Acta Cryst. (2008). E64, m1546 [ doi:10.1107/S1600536808036532 ]
2-sulfido-tetrasulfidocopper(I)dimolybdenum(VI) N,N-dimethylformamide solvateThe 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.
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.
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).
Data collection: SMART (Bruker, 1998); cell refinement: SAINT (Bruker, 1998); data reduction: SAINT (Bruker, 1998); program(s) used to solve structure: SHELXTL (Sheldrick, 2008); program(s) used to refine structure: SHELXTL (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).
| Fig. 1. The molecular structure of the title compound, with atom labels and 50% probability displacement ellipsoids. All H atoms have been omitted. |
| (C4H12N)3[CuMo2S8]·C3H7NO | F(000) = 1640 |
| Mr = 807.43 | Dx = 1.595 Mg m−3 |
| Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
| Hall symbol: -P 2yn | Cell parameters from 7032 reflections |
| a = 9.4380 (19) Å | θ = 1.2–26.1° |
| b = 20.336 (4) Å | µ = 1.87 mm−1 |
| c = 17.718 (4) Å | T = 293 K |
| β = 98.60 (3)° | Polyhedron, black red |
| V = 3362.4 (12) Å3 | 0.40 × 0.30 × 0.25 mm |
| Z = 4 |
| Bruker APEX CCD area-detector diffractometer | 6625 independent reflections |
| Radiation source: fine-focus sealed tube | 5061 reflections with I > 2σ(I) |
| graphite | Rint = 0.039 |
| φ and ω scans | θmax = 26.0°, θmin = 1.5° |
| Absorption correction: multi-scan (SADABS; Bruker, 1998) | h = −11→11 |
| Tmin = 0.527, Tmax = 0.618 | k = −24→25 |
| 17155 measured reflections | l = −21→21 |
| Refinement on F2 | Primary atom site location: structure-invariant direct methods |
| Least-squares matrix: full | Secondary atom site location: difference Fourier map |
| R[F2 > 2σ(F2)] = 0.042 | Hydrogen site location: inferred from neighbouring sites |
| wR(F2) = 0.136 | H-atom parameters constrained |
| S = 1.05 | w = 1/[σ2(Fo2) + (0.0646P)2] where P = (Fo2 + 2Fc2)/3 |
| 6625 reflections | (Δ/σ)max < 0.001 |
| 274 parameters | Δρmax = 0.93 e Å−3 |
| 0 restraints | Δρmin = −0.85 e Å−3 |
| (C4H12N)3[CuMo2S8]·C3H7NO | V = 3362.4 (12) Å3 |
| Mr = 807.43 | Z = 4 |
| Monoclinic, P21/n | Mo Kα radiation |
| a = 9.4380 (19) Å | µ = 1.87 mm−1 |
| b = 20.336 (4) Å | T = 293 K |
| c = 17.718 (4) Å | 0.40 × 0.30 × 0.25 mm |
| β = 98.60 (3)° |
| Bruker APEX CCD area-detector diffractometer | 6625 independent reflections |
| Absorption correction: multi-scan (SADABS; Bruker, 1998) | 5061 reflections with I > 2σ(I) |
| Tmin = 0.527, Tmax = 0.618 | Rint = 0.039 |
| 17155 measured reflections | θmax = 26.0° |
| R[F2 > 2σ(F2)] = 0.042 | H-atom parameters constrained |
| wR(F2) = 0.136 | Δρmax = 0.93 e Å−3 |
| S = 1.05 | Δρmin = −0.85 e Å−3 |
| 6625 reflections | Absolute structure: ? |
| 274 parameters | Flack parameter: ? |
| 0 restraints | Rogers parameter: ? |
| x | y | z | Uiso*/Ueq | ||
| Mo1 | 0.25496 (5) | 0.15816 (2) | 0.93899 (3) | 0.04775 (14) | |
| Mo2 | 0.31519 (5) | 0.05342 (2) | 0.66754 (3) | 0.04773 (14) | |
| Cu1 | 0.24065 (7) | 0.09541 (3) | 0.80223 (4) | 0.04912 (18) | |
| S1 | 0.11495 (15) | 0.18682 (7) | 0.83342 (8) | 0.0494 (3) | |
| S2 | 0.31587 (15) | 0.05454 (7) | 0.92589 (8) | 0.0489 (3) | |
| S3 | 0.12487 (15) | 0.02298 (7) | 0.71839 (8) | 0.0483 (3) | |
| S4 | 0.43472 (16) | 0.12836 (7) | 0.74081 (8) | 0.0514 (3) | |
| S5 | 0.45325 (16) | −0.03117 (8) | 0.65994 (8) | 0.0532 (3) | |
| S6 | 0.24512 (16) | 0.09507 (7) | 0.55703 (9) | 0.0543 (3) | |
| S7 | 0.44848 (16) | 0.21739 (7) | 0.95638 (8) | 0.0516 (3) | |
| S8 | 0.13280 (16) | 0.16860 (7) | 1.03204 (8) | 0.0522 (3) | |
| O1 | 0.1656 (5) | 0.1069 (2) | 1.2555 (3) | 0.0610 (11) | |
| N1 | 0.2487 (5) | 0.1922 (2) | 1.3279 (3) | 0.0500 (11) | |
| C11 | 0.2068 (7) | 0.1295 (3) | 1.3196 (4) | 0.0553 (14) | |
| H11A | 0.2088 | 0.1028 | 1.3624 | 0.066* | |
| C12 | 0.2912 (7) | 0.2217 (3) | 1.4013 (4) | 0.0605 (15) | |
| H12A | 0.3093 | 0.1879 | 1.4393 | 0.091* | |
| H12B | 0.2160 | 0.2499 | 1.4133 | 0.091* | |
| H12C | 0.3767 | 0.2471 | 1.4006 | 0.091* | |
| C13 | 0.2171 (7) | 0.2367 (3) | 1.2639 (4) | 0.0579 (15) | |
| H13A | 0.1901 | 0.2118 | 1.2179 | 0.087* | |
| H13B | 0.3006 | 0.2625 | 1.2592 | 0.087* | |
| H13C | 0.1398 | 0.2653 | 1.2719 | 0.087* | |
| N2 | 0.7731 (5) | 0.1115 (2) | 0.5453 (3) | 0.0507 (11) | |
| C21 | 0.8726 (7) | 0.1130 (3) | 0.4883 (4) | 0.0616 (16) | |
| H21A | 0.9607 | 0.0916 | 0.5089 | 0.092* | |
| H21B | 0.8918 | 0.1578 | 0.4761 | 0.092* | |
| H21C | 0.8301 | 0.0905 | 0.4429 | 0.092* | |
| C22 | 0.8482 (7) | 0.1530 (3) | 0.6068 (3) | 0.0549 (14) | |
| H22A | 0.9399 | 0.1340 | 0.6254 | 0.082* | |
| H22B | 0.7922 | 0.1557 | 0.6476 | 0.082* | |
| H22C | 0.8613 | 0.1963 | 0.5873 | 0.082* | |
| C23 | 0.6306 (7) | 0.1439 (3) | 0.5187 (4) | 0.0600 (15) | |
| H23A | 0.5717 | 0.1411 | 0.5583 | 0.090* | |
| H23B | 0.5839 | 0.1219 | 0.4738 | 0.090* | |
| H23C | 0.6457 | 0.1892 | 0.5070 | 0.090* | |
| C24 | 0.7503 (7) | 0.0474 (3) | 0.5762 (4) | 0.0557 (14) | |
| H24A | 0.8411 | 0.0269 | 0.5931 | 0.084* | |
| H24B | 0.6960 | 0.0207 | 0.5376 | 0.084* | |
| H24C | 0.6985 | 0.0519 | 0.6186 | 0.084* | |
| N3 | 0.7749 (5) | 0.0309 (2) | 0.8680 (3) | 0.0525 (11) | |
| C31 | 0.9019 (7) | −0.0048 (3) | 0.9017 (3) | 0.0554 (14) | |
| H31A | 0.9818 | 0.0248 | 0.9108 | 0.083* | |
| H31B | 0.9224 | −0.0389 | 0.8674 | 0.083* | |
| H31C | 0.8857 | −0.0241 | 0.9491 | 0.083* | |
| C32 | 0.7374 (7) | 0.0836 (3) | 0.9250 (4) | 0.0574 (14) | |
| H32A | 0.8146 | 0.1146 | 0.9350 | 0.086* | |
| H32B | 0.7231 | 0.0626 | 0.9719 | 0.086* | |
| H32C | 0.6513 | 0.1061 | 0.9036 | 0.086* | |
| C33 | 0.7972 (6) | 0.0578 (3) | 0.7979 (4) | 0.0577 (14) | |
| H33A | 0.8760 | 0.0881 | 0.8061 | 0.087* | |
| H33B | 0.7123 | 0.0805 | 0.7751 | 0.087* | |
| H33C | 0.8187 | 0.0232 | 0.7645 | 0.087* | |
| C34 | 0.6474 (4) | −0.01784 (16) | 0.85381 (19) | 0.0594 (14) | |
| H34A | 0.6675 | −0.0512 | 0.8185 | 0.089* | |
| H34B | 0.5620 | 0.0054 | 0.8329 | 0.089* | |
| H34C | 0.6339 | −0.0380 | 0.9012 | 0.089* | |
| N4 | 0.2179 (4) | 0.32703 (16) | 0.67898 (19) | 0.0504 (10) | |
| C41 | 0.2608 (4) | 0.27407 (16) | 0.63794 (19) | 0.0593 (15) | |
| H41A | 0.2482 | 0.2339 | 0.6647 | 0.089* | |
| H41B | 0.3599 | 0.2791 | 0.6325 | 0.089* | |
| H41C | 0.2037 | 0.2727 | 0.5883 | 0.089* | |
| C42 | 0.3149 (6) | 0.3291 (3) | 0.7528 (3) | 0.0522 (13) | |
| H42A | 0.3032 | 0.2897 | 0.7811 | 0.078* | |
| H42B | 0.2922 | 0.3666 | 0.7816 | 0.078* | |
| H42C | 0.4124 | 0.3322 | 0.7436 | 0.078* | |
| C43 | 0.2388 (6) | 0.3897 (3) | 0.6357 (3) | 0.0512 (13) | |
| H43A | 0.3368 | 0.3929 | 0.6276 | 0.077* | |
| H43B | 0.2152 | 0.4269 | 0.6647 | 0.077* | |
| H43C | 0.1774 | 0.3890 | 0.5873 | 0.077* | |
| C44 | 0.0667 (6) | 0.3221 (3) | 0.6915 (4) | 0.0560 (14) | |
| H44A | 0.0536 | 0.2824 | 0.7190 | 0.084* | |
| H44B | 0.0053 | 0.3214 | 0.6432 | 0.084* | |
| H44C | 0.0431 | 0.3593 | 0.7206 | 0.084* |
| U11 | U22 | U33 | U12 | U13 | U23 | |
| Mo1 | 0.0462 (3) | 0.0487 (3) | 0.0477 (3) | 0.00610 (19) | 0.00487 (19) | −0.00193 (19) |
| Mo2 | 0.0459 (3) | 0.0490 (3) | 0.0484 (3) | 0.00548 (19) | 0.00763 (19) | 0.00304 (19) |
| Cu1 | 0.0491 (4) | 0.0505 (4) | 0.0476 (4) | 0.0071 (3) | 0.0065 (3) | −0.0035 (3) |
| S1 | 0.0479 (7) | 0.0533 (7) | 0.0479 (7) | 0.0088 (6) | 0.0104 (6) | −0.0037 (6) |
| S2 | 0.0476 (7) | 0.0524 (7) | 0.0464 (7) | 0.0074 (6) | 0.0060 (5) | −0.0030 (6) |
| S3 | 0.0467 (7) | 0.0504 (7) | 0.0484 (7) | 0.0073 (5) | 0.0092 (6) | 0.0045 (6) |
| S4 | 0.0545 (8) | 0.0472 (7) | 0.0531 (7) | 0.0107 (6) | 0.0103 (6) | 0.0061 (6) |
| S5 | 0.0503 (8) | 0.0580 (8) | 0.0526 (7) | 0.0073 (6) | 0.0124 (6) | 0.0045 (6) |
| S6 | 0.0538 (8) | 0.0518 (8) | 0.0567 (8) | 0.0112 (6) | 0.0069 (6) | −0.0029 (6) |
| S7 | 0.0513 (7) | 0.0521 (7) | 0.0526 (7) | 0.0119 (6) | 0.0118 (6) | −0.0056 (6) |
| S8 | 0.0511 (7) | 0.0520 (7) | 0.0540 (8) | 0.0122 (6) | 0.0101 (6) | 0.0052 (6) |
| O1 | 0.058 (2) | 0.069 (3) | 0.056 (2) | 0.014 (2) | 0.0089 (19) | 0.022 (2) |
| N1 | 0.046 (2) | 0.050 (3) | 0.055 (3) | −0.0102 (19) | 0.011 (2) | 0.012 (2) |
| C11 | 0.053 (3) | 0.053 (3) | 0.061 (4) | −0.015 (3) | 0.010 (3) | 0.015 (3) |
| C12 | 0.062 (4) | 0.053 (3) | 0.068 (4) | −0.014 (3) | 0.014 (3) | 0.010 (3) |
| C13 | 0.063 (3) | 0.044 (3) | 0.061 (3) | 0.009 (3) | −0.006 (3) | −0.015 (3) |
| N2 | 0.051 (3) | 0.051 (3) | 0.051 (3) | −0.005 (2) | 0.011 (2) | 0.011 (2) |
| C21 | 0.060 (4) | 0.056 (3) | 0.061 (3) | 0.017 (3) | −0.015 (3) | 0.008 (3) |
| C22 | 0.051 (3) | 0.067 (4) | 0.050 (3) | 0.005 (3) | 0.017 (2) | 0.010 (3) |
| C23 | 0.067 (4) | 0.051 (3) | 0.054 (3) | 0.020 (3) | −0.015 (3) | 0.008 (3) |
| C24 | 0.054 (3) | 0.059 (3) | 0.055 (3) | 0.013 (3) | 0.008 (3) | 0.008 (3) |
| N3 | 0.056 (3) | 0.047 (2) | 0.054 (3) | −0.004 (2) | 0.009 (2) | −0.004 (2) |
| C31 | 0.067 (4) | 0.049 (3) | 0.051 (3) | 0.009 (3) | 0.011 (3) | 0.009 (2) |
| C32 | 0.056 (3) | 0.063 (4) | 0.054 (3) | −0.006 (3) | 0.009 (3) | 0.015 (3) |
| C33 | 0.040 (3) | 0.064 (4) | 0.070 (4) | −0.005 (2) | 0.009 (3) | 0.013 (3) |
| C34 | 0.059 (4) | 0.057 (3) | 0.062 (4) | 0.004 (3) | 0.011 (3) | 0.010 (3) |
| N4 | 0.049 (3) | 0.045 (2) | 0.057 (3) | −0.010 (2) | 0.006 (2) | 0.006 (2) |
| C41 | 0.066 (4) | 0.063 (4) | 0.049 (3) | 0.010 (3) | 0.009 (3) | 0.015 (3) |
| C42 | 0.047 (3) | 0.057 (3) | 0.054 (3) | −0.006 (2) | 0.011 (2) | 0.011 (3) |
| C43 | 0.050 (3) | 0.056 (3) | 0.050 (3) | −0.015 (2) | 0.015 (2) | −0.011 (2) |
| C44 | 0.053 (3) | 0.051 (3) | 0.059 (3) | 0.012 (3) | −0.005 (3) | 0.009 (3) |
| Mo1—S8 | 2.1589 (16) | C23—H23C | 0.9600 |
| Mo1—S7 | 2.1710 (17) | C24—H24A | 0.9600 |
| Mo1—S1 | 2.2013 (16) | C24—H24B | 0.9600 |
| Mo1—S2 | 2.2057 (15) | C24—H24C | 0.9600 |
| Mo1—Cu1 | 2.7241 (9) | N3—C33 | 1.401 (8) |
| Mo2—S6 | 2.1451 (17) | N3—C31 | 1.453 (8) |
| Mo2—S5 | 2.1742 (16) | N3—C32 | 1.549 (9) |
| Mo2—S4 | 2.2006 (17) | N3—C34 | 1.550 (6) |
| Mo2—S3 | 2.2148 (16) | C31—H31A | 0.9600 |
| Mo2—Cu1 | 2.7241 (10) | C31—H31B | 0.9600 |
| Cu1—S3 | 2.2549 (17) | C31—H31C | 0.9600 |
| Cu1—S1 | 2.3161 (15) | C32—H32A | 0.9600 |
| Cu1—S2 | 2.3518 (16) | C32—H32B | 0.9600 |
| Cu1—S4 | 2.3630 (17) | C32—H32C | 0.9600 |
| O1—C11 | 1.232 (8) | C33—H33A | 0.9600 |
| N1—C11 | 1.338 (8) | C33—H33B | 0.9600 |
| N1—C12 | 1.434 (9) | C33—H33C | 0.9600 |
| N1—C13 | 1.447 (8) | C34—H34A | 0.9600 |
| C11—H11A | 0.9300 | C34—H34B | 0.9600 |
| C12—H12A | 0.9600 | C34—H34C | 0.9600 |
| C12—H12B | 0.9600 | N4—C41 | 1.392 (9) |
| C12—H12C | 0.9600 | N4—C42 | 1.481 (7) |
| C13—H13A | 0.9600 | N4—C44 | 1.481 (7) |
| C13—H13B | 0.9600 | N4—C43 | 1.515 (7) |
| C13—H13C | 0.9600 | C41—H41A | 0.9600 |
| N2—C24 | 1.443 (8) | C41—H41B | 0.9600 |
| N2—C22 | 1.473 (8) | C41—H41C | 0.9600 |
| N2—C21 | 1.478 (9) | C42—H42A | 0.9600 |
| N2—C23 | 1.508 (7) | C42—H42B | 0.9600 |
| C21—H21A | 0.9600 | C42—H42C | 0.9600 |
| C21—H21B | 0.9600 | C43—H43A | 0.9600 |
| C21—H21C | 0.9600 | C43—H43B | 0.9600 |
| C22—H22A | 0.9600 | C43—H43C | 0.9600 |
| C22—H22B | 0.9600 | C44—H44A | 0.9600 |
| C22—H22C | 0.9600 | C44—H44B | 0.9600 |
| C23—H23A | 0.9600 | C44—H44C | 0.9600 |
| C23—H23B | 0.9600 | ||
| S8—Mo1—S7 | 111.79 (6) | H22B—C22—H22C | 109.5 |
| S8—Mo1—S1 | 107.55 (6) | N2—C23—H23A | 109.5 |
| S7—Mo1—S1 | 111.04 (6) | N2—C23—H23B | 109.5 |
| S8—Mo1—S2 | 110.59 (6) | H23A—C23—H23B | 109.5 |
| S7—Mo1—S2 | 108.54 (6) | N2—C23—H23C | 109.5 |
| S1—Mo1—S2 | 107.24 (6) | H23A—C23—H23C | 109.5 |
| S8—Mo1—Cu1 | 139.84 (5) | H23B—C23—H23C | 109.5 |
| S7—Mo1—Cu1 | 108.35 (5) | N2—C24—H24A | 109.5 |
| S1—Mo1—Cu1 | 54.87 (4) | N2—C24—H24B | 109.5 |
| S2—Mo1—Cu1 | 55.80 (4) | H24A—C24—H24B | 109.5 |
| S6—Mo2—S5 | 111.20 (6) | N2—C24—H24C | 109.5 |
| S6—Mo2—S4 | 109.02 (6) | H24A—C24—H24C | 109.5 |
| S5—Mo2—S4 | 108.98 (6) | H24B—C24—H24C | 109.5 |
| S6—Mo2—S3 | 108.88 (6) | C33—N3—C31 | 109.6 (5) |
| S5—Mo2—S3 | 109.52 (6) | C33—N3—C32 | 112.8 (5) |
| S4—Mo2—S3 | 109.21 (6) | C31—N3—C32 | 109.4 (5) |
| S6—Mo2—Cu1 | 126.23 (5) | C33—N3—C34 | 108.8 (4) |
| S5—Mo2—Cu1 | 122.54 (5) | C31—N3—C34 | 108.6 (4) |
| S4—Mo2—Cu1 | 56.14 (4) | C32—N3—C34 | 107.5 (4) |
| S3—Mo2—Cu1 | 53.12 (5) | N3—C31—H31A | 109.5 |
| S3—Cu1—S1 | 117.80 (6) | N3—C31—H31B | 109.5 |
| S3—Cu1—S2 | 115.59 (6) | H31A—C31—H31B | 109.5 |
| S1—Cu1—S2 | 98.94 (6) | N3—C31—H31C | 109.5 |
| S3—Cu1—S4 | 102.39 (6) | H31A—C31—H31C | 109.5 |
| S1—Cu1—S4 | 110.01 (6) | H31B—C31—H31C | 109.5 |
| S2—Cu1—S4 | 112.49 (6) | N3—C32—H32A | 109.5 |
| S3—Cu1—Mo2 | 51.78 (4) | N3—C32—H32B | 109.5 |
| S1—Cu1—Mo2 | 132.00 (5) | H32A—C32—H32B | 109.5 |
| S2—Cu1—Mo2 | 128.60 (4) | N3—C32—H32C | 109.5 |
| S4—Cu1—Mo2 | 50.66 (4) | H32A—C32—H32C | 109.5 |
| S3—Cu1—Mo1 | 147.85 (5) | H32B—C32—H32C | 109.5 |
| S1—Cu1—Mo1 | 51.01 (4) | N3—C33—H33A | 109.5 |
| S2—Cu1—Mo1 | 50.87 (4) | N3—C33—H33B | 109.5 |
| S4—Cu1—Mo1 | 109.76 (5) | H33A—C33—H33B | 109.5 |
| Mo2—Cu1—Mo1 | 160.24 (3) | N3—C33—H33C | 109.5 |
| Mo1—S1—Cu1 | 74.13 (5) | H33A—C33—H33C | 109.5 |
| Mo1—S2—Cu1 | 73.34 (5) | H33B—C33—H33C | 109.5 |
| Mo2—S3—Cu1 | 75.09 (5) | N3—C34—H34A | 109.5 |
| Mo2—S4—Cu1 | 73.20 (5) | N3—C34—H34B | 109.5 |
| C11—N1—C12 | 122.4 (5) | H34A—C34—H34B | 109.5 |
| C11—N1—C13 | 119.2 (5) | N3—C34—H34C | 109.5 |
| C12—N1—C13 | 116.6 (5) | H34A—C34—H34C | 109.5 |
| O1—C11—N1 | 120.3 (5) | H34B—C34—H34C | 109.5 |
| O1—C11—H11A | 119.9 | C41—N4—C42 | 107.0 (3) |
| N1—C11—H11A | 119.9 | C41—N4—C44 | 112.8 (3) |
| N1—C12—H12A | 109.5 | C42—N4—C44 | 110.6 (4) |
| N1—C12—H12B | 109.5 | C41—N4—C43 | 108.4 (3) |
| H12A—C12—H12B | 109.5 | C42—N4—C43 | 108.3 (4) |
| N1—C12—H12C | 109.5 | C44—N4—C43 | 109.5 (4) |
| H12A—C12—H12C | 109.5 | N4—C41—H41A | 109.5 |
| H12B—C12—H12C | 109.5 | N4—C41—H41B | 109.5 |
| N1—C13—H13A | 109.5 | H41A—C41—H41B | 109.5 |
| N1—C13—H13B | 109.5 | N4—C41—H41C | 109.5 |
| H13A—C13—H13B | 109.5 | H41A—C41—H41C | 109.5 |
| N1—C13—H13C | 109.5 | H41B—C41—H41C | 109.5 |
| H13A—C13—H13C | 109.5 | N4—C42—H42A | 109.5 |
| H13B—C13—H13C | 109.5 | N4—C42—H42B | 109.5 |
| C24—N2—C22 | 108.6 (5) | H42A—C42—H42B | 109.5 |
| C24—N2—C21 | 115.1 (5) | N4—C42—H42C | 109.5 |
| C22—N2—C21 | 102.0 (4) | H42A—C42—H42C | 109.5 |
| C24—N2—C23 | 109.7 (5) | H42B—C42—H42C | 109.5 |
| C22—N2—C23 | 106.8 (5) | N4—C43—H43A | 109.5 |
| C21—N2—C23 | 113.9 (5) | N4—C43—H43B | 109.5 |
| N2—C21—H21A | 109.5 | H43A—C43—H43B | 109.5 |
| N2—C21—H21B | 109.5 | N4—C43—H43C | 109.5 |
| H21A—C21—H21B | 109.5 | H43A—C43—H43C | 109.5 |
| N2—C21—H21C | 109.5 | H43B—C43—H43C | 109.5 |
| H21A—C21—H21C | 109.5 | N4—C44—H44A | 109.5 |
| H21B—C21—H21C | 109.5 | N4—C44—H44B | 109.5 |
| N2—C22—H22A | 109.5 | H44A—C44—H44B | 109.5 |
| N2—C22—H22B | 109.5 | N4—C44—H44C | 109.5 |
| H22A—C22—H22B | 109.5 | H44A—C44—H44C | 109.5 |
| N2—C22—H22C | 109.5 | H44B—C44—H44C | 109.5 |
| H22A—C22—H22C | 109.5 | ||
| S6—Mo2—Cu1—S3 | 87.24 (8) | S7—Mo1—Cu1—Mo2 | 3.80 (11) |
| S5—Mo2—Cu1—S3 | −90.96 (7) | S1—Mo1—Cu1—Mo2 | 107.05 (11) |
| S4—Mo2—Cu1—S3 | 176.95 (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—S1 | 173.89 (8) | S7—Mo1—S1—Cu1 | 98.15 (6) |
| S4—Mo2—Cu1—S1 | 81.80 (8) | S2—Mo1—S1—Cu1 | −20.28 (6) |
| S3—Mo2—Cu1—S1 | −95.15 (8) | S3—Cu1—S1—Mo1 | 143.57 (6) |
| S6—Mo2—Cu1—S2 | −178.47 (8) | S2—Cu1—S1—Mo1 | 18.32 (6) |
| S5—Mo2—Cu1—S2 | 3.34 (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—S2 | 94.29 (8) | S8—Mo1—S2—Cu1 | 137.04 (6) |
| S6—Mo2—Cu1—S4 | −89.71 (8) | S7—Mo1—S2—Cu1 | −99.99 (6) |
| S5—Mo2—Cu1—S4 | 92.10 (7) | S1—Mo1—S2—Cu1 | 20.04 (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—Mo1 | 83.75 (11) | S4—Cu1—S2—Mo1 | 97.75 (6) |
| S4—Mo2—Cu1—Mo1 | −8.35 (10) | Mo2—Cu1—S2—Mo1 | 154.55 (4) |
| S3—Mo2—Cu1—Mo1 | 174.71 (11) | S6—Mo2—S3—Cu1 | −121.63 (6) |
| S8—Mo1—Cu1—S3 | −5.97 (12) | S5—Mo2—S3—Cu1 | 116.59 (6) |
| S7—Mo1—Cu1—S3 | 175.98 (9) | S4—Mo2—S3—Cu1 | −2.69 (6) |
| S1—Mo1—Cu1—S3 | −80.77 (10) | S1—Cu1—S3—Mo2 | 123.21 (6) |
| S2—Mo1—Cu1—S3 | 75.63 (10) | S2—Cu1—S3—Mo2 | −120.22 (5) |
| S8—Mo1—Cu1—S1 | 74.81 (8) | S4—Cu1—S3—Mo2 | 2.42 (5) |
| S7—Mo1—Cu1—S1 | −103.25 (7) | Mo1—Cu1—S3—Mo2 | −176.64 (7) |
| S2—Mo1—Cu1—S1 | 156.40 (7) | S6—Mo2—S4—Cu1 | 121.44 (5) |
| S8—Mo1—Cu1—S2 | −81.60 (8) | S5—Mo2—S4—Cu1 | −117.02 (5) |
| S7—Mo1—Cu1—S2 | 100.35 (7) | S3—Mo2—S4—Cu1 | 2.59 (5) |
| S1—Mo1—Cu1—S2 | −156.40 (7) | S3—Cu1—S4—Mo2 | −2.46 (5) |
| S8—Mo1—Cu1—S4 | 175.01 (7) | S1—Cu1—S4—Mo2 | −128.49 (5) |
| S7—Mo1—Cu1—S4 | −3.04 (6) | S2—Cu1—S4—Mo2 | 122.26 (6) |
| S1—Mo1—Cu1—S4 | 100.20 (7) | Mo1—Cu1—S4—Mo2 | 177.01 (3) |
| S2—Mo1—Cu1—S4 | −103.39 (6) | C12—N1—C11—O1 | 177.0 (6) |
| S8—Mo1—Cu1—Mo2 | −178.14 (9) | C13—N1—C11—O1 | 13.0 (9) |
Bruker (1998). SMART, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.
Maiti, B., Pal, K. & Sarkar, S. (2004). Inorg. Chem. Commun. 7, 1027–1029.
Müller, A., Bögge, H., Schimanski, U., Penk, M., Nieradzik, K., Dartmann, M., Krickemeyer, E., Schimanski, J., Römer, C., Römer, M., Dornfeld, H., Wienböker, U., Hellmann, W. & Zimmermann, M. (1989). Monatsh. Chem. 120, 367–391.
Niu, Y.-Y., Chen, T.-N., Liu, S.-X., Song, Y.-L., Wang, Y.-X., Xue, Z.-L. & Xin, X.-Q. (2002). J. Chem. Soc. Dalton Trans. pp. 1980–1984.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122.
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.