicating a largest deviation from ideal linear array in the title salt.

Experimental

0.75 mmol of Cu2S powder was added to a solution of [NH4]2MoS4 (1 mmol in 10 ml DMF) and stirred for 4 h. at room temperature. After filtration, the filtrate was carefully laid on the surface with DMF (3 ml) and saturated (Me4N)NO3 solution (5 ml in methanol), successively. Black red polyhedric crystals of the title compound were obtained after two weeks.

Refinement

All H atoms were positioned geometrically and refined using a riding model, with C—H = 0.93 Å for aldehydic H atom and C—H = 0.96 Å for methyl groups. Isotropic displacement parameters for H atoms were calculated as Uiso(H) = 1.5Ueq(carrier C), except for H11A: Uiso(H11A) = 1.2Ueq(C11).

Figures

Fig. 1.
The molecular structure of the title compound, with atom labels and 50% probability displacement ellipsoids. All H atoms have been omitted.

Crystal data

(C4H12N)3[CuMo2S8]·C3H7NOF000 = 1640
Mr = 807.43Dx = 1.595 Mg m3
Monoclinic, P21/nMo Kα radiation λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 7032 reflections
a = 9.4380 (19) Åθ = 1.2–26.1º
b = 20.336 (4) ŵ = 1.87 mm1
c = 17.718 (4) ÅT = 293 (2) K
β = 98.60 (3)ºPolyhedron, black red
V = 3362.4 (12) Å30.40 × 0.30 × 0.25 mm
Z = 4

Data collection

Bruker APEX CCD area-detector diffractometer6625 independent reflections
Radiation source: fine-focus sealed tube5061 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.039
T = 293(2) Kθmax = 26.0º
[var phi] and ω scansθmin = 1.5º
Absorption correction: multi-scan(SADABS; Bruker, 1998)h = −11→11
Tmin = 0.527, Tmax = 0.618k = −24→25
17155 measured reflectionsl = −21→21

Refinement

Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.042H-atom parameters constrained
wR(F2) = 0.136  w = 1/[σ2(Fo2) + (0.0646P)2] where P = (Fo2 + 2Fc2)/3
S = 1.05(Δ/σ)max < 0.001
6625 reflectionsΔρmax = 0.93 e Å3
274 parametersΔρmin = −0.85 e Å3
Primary atom site location: structure-invariant direct methodsExtinction correction: none

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2)

xyzUiso*/Ueq
Mo10.25496 (5)0.15816 (2)0.93899 (3)0.04775 (14)
Mo20.31519 (5)0.05342 (2)0.66754 (3)0.04773 (14)
Cu10.24065 (7)0.09541 (3)0.80223 (4)0.04912 (18)
S10.11495 (15)0.18682 (7)0.83342 (8)0.0494 (3)
S20.31587 (15)0.05454 (7)0.92589 (8)0.0489 (3)
S30.12487 (15)0.02298 (7)0.71839 (8)0.0483 (3)
S40.43472 (16)0.12836 (7)0.74081 (8)0.0514 (3)
S50.45325 (16)−0.03117 (8)0.65994 (8)0.0532 (3)
S60.24512 (16)0.09507 (7)0.55703 (9)0.0543 (3)
S70.44848 (16)0.21739 (7)0.95638 (8)0.0516 (3)
S80.13280 (16)0.16860 (7)1.03204 (8)0.0522 (3)
O10.1656 (5)0.1069 (2)1.2555 (3)0.0610 (11)
N10.2487 (5)0.1922 (2)1.3279 (3)0.0500 (11)
C110.2068 (7)0.1295 (3)1.3196 (4)0.0553 (14)
H11A0.20880.10281.36240.066*
C120.2912 (7)0.2217 (3)1.4013 (4)0.0605 (15)
H12A0.30930.18791.43930.091*
H12B0.21600.24991.41330.091*
H12C0.37670.24711.40060.091*
C130.2171 (7)0.2367 (3)1.2639 (4)0.0579 (15)
H13A0.19010.21181.21790.087*
H13B0.30060.26251.25920.087*
H13C0.13980.26531.27190.087*
N20.7731 (5)0.1115 (2)0.5453 (3)0.0507 (11)
C210.8726 (7)0.1130 (3)0.4883 (4)0.0616 (16)
H21A0.96070.09160.50890.092*
H21B0.89180.15780.47610.092*
H21C0.83010.09050.44290.092*
C220.8482 (7)0.1530 (3)0.6068 (3)0.0549 (14)
H22A0.93990.13400.62540.082*
H22B0.79220.15570.64760.082*
H22C0.86130.19630.58730.082*
C230.6306 (7)0.1439 (3)0.5187 (4)0.0600 (15)
H23A0.57170.14110.55830.090*
H23B0.58390.12190.47380.090*
H23C0.64570.18920.50700.090*
C240.7503 (7)0.0474 (3)0.5762 (4)0.0557 (14)
H24A0.84110.02690.59310.084*
H24B0.69600.02070.53760.084*
H24C0.69850.05190.61860.084*
N30.7749 (5)0.0309 (2)0.8680 (3)0.0525 (11)
C310.9019 (7)−0.0048 (3)0.9017 (3)0.0554 (14)
H31A0.98180.02480.91080.083*
H31B0.9224−0.03890.86740.083*
H31C0.8857−0.02410.94910.083*
C320.7374 (7)0.0836 (3)0.9250 (4)0.0574 (14)
H32A0.81460.11460.93500.086*
H32B0.72310.06260.97190.086*
H32C0.65130.10610.90360.086*
C330.7972 (6)0.0578 (3)0.7979 (4)0.0577 (14)
H33A0.87600.08810.80610.087*
H33B0.71230.08050.77510.087*
H33C0.81870.02320.76450.087*
C340.6474 (4)−0.01784 (16)0.85381 (19)0.0594 (14)
H34A0.6675−0.05120.81850.089*
H34B0.56200.00540.83290.089*
H34C0.6339−0.03800.90120.089*
N40.2179 (4)0.32703 (16)0.67898 (19)0.0504 (10)
C410.2608 (4)0.27407 (16)0.63794 (19)0.0593 (15)
H41A0.24820.23390.66470.089*
H41B0.35990.27910.63250.089*
H41C0.20370.27270.58830.089*
C420.3149 (6)0.3291 (3)0.7528 (3)0.0522 (13)
H42A0.30320.28970.78110.078*
H42B0.29220.36660.78160.078*
H42C0.41240.33220.74360.078*
C430.2388 (6)0.3897 (3)0.6357 (3)0.0512 (13)
H43A0.33680.39290.62760.077*
H43B0.21520.42690.66470.077*
H43C0.17740.38900.58730.077*
C440.0667 (6)0.3221 (3)0.6915 (4)0.0560 (14)
H44A0.05360.28240.71900.084*
H44B0.00530.32140.64320.084*
H44C0.04310.35930.72060.084*

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
Mo10.0462 (3)0.0487 (3)0.0477 (3)0.00610 (19)0.00487 (19)−0.00193 (19)
Mo20.0459 (3)0.0490 (3)0.0484 (3)0.00548 (19)0.00763 (19)0.00304 (19)
Cu10.0491 (4)0.0505 (4)0.0476 (4)0.0071 (3)0.0065 (3)−0.0035 (3)
S10.0479 (7)0.0533 (7)0.0479 (7)0.0088 (6)0.0104 (6)−0.0037 (6)
S20.0476 (7)0.0524 (7)0.0464 (7)0.0074 (6)0.0060 (5)−0.0030 (6)
S30.0467 (7)0.0504 (7)0.0484 (7)0.0073 (5)0.0092 (6)0.0045 (6)
S40.0545 (8)0.0472 (7)0.0531 (7)0.0107 (6)0.0103 (6)0.0061 (6)
S50.0503 (8)0.0580 (8)0.0526 (7)0.0073 (6)0.0124 (6)0.0045 (6)
S60.0538 (8)0.0518 (8)0.0567 (8)0.0112 (6)0.0069 (6)−0.0029 (6)
S70.0513 (7)0.0521 (7)0.0526 (7)0.0119 (6)0.0118 (6)−0.0056 (6)
S80.0511 (7)0.0520 (7)0.0540 (8)0.0122 (6)0.0101 (6)0.0052 (6)
O10.058 (2)0.069 (3)0.056 (2)0.014 (2)0.0089 (19)0.022 (2)
N10.046 (2)0.050 (3)0.055 (3)−0.0102 (19)0.011 (2)0.012 (2)
C110.053 (3)0.053 (3)0.061 (4)−0.015 (3)0.010 (3)0.015 (3)
C120.062 (4)0.053 (3)0.068 (4)−0.014 (3)0.014 (3)0.010 (3)
C130.063 (3)0.044 (3)0.061 (3)0.009 (3)−0.006 (3)−0.015 (3)
N20.051 (3)0.051 (3)0.051 (3)−0.005 (2)0.011 (2)0.011 (2)
C210.060 (4)0.056 (3)0.061 (3)0.017 (3)−0.015 (3)0.008 (3)
C220.051 (3)0.067 (4)0.050 (3)0.005 (3)0.017 (2)0.010 (3)
C230.067 (4)0.051 (3)0.054 (3)0.020 (3)−0.015 (3)0.008 (3)
C240.054 (3)0.059 (3)0.055 (3)0.013 (3)0.008 (3)0.008 (3)
N30.056 (3)0.047 (2)0.054 (3)−0.004 (2)0.009 (2)−0.004 (2)
C310.067 (4)0.049 (3)0.051 (3)0.009 (3)0.011 (3)0.009 (2)
C320.056 (3)0.063 (4)0.054 (3)−0.006 (3)0.009 (3)0.015 (3)
C330.040 (3)0.064 (4)0.070 (4)−0.005 (2)0.009 (3)0.013 (3)
C340.059 (4)0.057 (3)0.062 (4)0.004 (3)0.011 (3)0.010 (3)
N40.049 (3)0.045 (2)0.057 (3)−0.010 (2)0.006 (2)0.006 (2)
C410.066 (4)0.063 (4)0.049 (3)0.010 (3)0.009 (3)0.015 (3)
C420.047 (3)0.057 (3)0.054 (3)−0.006 (2)0.011 (2)0.011 (3)
C430.050 (3)0.056 (3)0.050 (3)−0.015 (2)0.015 (2)−0.011 (2)
C440.053 (3)0.051 (3)0.059 (3)0.012 (3)−0.005 (3)0.009 (3)

Geometric parameters (Å, °)

Mo1—S82.1589 (16)C23—H23C0.9600
Mo1—S72.1710 (17)C24—H24A0.9600
Mo1—S12.2013 (16)C24—H24B0.9600
Mo1—S22.2057 (15)C24—H24C0.9600
Mo1—Cu12.7241 (9)N3—C331.401 (8)
Mo2—S62.1451 (17)N3—C311.453 (8)
Mo2—S52.1742 (16)N3—C321.549 (9)
Mo2—S42.2006 (17)N3—C341.550 (6)
Mo2—S32.2148 (16)C31—H31A0.9600
Mo2—Cu12.7241 (10)C31—H31B0.9600
Cu1—S32.2549 (17)C31—H31C0.9600
Cu1—S12.3161 (15)C32—H32A0.9600
Cu1—S22.3518 (16)C32—H32B0.9600
Cu1—S42.3630 (17)C32—H32C0.9600
O1—C111.232 (8)C33—H33A0.9600
N1—C111.338 (8)C33—H33B0.9600
N1—C121.434 (9)C33—H33C0.9600
N1—C131.447 (8)C34—H34A0.9600
C11—H11A0.9300C34—H34B0.9600
C12—H12A0.9600C34—H34C0.9600
C12—H12B0.9600N4—C411.392 (9)
C12—H12C0.9600N4—C421.481 (7)
C13—H13A0.9600N4—C441.481 (7)
C13—H13B0.9600N4—C431.515 (7)
C13—H13C0.9600C41—H41A0.9600
N2—C241.443 (8)C41—H41B0.9600
N2—C221.473 (8)C41—H41C0.9600
N2—C211.478 (9)C42—H42A0.9600
N2—C231.508 (7)C42—H42B0.9600
C21—H21A0.9600C42—H42C0.9600
C21—H21B0.9600C43—H43A0.9600
C21—H21C0.9600C43—H43B0.9600
C22—H22A0.9600C43—H43C0.9600
C22—H22B0.9600C44—H44A0.9600
C22—H22C0.9600C44—H44B0.9600
C23—H23A0.9600C44—H44C0.9600
C23—H23B0.9600
S8—Mo1—S7111.79 (6)H22B—C22—H22C109.5
S8—Mo1—S1107.55 (6)N2—C23—H23A109.5
S7—Mo1—S1111.04 (6)N2—C23—H23B109.5
S8—Mo1—S2110.59 (6)H23A—C23—H23B109.5
S7—Mo1—S2108.54 (6)N2—C23—H23C109.5
S1—Mo1—S2107.24 (6)H23A—C23—H23C109.5
S8—Mo1—Cu1139.84 (5)H23B—C23—H23C109.5
S7—Mo1—Cu1108.35 (5)N2—C24—H24A109.5
S1—Mo1—Cu154.87 (4)N2—C24—H24B109.5
S2—Mo1—Cu155.80 (4)H24A—C24—H24B109.5
S6—Mo2—S5111.20 (6)N2—C24—H24C109.5
S6—Mo2—S4109.02 (6)H24A—C24—H24C109.5
S5—Mo2—S4108.98 (6)H24B—C24—H24C109.5
S6—Mo2—S3108.88 (6)C33—N3—C31109.6 (5)
S5—Mo2—S3109.52 (6)C33—N3—C32112.8 (5)
S4—Mo2—S3109.21 (6)C31—N3—C32109.4 (5)
S6—Mo2—Cu1126.23 (5)C33—N3—C34108.8 (4)
S5—Mo2—Cu1122.54 (5)C31—N3—C34108.6 (4)
S4—Mo2—Cu156.14 (4)C32—N3—C34107.5 (4)
S3—Mo2—Cu153.12 (5)N3—C31—H31A109.5
S3—Cu1—S1117.80 (6)N3—C31—H31B109.5
S3—Cu1—S2115.59 (6)H31A—C31—H31B109.5
S1—Cu1—S298.94 (6)N3—C31—H31C109.5
S3—Cu1—S4102.39 (6)H31A—C31—H31C109.5
S1—Cu1—S4110.01 (6)H31B—C31—H31C109.5
S2—Cu1—S4112.49 (6)N3—C32—H32A109.5
S3—Cu1—Mo251.78 (4)N3—C32—H32B109.5
S1—Cu1—Mo2132.00 (5)H32A—C32—H32B109.5
S2—Cu1—Mo2128.60 (4)N3—C32—H32C109.5
S4—Cu1—Mo250.66 (4)H32A—C32—H32C109.5
S3—Cu1—Mo1147.85 (5)H32B—C32—H32C109.5
S1—Cu1—Mo151.01 (4)N3—C33—H33A109.5
S2—Cu1—Mo150.87 (4)N3—C33—H33B109.5
S4—Cu1—Mo1109.76 (5)H33A—C33—H33B109.5
Mo2—Cu1—Mo1160.24 (3)N3—C33—H33C109.5
Mo1—S1—Cu174.13 (5)H33A—C33—H33C109.5
Mo1—S2—Cu173.34 (5)H33B—C33—H33C109.5
Mo2—S3—Cu175.09 (5)N3—C34—H34A109.5
Mo2—S4—Cu173.20 (5)N3—C34—H34B109.5
C11—N1—C12122.4 (5)H34A—C34—H34B109.5
C11—N1—C13119.2 (5)N3—C34—H34C109.5
C12—N1—C13116.6 (5)H34A—C34—H34C109.5
O1—C11—N1120.3 (5)H34B—C34—H34C109.5
O1—C11—H11A119.9C41—N4—C42107.0 (3)
N1—C11—H11A119.9C41—N4—C44112.8 (3)
N1—C12—H12A109.5C42—N4—C44110.6 (4)
N1—C12—H12B109.5C41—N4—C43108.4 (3)
H12A—C12—H12B109.5C42—N4—C43108.3 (4)
N1—C12—H12C109.5C44—N4—C43109.5 (4)
H12A—C12—H12C109.5N4—C41—H41A109.5
H12B—C12—H12C109.5N4—C41—H41B109.5
N1—C13—H13A109.5H41A—C41—H41B109.5
N1—C13—H13B109.5N4—C41—H41C109.5
H13A—C13—H13B109.5H41A—C41—H41C109.5
N1—C13—H13C109.5H41B—C41—H41C109.5
H13A—C13—H13C109.5N4—C42—H42A109.5
H13B—C13—H13C109.5N4—C42—H42B109.5
C24—N2—C22108.6 (5)H42A—C42—H42B109.5
C24—N2—C21115.1 (5)N4—C42—H42C109.5
C22—N2—C21102.0 (4)H42A—C42—H42C109.5
C24—N2—C23109.7 (5)H42B—C42—H42C109.5
C22—N2—C23106.8 (5)N4—C43—H43A109.5
C21—N2—C23113.9 (5)N4—C43—H43B109.5
N2—C21—H21A109.5H43A—C43—H43B109.5
N2—C21—H21B109.5N4—C43—H43C109.5
H21A—C21—H21B109.5H43A—C43—H43C109.5
N2—C21—H21C109.5H43B—C43—H43C109.5
H21A—C21—H21C109.5N4—C44—H44A109.5
H21B—C21—H21C109.5N4—C44—H44B109.5
N2—C22—H22A109.5H44A—C44—H44B109.5
N2—C22—H22B109.5N4—C44—H44C109.5
H22A—C22—H22B109.5H44A—C44—H44C109.5
N2—C22—H22C109.5H44B—C44—H44C109.5
H22A—C22—H22C109.5
S6—Mo2—Cu1—S387.24 (8)S7—Mo1—Cu1—Mo23.80 (11)
S5—Mo2—Cu1—S3−90.96 (7)S1—Mo1—Cu1—Mo2107.05 (11)
S4—Mo2—Cu1—S3176.95 (6)S2—Mo1—Cu1—Mo2−96.54 (10)
S6—Mo2—Cu1—S1−7.91 (9)S8—Mo1—S1—Cu1−139.25 (6)
S5—Mo2—Cu1—S1173.89 (8)S7—Mo1—S1—Cu198.15 (6)
S4—Mo2—Cu1—S181.80 (8)S2—Mo1—S1—Cu1−20.28 (6)
S3—Mo2—Cu1—S1−95.15 (8)S3—Cu1—S1—Mo1143.57 (6)
S6—Mo2—Cu1—S2−178.47 (8)S2—Cu1—S1—Mo118.32 (6)
S5—Mo2—Cu1—S23.34 (9)S4—Cu1—S1—Mo1−99.67 (6)
S4—Mo2—Cu1—S2−88.76 (8)Mo2—Cu1—S1—Mo1−154.22 (5)
S3—Mo2—Cu1—S294.29 (8)S8—Mo1—S2—Cu1137.04 (6)
S6—Mo2—Cu1—S4−89.71 (8)S7—Mo1—S2—Cu1−99.99 (6)
S5—Mo2—Cu1—S492.10 (7)S1—Mo1—S2—Cu120.04 (6)
S3—Mo2—Cu1—S4−176.95 (6)S3—Cu1—S2—Mo1−145.14 (5)
S6—Mo2—Cu1—Mo1−98.05 (11)S1—Cu1—S2—Mo1−18.36 (6)
S5—Mo2—Cu1—Mo183.75 (11)S4—Cu1—S2—Mo197.75 (6)
S4—Mo2—Cu1—Mo1−8.35 (10)Mo2—Cu1—S2—Mo1154.55 (4)
S3—Mo2—Cu1—Mo1174.71 (11)S6—Mo2—S3—Cu1−121.63 (6)
S8—Mo1—Cu1—S3−5.97 (12)S5—Mo2—S3—Cu1116.59 (6)
S7—Mo1—Cu1—S3175.98 (9)S4—Mo2—S3—Cu1−2.69 (6)
S1—Mo1—Cu1—S3−80.77 (10)S1—Cu1—S3—Mo2123.21 (6)
S2—Mo1—Cu1—S375.63 (10)S2—Cu1—S3—Mo2−120.22 (5)
S8—Mo1—Cu1—S174.81 (8)S4—Cu1—S3—Mo22.42 (5)
S7—Mo1—Cu1—S1−103.25 (7)Mo1—Cu1—S3—Mo2−176.64 (7)
S2—Mo1—Cu1—S1156.40 (7)S6—Mo2—S4—Cu1121.44 (5)
S8—Mo1—Cu1—S2−81.60 (8)S5—Mo2—S4—Cu1−117.02 (5)
S7—Mo1—Cu1—S2100.35 (7)S3—Mo2—S4—Cu12.59 (5)
S1—Mo1—Cu1—S2−156.40 (7)S3—Cu1—S4—Mo2−2.46 (5)
S8—Mo1—Cu1—S4175.01 (7)S1—Cu1—S4—Mo2−128.49 (5)
S7—Mo1—Cu1—S4−3.04 (6)S2—Cu1—S4—Mo2122.26 (6)
S1—Mo1—Cu1—S4100.20 (7)Mo1—Cu1—S4—Mo2177.01 (3)
S2—Mo1—Cu1—S4−103.39 (6)C12—N1—C11—O1177.0 (6)
S8—Mo1—Cu1—Mo2−178.14 (9)C13—N1—C11—O113.0 (9)

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: BH2199).

References

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