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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.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536808036532/bh2199sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536808036532/bh2199Isup2.hkl
Contains datablock I

CCDC reference: 712303

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](O-C) = 0.009 Å
  • R factor = 0.042
  • wR factor = 0.136
  • Data-to-parameter ratio = 24.2

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT232_ALERT_2_B Hirshfeld Test Diff (M-X) Mo1 -- S7 .. 12.52 su PLAT232_ALERT_2_B Hirshfeld Test Diff (M-X) Mo2 -- S4 .. 10.60 su PLAT232_ALERT_2_B Hirshfeld Test Diff (M-X) Mo2 -- S6 .. 11.28 su
Alert level C Value of measurement temperature given = 293.000 Value of melting point given = 0.000 PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Mo1 -- S1 .. 6.17 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Mo2 -- S5 .. 6.35 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Cu1 -- S3 .. 9.28 su PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 4 C3 H7 N O
Alert level G PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K
0 ALERT level A = In general: serious problem 3 ALERT level B = Potentially serious problem 5 ALERT level C = Check and explain 2 ALERT level G = General alerts; check 3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 6 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Comment top

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.

Related literature top

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

Experimental top

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 top

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).

Computing details top

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).

Figures top
[Figure 1] Fig. 1. The molecular structure of the title compound, with atom labels and 50% probability displacement ellipsoids. All H atoms have been omitted.
Tris(tetramethylammonium) tetra-µ2-sulfido-tetrasulfidocopper(I)dimolybdenum(VI) N,N-dimethylformamide solvate top
Crystal data top
(C4H12N)3[CuMo2S8]·C3H7NOF(000) = 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 = 1.2–26.1°
b = 20.336 (4) ŵ = 1.87 mm1
c = 17.718 (4) ÅT = 293 K
β = 98.60 (3)°Polyhedron, black red
V = 3362.4 (12) Å30.40 × 0.30 × 0.25 mm
Z = 4
Data collection top
Bruker APEX CCD area-detector
diffractometer
6625 independent reflections
Radiation source: fine-focus sealed tube5061 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.039
ϕ and ω scansθmax = 26.0°, θmin = 1.5°
Absorption correction: multi-scan
(SADABS; Bruker, 1998)
h = 1111
Tmin = 0.527, Tmax = 0.618k = 2425
17155 measured reflectionsl = 2121
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.042Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.136H-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 parametersΔρmax = 0.93 e Å3
0 restraintsΔρmin = 0.85 e Å3
Crystal data top
(C4H12N)3[CuMo2S8]·C3H7NOV = 3362.4 (12) Å3
Mr = 807.43Z = 4
Monoclinic, P21/nMo Kα radiation
a = 9.4380 (19) ŵ = 1.87 mm1
b = 20.336 (4) ÅT = 293 K
c = 17.718 (4) Å0.40 × 0.30 × 0.25 mm
β = 98.60 (3)°
Data collection top
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 = 0.618Rint = 0.039
17155 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0420 restraints
wR(F2) = 0.136H-atom parameters constrained
S = 1.05Δρmax = 0.93 e Å3
6625 reflectionsΔρmin = 0.85 e Å3
274 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
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*
H31B0.92240.03890.86740.083*
H31C0.88570.02410.94910.083*
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)
H34A0.66750.05120.81850.089*
H34B0.56200.00540.83290.089*
H34C0.63390.03800.90120.089*
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) top
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, º) top
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—S390.96 (7)S1—Mo1—Cu1—Mo2107.05 (11)
S4—Mo2—Cu1—S3176.95 (6)S2—Mo1—Cu1—Mo296.54 (10)
S6—Mo2—Cu1—S17.91 (9)S8—Mo1—S1—Cu1139.25 (6)
S5—Mo2—Cu1—S1173.89 (8)S7—Mo1—S1—Cu198.15 (6)
S4—Mo2—Cu1—S181.80 (8)S2—Mo1—S1—Cu120.28 (6)
S3—Mo2—Cu1—S195.15 (8)S3—Cu1—S1—Mo1143.57 (6)
S6—Mo2—Cu1—S2178.47 (8)S2—Cu1—S1—Mo118.32 (6)
S5—Mo2—Cu1—S23.34 (9)S4—Cu1—S1—Mo199.67 (6)
S4—Mo2—Cu1—S288.76 (8)Mo2—Cu1—S1—Mo1154.22 (5)
S3—Mo2—Cu1—S294.29 (8)S8—Mo1—S2—Cu1137.04 (6)
S6—Mo2—Cu1—S489.71 (8)S7—Mo1—S2—Cu199.99 (6)
S5—Mo2—Cu1—S492.10 (7)S1—Mo1—S2—Cu120.04 (6)
S3—Mo2—Cu1—S4176.95 (6)S3—Cu1—S2—Mo1145.14 (5)
S6—Mo2—Cu1—Mo198.05 (11)S1—Cu1—S2—Mo118.36 (6)
S5—Mo2—Cu1—Mo183.75 (11)S4—Cu1—S2—Mo197.75 (6)
S4—Mo2—Cu1—Mo18.35 (10)Mo2—Cu1—S2—Mo1154.55 (4)
S3—Mo2—Cu1—Mo1174.71 (11)S6—Mo2—S3—Cu1121.63 (6)
S8—Mo1—Cu1—S35.97 (12)S5—Mo2—S3—Cu1116.59 (6)
S7—Mo1—Cu1—S3175.98 (9)S4—Mo2—S3—Cu12.69 (6)
S1—Mo1—Cu1—S380.77 (10)S1—Cu1—S3—Mo2123.21 (6)
S2—Mo1—Cu1—S375.63 (10)S2—Cu1—S3—Mo2120.22 (5)
S8—Mo1—Cu1—S174.81 (8)S4—Cu1—S3—Mo22.42 (5)
S7—Mo1—Cu1—S1103.25 (7)Mo1—Cu1—S3—Mo2176.64 (7)
S2—Mo1—Cu1—S1156.40 (7)S6—Mo2—S4—Cu1121.44 (5)
S8—Mo1—Cu1—S281.60 (8)S5—Mo2—S4—Cu1117.02 (5)
S7—Mo1—Cu1—S2100.35 (7)S3—Mo2—S4—Cu12.59 (5)
S1—Mo1—Cu1—S2156.40 (7)S3—Cu1—S4—Mo22.46 (5)
S8—Mo1—Cu1—S4175.01 (7)S1—Cu1—S4—Mo2128.49 (5)
S7—Mo1—Cu1—S43.04 (6)S2—Cu1—S4—Mo2122.26 (6)
S1—Mo1—Cu1—S4100.20 (7)Mo1—Cu1—S4—Mo2177.01 (3)
S2—Mo1—Cu1—S4103.39 (6)C12—N1—C11—O1177.0 (6)
S8—Mo1—Cu1—Mo2178.14 (9)C13—N1—C11—O113.0 (9)

Experimental details

Crystal data
Chemical formula(C4H12N)3[CuMo2S8]·C3H7NO
Mr807.43
Crystal system, space groupMonoclinic, P21/n
Temperature (K)293
a, b, c (Å)9.4380 (19), 20.336 (4), 17.718 (4)
β (°) 98.60 (3)
V3)3362.4 (12)
Z4
Radiation typeMo Kα
µ (mm1)1.87
Crystal size (mm)0.40 × 0.30 × 0.25
Data collection
DiffractometerBruker APEX CCD area-detector
diffractometer
Absorption correctionMulti-scan
(SADABS; Bruker, 1998)
Tmin, Tmax0.527, 0.618
No. of measured, independent and
observed [I > 2σ(I)] reflections
17155, 6625, 5061
Rint0.039
(sin θ/λ)max1)0.617
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.042, 0.136, 1.05
No. of reflections6625
No. of parameters274
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.93, 0.85

Computer programs: SMART (Bruker, 1998), SAINT (Bruker, 1998), SHELXTL (Sheldrick, 2008).

 

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