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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 70| Part 7| July 2014| Pages m240-m241
https://doi.org/10.1107/S1600536814012501

μ2-Acetato-κ2O:O′-(4,4′-bi­pyridyl-κN)tris­­(di­ethyl di­thio­phosphato-κ2S,S′)-μ3-sulfido-tri-μ2-sulfido-trimolybdenum(IV) di­ethyl ether monosolvate

Keisuke Kawamotoa* and Isamu Kinoshitaa

aDepartment of Chemistry, Graduate School of Science, Osaka City University, Sumiyoshi-Ku, Osaka 558-8585, Japan
*Correspondence e-mail: [email protected]

(Received 19 May 2014; accepted 29 May 2014; online 4 June 2014)

In the title compound, [Mo3(CH3COO)(C4H10O2PS2)3S4(C10H8N2)]·C4H10O, the complex mol­ecule has a trinuclear incomplete cuboidal structure which is coordinated by three kinds of ligands, namely, diethyl di­thio­phosphate, acetate and 4,4′-bipyridyl. If Mo—Mo bonds are ignored, each Mo atom can be considered as six-coordinated in a distorted octa­hedral geometry. The Mo—Mo distance of 2.6880 (5) Å for two the Mo atoms bridged by the acetate ligand is shorter than the other two Mo—Mo distances [2.7490 (5) and 2.7566 (5) Å]. One ethyl group is disordered between two conformations in a 0.65 (3):0.35 (3) ratio. In the crystal, weak C—H⋯O inter­actions link the trinuclear mol­ecules related by translation in [100] into chains. The crystal packing exhibits short inter­molecular S⋯S contacts of 3.1886 (13) Å. In other words, in this crystal packing, a supramolecular structure is constructed by the C—H⋯O and S⋯S interactions.

CCDC reference: 1005735

Related literature

For related compounds and their crystal structures, see: Hernandez-Molina et al. (2011[Hernandez-Molina, R., Gonzalez-Platas, J., Kovalenko, K. A., Sokolov, M. N., Virovets, A. V., Llisar, R. & Vicent, C. (2011). Eur. J. Inorg. Chem. 683-693.]); Ogino et al. (1998[Ogino, H., Inomata, S. & Tobita, H. (1998). Chem. Rev. 98, 2093-2121.]); Tang et al. (2001[Tang, Y. H., Qin, Y. Y., Wu, L., Li, Z. J., Kang, Y. & Yao, Y. G. (2001). Polyhedron, 20, 2911-2916.]); Yao et al. (1995[Yao, Y., Akashi, H., Sakane, G., Shibahara, T. & Ohtaki, H. (1995). Inorg. Chem. 34, 42-48.]).

[Scheme 1]

Experimental

Crystal data

  • [Mo3(C2H3O2)(C4H10O2PS2)3S4(C10H8N2)]·C4H10O

  • Mr = 1261.06

  • Monoclinic, P 21 /c

  • a = 13.1573 (16) Å

  • b = 27.647 (3) Å

  • c = 14.2153 (17) Å

  • β = 107.7183 (16)°

  • V = 4925.6 (10) Å3

  • Z = 4

  • Mo Kα radiation

  • μ = 1.32 mm−1

  • T = 153 K

  • 0.19 × 0.16 × 0.03 mm
Data collection

  • Rigaku Saturn724 diffractometer

  • Absorption correction: multi-scan (REQAB; Rigaku, 1998[Rigaku (1998). REQAB. Rigaku Corporation, Tokyo, Japan.]) Tmin = 0.778, Tmax = 0.961

  • 40597 measured reflections

  • 11260 independent reflections

  • 9267 reflections with F2 > 2σ(F2)

  • Rint = 0.041
Refinement

  • R[F2 > 2σ(F2)] = 0.040

  • wR(F2) = 0.095

  • S = 1.08

  • 11260 reflections

  • 506 parameters

  • 1 restraint

  • H-atom parameters constrained

  • Δρmax = 0.78 e Å−3

  • Δρmin = −0.73 e Å−3

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A D⋯A D—H⋯A
C11—H11B⋯O5i 0.99 2.38 3.335 (7) 161
Symmetry code: (i) x-1, y, z.

Data collection: CrystalClear (Rigaku, 2010[Rigaku (2010). CrystalClear and CrystalStructure. Rigaku Corporation, Tokyo, Japan.]); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: SIR92 (Altomare et al., 1994[Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M. C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: CrystalStructure (Rigaku, 2010[Rigaku (2010). CrystalClear and CrystalStructure. Rigaku Corporation, Tokyo, Japan.]); software used to prepare material for publication: CrystalStructure.

Supporting information

CCDC reference: 1005735

Crystal structure: contains datablocks General, I. DOI: https://doi.org/10.1107/S1600536814012501/cv5459sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536814012501/cv5459Isup2.hkl

checkCIF report


Comment top

Mo3S4 clusters with diethyl dithiophosphate (dtp) ligand have been previously reported (Tang et al., 2001; Yao et al., 1995). In this study, complex of [Mo3S4(dtp)4(CH3CN)] (1) as starting material has been prepared by the reaction of [Mo3S4(H2O)9]4+ with Hdtp obtained by dissolving P4S10 in EtOH. Complex 1 reacts with acetate ion in pyridine, and then complex of [Mo3S4(dtp)3(µ2-OAc)(pyridine)] (2) was obtained. The pyridine in complex 2 loosely coordinates to the Mo3S4 core. Therefore, as estimating by VT-1H NMR spectroscopy and mass spectrometry, the pyridine molecule liberates from Mo3S4(dtp)3(µ2-OAc) core in solution (Hernandez-Molina et al., 2011). In our material, the 4,4'-bipyridine ligand also easily liberates from Mo3S4(dtp)3(µ2-OAc) core in solution as estimated by using mass spectrometry.

In general, the metal-metal distances of the sulfur bridged complexes increase with the increase of the negative charge of the cluster center (Ogino et al., 1998; Tang et al., 2001). In the title compound, the Mo3—N1 distance of 2.335 (5) Å is shorter than that in2 [2.385 (9) Å], which has the same framework of [Mo3S4(dtp)3(µ2-OAc)(L)] with the title compound. Furthermore, the average Mo—Mo distance in the title compound [2.731[1] Å] is also shorter than that in 2 [2.738[2] Å]. This shortening of Mo—Mo distnace is probably caused by the electron donating ability of N donating atom of 4,4'-bipyridine ligand.

Related literature top

For related compounds and their crystal structures, see: Hernandez-Molina et al. (2011); Ogino et al. (1998); Tang et al. (2001); Yao et al. (1995).

Experimental top

The title compound was synthesized from [Mo3S4(dtp)4(CH3CN) (1) (dtp = diethyl dithiophosphate), which was prepared by the literature method (Yao et al., 1995). To a solution of complex 1 (251 mg, 0.21 mmol) in 10 ml of EtOH was added excess 4,4'-bipyridine (415 mg, 2.65 mmol) and acetate anhydride (0.5 ml). After 4 h of stirring at 85°C, a brown powder was obtained (Yield: 176 mg, 70%). Red platelet single crystals of [Mo3S4(dtp)3(µ2-OAc)(4,4'-bpy)] suitable for X-ray analysis were obtained by vapor diffusion of the CHCl3 solution with external Et2O.

Refinement top

All H atoms were geometrically positioned [C—H 0.95–0.99 Å] and refined as riding, with Uiso(H) = 1.2–1.5 Ueq (C). The ethyl group attached to O3 was treated as disordered between two conformations with the occupancies refined to 0.65 (3) and 0.35 (3).

Structure description top

Mo3S4 clusters with diethyl dithiophosphate (dtp) ligand have been previously reported (Tang et al., 2001; Yao et al., 1995). In this study, complex of [Mo3S4(dtp)4(CH3CN)] (1) as starting material has been prepared by the reaction of [Mo3S4(H2O)9]4+ with Hdtp obtained by dissolving P4S10 in EtOH. Complex 1 reacts with acetate ion in pyridine, and then complex of [Mo3S4(dtp)3(µ2-OAc)(pyridine)] (2) was obtained. The pyridine in complex 2 loosely coordinates to the Mo3S4 core. Therefore, as estimating by VT-1H NMR spectroscopy and mass spectrometry, the pyridine molecule liberates from Mo3S4(dtp)3(µ2-OAc) core in solution (Hernandez-Molina et al., 2011). In our material, the 4,4'-bipyridine ligand also easily liberates from Mo3S4(dtp)3(µ2-OAc) core in solution as estimated by using mass spectrometry.

In general, the metal-metal distances of the sulfur bridged complexes increase with the increase of the negative charge of the cluster center (Ogino et al., 1998; Tang et al., 2001). In the title compound, the Mo3—N1 distance of 2.335 (5) Å is shorter than that in2 [2.385 (9) Å], which has the same framework of [Mo3S4(dtp)3(µ2-OAc)(L)] with the title compound. Furthermore, the average Mo—Mo distance in the title compound [2.731[1] Å] is also shorter than that in 2 [2.738[2] Å]. This shortening of Mo—Mo distnace is probably caused by the electron donating ability of N donating atom of 4,4'-bipyridine ligand.

For related compounds and their crystal structures, see: Hernandez-Molina et al. (2011); Ogino et al. (1998); Tang et al. (2001); Yao et al. (1995).

Computing details top

Data collection: CrystalClear (Rigaku, 2010); cell refinement: CrystalClear (Rigaku, 2010); data reduction: CrystalClear (Rigaku, 2010); program(s) used to solve structure: SIR92 (Altomare et al., 1994); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: CrystalStructure (Rigaku, 2010); software used to prepare material for publication: CrystalStructure (Rigaku, 2010).

Figures top
[Figure 1] Fig. 1. The molecular structure of the title compound with the atom-labeling scheme (except of C and H atoms). Displacement elipsoids are drawn at the 50% probability level. Both components of the disordered ethyl group (attached to O3) are shown.
µ2-Acetato-κ2O:O'-(4,4'-bipyridyl-κN)tris(diethyl dithiophosphato-κ2S,S')-µ3-sulfido-tri-µ2-sulfido-trimolybdenum(IV) diethyl ether solvate top
Crystal data top
[Mo3(C2H3O2)(C4H10O2PS2)3S4(C10H8N2)]·C4H10OF(000) = 2544.00
Mr = 1261.06Dx = 1.700 Mg m−3
Monoclinic, P21/cMo Kα radiation, λ = 0.71075 Å
Hall symbol: -P 2ybcCell parameters from 12390 reflections
a = 13.1573 (16) Åθ = 3.0–27.5°
b = 27.647 (3) ŵ = 1.32 mm−1
c = 14.2153 (17) ÅT = 153 K
β = 107.7183 (16)°Platelet, red
V = 4925.6 (10) Å30.19 × 0.16 × 0.03 mm
Z = 4
Data collection top
Rigaku Saturn724
diffractometer		9267 reflections with F2 > 2σ(F2)
Detector resolution: 7.111 pixels mm-1Rint = 0.041
ω scansθmax = 27.5°
Absorption correction: multi-scan
(REQAB; Rigaku, 1998)		h = −16→17
Tmin = 0.778, Tmax = 0.961k = −35→35
40597 measured reflectionsl = −18→18
11260 independent reflections
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.040Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.095H-atom parameters constrained
S = 1.08 w = 1/[σ2(Fo2) + (0.035P)2 + 9.5598P]
where P = (Fo2 + 2Fc2)/3
11260 reflections(Δ/σ)max < 0.001
506 parametersΔρmax = 0.78 e Å−3
1 restraintΔρmin = −0.73 e Å−3
Primary atom site location: structure-invariant direct methods
Crystal data top
[Mo3(C2H3O2)(C4H10O2PS2)3S4(C10H8N2)]·C4H10OV = 4925.6 (10) Å3
Mr = 1261.06Z = 4
Monoclinic, P21/cMo Kα radiation
a = 13.1573 (16) ŵ = 1.32 mm−1
b = 27.647 (3) ÅT = 153 K
c = 14.2153 (17) Å0.19 × 0.16 × 0.03 mm
β = 107.7183 (16)°
Data collection top
Rigaku Saturn724
diffractometer		11260 independent reflections
Absorption correction: multi-scan
(REQAB; Rigaku, 1998)		9267 reflections with F2 > 2σ(F2)
Tmin = 0.778, Tmax = 0.961Rint = 0.041
40597 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0401 restraint
wR(F2) = 0.095H-atom parameters constrained
S = 1.08Δρmax = 0.78 e Å−3
11260 reflectionsΔρmin = −0.73 e Å−3
506 parameters
Special details top

Geometry. ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY

Refinement. Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F2. R-factor (gt) are based on F. The threshold expression of F2 > 2.0 σ(F2) is used only for calculating R-factor (gt).

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Mo20.10154 (2)−0.060421 (11)0.19523 (2)0.01958 (8)
Mo10.24940 (2)0.009996 (11)0.23468 (2)0.01978 (8)
Mo30.04169 (2)0.033251 (11)0.21877 (2)0.01827 (7)
S10.21446 (7)−0.04305 (3)0.10469 (6)0.02303 (18)
S20.15391 (7)−0.01529 (3)0.34076 (6)0.02047 (17)
S3−0.03765 (7)−0.01806 (3)0.09060 (6)0.02140 (18)
S40.15061 (7)0.07198 (3)0.14388 (6)0.02183 (18)
S5−0.00065 (8)−0.10961 (4)0.28613 (7)0.0287 (2)
S60.04814 (8)−0.13499 (4)0.08405 (7)0.0290 (2)
S70.35744 (8)0.06451 (4)0.37431 (7)0.0276 (2)
S80.40698 (8)0.03446 (4)0.17530 (7)0.0302 (2)
S9−0.10014 (8)0.09694 (3)0.13671 (7)0.02602 (19)
S10−0.10271 (8)0.01686 (4)0.30145 (7)0.0263 (2)
P1−0.02992 (9)−0.15765 (4)0.17586 (7)0.0280 (2)
P20.46696 (8)0.06937 (4)0.30288 (8)0.0290 (3)
P3−0.17135 (8)0.07802 (4)0.23600 (7)0.0267 (2)
O10.2373 (2)−0.10679 (10)0.28332 (19)0.0275 (6)
O20.3601 (3)−0.04657 (10)0.31748 (19)0.0292 (6)
O3−0.0006 (3)−0.21110 (10)0.2143 (3)0.0379 (7)
O4−0.1523 (3)−0.16713 (11)0.1248 (2)0.0357 (7)
O50.5800 (3)0.05161 (11)0.3666 (3)0.0394 (8)
O60.5017 (3)0.12277 (11)0.2904 (3)0.0391 (7)
O7−0.1620 (3)0.12055 (10)0.3116 (2)0.0349 (7)
O8−0.2960 (2)0.07256 (11)0.1910 (2)0.0346 (7)
O90.5009 (4)0.22604 (17)0.9179 (4)0.0829 (14)
N10.0886 (3)0.09178 (11)0.3430 (2)0.0212 (6)
N20.2054 (4)0.27667 (14)0.7073 (3)0.0439 (10)
C10.3303 (4)−0.08972 (15)0.3243 (3)0.0295 (9)
C20.4110 (4)−0.12299 (17)0.3901 (4)0.0474 (12)
C30.1102 (5)−0.22189 (19)0.2713 (5)0.0655 (17)
C4A0.1481 (19)−0.2603 (11)0.239 (4)0.122 (18)0.35 (3)
C4B0.1189 (9)−0.2652 (4)0.3227 (12)0.081 (6)0.65 (3)
C5−0.2205 (4)−0.1297 (2)0.0645 (4)0.0530 (14)
C6−0.2903 (7)−0.1074 (4)0.1084 (6)0.114 (4)
C70.5974 (4)0.00443 (17)0.4150 (4)0.0416 (11)
C80.6389 (5)−0.0311 (2)0.3569 (5)0.0626 (17)
C90.4255 (5)0.15613 (19)0.2282 (5)0.0586 (15)
C100.4810 (7)0.1953 (3)0.1974 (7)0.109 (3)
C11−0.1951 (5)0.1142 (2)0.3999 (4)0.0516 (14)
C12−0.1868 (6)0.1610 (3)0.4514 (5)0.0699 (18)
C13−0.3411 (4)0.03861 (17)0.1090 (4)0.0388 (11)
C14−0.4114 (4)0.0658 (2)0.0244 (4)0.0504 (13)
C150.1053 (3)0.13808 (13)0.3217 (3)0.0263 (8)
C160.0997 (3)0.08171 (13)0.4387 (3)0.0218 (7)
C170.1278 (4)0.17474 (14)0.3906 (3)0.0279 (8)
C180.1240 (3)0.11629 (13)0.5119 (3)0.0249 (8)
C190.1377 (3)0.16418 (13)0.4890 (3)0.0247 (8)
C200.1608 (4)0.20292 (14)0.5646 (3)0.0285 (9)
C210.1182 (4)0.24874 (15)0.5430 (3)0.0397 (11)
C220.2260 (4)0.19456 (15)0.6596 (3)0.0346 (10)
C230.1433 (5)0.28370 (16)0.6162 (4)0.0474 (13)
C240.2458 (5)0.23228 (16)0.7277 (3)0.0442 (12)
C250.5100 (6)0.2665 (3)0.9833 (6)0.084 (2)
C260.3979 (6)0.2842 (3)0.9759 (6)0.091 (3)
C270.6064 (8)0.2053 (3)0.9270 (8)0.116 (4)
C280.5875 (10)0.1690 (4)0.8416 (7)0.158 (6)
H2A0.4733−0.12540.36620.0569*
H2B0.3794−0.15510.38960.0569*
H2C0.4332−0.11020.45760.0569*
H5A−0.1745−0.10450.04910.0636*
H5B−0.2631−0.14440.00130.0636*
H6A−0.2492−0.09160.16990.1367*
H6B−0.3375−0.13180.12280.1367*
H6C−0.3332−0.08320.06310.1367*
H7A0.5293−0.00760.42230.0499*
H7B0.64910.00780.48190.0499*
H8A0.7016−0.01750.34300.0751*
H8B0.5834−0.03810.29470.0751*
H8C0.6590−0.06100.39500.0751*
H9A0.38010.13890.16940.0703*
H9B0.37880.16930.26510.0703*
H10A0.52680.18220.16050.1313*
H10B0.52500.21270.25570.1313*
H10C0.42900.21760.15520.1313*
H11A−0.14890.09000.44410.0619*
H11B−0.26970.10240.38120.0619*
H12A−0.11200.17130.47430.0838*
H12B−0.21370.15760.50820.0838*
H12C−0.22920.18530.40600.0838*
H13A−0.38250.01310.12990.0465*
H13B−0.28300.02290.08960.0465*
H14A−0.37100.09220.00680.0605*
H14B−0.47180.07910.04260.0605*
H14C−0.43790.0440−0.03220.0605*
H150.10120.14580.25550.0315*
H160.09030.04920.45630.0261*
H170.13660.20700.37120.0334*
H180.13130.10740.57820.0299*
H210.07220.25610.47890.0476*
H220.25700.16360.67810.0415*
H230.11370.31500.59950.0569*
H240.29080.22600.79280.0531*
H25A0.55110.29280.96450.1005*
H25B0.54790.25671.05200.1005*
H26A0.40270.31181.02030.1089*
H26B0.35790.25800.99490.1089*
H26C0.36120.29410.90780.1089*
H27A0.63580.18880.99130.1394*
H27B0.65690.23090.92130.1394*
H28A0.55800.18600.77860.1895*
H28B0.53710.14410.84830.1895*
H28C0.65530.15380.84330.1895*
H4A0.1555−0.19370.26830.0786*0.35 (3)
H4B0.1143−0.22700.34130.0786*0.35 (3)
H4C0.1542−0.22370.22590.0786*0.65 (3)
H4D0.1385−0.19530.31870.0786*0.65 (3)
H4E0.2220−0.26580.27980.1462*0.35 (3)
H4F0.1459−0.25530.17030.1462*0.35 (3)
H4G0.1047−0.28860.24330.1462*0.35 (3)
H4H0.1939−0.27120.35960.0969*0.65 (3)
H4I0.0922−0.29180.27600.0969*0.65 (3)
H4J0.0768−0.26340.36880.0969*0.65 (3)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mo20.01993 (15)0.02225 (16)0.01681 (14)−0.00049 (12)0.00596 (11)−0.00109 (11)
Mo10.01735 (14)0.02572 (17)0.01616 (14)−0.00130 (12)0.00493 (11)−0.00018 (11)
Mo30.01806 (15)0.02209 (16)0.01506 (13)−0.00112 (12)0.00562 (11)−0.00143 (11)
S10.0219 (5)0.0294 (5)0.0194 (4)−0.0004 (4)0.0088 (4)−0.0028 (4)
S20.0219 (5)0.0240 (5)0.0155 (4)−0.0014 (4)0.0057 (4)−0.0005 (4)
S30.0203 (4)0.0250 (5)0.0176 (4)−0.0009 (4)0.0039 (4)−0.0027 (4)
S40.0222 (5)0.0261 (5)0.0177 (4)−0.0012 (4)0.0068 (4)0.0017 (4)
S50.0359 (6)0.0294 (5)0.0238 (5)−0.0057 (5)0.0137 (4)−0.0007 (4)
S60.0360 (6)0.0274 (5)0.0257 (5)−0.0042 (4)0.0125 (4)−0.0055 (4)
S70.0249 (5)0.0362 (6)0.0199 (4)−0.0078 (4)0.0040 (4)−0.0022 (4)
S80.0226 (5)0.0429 (6)0.0274 (5)−0.0036 (5)0.0110 (4)−0.0002 (4)
S90.0252 (5)0.0290 (5)0.0233 (5)0.0040 (4)0.0065 (4)0.0004 (4)
S100.0239 (5)0.0316 (5)0.0270 (5)−0.0027 (4)0.0133 (4)−0.0010 (4)
P10.0328 (6)0.0246 (5)0.0262 (5)−0.0052 (5)0.0087 (4)−0.0005 (4)
P20.0211 (5)0.0355 (6)0.0278 (5)−0.0059 (5)0.0037 (4)0.0045 (5)
P30.0216 (5)0.0329 (6)0.0265 (5)0.0002 (4)0.0087 (4)−0.0072 (4)
O10.0259 (14)0.0293 (14)0.0251 (13)0.0030 (12)0.0042 (11)0.0004 (11)
O20.0289 (15)0.0294 (15)0.0290 (14)−0.0010 (12)0.0085 (12)0.0007 (12)
O30.0474 (19)0.0248 (15)0.0384 (17)−0.0039 (14)0.0086 (14)0.0013 (13)
O40.0332 (16)0.0379 (17)0.0340 (16)−0.0098 (13)0.0074 (13)0.0007 (13)
O50.0220 (14)0.0494 (19)0.0414 (17)−0.0084 (14)0.0016 (13)0.0112 (15)
O60.0336 (16)0.0388 (17)0.0441 (17)−0.0099 (14)0.0108 (14)0.0074 (14)
O70.0366 (17)0.0388 (17)0.0325 (15)0.0007 (14)0.0151 (13)−0.0123 (13)
O80.0203 (14)0.0486 (18)0.0353 (16)0.0021 (13)0.0087 (12)−0.0126 (14)
O90.090 (4)0.082 (4)0.074 (3)−0.005 (3)0.020 (3)−0.024 (3)
N10.0240 (16)0.0240 (16)0.0168 (14)−0.0003 (13)0.0079 (12)−0.0009 (12)
N20.068 (3)0.036 (2)0.0294 (19)−0.015 (2)0.0165 (19)−0.0113 (16)
C10.029 (2)0.034 (3)0.0259 (19)0.0043 (18)0.0094 (16)0.0016 (16)
C20.041 (3)0.039 (3)0.051 (3)0.008 (3)−0.002 (3)0.010 (3)
C30.052 (4)0.040 (3)0.088 (5)0.006 (3)−0.004 (3)0.014 (3)
C4A0.069 (15)0.10 (2)0.18 (4)0.018 (14)0.008 (19)−0.07 (3)
C4B0.063 (7)0.062 (7)0.100 (11)−0.003 (6)−0.000 (7)0.044 (7)
C50.039 (3)0.066 (4)0.051 (3)−0.006 (3)0.010 (3)0.021 (3)
C60.099 (7)0.156 (9)0.093 (6)0.073 (6)0.039 (5)0.056 (6)
C70.028 (3)0.051 (3)0.040 (3)−0.005 (2)0.0026 (19)0.018 (2)
C80.049 (4)0.070 (4)0.080 (4)0.022 (3)0.037 (3)0.034 (4)
C90.060 (4)0.042 (3)0.063 (4)−0.002 (3)0.004 (3)0.019 (3)
C100.112 (7)0.081 (6)0.149 (9)0.005 (5)0.059 (7)0.056 (6)
C110.048 (3)0.066 (4)0.053 (3)−0.023 (3)0.034 (3)−0.033 (3)
C120.084 (5)0.079 (5)0.052 (4)0.011 (4)0.028 (4)−0.030 (3)
C130.023 (2)0.054 (3)0.040 (3)−0.003 (2)0.0096 (18)−0.014 (2)
C140.035 (3)0.078 (4)0.038 (3)0.009 (3)0.010 (2)−0.005 (3)
C150.034 (2)0.027 (2)0.0187 (17)−0.0028 (17)0.0091 (15)−0.0018 (15)
C160.0244 (18)0.0238 (18)0.0178 (16)−0.0007 (15)0.0076 (14)−0.0001 (14)
C170.038 (3)0.0239 (19)0.0227 (18)−0.0050 (17)0.0111 (16)−0.0010 (15)
C180.029 (2)0.029 (2)0.0179 (16)−0.0009 (16)0.0090 (15)0.0010 (14)
C190.029 (2)0.0255 (19)0.0196 (17)−0.0008 (16)0.0076 (15)−0.0024 (14)
C200.037 (3)0.027 (2)0.0223 (18)−0.0045 (17)0.0102 (17)−0.0042 (15)
C210.063 (3)0.027 (3)0.023 (2)0.004 (2)0.006 (2)−0.0006 (16)
C220.047 (3)0.030 (3)0.0241 (19)−0.0031 (19)0.0065 (18)−0.0040 (16)
C230.078 (4)0.026 (3)0.036 (3)0.003 (3)0.015 (3)−0.0043 (19)
C240.066 (4)0.038 (3)0.023 (2)−0.011 (3)0.005 (2)−0.0072 (18)
C250.082 (5)0.092 (6)0.077 (5)−0.017 (5)0.024 (4)−0.027 (4)
C260.082 (6)0.105 (6)0.085 (6)−0.003 (5)0.024 (5)−0.029 (5)
C270.116 (8)0.097 (7)0.162 (10)0.009 (6)0.083 (7)−0.036 (6)
C280.266 (15)0.137 (9)0.084 (7)0.097 (10)0.073 (8)0.005 (6)
Geometric parameters (Å, º) top
Mo2—Mo12.6880 (5)C20—C221.380 (5)
Mo2—Mo32.7566 (5)C21—C231.384 (6)
Mo2—S12.2931 (11)C22—C241.393 (6)
Mo2—S22.3332 (9)C25—C261.527 (12)
Mo2—S32.2978 (9)C27—C281.536 (14)
Mo2—S52.5267 (12)C2—H2A0.980
Mo2—S62.5624 (11)C2—H2B0.980
Mo2—O12.245 (3)C2—H2C0.980
Mo1—Mo32.7490 (5)C3—H4A0.990
Mo1—S12.2934 (9)C3—H4B0.990
Mo1—S22.3440 (11)C3—H4C0.990
Mo1—S42.2959 (9)C3—H4D0.990
Mo1—S72.5524 (10)C4A—H4E0.980
Mo1—S82.5561 (13)C4A—H4F0.980
Mo1—O22.216 (3)C4A—H4G0.980
Mo3—S22.3302 (9)C4B—H4H0.980
Mo3—S32.2943 (9)C4B—H4I0.980
Mo3—S42.2939 (11)C4B—H4J0.980
Mo3—S92.5726 (10)C5—H5A0.990
Mo3—S102.5604 (13)C5—H5B0.990
Mo3—N12.335 (3)C6—H6A0.980
S5—P12.0005 (15)C6—H6B0.980
S6—P11.9916 (17)C6—H6C0.980
S7—P22.0040 (18)C7—H7A0.990
S8—P21.9930 (15)C7—H7B0.990
S9—P31.9871 (17)C8—H8A0.980
S10—P32.0072 (15)C8—H8B0.980
P1—O31.582 (3)C8—H8C0.980
P1—O41.573 (3)C9—H9A0.990
P2—O51.566 (3)C9—H9B0.990
P2—O61.571 (4)C10—H10A0.980
P3—O71.572 (3)C10—H10B0.980
P3—O81.576 (3)C10—H10C0.980
O1—C11.275 (5)C11—H11A0.990
O2—C11.269 (5)C11—H11B0.990
O3—C31.467 (7)C12—H12A0.980
O4—C51.464 (6)C12—H12B0.980
O5—C71.460 (6)C12—H12C0.980
O6—C91.449 (6)C13—H13A0.990
O7—C111.459 (7)C13—H13B0.990
O8—C131.474 (6)C14—H14A0.980
O9—C251.437 (9)C14—H14B0.980
O9—C271.471 (12)C14—H14C0.980
N1—C151.348 (5)C15—H150.950
N1—C161.353 (5)C16—H160.950
N2—C231.319 (6)C17—H170.950
N2—C241.334 (6)C18—H180.950
C1—C21.498 (6)C21—H210.950
C3—C4A1.31 (4)C22—H220.950
C3—C4B1.390 (14)C23—H230.950
C5—C61.400 (12)C24—H240.950
C7—C81.489 (9)C25—H25A0.990
C9—C101.447 (11)C25—H25B0.990
C11—C121.476 (9)C26—H26A0.980
C13—C141.479 (7)C26—H26B0.980
C15—C171.377 (6)C26—H26C0.980
C16—C181.377 (5)C27—H27A0.990
C17—C191.397 (6)C27—H27B0.990
C18—C191.388 (6)C28—H28A0.980
C19—C201.482 (6)C28—H28B0.980
C20—C211.382 (6)C28—H28C0.980
S1···C13.292 (4)C26···H2Axi3.4419
S2···C13.163 (5)C26···H2Bxi3.4125
S2···C163.201 (4)C26···H9Bviii3.2002
S4···C153.317 (4)C26···H10Cxii3.0682
S5···C33.463 (6)C26···H17viii3.3132
S6···C33.493 (7)C26···H243.0195
S6···C53.464 (6)C27···H10Bviii3.2606
S7···N13.510 (4)C27···H14Axvii3.3072
S7···C73.457 (5)C27···H4Hxi3.4177
S7···C93.559 (7)C28···H2Aii3.0625
S8···C93.439 (6)C28···H2Bii3.4649
S9···C133.471 (5)C28···H10Bviii3.5011
S9···C153.344 (4)C28···H14Axvii3.0885
S10···C113.423 (6)H2A···C26ix3.4419
S10···C133.530 (4)H2A···C28ii3.0625
S10···C163.309 (4)H2A···H25Aix3.3877
P1···C63.548 (9)H2A···H25Bix3.5015
P2···O23.531 (3)H2A···H26Aix2.5847
P2···C83.515 (6)H2A···H28Aii2.5875
P3···N13.315 (3)H2A···H28Bii3.0546
O1···C33.575 (7)H2A···H28Cii3.0464
O2···C73.320 (5)H2B···C25ix2.9110
O2···C83.563 (7)H2B···C26ix3.4125
O7···N13.287 (5)H2B···C28ii3.4649
O7···C153.508 (6)H2B···H12Biv2.9655
O7···C163.534 (5)H2B···H25Aix2.4602
O8···C113.083 (6)H2B···H25Bix2.6585
N1···C192.814 (5)H2B···H26Aix2.9086
N2···C202.809 (6)H2B···H28Aii2.8846
C15···C182.708 (6)H2B···H28Cii3.2018
C16···C172.716 (6)H2C···S7ii3.2996
C17···C213.011 (6)H2C···P2ii3.4451
C18···C223.029 (6)H2C···O5ii3.0264
C21···C242.690 (6)H2C···O6ii3.4373
C22···C232.689 (7)H2C···C7ii3.5264
S1···S3i3.4702 (11)H2C···C25ix3.5350
S3···S1i3.4702 (11)H2C···H7Bii3.2406
S3···S3i3.1886 (14)H2C···H11Biv3.5951
S3···S4i3.5392 (12)H2C···H12Biv3.3377
S4···S3i3.5392 (12)H2C···H25Aix2.8835
S6···S9i3.5679 (16)H2C···H26Aix2.9995
S7···C7ii3.445 (5)H5A···S4i2.9932
S9···S6i3.5679 (16)H5A···H9Ai3.5709
O4···C21iii3.457 (6)H5A···H23iii3.3284
O4···C22iv3.568 (6)H5B···S4i3.5083
O4···C24iv3.275 (7)H5B···C9i3.3273
O5···O8v3.422 (5)H5B···C23iii3.2909
O5···C11v3.335 (7)H5B···H9Ai2.4505
O7···C4Avi3.39 (3)H5B···H10Ci3.2950
O8···O5vii3.422 (5)H5B···H23iii2.9821
N2···C9viii3.377 (8)H5B···H26Biv3.3870
N2···C15viii3.352 (6)H6A···H8Avii3.4127
N2···C17viii3.354 (7)H6A···H8Bvii3.5453
C2···C25ix3.537 (9)H6A···H18iv3.4690
C2···C28ii3.536 (12)H6A···H22iv2.9619
C4A···O7iii3.39 (3)H6B···O9iv3.3142
C7···S7ii3.445 (5)H6B···C22iv3.4593
C9···N2x3.377 (8)H6B···C24iv3.4818
C11···O5vii3.335 (7)H6B···H14Bxiii3.2176
C15···N2x3.352 (6)H6B···H22iv2.8420
C17···N2x3.354 (7)H6B···H24iv2.8543
C17···C26x3.573 (9)H6B···H28Biv2.7998
C21···O4vi3.457 (6)H6C···S8i3.4986
C22···O4iv3.568 (6)H6C···C14xiii3.2438
C24···O4iv3.275 (7)H6C···H9Ai3.5260
C25···C2xi3.537 (9)H6C···H14Bxiii2.5497
C26···C17viii3.573 (9)H6C···H14Cxiii3.1028
C28···C2ii3.536 (12)H7A···S7ii3.2294
Mo3···H153.2133H7A···C7ii3.2370
Mo3···H163.2695H7A···H7Aii2.5855
S2···H162.7230H7A···H7Bii3.0512
S3···H5A2.9422H7B···S2ii3.0237
S3···H13B3.4162H7B···S7ii2.8786
S4···H9A3.4637H7B···O2ii3.0842
S4···H152.7820H7B···C1ii3.5135
S5···H5A3.4512H7B···H2Cii3.2406
S5···H6A3.2217H7B···H7Aii3.0512
S5···H4A3.1626H7B···H11Bv3.3117
S5···H4B3.5647H8A···S10v2.9675
S5···H4D2.9429H8A···O8v3.3022
S6···H5A2.9408H8A···C13v3.5560
S6···H4A3.0390H8A···H6Av3.4127
S6···H4C3.2110H8A···H11Bv3.3610
S6···H4D3.5920H8A···H13Av3.0119
S7···H7A2.9354H8A···H16ii3.4138
S7···H9B3.3392H8A···H18ii3.2809
S8···H7A3.5827H8B···H6Av3.5453
S8···H8B3.1449H8B···H13Av2.8851
S8···H9A2.9061H8C···S7ii3.3529
S9···H13B3.0731H8C···C16ii3.3807
S9···H14A3.4819H8C···C18ii3.1537
S9···H152.9956H8C···H16ii3.3483
S10···H11A3.0522H8C···H18ii2.9601
S10···H13B3.2214H8C···H22ii3.3243
S10···H162.9486H9A···N2x3.4324
P1···H5A2.6332H9A···C5i3.3584
P1···H5B3.3272H9A···H5Ai3.5709
P1···H6A3.3927H9A···H5Bi2.4505
P1···H4A2.5918H9A···H6Ci3.5260
P1···H4B3.1762H9A···H14Bv3.4509
P1···H4C2.9418H9A···H23x3.5746
P1···H4D2.7158H9B···N2x2.6407
P1···H4F3.5708H9B···C23x3.4323
P2···H7A2.6904H9B···C24x3.1914
P2···H7B3.3771H9B···C25x3.5346
P2···H8B3.3602H9B···C26x3.2002
P2···H9A2.6980H9B···H23x3.5917
P2···H9B2.9811H9B···H24x3.1866
P3···H11A2.9004H9B···H25Ax3.2194
P3···H11B2.8305H9B···H26Ax3.5830
P3···H13A3.2653H9B···H26Cx2.3416
P3···H13B2.6366H10A···O9xiv3.5739
P3···H14A3.5300H10A···C25xiv3.3903
O1···H2A3.0104H10A···H14Bv3.3083
O1···H2B2.4175H10A···H25Bxiv2.6381
O1···H2C2.9837H10A···H26Bxiv3.4193
O1···H4A2.6147H10A···H27Axiv3.1581
O1···H4C3.4296H10A···H4Exviii3.4652
O1···H4D2.8860H10B···O9x2.9543
O2···H2A2.6109H10B···C25x3.3501
O2···H2B3.1567H10B···C27x3.2606
O2···H2C2.6124H10B···C28x3.5011
O2···H7A2.5136H10B···H12Cv3.3740
O2···H8B3.0616H10B···H25Ax2.8861
O3···H4E3.1739H10B···H25Bxiv3.2389
O3···H4F2.5160H10B···H26Cx3.4916
O3···H4G2.5157H10B···H27Bx2.9158
O3···H4H3.2180H10B···H28Ax2.8396
O3···H4I2.5652H10B···H4Exviii3.5649
O3···H4J2.5671H10C···N2x3.2493
O4···H6A2.6253H10C···C24x3.2106
O4···H6B2.6180H10C···C25xiv3.2431
O4···H6C3.2490H10C···C26xiv3.0682
O5···H8A2.5785H10C···H5Bi3.2950
O5···H8B2.6873H10C···H24x3.4249
O5···H8C3.2678H10C···H25Bxiv2.6762
O6···H10A2.5660H10C···H26Axiv3.1897
O6···H10B2.5700H10C···H26Bxiv2.4528
O6···H10C3.2198H10C···H28Ax3.3548
O7···H12A2.6117H11A···O5vii3.5596
O7···H12B3.2380H11B···P2vii3.4255
O7···H12C2.5526H11B···O5vii2.3830
O8···H11A3.5609H11B···O6vii2.9446
O8···H11B2.7456H11B···C7vii3.3374
O8···H14A2.5601H11B···H2Civ3.5951
O8···H14B2.6201H11B···H7Bvii3.3117
O8···H14C3.2509H11B···H8Avii3.3610
O9···H26A3.2488H12A···C4Avi3.4824
O9···H26B2.6025H12A···H4Biv3.0483
O9···H26C2.6039H12A···H4Div3.1385
O9···H28A2.5719H12A···H4Fvi2.8264
O9···H28B2.5736H12A···H4Gvi3.3149
O9···H28C3.2484H12A···H4Jiv3.3231
N1···H173.2480H12B···O1iv3.3780
N1···H183.2467H12B···C2iv3.4677
N2···H213.2359H12B···C3iv3.4984
N2···H223.2521H12B···H2Biv2.9655
C1···H7A3.4251H12B···H2Civ3.3377
C2···H7A3.5176H12B···H25Axv3.2661
C6···H13A3.5913H12B···H27Bxv3.5573
C8···H2A3.4267H12B···H4Aiv3.1926
C13···H6C3.4373H12B···H4Biv2.8741
C15···H163.1563H12B···H4Div2.5766
C16···H11A3.3031H12B···H4Jiv3.5966
C16···H153.1554H12C···C4Avi2.9987
C17···H183.2425H12C···H10Bvii3.3740
C17···H212.7810H12C···H25Axv3.2975
C18···H11A3.4988H12C···H27Bxv2.8033
C18···H12A3.3503H12C···H4Cvi3.4564
C18···H173.2431H12C···H4Evi2.9933
C18···H222.7994H12C···H4Fvi2.4081
C19···H12A3.2332H12C···H4Gvi3.1346
C19···H153.2458H13A···S8vii3.0855
C19···H163.2446H13A···C8vii3.3811
C19···H212.6737H13A···H8Avii3.0119
C19···H222.6685H13A···H8Bvii2.8851
C20···H12A3.5347H13A···H14Cxiii2.8307
C20···H172.6721H13B···S1i3.2034
C20···H182.6857H14A···S1i3.2546
C20···H233.2290H14A···C27xvi3.3072
C20···H243.2359H14A···C28xvi3.0885
C21···H12A3.5930H14A···H27Axvi2.6815
C21···H172.7778H14A···H28Bxvi2.6335
C21···H223.2294H14A···H28Cxvi2.9842
C22···H182.7973H14B···S8vii3.0751
C22···H213.2287H14B···C6xiii3.3045
C23···H243.1060H14B···H6Bxiii3.2176
C24···H233.1063H14B···H6Cxiii2.5497
C25···H27A2.6934H14B···H9Avii3.4509
C25···H27B2.5540H14B···H10Avii3.3083
C27···H25A2.6281H14B···H14Cxiii3.5946
C27···H25B2.5694H14B···H27Axvi3.5141
H2A···H7A3.3802H14B···H28Bxvi3.3266
H2A···H8B3.1406H14C···S1i3.3983
H2A···H8C2.9492H14C···S8i3.0848
H2B···H4A3.1145H14C···C13xiii3.5963
H2B···H4D3.2178H14C···H6Cxiii3.1028
H2C···H7A3.2072H14C···H13Axiii2.8307
H5A···H6A2.2512H14C···H14Bxiii3.5946
H5A···H6B2.7636H14C···H14Cxiii3.2167
H5A···H6C2.2374H14C···H28Bxvi3.2106
H5B···H6A2.7634H15···N2x2.7404
H5B···H6B2.2571H15···C23x2.9484
H5B···H6C2.2315H15···H23x2.5171
H6A···H13A3.3442H15···H4Gvi3.2644
H6A···H13B3.3495H15···H4Ivi2.9924
H6C···H13A2.9644H15···H4Jvi3.5197
H6C···H13B3.0048H16···H8Aii3.4138
H7A···H8A2.8354H16···H8Cii3.3483
H7A···H8B2.3013H17···O3vi2.9130
H7A···H8C2.3752H17···O4vi3.4859
H7B···H8A2.3859H17···N2x2.7812
H7B···H8B2.8342H17···C24x3.2904
H7B···H8C2.2918H17···C26x3.3132
H9A···H10A2.3072H17···H24x3.1885
H9A···H10B2.8077H17···H26Ax3.5352
H9A···H10C2.2966H17···H26Bx3.0637
H9B···H10A2.8076H17···H26Cx2.8398
H9B···H10B2.3043H17···H4Gvi3.0989
H9B···H10C2.2995H17···H4Ivi3.0996
H11A···H12A2.3120H18···S5iv2.9490
H11A···H12B2.3511H18···C8ii3.5701
H11A···H12C2.8306H18···H6Aiv3.4690
H11A···H163.2978H18···H8Aii3.2809
H11B···H12A2.8302H18···H8Cii2.9601
H11B···H12B2.3071H21···S6vi3.3923
H11B···H12C2.3563H21···P1vi3.1759
H12A···H183.5605H21···O3vi2.7702
H12A···H213.3595H21···O4vi2.9537
H13A···H14A2.8340H21···C4Avi3.5705
H13A···H14B2.3162H21···H4Cvi3.5188
H13A···H14C2.3559H21···H4Fvi3.0214
H13B···H14A2.3604H21···H4Gvi3.5283
H13B···H14B2.8337H21···H4Jiv3.3398
H13B···H14C2.3117H22···O4iv3.4800
H15···H172.3051H22···C6iv3.3176
H16···H182.3041H22···H6Aiv2.9619
H17···H212.3865H22···H6Biv2.8420
H18···H222.3952H22···H8Cii3.3243
H21···H232.3067H22···H26Ax3.4343
H22···H242.3215H23···S4viii3.1943
H25A···H26A2.3787H23···S6vi3.1414
H25A···H26B2.8712H23···O4vi3.4132
H25A···H26C2.3814H23···C5vi3.4274
H25A···H27A3.0660H23···C15viii3.4464
H25A···H27B2.4023H23···H5Avi3.3284
H25B···H26A2.3777H23···H5Bvi2.9821
H25B···H26B2.3825H23···H9Aviii3.5746
H25B···H26C2.8712H23···H9Bviii3.5917
H25B···H27A2.4917H23···H15viii2.5171
H25B···H27B2.7642H23···H4Jiv3.0345
H27A···H28A2.8837H24···O4iv2.9402
H27A···H28B2.3953H24···O92.7956
H27A···H28C2.4001H24···C6iv3.5677
H27B···H28A2.3962H24···C253.4865
H27B···H28B2.8838H24···C263.0195
H27B···H28C2.3991H24···H6Biv2.8543
H4A···H4E2.1634H24···H9Bviii3.1866
H4A···H4F2.1791H24···H10Cviii3.4249
H4A···H4G2.7034H24···H17viii3.1885
H4B···H4E2.1634H24···H26B2.8758
H4B···H4F2.7036H24···H26C2.4808
H4B···H4G2.1794H25A···O6viii3.3194
H4C···H4H2.2368H25A···C2xi3.0510
H4C···H4I2.2514H25A···C9viii3.5543
H4C···H4J2.7617H25A···H2Axi3.3877
H4D···H4H2.2384H25A···H2Bxi2.4602
H4D···H4I2.7619H25A···H2Cxi2.8835
H4D···H4J2.2499H25A···H9Bviii3.2194
S1···H13Bi3.2034H25A···H10Bviii2.8861
S1···H14Ai3.2546H25A···H12Bxix3.2661
S1···H14Ci3.3983H25A···H12Cxix3.2975
S1···H28Cii3.4759H25B···C2xi3.4306
S2···H7Bii3.0237H25B···C10xii3.0055
S4···H5Ai2.9932H25B···H2Axi3.5015
S4···H5Bi3.5083H25B···H2Bxi2.6585
S4···H23x3.1943H25B···H10Axii2.6381
S5···H18iv2.9490H25B···H10Bxii3.2389
S6···H21iii3.3923H25B···H10Cxii2.6762
S6···H23iii3.1414H25B···H28Aviii3.5568
S7···H2Cii3.2996H25B···H4Exi3.2955
S7···H7Aii3.2294H25B···H4Hxi3.3334
S7···H7Bii2.8786H26A···C2xi2.9966
S7···H8Cii3.3529H26A···C17viii3.5438
S8···H6Ci3.4986H26A···C19viii3.4432
S8···H13Av3.0855H26A···C20viii3.4517
S8···H14Bv3.0751H26A···C22viii3.4868
S8···H14Ci3.0848H26A···H2Axi2.5847
S9···H4Ivi3.3077H26A···H2Bxi2.9086
S10···H8Avii2.9675H26A···H2Cxi2.9995
P1···H21iii3.1759H26A···H9Bviii3.5830
P2···H2Cii3.4451H26A···H10Cxii3.1897
P2···H11Bv3.4255H26A···H17viii3.5352
O1···H12Biv3.3780H26A···H22viii3.4343
O1···H28Cii2.9104H26B···C10xii3.3290
O2···H7Bii3.0842H26B···C17viii3.4767
O3···H17iii2.9130H26B···C19viii3.5897
O3···H21iii2.7702H26B···C20viii3.2312
O4···H17iii3.4859H26B···C21viii3.4303
O4···H21iii2.9537H26B···C22viii3.5617
O4···H22iv3.4800H26B···H5Biv3.3870
O4···H23iii3.4132H26B···H10Axii3.4193
O4···H24iv2.9402H26B···H10Cxii2.4528
O5···H2Cii3.0264H26B···H17viii3.0637
O5···H11Av3.5596H26B···H242.8758
O5···H11Bv2.3830H26C···N23.0003
O6···H2Cii3.4373H26C···C9viii3.2319
O6···H11Bv2.9446H26C···C17viii3.1259
O6···H25Ax3.3194H26C···C243.0682
O7···H4Evi3.4004H26C···H9Bviii2.3416
O7···H4Fvi3.4448H26C···H10Bviii3.4916
O7···H4Gvi2.8015H26C···H17viii2.8398
O7···H4Ivi2.9944H26C···H242.4808
O8···H8Avii3.3022H27A···C14xvii3.5130
O9···H6Biv3.3142H27A···H10Axii3.1581
O9···H10Axii3.5739H27A···H14Axvii2.6815
O9···H10Bviii2.9543H27A···H14Bxvii3.5141
O9···H242.7956H27A···H4Exi3.4585
N2···H9Aviii3.4324H27A···H4Hxi2.8018
N2···H9Bviii2.6407H27B···C12xix3.5788
N2···H10Cviii3.2493H27B···H10Bviii2.9158
N2···H15viii2.7404H27B···H12Bxix3.5573
N2···H17viii2.7812H27B···H12Cxix2.8033
N2···H26C3.0003H27B···H4Fii3.3072
N2···H4Jiv3.5556H27B···H4Hxi3.1365
C1···H7Bii3.5135H28A···C1ii3.5623
C1···H28Aii3.5623H28A···C2ii3.0896
C1···H28Cii3.0206H28A···C10viii3.5244
C2···H12Biv3.4677H28A···H2Aii2.5875
C2···H25Aix3.0510H28A···H2Bii2.8846
C2···H25Bix3.4306H28A···H10Bviii2.8396
C2···H26Aix2.9966H28A···H10Cviii3.3548
C2···H28Aii3.0896H28A···H25Bx3.5568
C2···H28Cii3.2764H28B···C14xvii3.2218
C3···H12Biv3.4984H28B···H2Aii3.0546
C4A···H12Aiii3.4824H28B···H6Biv2.7998
C4A···H12Ciii2.9987H28B···H14Axvii2.6335
C4A···H21iii3.5705H28B···H14Bxvii3.3266
C5···H9Ai3.3584H28B···H14Cxvii3.2106
C5···H23iii3.4274H28C···S1ii3.4759
C6···H14Bxiii3.3045H28C···O1ii2.9104
C6···H22iv3.3176H28C···C1ii3.0206
C6···H24iv3.5677H28C···C2ii3.2764
C7···H2Cii3.5264H28C···H2Aii3.0464
C7···H7Aii3.2370H28C···H2Bii3.2018
C7···H11Bv3.3374H28C···H14Axvii2.9842
C8···H13Av3.3811H28C···H4Aii3.5126
C8···H18ii3.5701H28C···H4Cii3.5341
C9···H5Bi3.3273H4A···H12Biv3.1926
C9···H25Ax3.5543H4A···H28Cii3.5126
C9···H26Cx3.2319H4B···C12iv3.3469
C10···H25Bxiv3.0055H4B···H12Aiv3.0483
C10···H26Bxiv3.3290H4B···H12Biv2.8741
C10···H28Ax3.5244H4C···H12Ciii3.4564
C12···H27Bxv3.5788H4C···H21iii3.5188
C12···H4Biv3.3469H4C···H28Cii3.5341
C12···H4Div3.2737H4D···C12iv3.2737
C12···H4Fvi3.0341H4D···H12Aiv3.1385
C12···H4Gvi3.5485H4D···H12Biv2.5766
C13···H8Avii3.5560H4E···O7iii3.4004
C13···H14Cxiii3.5963H4E···H10Axx3.4652
C14···H6Cxiii3.2438H4E···H10Bxx3.5649
C14···H27Axvi3.5130H4E···H12Ciii2.9933
C14···H28Bxvi3.2218H4E···H25Bix3.2955
C15···H23x3.4464H4E···H27Aix3.4585
C15···H4Gvi3.3235H4F···O7iii3.4448
C15···H4Ivi3.2002H4F···C12iii3.0341
C16···H8Cii3.3807H4F···H12Aiii2.8264
C17···H26Ax3.5438H4F···H12Ciii2.4081
C17···H26Bx3.4767H4F···H21iii3.0214
C17···H26Cx3.1259H4F···H27Bii3.3072
C17···H4Gvi3.2354H4G···O7iii2.8015
C17···H4Ivi3.2663H4G···C12iii3.5485
C18···H8Cii3.1537H4G···C15iii3.3235
C19···H26Ax3.4432H4G···C17iii3.2354
C19···H26Bx3.5897H4G···H12Aiii3.3149
C20···H26Ax3.4517H4G···H12Ciii3.1346
C20···H26Bx3.2312H4G···H15iii3.2644
C21···H26Bx3.4303H4G···H17iii3.0989
C21···H4Jiv3.2046H4G···H21iii3.5283
C22···H6Biv3.4593H4H···C27ix3.4177
C22···H26Ax3.4868H4H···H25Bix3.3334
C22···H26Bx3.5617H4H···H27Aix2.8018
C23···H5Bvi3.2909H4H···H27Bix3.1365
C23···H9Bviii3.4323H4I···S9iii3.3077
C23···H15viii2.9484H4I···O7iii2.9944
C23···H4Jiv3.0201H4I···C15iii3.2002
C24···H6Biv3.4818H4I···C17iii3.2663
C24···H9Bviii3.1914H4I···H15iii2.9924
C24···H10Cviii3.2106H4I···H17iii3.0996
C24···H17viii3.2904H4J···N2iv3.5556
C24···H26C3.0682H4J···C21iv3.2046
C25···H2Bxi2.9110H4J···C23iv3.0201
C25···H2Cxi3.5350H4J···H12Aiv3.3231
C25···H9Bviii3.5346H4J···H12Biv3.5966
C25···H10Axii3.3903H4J···H15iii3.5197
C25···H10Bviii3.3501H4J···H21iv3.3398
C25···H10Cxii3.2431H4J···H23iv3.0345
C25···H243.4865
Mo1—Mo2—Mo360.634 (13)N1—C15—C17123.6 (4)
Mo1—Mo2—S154.13 (3)N1—C16—C18123.1 (4)
Mo1—Mo2—S255.11 (3)C15—C17—C19119.5 (4)
Mo1—Mo2—S398.60 (3)C16—C18—C19120.1 (4)
Mo1—Mo2—S5138.34 (3)C17—C19—C18117.1 (4)
Mo1—Mo2—S6139.16 (3)C17—C19—C20120.8 (4)
Mo1—Mo2—O183.95 (7)C18—C19—C20122.1 (4)
Mo3—Mo2—S197.42 (3)C19—C20—C21121.4 (4)
Mo3—Mo2—S253.71 (3)C19—C20—C22121.2 (4)
Mo3—Mo2—S353.05 (3)C21—C20—C22117.4 (4)
Mo3—Mo2—S5103.14 (3)C20—C21—C23119.0 (4)
Mo3—Mo2—S6142.74 (3)C20—C22—C24118.9 (4)
Mo3—Mo2—O1132.60 (7)N2—C23—C21124.8 (5)
S1—Mo2—S2108.58 (4)N2—C24—C22124.1 (4)
S1—Mo2—S393.14 (4)O9—C25—C26108.4 (6)
S1—Mo2—S5159.43 (4)O9—C27—C28105.3 (8)
S1—Mo2—S685.71 (4)C1—C2—H2A109.469
S1—Mo2—O183.75 (9)C1—C2—H2B109.470
S2—Mo2—S3105.28 (4)C1—C2—H2C109.476
S2—Mo2—S583.91 (4)H2A—C2—H2B109.470
S2—Mo2—S6158.23 (4)H2A—C2—H2C109.479
S2—Mo2—O180.83 (8)H2B—C2—H2C109.462
S3—Mo2—S599.32 (4)O3—C3—H4A108.998
S3—Mo2—S689.77 (3)O3—C3—H4B108.979
S3—Mo2—O1173.80 (8)O3—C3—H4C109.217
S5—Mo2—S678.09 (4)O3—C3—H4D109.218
S5—Mo2—O182.21 (9)C4A—C3—H4A108.975
S6—Mo2—O184.66 (7)C4A—C3—H4B108.979
Mo2—Mo1—Mo360.919 (13)C4B—C3—H4C109.203
Mo2—Mo1—S154.12 (3)C4B—C3—H4D109.211
Mo2—Mo1—S254.73 (3)H4A—C3—H4B107.773
Mo2—Mo1—S499.98 (3)H4C—C3—H4D107.903
Mo2—Mo1—S7141.85 (3)C3—C4A—H4E109.471
Mo2—Mo1—S8136.97 (3)C3—C4A—H4F109.474
Mo2—Mo1—O285.23 (8)C3—C4A—H4G109.473
Mo3—Mo1—S197.63 (3)H4E—C4A—H4F109.471
Mo3—Mo1—S253.74 (3)H4E—C4A—H4G109.468
Mo3—Mo1—S453.17 (3)H4F—C4A—H4G109.470
Mo3—Mo1—S7103.32 (3)C3—C4B—H4H109.468
Mo3—Mo1—S8142.84 (3)C3—C4B—H4I109.477
Mo3—Mo1—O2133.25 (9)C3—C4B—H4J109.470
S1—Mo1—S2108.20 (4)H4H—C4B—H4I109.470
S1—Mo1—S494.82 (3)H4H—C4B—H4J109.468
S1—Mo1—S7158.72 (4)H4I—C4B—H4J109.473
S1—Mo1—S883.51 (4)O4—C5—H5A108.557
S1—Mo1—O285.12 (8)O4—C5—H5B108.563
S2—Mo1—S4105.17 (4)C6—C5—H5A108.557
S2—Mo1—S787.51 (4)C6—C5—H5B108.561
S2—Mo1—S8159.85 (3)H5A—C5—H5B107.550
S2—Mo1—O280.93 (9)C5—C6—H6A109.482
S4—Mo1—S794.73 (4)C5—C6—H6B109.466
S4—Mo1—S889.67 (4)C5—C6—H6C109.472
S4—Mo1—O2173.54 (9)H6A—C6—H6B109.464
S7—Mo1—S877.57 (4)H6A—C6—H6C109.469
S7—Mo1—O283.29 (7)H6B—C6—H6C109.474
S8—Mo1—O283.91 (9)O5—C7—H7A109.431
Mo2—Mo3—Mo158.447 (11)O5—C7—H7B109.426
Mo2—Mo3—S253.81 (3)C8—C7—H7A109.435
Mo2—Mo3—S353.17 (3)C8—C7—H7B109.437
Mo2—Mo3—S498.06 (3)H7A—C7—H7B108.034
Mo2—Mo3—S9141.49 (3)C7—C8—H8A109.485
Mo2—Mo3—S1099.71 (3)C7—C8—H8B109.480
Mo2—Mo3—N1136.32 (7)C7—C8—H8C109.469
Mo1—Mo3—S254.21 (3)H8A—C8—H8B109.472
Mo1—Mo3—S396.97 (3)H8A—C8—H8C109.453
Mo1—Mo3—S453.24 (3)H8B—C8—H8C109.469
Mo1—Mo3—S9139.74 (3)O6—C9—H9A109.657
Mo1—Mo3—S10141.15 (3)O6—C9—H9B109.669
Mo1—Mo3—N194.15 (8)C10—C9—H9A109.670
S2—Mo3—S3105.49 (4)C10—C9—H9B109.662
S2—Mo3—S4105.68 (4)H9A—C9—H9B108.176
S2—Mo3—S9159.97 (4)C9—C10—H10A109.481
S2—Mo3—S1086.97 (4)C9—C10—H10B109.483
S2—Mo3—N182.79 (8)C9—C10—H10C109.474
S3—Mo3—S496.75 (4)H10A—C10—H10B109.465
S3—Mo3—S988.35 (3)H10A—C10—H10C109.461
S3—Mo3—S1091.91 (4)H10B—C10—H10C109.464
S3—Mo3—N1168.68 (8)O7—C11—H11A109.893
S4—Mo3—S986.53 (4)O7—C11—H11B109.888
S4—Mo3—S10162.05 (4)C12—C11—H11A109.884
S4—Mo3—N188.20 (9)C12—C11—H11B109.887
S9—Mo3—S1078.00 (4)H11A—C11—H11B108.302
S9—Mo3—N181.78 (8)C11—C12—H12A109.462
S10—Mo3—N180.68 (9)C11—C12—H12B109.471
Mo2—S1—Mo171.76 (3)C11—C12—H12C109.464
Mo2—S2—Mo170.16 (3)H12A—C12—H12B109.476
Mo2—S2—Mo372.47 (3)H12A—C12—H12C109.477
Mo1—S2—Mo372.05 (3)H12B—C12—H12C109.477
Mo2—S3—Mo373.78 (3)O8—C13—H13A109.952
Mo1—S4—Mo373.59 (3)O8—C13—H13B109.941
Mo2—S5—P187.83 (6)C14—C13—H13A109.942
Mo2—S6—P187.03 (5)C14—C13—H13B109.938
Mo1—S7—P287.81 (5)H13A—C13—H13B108.342
Mo1—S8—P287.94 (6)C13—C14—H14A109.474
Mo3—S9—P386.07 (5)C13—C14—H14B109.477
Mo3—S10—P386.00 (6)C13—C14—H14C109.471
S5—P1—S6106.85 (7)H14A—C14—H14B109.467
S5—P1—O3112.41 (13)H14A—C14—H14C109.465
S5—P1—O4113.48 (14)H14B—C14—H14C109.474
S6—P1—O3113.57 (16)N1—C15—H15118.190
S6—P1—O4114.14 (13)C17—C15—H15118.198
O3—P1—O496.40 (17)N1—C16—H16118.428
S7—P2—S8106.38 (7)C18—C16—H16118.430
S7—P2—O5112.85 (15)C15—C17—H17120.245
S7—P2—O6113.51 (15)C19—C17—H17120.233
S8—P2—O5114.71 (14)C16—C18—H18119.959
S8—P2—O6113.61 (14)C19—C18—H18119.951
O5—P2—O695.87 (16)C20—C21—H21120.488
S9—P3—S10107.94 (7)C23—C21—H21120.495
S9—P3—O7109.43 (14)C20—C22—H22120.555
S9—P3—O8113.24 (13)C24—C22—H22120.546
S10—P3—O7112.49 (12)N2—C23—H23117.622
S10—P3—O8111.92 (13)C21—C23—H23117.625
O7—P3—O8101.80 (17)N2—C24—H24117.965
Mo2—O1—C1122.2 (3)C22—C24—H24117.978
Mo1—O2—C1122.4 (3)O9—C25—H25A110.009
P1—O3—C3118.5 (3)O9—C25—H25B110.010
P1—O4—C5120.8 (3)C26—C25—H25A110.003
P2—O5—C7122.5 (3)C26—C25—H25B110.012
P2—O6—C9119.7 (3)H25A—C25—H25B108.368
P3—O7—C11121.1 (3)C25—C26—H26A109.471
P3—O8—C13120.0 (3)C25—C26—H26B109.467
C25—O9—C27110.9 (6)C25—C26—H26C109.468
Mo3—N1—C15120.8 (3)H26A—C26—H26B109.475
Mo3—N1—C16122.7 (3)H26A—C26—H26C109.474
C15—N1—C16116.5 (3)H26B—C26—H26C109.472
C23—N2—C24115.8 (4)O9—C27—H27A110.693
O1—C1—O2126.1 (4)O9—C27—H27B110.669
O1—C1—C2117.2 (4)C28—C27—H27A110.702
O2—C1—C2116.6 (4)C28—C27—H27B110.678
O3—C3—C4A113.0 (13)H27A—C27—H27B108.793
O3—C3—C4B112.0 (7)C27—C28—H28A109.477
O4—C5—C6114.8 (6)C27—C28—H28B109.468
O5—C7—C8111.0 (5)C27—C28—H28C109.474
O6—C9—C10110.0 (5)H28A—C28—H28B109.480
O7—C11—C12109.0 (5)H28A—C28—H28C109.477
O8—C13—C14108.7 (4)H28B—C28—H28C109.451
Mo1—Mo2—Mo3—Mo10.0S4—Mo1—Mo3—S10−164.92 (4)
Mo1—Mo2—Mo3—S2−66.4S4—Mo1—Mo3—N1−84.64 (3)
Mo1—Mo2—Mo3—S3129.640 (14)Mo3—Mo1—S7—P2−145.52 (3)
Mo1—Mo2—Mo3—S437.218 (11)S7—Mo1—Mo3—Mo2−142.47 (3)
Mo1—Mo2—Mo3—S9131.80 (3)S7—Mo1—Mo3—S2−76.76 (3)
Mo1—Mo2—Mo3—S10−145.299 (13)S7—Mo1—Mo3—S3179.15 (3)
Mo1—Mo2—Mo3—N1−58.68 (14)S7—Mo1—Mo3—S485.91 (3)
Mo3—Mo2—Mo1—Mo30.0S7—Mo1—Mo3—S983.44 (4)
Mo3—Mo2—Mo1—S1−126.147 (12)S7—Mo1—Mo3—S10−79.01 (4)
Mo3—Mo2—Mo1—S264.2S7—Mo1—Mo3—N11.27 (3)
Mo3—Mo2—Mo1—S4−37.414 (12)Mo3—Mo1—S8—P299.41 (4)
Mo3—Mo2—Mo1—S773.66 (2)S8—Mo1—Mo3—Mo2130.62 (5)
Mo3—Mo2—Mo1—S8−137.777 (19)S8—Mo1—Mo3—S2−163.68 (5)
Mo3—Mo2—Mo1—O2146.435 (14)S8—Mo1—Mo3—S392.23 (5)
Mo1—Mo2—S1—Mo10.0S8—Mo1—Mo3—S4−1.01 (5)
S1—Mo2—Mo1—Mo3126.15 (3)S8—Mo1—Mo3—S9−3.48 (5)
S1—Mo2—Mo1—S10.00 (3)S8—Mo1—Mo3—S10−165.92 (4)
S1—Mo2—Mo1—S2−169.67 (3)S8—Mo1—Mo3—N1−85.64 (5)
S1—Mo2—Mo1—S488.73 (3)Mo3—Mo1—O2—C141.1 (3)
S1—Mo2—Mo1—S7−160.19 (4)O2—Mo1—Mo3—Mo2−49.16 (10)
S1—Mo2—Mo1—S8−11.63 (3)O2—Mo1—Mo3—S216.55 (10)
S1—Mo2—Mo1—O2−87.42 (3)O2—Mo1—Mo3—S3−87.54 (10)
Mo1—Mo2—S2—Mo1−0.0O2—Mo1—Mo3—S4179.22 (10)
Mo1—Mo2—S2—Mo376.72 (3)O2—Mo1—Mo3—S9176.75 (10)
S2—Mo2—Mo1—Mo3−64.18 (3)O2—Mo1—Mo3—S1014.31 (10)
S2—Mo2—Mo1—S1169.67 (3)O2—Mo1—Mo3—N194.58 (10)
S2—Mo2—Mo1—S2−0.00 (3)S1—Mo1—S2—Mo2−8.80 (3)
S2—Mo2—Mo1—S4−101.59 (3)S1—Mo1—S2—Mo3−86.11 (3)
S2—Mo2—Mo1—S79.48 (3)S2—Mo1—S1—Mo28.86 (3)
S2—Mo2—Mo1—S8158.04 (3)S1—Mo1—S4—Mo395.93 (3)
S2—Mo2—Mo1—O282.25 (3)S4—Mo1—S1—Mo2−98.84 (3)
Mo1—Mo2—S3—Mo3−42.75 (3)S1—Mo1—S7—P224.12 (11)
S3—Mo2—Mo1—Mo338.49 (3)S7—Mo1—S1—Mo2144.77 (9)
S3—Mo2—Mo1—S1−87.65 (3)S1—Mo1—S8—P2−166.51 (4)
S3—Mo2—Mo1—S2102.67 (3)S8—Mo1—S1—Mo2172.04 (3)
S3—Mo2—Mo1—S41.08 (3)S1—Mo1—O2—C1−54.8 (2)
S3—Mo2—Mo1—S7112.16 (4)O2—Mo1—S1—Mo287.64 (9)
S3—Mo2—Mo1—S8−99.28 (3)S2—Mo1—S4—Mo3−14.41 (3)
S3—Mo2—Mo1—O2−175.07 (3)S4—Mo1—S2—Mo291.62 (3)
Mo1—Mo2—S5—P1−160.76 (2)S4—Mo1—S2—Mo314.30 (3)
S5—Mo2—Mo1—Mo3−76.12 (4)S2—Mo1—S7—P2162.70 (4)
S5—Mo2—Mo1—S1157.73 (5)S7—Mo1—S2—Mo2−174.15 (3)
S5—Mo2—Mo1—S2−11.94 (4)S7—Mo1—S2—Mo3108.53 (3)
S5—Mo2—Mo1—S4−113.54 (4)S2—Mo1—S8—P2−39.45 (12)
S5—Mo2—Mo1—S7−2.46 (5)S8—Mo1—S2—Mo2−132.21 (10)
S5—Mo2—Mo1—S8146.10 (4)S8—Mo1—S2—Mo3150.47 (10)
S5—Mo2—Mo1—O270.31 (5)S2—Mo1—O2—C154.5 (2)
Mo1—Mo2—S6—P1160.39 (2)O2—Mo1—S2—Mo2−90.56 (7)
S6—Mo2—Mo1—Mo3138.21 (4)O2—Mo1—S2—Mo3−167.87 (7)
S6—Mo2—Mo1—S112.06 (4)S4—Mo1—S7—P2−92.28 (4)
S6—Mo2—Mo1—S2−157.61 (4)S7—Mo1—S4—Mo3−103.11 (4)
S6—Mo2—Mo1—S4100.79 (4)S4—Mo1—S8—P298.61 (4)
S6—Mo2—Mo1—S7−148.13 (4)S8—Mo1—S4—Mo3179.39 (3)
S6—Mo2—Mo1—S80.43 (5)S7—Mo1—S8—P23.69 (4)
S6—Mo2—Mo1—O2−75.36 (4)S8—Mo1—S7—P2−3.67 (4)
Mo1—Mo2—O1—C12.5 (2)S7—Mo1—O2—C1143.1 (3)
O1—Mo2—Mo1—Mo3−147.21 (8)O2—Mo1—S7—P281.54 (9)
O1—Mo2—Mo1—S186.64 (8)S8—Mo1—O2—C1−138.8 (3)
O1—Mo2—Mo1—S2−83.03 (8)O2—Mo1—S8—P2−80.75 (8)
O1—Mo2—Mo1—S4175.38 (8)Mo2—Mo3—S2—Mo2−0.0
O1—Mo2—Mo1—S7−73.55 (8)Mo2—Mo3—S2—Mo174.22 (3)
O1—Mo2—Mo1—S875.01 (8)Mo2—Mo3—S3—Mo2−0.0
O1—Mo2—Mo1—O2−0.77 (8)Mo2—Mo3—S4—Mo1−40.044 (19)
Mo3—Mo2—S1—Mo145.210 (18)Mo2—Mo3—S9—P399.86 (5)
S1—Mo2—Mo3—Mo1−41.29 (2)Mo2—Mo3—S10—P3−150.03 (3)
S1—Mo2—Mo3—S2−107.64 (3)Mo2—Mo3—N1—C15135.42 (15)
S1—Mo2—Mo3—S388.35 (3)Mo2—Mo3—N1—C16−45.2 (3)
S1—Mo2—Mo3—S4−4.07 (3)Mo1—Mo3—S2—Mo2−74.22 (3)
S1—Mo2—Mo3—S990.51 (3)Mo1—Mo3—S2—Mo10.0
S1—Mo2—Mo3—S10173.41 (2)Mo1—Mo3—S3—Mo241.38 (3)
S1—Mo2—Mo3—N1−99.95 (3)Mo1—Mo3—S4—Mo10.0
Mo3—Mo2—S2—Mo1−76.72 (3)Mo1—Mo3—S9—P3−159.56 (3)
Mo3—Mo2—S2—Mo3−0.0Mo1—Mo3—S10—P3159.31 (3)
S2—Mo2—Mo3—Mo166.35 (3)Mo1—Mo3—N1—C1588.5 (2)
S2—Mo2—Mo3—S20.00 (3)Mo1—Mo3—N1—C16−92.0 (2)
S2—Mo2—Mo3—S3−164.01 (4)S2—Mo3—S3—Mo2−13.34 (4)
S2—Mo2—Mo3—S4103.57 (4)S3—Mo3—S2—Mo213.23 (4)
S2—Mo2—Mo3—S9−161.84 (4)S3—Mo3—S2—Mo187.45 (4)
S2—Mo2—Mo3—S10−78.95 (4)S2—Mo3—S4—Mo114.53 (3)
S2—Mo2—Mo3—N17.69 (4)S4—Mo3—S2—Mo2−88.57 (3)
Mo3—Mo2—S3—Mo3−0.0S4—Mo3—S2—Mo1−14.35 (3)
S3—Mo2—Mo3—Mo1−129.64 (4)S2—Mo3—S9—P3−32.90 (11)
S3—Mo2—Mo3—S2164.01 (4)S9—Mo3—S2—Mo2145.50 (9)
S3—Mo2—Mo3—S30.00 (4)S9—Mo3—S2—Mo1−140.28 (9)
S3—Mo2—Mo3—S4−92.42 (4)S2—Mo3—S10—P3157.48 (4)
S3—Mo2—Mo3—S92.16 (4)S10—Mo3—S2—Mo2104.37 (3)
S3—Mo2—Mo3—S1085.06 (4)S10—Mo3—S2—Mo1178.59 (3)
S3—Mo2—Mo3—N1171.70 (4)S2—Mo3—N1—C15141.7 (3)
Mo3—Mo2—S5—P1138.91 (3)S2—Mo3—N1—C16−38.9 (2)
S5—Mo2—Mo3—Mo1138.50 (3)N1—Mo3—S2—Mo2−174.66 (9)
S5—Mo2—Mo3—S272.14 (3)N1—Mo3—S2—Mo1−100.43 (9)
S5—Mo2—Mo3—S3−91.86 (3)S3—Mo3—S4—Mo1−93.68 (3)
S5—Mo2—Mo3—S4175.71 (3)S4—Mo3—S3—Mo295.04 (3)
S5—Mo2—Mo3—S9−89.70 (4)S3—Mo3—S9—P3101.59 (4)
S5—Mo2—Mo3—S10−6.80 (3)S9—Mo3—S3—Mo2−178.65 (4)
S5—Mo2—Mo3—N179.83 (3)S3—Mo3—S10—P3−97.10 (4)
Mo3—Mo2—S6—P1−93.21 (5)S10—Mo3—S3—Mo2−100.72 (3)
S6—Mo2—Mo3—Mo1−133.96 (5)S4—Mo3—S9—P3−161.54 (4)
S6—Mo2—Mo3—S2159.68 (5)S9—Mo3—S4—Mo1178.40 (3)
S6—Mo2—Mo3—S3−4.32 (5)S4—Mo3—N1—C1535.6 (2)
S6—Mo2—Mo3—S4−96.75 (5)S4—Mo3—N1—C16−145.0 (2)
S6—Mo2—Mo3—S9−2.16 (6)N1—Mo3—S4—Mo196.53 (7)
S6—Mo2—Mo3—S1080.74 (5)S9—Mo3—S10—P3−9.20 (3)
S6—Mo2—Mo3—N1167.37 (5)S10—Mo3—S9—P39.29 (3)
Mo3—Mo2—O1—C1−37.4 (3)S9—Mo3—N1—C15−51.1 (2)
O1—Mo2—Mo3—Mo147.02 (11)S9—Mo3—N1—C16128.3 (3)
O1—Mo2—Mo3—S2−19.33 (11)N1—Mo3—S9—P3−72.85 (9)
O1—Mo2—Mo3—S3176.66 (11)S10—Mo3—N1—C15−130.2 (2)
O1—Mo2—Mo3—S484.24 (11)S10—Mo3—N1—C1649.2 (2)
O1—Mo2—Mo3—S9178.83 (11)N1—Mo3—S10—P374.30 (8)
O1—Mo2—Mo3—S10−98.28 (11)Mo2—S5—P1—S63.82 (5)
O1—Mo2—Mo3—N1−11.64 (12)Mo2—S5—P1—O3129.05 (7)
S1—Mo2—S2—Mo18.82 (3)Mo2—S5—P1—O4−122.87 (6)
S1—Mo2—S2—Mo385.54 (4)Mo2—S6—P1—S5−3.77 (5)
S2—Mo2—S1—Mo1−8.93 (3)Mo2—S6—P1—O3−128.29 (6)
S1—Mo2—S3—Mo3−96.93 (3)Mo2—S6—P1—O4122.52 (7)
S3—Mo2—S1—Mo198.35 (3)Mo1—S7—P2—S84.79 (5)
S1—Mo2—S5—P1−41.69 (10)Mo1—S7—P2—O5−121.83 (6)
S5—Mo2—S1—Mo1−134.19 (8)Mo1—S7—P2—O6130.45 (6)
S1—Mo2—S6—P1170.16 (4)Mo1—S8—P2—S7−4.78 (5)
S6—Mo2—S1—Mo1−172.13 (3)Mo1—S8—P2—O5120.71 (7)
S1—Mo2—O1—C157.0 (2)Mo1—S8—P2—O6−130.39 (6)
O1—Mo2—S1—Mo1−87.04 (7)Mo3—S9—P3—S10−12.23 (5)
S2—Mo2—S3—Mo313.31 (4)Mo3—S9—P3—O7110.50 (5)
S3—Mo2—S2—Mo1−89.92 (4)Mo3—S9—P3—O8−136.70 (6)
S3—Mo2—S2—Mo3−13.19 (4)Mo3—S10—P3—S912.29 (5)
S2—Mo2—S5—P1−170.59 (4)Mo3—S10—P3—O7−108.55 (7)
S5—Mo2—S2—Mo1172.05 (3)Mo3—S10—P3—O8137.56 (6)
S5—Mo2—S2—Mo3−111.23 (4)S5—P1—O3—C3−60.3 (3)
S2—Mo2—S6—P137.79 (11)S5—P1—O4—C569.4 (3)
S6—Mo2—S2—Mo1137.81 (9)S6—P1—O3—C361.1 (3)
S6—Mo2—S2—Mo3−145.47 (9)S6—P1—O4—C5−53.4 (3)
S2—Mo2—O1—C1−53.1 (2)O3—P1—O4—C5−172.8 (3)
O1—Mo2—S2—Mo188.99 (8)O4—P1—O3—C3−179.0 (3)
O1—Mo2—S2—Mo3165.71 (9)S7—P2—O5—C752.4 (3)
S3—Mo2—S5—P184.87 (4)S7—P2—O6—C9−66.6 (3)
S5—Mo2—S3—Mo399.49 (4)S8—P2—O5—C7−69.6 (3)
S3—Mo2—S6—P1−96.67 (4)S8—P2—O6—C955.2 (3)
S6—Mo2—S3—Mo3177.38 (4)O5—P2—O6—C9175.4 (3)
S5—Mo2—S6—P12.92 (4)O6—P2—O5—C7171.0 (3)
S6—Mo2—S5—P1−2.90 (4)S9—P3—O7—C11−171.99 (16)
S5—Mo2—O1—C1−138.1 (3)S9—P3—O8—C1357.4 (3)
O1—Mo2—S5—P1−89.05 (8)S10—P3—O7—C11−52.0 (3)
S6—Mo2—O1—C1143.2 (3)S10—P3—O8—C13−64.9 (3)
O1—Mo2—S6—P186.06 (9)O7—P3—O8—C13174.8 (3)
Mo2—Mo1—Mo3—Mo20.0O8—P3—O7—C1167.9 (3)
Mo2—Mo1—Mo3—S265.706 (11)Mo2—O1—C1—O2−3.8 (6)
Mo2—Mo1—Mo3—S3−38.384 (11)Mo2—O1—C1—C2173.5 (2)
Mo2—Mo1—Mo3—S4−131.623 (14)Mo1—O2—C1—O12.8 (6)
Mo2—Mo1—Mo3—S9−134.09 (3)Mo1—O2—C1—C2−174.6 (2)
Mo2—Mo1—Mo3—S1063.46 (2)P1—O3—C3—C4A−130.7 (4)
Mo2—Mo1—Mo3—N1143.738 (14)P1—O3—C3—C4B163.3 (4)
Mo2—Mo1—S1—Mo20.0P1—O4—C5—C6−106.7 (4)
Mo2—Mo1—S2—Mo2−0.0P2—O5—C7—C8100.0 (4)
Mo2—Mo1—S2—Mo3−77.31 (2)P2—O6—C9—C10−158.5 (3)
Mo2—Mo1—S4—Mo341.55 (3)P3—O7—C11—C12−174.7 (2)
Mo2—Mo1—S7—P2154.96 (3)P3—O8—C13—C14−122.1 (3)
Mo2—Mo1—S8—P2−157.05 (2)C25—O9—C27—C28−170.2 (6)
Mo2—Mo1—O2—C1−0.5 (2)C27—O9—C25—C26−176.0 (6)
Mo3—Mo1—S1—Mo2−45.398 (19)Mo3—N1—C15—C17176.6 (3)
S1—Mo1—Mo3—Mo241.31 (3)Mo3—N1—C16—C18−177.8 (2)
S1—Mo1—Mo3—S2107.01 (3)C15—N1—C16—C181.6 (5)
S1—Mo1—Mo3—S32.92 (3)C16—N1—C15—C17−2.8 (6)
S1—Mo1—Mo3—S4−90.32 (3)C23—N2—C24—C220.1 (8)
S1—Mo1—Mo3—S9−92.79 (3)C24—N2—C23—C210.2 (9)
S1—Mo1—Mo3—S10104.77 (3)N1—C15—C17—C192.0 (6)
S1—Mo1—Mo3—N1−174.95 (3)N1—C16—C18—C190.4 (6)
Mo3—Mo1—S2—Mo277.31 (2)C15—C17—C19—C180.1 (6)
Mo3—Mo1—S2—Mo30.0C15—C17—C19—C20−179.4 (4)
S2—Mo1—Mo3—Mo2−65.71 (3)C16—C18—C19—C17−1.2 (6)
S2—Mo1—Mo3—S20.00 (3)C16—C18—C19—C20178.3 (4)
S2—Mo1—Mo3—S3−104.09 (3)C17—C19—C20—C2136.6 (6)
S2—Mo1—Mo3—S4162.67 (3)C17—C19—C20—C22−143.4 (4)
S2—Mo1—Mo3—S9160.20 (4)C18—C19—C20—C21−142.9 (4)
S2—Mo1—Mo3—S10−2.24 (3)C18—C19—C20—C2237.1 (6)
S2—Mo1—Mo3—N178.03 (3)C19—C20—C21—C23−179.4 (4)
Mo3—Mo1—S4—Mo30.0C19—C20—C22—C24179.6 (4)
S4—Mo1—Mo3—Mo2131.62 (3)C21—C20—C22—C24−0.3 (7)
S4—Mo1—Mo3—S2−162.67 (3)C22—C20—C21—C230.6 (7)
S4—Mo1—Mo3—S393.24 (3)C20—C21—C23—N2−0.6 (9)
S4—Mo1—Mo3—S40.00 (3)C20—C22—C24—N2−0.0 (8)
S4—Mo1—Mo3—S9−2.47 (3)
Symmetry codes: (i) −x, −y, −z; (ii) −x+1, −y, −z+1; (iii) −x, y−1/2, −z+1/2; (iv) −x, −y, −z+1; (v) x+1, y, z; (vi) −x, y+1/2, −z+1/2; (vii) x−1, y, z; (viii) x, −y+1/2, z+1/2; (ix) −x+1, y−1/2, −z+3/2; (x) x, −y+1/2, z−1/2; (xi) −x+1, y+1/2, −z+3/2; (xii) x, y, z+1; (xiii) −x−1, −y, −z; (xiv) x, y, z−1; (xv) x−1, −y+1/2, z−1/2; (xvi) x−1, y, z−1; (xvii) x+1, y, z+1; (xviii) −x+1, y+1/2, −z+1/2; (xix) x+1, −y+1/2, z+1/2; (xx) −x+1, y−1/2, −z+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C11—H11B···O5vii0.992.383.335 (7)161
Symmetry code: (vii) x−1, y, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C11—H11B···O5i0.992.383.335 (7)161
Symmetry code: (i) x−1, y, z.
 

Acknowledgements

We thank Professor Takashi Shibahara of Okayama University of Science and Professor Kiyoshi Isobe of Osaka City University for helpful discussions and suggestions regarding the preparation of [Mo3S4(H2O)9]4+.

References

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 First citationYao, Y., Akashi, H., Sakane, G., Shibahara, T. & Ohtaki, H. (1995). Inorg. Chem. 34, 42–48.  CSD CrossRef CAS Web of Science Google Scholar

This is an open-access article distributed under the terms of the Creative Commons Attribution (CC-BY) Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890
Volume 70| Part 7| July 2014| Pages m240-m241
https://doi.org/10.1107/S1600536814012501
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