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The title compound, [(C2H5)4N][Mo3Cl6O(C2H3O2)3], has been synthesized by the reaction of MoCl3·3H2O with CH3COOH. The structure is a polymorph of the structure reported by Chen, Lu, Huang, Huang & Huang [Chin. J. Struct. Chem. (1993). 12, 117–123]. The crystal contains discrete cations and anions. The mono-oxo-capped trinuclear Mo cluster anion consists of three Cl atoms and three acetate groups that bridge the three edges of the Mo triangle; each Mo atom is also coordinated by one terminal Cl atom. The coordination around Mo is a distorted octahedron.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802013892/bt6175sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536802013892/bt6175Isup2.hkl
Contains datablock I

CCDC reference: 197452

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.020 Å
  • R factor = 0.071
  • wR factor = 0.157
  • Data-to-parameter ratio = 17.5

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry








Comment top

A series of trinuclear Mo3 cluster compounds with the cluster anions {[Mo33-O)(µ-X)3(µ-O2R)3X3] (R = H, –CH3, –C2H5, X = Cl, Br)} have been synthesized and structurally characterized (Cotton et al., 1991a,b; Zhuang et al., 1985, 1996; Chen et al., 1993; Wu et al., 1984; Lin & Chen, 1988). As an extension of these works, we here report the synthesis and crystal structure of the title compound, (I), which was synthesized in a similar way to that described by Chen et al. (1993). However, the two crystal structures are polymorphs.

A view of the structure of (I) is shown in Fig. 1. The three Mo atoms of the cluster anion form an approximately equilateral triangle. On the side of the Mo3 plane, one µ3-O atom binds the three Mo atoms together to form an Mo3O mono-capped cluster skeleton. The three acetate (Ac) ligands and the µ3-O atom are situated on the same side of the plane. In addition, three terminal Cl atoms and three bridging Cl atoms are situated on the other side of the Mo3 plane. Each unit cell consists of four formula units of [Et4N][Mo3OCl6(Ac)3], which are discrete ions. The synthetic route and chemical composition of the title complex is identical to that of the complex reported by Chen et al. (1993). However, both structures are polymorphs. This reflects the diversity of crystal packing of this series of trinuclear Mo cluster compounds. The formal oxidation state of the Mo atoms is 3.33, so that the Mo3 core possesses eight electrons to form three metal–metal bonds. The average Mo—Mo distance [2.5778 (14) Å] is consistent with an eight-electron system.

Experimental top

A mixture of 5.2 g (20 mmol) of MoCl3·3H2O in 40 ml of acetic acid was refluxed at 353 K for 2 h. After cooling, 40 ml of ethanol saturated by HCl and 2.0 g (7.8 mmol) of (Et)4NI was added and the mixture was stirred for 1 h. Several days later, crude crystals precipitated. On recrystallization from CH2Cl2, black single crystals were obtained.

Refinement top

H atoms were all set to calculated positions and not refined.

Computing details top

Data collection: SMART (Siemens, 1995); cell refinement: SAINT (Siemens, 1995); data reduction: XPREP (Sheldrick, 1991); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP (Sheldrick, 1991); software used to prepare material for publication: SHELXL97.

Figures top
[Figure 1] Fig. 1. A view of the structure of the title compound, showing 30% probability displacement ellipsoids. H atoms have been omitted for clarity.
(I) top
Crystal data top
(C2H5N)[Mo3Cl6O(C2H3O2)3]Z = 4
Mr = 823.90F(000) = 1616
Triclinic, P1Dx = 1.972 Mg m3
a = 7.9356 (1) ÅMo Kα radiation, λ = 0.71073 Å
b = 14.4258 (1) ÅCell parameters from 6220 reflections
c = 24.4415 (4) Åθ = 0.8–25.1°
α = 96.613 (1)°µ = 1.95 mm1
β = 92.518 (1)°T = 293 K
γ = 91.815 (1)°Prism, black
V = 2774.80 (6) Å30.84 × 0.20 × 0.02 mm
Data collection top
Siemens SMART CCD
diffractometer
9771 independent reflections
Radiation source: fine-focus sealed tube7292 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.041
ϕ and ω scansθmax = 25.1°, θmin = 0.8°
Absorption correction: empirical (using intensity measurements)
(SADABS; Sheldrick, 1996)
h = 99
Tmin = 0.680, Tmax = 1.000k = 1517
14579 measured reflectionsl = 2926
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)] = 0.071Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.157H-atom parameters constrained
S = 1.07 w = 1/[σ2(Fo2) + 55.1956P]
where P = (Fo2 + 2Fc2)/3
9771 reflections(Δ/σ)max = 0.005
559 parametersΔρmax = 0.80 e Å3
0 restraintsΔρmin = 0.81 e Å3
Crystal data top
(C2H5N)[Mo3Cl6O(C2H3O2)3]γ = 91.815 (1)°
Mr = 823.90V = 2774.80 (6) Å3
Triclinic, P1Z = 4
a = 7.9356 (1) ÅMo Kα radiation
b = 14.4258 (1) ŵ = 1.95 mm1
c = 24.4415 (4) ÅT = 293 K
α = 96.613 (1)°0.84 × 0.20 × 0.02 mm
β = 92.518 (1)°
Data collection top
Siemens SMART CCD
diffractometer
9771 independent reflections
Absorption correction: empirical (using intensity measurements)
(SADABS; Sheldrick, 1996)
7292 reflections with I > 2σ(I)
Tmin = 0.680, Tmax = 1.000Rint = 0.041
14579 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0710 restraints
wR(F2) = 0.157H-atom parameters constrained
S = 1.07 w = 1/[σ2(Fo2) + 55.1956P]
where P = (Fo2 + 2Fc2)/3
9771 reflectionsΔρmax = 0.80 e Å3
559 parametersΔρmin = 0.81 e Å3
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Mo60.69390 (12)0.11122 (7)0.39186 (4)0.0368 (2)
Mo20.22701 (13)0.12059 (7)0.10533 (4)0.0397 (2)
Mo30.36214 (13)0.26659 (7)0.13669 (4)0.0398 (2)
Mo50.73040 (12)0.25706 (7)0.46432 (4)0.0362 (2)
Mo10.23874 (12)0.27048 (7)0.03718 (4)0.0382 (2)
Mo40.82278 (13)0.26484 (7)0.36521 (4)0.0391 (2)
Cl80.4600 (4)0.1752 (2)0.44300 (13)0.0500 (7)
Cl70.6312 (4)0.3743 (2)0.40919 (12)0.0476 (7)
Cl90.5832 (4)0.1835 (2)0.31459 (13)0.0510 (8)
Cl10.0231 (4)0.1937 (2)0.05651 (13)0.0489 (7)
Cl30.1564 (4)0.3845 (2)0.09652 (13)0.0482 (7)
Cl110.6126 (4)0.3444 (2)0.54238 (13)0.0521 (8)
Cl40.0944 (4)0.3673 (2)0.03834 (13)0.0558 (8)
Cl20.1377 (4)0.1886 (2)0.18511 (12)0.0510 (7)
Cl60.3975 (5)0.3570 (2)0.21331 (14)0.0622 (9)
Cl100.8318 (5)0.3646 (2)0.29225 (13)0.0602 (9)
Cl120.5202 (4)0.0258 (2)0.35826 (14)0.0530 (8)
Cl50.0636 (4)0.0122 (2)0.13473 (15)0.0616 (9)
O140.9010 (8)0.1849 (5)0.4221 (3)0.0342 (16)
O130.4228 (9)0.1900 (5)0.0772 (3)0.0388 (17)
O100.7550 (10)0.0364 (5)0.4569 (3)0.0405 (18)
O50.5505 (9)0.3465 (6)0.1020 (3)0.046 (2)
O120.9833 (10)0.1812 (5)0.3191 (3)0.0439 (19)
O110.8755 (10)0.0473 (5)0.3432 (3)0.0396 (18)
O90.7905 (10)0.1633 (5)0.5195 (3)0.0410 (18)
O80.9480 (9)0.3402 (5)0.4881 (3)0.0414 (18)
O20.2718 (10)0.0505 (6)0.0375 (3)0.047 (2)
O30.4213 (11)0.0456 (6)0.1533 (3)0.052 (2)
O71.0235 (10)0.3480 (6)0.4019 (3)0.048 (2)
O40.5359 (10)0.1736 (6)0.1807 (3)0.050 (2)
O10.2837 (10)0.1805 (6)0.0217 (3)0.050 (2)
O60.4457 (10)0.3482 (6)0.0159 (3)0.048 (2)
C110.9857 (15)0.0940 (9)0.3200 (4)0.046 (3)
C10.2924 (15)0.0934 (10)0.0102 (5)0.051 (3)
C30.5353 (16)0.0858 (9)0.1790 (5)0.049 (3)
C50.5578 (15)0.3674 (8)0.0504 (5)0.045 (3)
C100.8372 (16)0.0139 (9)0.5491 (5)0.052 (3)
H10A0.86030.05170.58380.077*
H10B0.93590.01940.53880.077*
H10C0.74560.02980.55250.077*
C90.7898 (14)0.0757 (9)0.5056 (5)0.044 (3)
C60.7068 (16)0.4188 (10)0.0306 (6)0.061 (4)
H6A0.69830.43040.00890.091*
H6B0.71040.47710.04590.091*
H6C0.80790.38210.04200.091*
C121.1214 (17)0.0416 (10)0.2906 (6)0.061 (4)
H12A1.10790.02360.29460.092*
H12B1.22980.06480.30630.092*
H12C1.11360.05020.25230.092*
C71.0493 (16)0.3649 (8)0.4531 (5)0.045 (3)
C40.6768 (18)0.0276 (11)0.2088 (6)0.069 (4)
H4A0.66160.03690.20420.104*
H4B0.78190.04680.19400.104*
H4C0.67810.03540.24730.104*
C81.2075 (16)0.4187 (9)0.4754 (6)0.062 (4)
H8A1.27360.43320.44530.093*
H8B1.27180.38170.49840.093*
H8C1.17830.47550.49670.093*
C20.3262 (17)0.0345 (11)0.0559 (6)0.066 (4)
H2A0.33950.07430.08950.099*
H2B0.42760.00320.04660.099*
H2C0.23320.00530.06060.099*
C130.1502 (18)0.3095 (10)0.7284 (5)0.061 (4)
H13A0.09570.25350.73890.073*
H13B0.26960.30760.73830.073*
C180.2127 (19)0.2066 (10)0.5789 (6)0.066 (4)
H18A0.26800.15000.56730.099*
H18B0.27220.25850.56630.099*
H18C0.09880.20260.56360.099*
C200.3920 (19)0.4114 (10)0.6635 (6)0.068 (4)
H20A0.43220.46700.64930.102*
H20B0.45520.35930.64890.102*
H20C0.40610.41940.70300.102*
C170.211 (2)0.2206 (9)0.6416 (6)0.065 (4)
H17A0.15300.16700.65380.078*
H17B0.32660.22230.65650.078*
C190.2077 (19)0.3934 (9)0.6468 (6)0.062 (4)
H19A0.14610.44710.66130.075*
H19B0.19510.38820.60690.075*
C160.1645 (18)0.2270 (12)0.6631 (6)0.078 (5)
H16A0.27910.23310.65010.117*
H16B0.15990.22870.70250.117*
H16C0.12340.16870.64690.117*
C211.105 (2)0.3311 (11)0.1646 (6)0.072 (4)
H21A1.07940.38370.19100.086*
H21B1.07680.34790.12810.086*
C150.0565 (17)0.3063 (11)0.6471 (6)0.069 (4)
H15A0.10360.36460.66200.082*
H15B0.06400.30400.60720.082*
C231.342 (2)0.2272 (10)0.1351 (6)0.072 (4)
H23A1.28840.17500.15030.086*
H23B1.46280.22090.13920.086*
C241.293 (2)0.2195 (12)0.0744 (6)0.088 (5)
H24A1.33040.16150.05650.131*
H24B1.34490.27050.05860.131*
H24C1.17250.22140.06940.131*
C281.314 (2)0.3886 (13)0.2696 (7)0.095 (6)
H28A1.35220.37580.30570.142*
H28B1.19420.39750.26920.142*
H28C1.37090.44410.26070.142*
C251.379 (3)0.3995 (11)0.1495 (8)0.092 (6)
H25A1.34430.45480.17210.111*
H25B1.33670.40350.11210.111*
C140.079 (2)0.3933 (12)0.7609 (6)0.087 (5)
H14A0.09880.38950.79960.130*
H14B0.03970.39470.75240.130*
H14C0.13400.44920.75140.130*
C271.351 (2)0.3071 (12)0.2277 (6)0.088 (5)
H27A1.47140.29810.22940.105*
H27B1.29590.25130.23830.105*
C220.993 (2)0.2490 (13)0.1741 (8)0.099 (6)
H22A0.87720.26510.17040.148*
H22B1.01720.23260.21060.148*
H22C1.01410.19690.14750.148*
C261.569 (3)0.4016 (16)0.1502 (10)0.126 (8)
H26A1.60860.45720.13600.189*
H26B1.60530.34770.12770.189*
H26C1.61290.40140.18740.189*
N10.1278 (13)0.3082 (7)0.6656 (4)0.049 (3)
N21.2964 (15)0.3163 (7)0.1693 (4)0.058 (3)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mo60.0367 (5)0.0361 (5)0.0373 (5)0.0032 (4)0.0019 (4)0.0037 (4)
Mo20.0402 (6)0.0425 (6)0.0369 (5)0.0026 (4)0.0015 (4)0.0066 (4)
Mo30.0399 (6)0.0457 (6)0.0341 (5)0.0017 (4)0.0034 (4)0.0081 (4)
Mo50.0364 (5)0.0356 (5)0.0363 (5)0.0019 (4)0.0016 (4)0.0035 (4)
Mo10.0360 (5)0.0463 (6)0.0323 (5)0.0059 (4)0.0017 (4)0.0050 (4)
Mo40.0445 (6)0.0372 (5)0.0361 (5)0.0056 (4)0.0020 (4)0.0059 (4)
Cl80.0404 (16)0.0472 (17)0.0606 (19)0.0016 (13)0.0040 (14)0.0021 (14)
Cl70.0526 (18)0.0428 (16)0.0499 (17)0.0153 (14)0.0055 (14)0.0112 (13)
Cl90.0553 (18)0.0499 (18)0.0472 (17)0.0063 (14)0.0110 (14)0.0078 (14)
Cl10.0385 (15)0.0565 (18)0.0510 (18)0.0069 (13)0.0043 (13)0.0041 (14)
Cl30.0484 (17)0.0458 (17)0.0506 (17)0.0053 (14)0.0023 (14)0.0101 (14)
Cl110.0545 (18)0.0524 (18)0.0483 (17)0.0036 (15)0.0094 (14)0.0019 (14)
Cl40.0507 (18)0.067 (2)0.0465 (18)0.0119 (16)0.0122 (14)0.0051 (15)
Cl20.0588 (19)0.0577 (19)0.0377 (16)0.0017 (15)0.0114 (14)0.0077 (14)
Cl60.075 (2)0.065 (2)0.0494 (19)0.0062 (18)0.0091 (17)0.0228 (16)
Cl100.087 (3)0.0516 (19)0.0456 (18)0.0096 (17)0.0106 (17)0.0163 (15)
Cl120.0469 (17)0.0489 (18)0.060 (2)0.0040 (14)0.0059 (15)0.0016 (15)
Cl50.061 (2)0.054 (2)0.069 (2)0.0130 (16)0.0065 (17)0.0003 (16)
O140.031 (4)0.038 (4)0.033 (4)0.003 (3)0.007 (3)0.004 (3)
O130.038 (4)0.049 (5)0.030 (4)0.001 (4)0.003 (3)0.009 (3)
O100.047 (5)0.034 (4)0.040 (5)0.001 (3)0.004 (4)0.003 (3)
O50.036 (4)0.058 (5)0.047 (5)0.011 (4)0.000 (4)0.014 (4)
O120.053 (5)0.041 (5)0.040 (4)0.007 (4)0.009 (4)0.008 (4)
O110.046 (5)0.035 (4)0.037 (4)0.012 (4)0.000 (4)0.002 (3)
O90.052 (5)0.039 (5)0.031 (4)0.000 (4)0.002 (3)0.001 (3)
O80.040 (4)0.044 (5)0.038 (4)0.005 (4)0.007 (4)0.001 (4)
O20.046 (5)0.052 (5)0.044 (5)0.001 (4)0.002 (4)0.015 (4)
O30.058 (5)0.043 (5)0.053 (5)0.001 (4)0.003 (4)0.003 (4)
O70.055 (5)0.049 (5)0.042 (5)0.003 (4)0.008 (4)0.014 (4)
O40.043 (5)0.061 (6)0.041 (5)0.003 (4)0.016 (4)0.001 (4)
O10.050 (5)0.061 (6)0.041 (5)0.008 (4)0.000 (4)0.014 (4)
O60.041 (5)0.055 (5)0.047 (5)0.008 (4)0.002 (4)0.002 (4)
C110.046 (7)0.062 (9)0.027 (6)0.005 (6)0.003 (5)0.004 (6)
C10.037 (7)0.072 (10)0.045 (8)0.003 (6)0.005 (6)0.018 (7)
C30.050 (8)0.055 (8)0.040 (7)0.003 (6)0.011 (6)0.002 (6)
C50.048 (7)0.034 (6)0.057 (8)0.009 (5)0.004 (6)0.015 (6)
C100.060 (8)0.053 (8)0.045 (7)0.007 (6)0.008 (6)0.019 (6)
C90.031 (6)0.057 (8)0.044 (7)0.002 (5)0.009 (5)0.009 (6)
C60.046 (8)0.067 (9)0.067 (9)0.018 (7)0.003 (7)0.005 (7)
C120.055 (8)0.063 (9)0.067 (9)0.020 (7)0.011 (7)0.008 (7)
C70.051 (7)0.034 (6)0.053 (8)0.009 (5)0.005 (6)0.010 (6)
C40.063 (9)0.085 (11)0.054 (8)0.029 (8)0.013 (7)0.007 (8)
C80.047 (8)0.057 (8)0.079 (10)0.015 (6)0.007 (7)0.000 (7)
C20.057 (9)0.087 (11)0.060 (9)0.006 (8)0.002 (7)0.038 (8)
C130.062 (9)0.072 (10)0.047 (8)0.010 (7)0.001 (7)0.003 (7)
C180.077 (10)0.056 (9)0.064 (9)0.009 (7)0.015 (8)0.007 (7)
C200.088 (11)0.068 (10)0.049 (8)0.008 (8)0.000 (8)0.015 (7)
C170.088 (11)0.043 (8)0.065 (9)0.014 (7)0.004 (8)0.004 (7)
C190.086 (11)0.051 (8)0.051 (8)0.001 (7)0.003 (7)0.012 (6)
C160.058 (9)0.101 (13)0.068 (10)0.021 (9)0.006 (8)0.009 (9)
C210.086 (11)0.073 (10)0.054 (9)0.031 (9)0.014 (8)0.004 (8)
C150.053 (8)0.082 (11)0.069 (10)0.007 (8)0.005 (7)0.001 (8)
C230.076 (10)0.060 (9)0.081 (11)0.012 (8)0.001 (8)0.009 (8)
C240.104 (14)0.096 (13)0.063 (10)0.028 (11)0.012 (9)0.003 (9)
C280.113 (15)0.108 (15)0.058 (10)0.002 (12)0.004 (10)0.002 (10)
C250.135 (18)0.055 (10)0.091 (13)0.000 (10)0.006 (12)0.026 (9)
C140.102 (14)0.094 (13)0.062 (10)0.014 (11)0.020 (9)0.002 (9)
C270.101 (13)0.097 (13)0.068 (11)0.006 (10)0.030 (10)0.034 (10)
C220.088 (13)0.099 (14)0.104 (15)0.018 (11)0.022 (11)0.021 (11)
C260.113 (18)0.126 (19)0.15 (2)0.018 (15)0.030 (15)0.040 (16)
N10.061 (7)0.039 (6)0.047 (6)0.011 (5)0.000 (5)0.001 (5)
N20.078 (8)0.049 (6)0.046 (6)0.007 (6)0.009 (6)0.011 (5)
Geometric parameters (Å, º) top
Mo6—O141.995 (7)Mo4—O72.070 (8)
Mo6—O102.071 (7)Mo4—Cl92.417 (3)
Mo6—O112.079 (7)Mo4—Cl102.419 (3)
Mo6—Cl92.406 (3)Mo4—Cl72.422 (3)
Mo6—Cl122.415 (3)O10—C91.272 (13)
Mo6—Cl82.430 (3)O5—C51.265 (14)
Mo6—Mo42.5746 (14)O12—C111.262 (14)
Mo6—Mo52.5894 (14)O11—C111.279 (14)
Mo2—O131.981 (7)O9—C91.269 (14)
Mo2—O22.078 (8)O8—C71.270 (14)
Mo2—O32.089 (8)O2—C11.274 (15)
Mo2—Cl22.405 (3)O3—C31.272 (15)
Mo2—Cl52.406 (3)O7—C71.255 (14)
Mo2—Cl12.418 (3)O4—C31.272 (15)
Mo2—Mo32.5722 (14)O1—C11.256 (15)
Mo2—Mo12.5798 (14)O6—C51.259 (14)
Mo3—O131.992 (7)C11—C121.496 (16)
Mo3—O52.068 (8)C1—C21.507 (17)
Mo3—O42.068 (8)C3—C41.491 (16)
Mo3—Cl32.413 (3)C5—C61.485 (16)
Mo3—Cl62.414 (3)C10—C91.508 (16)
Mo3—Cl22.417 (3)C7—C81.502 (16)
Mo3—Mo12.5756 (13)C13—C141.51 (2)
Mo5—O141.986 (7)C13—N11.536 (16)
Mo5—O92.070 (7)C18—C171.524 (18)
Mo5—O82.092 (7)C20—C191.508 (19)
Mo5—Cl112.404 (3)C17—N11.513 (15)
Mo5—Cl72.411 (3)C19—N11.493 (16)
Mo5—Cl82.423 (3)C16—C151.51 (2)
Mo5—Mo42.5751 (14)C21—C221.50 (2)
Mo1—O131.985 (7)C21—N21.542 (18)
Mo1—O62.070 (8)C15—N11.510 (16)
Mo1—O12.080 (8)C23—N21.511 (17)
Mo1—Cl42.406 (3)C23—C241.51 (2)
Mo1—Cl32.409 (3)C28—C271.51 (2)
Mo1—Cl12.425 (3)C25—N21.488 (18)
Mo4—O141.997 (7)C25—C261.50 (3)
Mo4—O122.063 (8)C27—N21.495 (17)
O14—Mo6—O1081.2 (3)O13—Mo1—Cl4157.7 (2)
O14—Mo6—O1179.2 (3)O6—Mo1—Cl484.7 (2)
O10—Mo6—O1192.5 (3)O1—Mo1—Cl484.3 (3)
O14—Mo6—Cl9107.6 (2)O13—Mo1—Cl3107.3 (2)
O10—Mo6—Cl9171.1 (2)O6—Mo1—Cl389.5 (2)
O11—Mo6—Cl990.5 (2)O1—Mo1—Cl3172.1 (2)
O14—Mo6—Cl12157.5 (2)Cl4—Mo1—Cl388.18 (12)
O10—Mo6—Cl1284.1 (2)O13—Mo1—Cl1106.8 (2)
O11—Mo6—Cl1284.5 (2)O6—Mo1—Cl1173.5 (2)
Cl9—Mo6—Cl1287.87 (11)O1—Mo1—Cl189.3 (2)
O14—Mo6—Cl8106.7 (2)Cl4—Mo1—Cl189.26 (11)
O10—Mo6—Cl888.8 (2)Cl3—Mo1—Cl188.16 (11)
O11—Mo6—Cl8174.0 (2)O13—Mo1—Mo349.8 (2)
Cl9—Mo6—Cl887.41 (11)O6—Mo1—Mo384.9 (2)
Cl12—Mo6—Cl889.86 (11)O1—Mo1—Mo3130.1 (2)
O14—Mo6—Mo449.9 (2)Cl4—Mo1—Mo3144.41 (10)
O10—Mo6—Mo4130.7 (2)Cl3—Mo1—Mo357.80 (8)
O11—Mo6—Mo485.0 (2)Cl1—Mo1—Mo398.90 (8)
Cl9—Mo6—Mo457.94 (8)O13—Mo1—Mo249.3 (2)
Cl12—Mo6—Mo4144.06 (9)O6—Mo1—Mo2128.7 (2)
Cl8—Mo6—Mo498.51 (8)O1—Mo1—Mo285.4 (2)
O14—Mo6—Mo549.3 (2)Cl4—Mo1—Mo2145.42 (9)
O10—Mo6—Mo585.3 (2)Cl3—Mo1—Mo299.56 (8)
O11—Mo6—Mo5128.3 (2)Cl1—Mo1—Mo257.68 (8)
Cl9—Mo6—Mo599.42 (8)Mo3—Mo1—Mo259.86 (4)
Cl12—Mo6—Mo5145.94 (9)O14—Mo4—O1280.5 (3)
Cl8—Mo6—Mo557.62 (8)O14—Mo4—O780.4 (3)
Mo4—Mo6—Mo559.82 (4)O12—Mo4—O791.4 (3)
O13—Mo2—O280.8 (3)O14—Mo4—Cl9107.1 (2)
O13—Mo2—O380.4 (3)O12—Mo4—Cl989.8 (2)
O2—Mo2—O392.6 (3)O7—Mo4—Cl9172.5 (2)
O13—Mo2—Cl2107.6 (2)O14—Mo4—Cl10160.1 (2)
O2—Mo2—Cl2171.5 (2)O12—Mo4—Cl1085.9 (2)
O3—Mo2—Cl290.0 (3)O7—Mo4—Cl1085.6 (2)
O13—Mo2—Cl5157.9 (2)Cl9—Mo4—Cl1087.16 (12)
O2—Mo2—Cl584.5 (2)O14—Mo4—Cl7106.9 (2)
O3—Mo2—Cl583.9 (2)O12—Mo4—Cl7172.6 (2)
Cl2—Mo2—Cl587.75 (12)O7—Mo4—Cl789.0 (2)
O13—Mo2—Cl1107.2 (2)Cl9—Mo4—Cl788.79 (11)
O2—Mo2—Cl188.9 (2)Cl10—Mo4—Cl786.72 (11)
O3—Mo2—Cl1172.4 (2)O14—Mo4—Mo649.8 (2)
Cl2—Mo2—Cl187.40 (11)O12—Mo4—Mo685.7 (2)
Cl5—Mo2—Cl188.84 (12)O7—Mo4—Mo6129.9 (2)
O13—Mo2—Mo349.8 (2)Cl9—Mo4—Mo657.54 (8)
O2—Mo2—Mo3130.3 (2)Cl10—Mo4—Mo6143.66 (10)
O3—Mo2—Mo385.5 (2)Cl7—Mo4—Mo699.71 (8)
Cl2—Mo2—Mo357.99 (8)O14—Mo4—Mo549.5 (2)
Cl5—Mo2—Mo3144.07 (10)O12—Mo4—Mo5129.8 (2)
Cl1—Mo2—Mo399.17 (8)O7—Mo4—Mo585.3 (2)
O13—Mo2—Mo149.5 (2)Cl9—Mo4—Mo599.54 (9)
O2—Mo2—Mo185.2 (2)Cl10—Mo4—Mo5143.23 (9)
O3—Mo2—Mo1129.6 (2)Cl7—Mo4—Mo557.59 (8)
Cl2—Mo2—Mo199.28 (9)Mo6—Mo4—Mo560.37 (4)
Cl5—Mo2—Mo1145.34 (10)Mo5—Cl8—Mo664.49 (8)
Cl1—Mo2—Mo157.94 (8)Mo5—Cl7—Mo464.39 (8)
Mo3—Mo2—Mo159.99 (4)Mo6—Cl9—Mo464.52 (8)
O13—Mo3—O580.6 (3)Mo2—Cl1—Mo164.38 (8)
O13—Mo3—O480.7 (3)Mo1—Cl3—Mo364.57 (8)
O5—Mo3—O492.1 (3)Mo2—Cl2—Mo364.47 (8)
O13—Mo3—Cl3106.9 (2)Mo5—O14—Mo681.1 (3)
O5—Mo3—Cl389.1 (2)Mo5—O14—Mo480.5 (3)
O4—Mo3—Cl3172.4 (3)Mo6—O14—Mo480.3 (2)
O13—Mo3—Cl6159.4 (2)Mo2—O13—Mo181.2 (3)
O5—Mo3—Cl685.2 (2)Mo2—O13—Mo380.7 (3)
O4—Mo3—Cl684.9 (3)Mo1—O13—Mo380.7 (3)
Cl3—Mo3—Cl687.68 (12)C9—O10—Mo6122.4 (7)
O13—Mo3—Cl2106.8 (2)C5—O5—Mo3122.5 (7)
O5—Mo3—Cl2172.6 (2)C11—O12—Mo4122.8 (8)
O4—Mo3—Cl289.5 (3)C11—O11—Mo6122.4 (7)
Cl3—Mo3—Cl288.42 (11)C9—O9—Mo5122.6 (7)
Cl6—Mo3—Cl287.73 (12)C7—O8—Mo5122.0 (8)
O13—Mo3—Mo249.5 (2)C1—O2—Mo2122.3 (8)
O5—Mo3—Mo2129.8 (2)C3—O3—Mo2122.1 (8)
O4—Mo3—Mo285.4 (2)C7—O7—Mo4123.4 (8)
Cl3—Mo3—Mo299.66 (8)C3—O4—Mo3123.3 (8)
Cl6—Mo3—Mo2143.94 (10)C1—O1—Mo1122.4 (8)
Cl2—Mo3—Mo257.54 (8)C5—O6—Mo1123.2 (8)
O13—Mo3—Mo149.5 (2)O12—C11—O11123.6 (11)
O5—Mo3—Mo185.4 (2)O12—C11—C12118.3 (12)
O4—Mo3—Mo1130.0 (2)O11—C11—C12118.0 (12)
Cl3—Mo3—Mo157.64 (8)O1—C1—O2124.6 (12)
Cl6—Mo3—Mo1144.14 (10)O1—C1—C2118.2 (12)
Cl2—Mo3—Mo199.08 (8)O2—C1—C2117.1 (13)
Mo2—Mo3—Mo160.15 (4)O3—C3—O4123.6 (11)
O14—Mo5—O980.5 (3)O3—C3—C4118.7 (12)
O14—Mo5—O879.6 (3)O4—C3—C4117.7 (12)
O9—Mo5—O892.3 (3)O6—C5—O5123.7 (11)
O14—Mo5—Cl11157.4 (2)O6—C5—C6119.1 (12)
O9—Mo5—Cl1184.4 (2)O5—C5—C6117.2 (11)
O8—Mo5—Cl1184.3 (2)O9—C9—O10124.4 (11)
O14—Mo5—Cl7107.7 (2)O9—C9—C10118.1 (11)
O9—Mo5—Cl7171.8 (2)O10—C9—C10117.5 (11)
O8—Mo5—Cl789.8 (2)O7—C7—O8123.9 (11)
Cl11—Mo5—Cl787.89 (11)O7—C7—C8119.0 (12)
O14—Mo5—Cl8107.2 (2)O8—C7—C8117.1 (11)
O9—Mo5—Cl889.6 (2)C14—C13—N1114.3 (12)
O8—Mo5—Cl8173.1 (2)N1—C17—C18114.9 (11)
Cl11—Mo5—Cl889.34 (11)N1—C19—C20115.6 (11)
Cl7—Mo5—Cl887.52 (11)C22—C21—N2115.7 (12)
O14—Mo5—Mo449.9 (2)C16—C15—N1116.2 (12)
O9—Mo5—Mo4130.1 (2)N2—C23—C24116.2 (12)
O8—Mo5—Mo485.2 (2)N2—C25—C26116.2 (15)
Cl11—Mo5—Mo4144.26 (9)N2—C27—C28115.8 (13)
Cl7—Mo5—Mo458.02 (8)C19—N1—C15106.7 (10)
Cl8—Mo5—Mo498.69 (9)C19—N1—C17111.3 (11)
O14—Mo5—Mo649.6 (2)C15—N1—C17111.0 (11)
O9—Mo5—Mo685.3 (2)C19—N1—C13111.2 (10)
O8—Mo5—Mo6128.8 (2)C15—N1—C13111.4 (10)
Cl11—Mo5—Mo6145.66 (9)C17—N1—C13105.3 (10)
Cl7—Mo5—Mo699.60 (8)C25—N2—C27111.5 (13)
Cl8—Mo5—Mo657.90 (8)C25—N2—C23111.3 (12)
Mo4—Mo5—Mo659.80 (4)C27—N2—C23106.9 (11)
O13—Mo1—O679.7 (3)C25—N2—C21105.9 (12)
O13—Mo1—O180.6 (3)C27—N2—C21110.2 (12)
O6—Mo1—O192.2 (3)C23—N2—C21111.1 (11)

Experimental details

Crystal data
Chemical formula(C2H5N)[Mo3Cl6O(C2H3O2)3]
Mr823.90
Crystal system, space groupTriclinic, P1
Temperature (K)293
a, b, c (Å)7.9356 (1), 14.4258 (1), 24.4415 (4)
α, β, γ (°)96.613 (1), 92.518 (1), 91.815 (1)
V3)2774.80 (6)
Z4
Radiation typeMo Kα
µ (mm1)1.95
Crystal size (mm)0.84 × 0.20 × 0.02
Data collection
DiffractometerSiemens SMART CCD
diffractometer
Absorption correctionEmpirical (using intensity measurements)
(SADABS; Sheldrick, 1996)
Tmin, Tmax0.680, 1.000
No. of measured, independent and
observed [I > 2σ(I)] reflections
14579, 9771, 7292
Rint0.041
(sin θ/λ)max1)0.598
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.071, 0.157, 1.07
No. of reflections9771
No. of parameters559
H-atom treatmentH-atom parameters constrained
w = 1/[σ2(Fo2) + 55.1956P]
where P = (Fo2 + 2Fc2)/3
Δρmax, Δρmin (e Å3)0.80, 0.81

Computer programs: SMART (Siemens, 1995), SAINT (Siemens, 1995), XPREP (Sheldrick, 1991), SHELXS97 (Sheldrick, 1990), SHELXL97 (Sheldrick, 1997), XP (Sheldrick, 1991), SHELXL97.

Selected geometric parameters (Å, º) top
Mo6—O141.995 (7)Mo3—Cl22.417 (3)
Mo6—O102.071 (7)Mo3—Mo12.5756 (13)
Mo6—O112.079 (7)Mo5—O141.986 (7)
Mo6—Cl92.406 (3)Mo5—O92.070 (7)
Mo6—Cl122.415 (3)Mo5—O82.092 (7)
Mo6—Cl82.430 (3)Mo5—Cl112.404 (3)
Mo6—Mo42.5746 (14)Mo5—Cl72.411 (3)
Mo6—Mo52.5894 (14)Mo5—Cl82.423 (3)
Mo2—O131.981 (7)Mo5—Mo42.5751 (14)
Mo2—O22.078 (8)Mo1—O131.985 (7)
Mo2—O32.089 (8)Mo1—O62.070 (8)
Mo2—Cl22.405 (3)Mo1—O12.080 (8)
Mo2—Cl52.406 (3)Mo1—Cl42.406 (3)
Mo2—Cl12.418 (3)Mo1—Cl32.409 (3)
Mo2—Mo32.5722 (14)Mo1—Cl12.425 (3)
Mo2—Mo12.5798 (14)Mo4—O141.997 (7)
Mo3—O131.992 (7)Mo4—O122.063 (8)
Mo3—O52.068 (8)Mo4—O72.070 (8)
Mo3—O42.068 (8)Mo4—Cl92.417 (3)
Mo3—Cl32.413 (3)Mo4—Cl102.419 (3)
Mo3—Cl62.414 (3)Mo4—Cl72.422 (3)
O14—Mo6—O1081.2 (3)O8—Mo5—Cl8173.1 (2)
O14—Mo6—O1179.2 (3)Cl11—Mo5—Cl889.34 (11)
O10—Mo6—O1192.5 (3)Cl7—Mo5—Cl887.52 (11)
O14—Mo6—Cl9107.6 (2)O14—Mo5—Mo449.9 (2)
O10—Mo6—Cl9171.1 (2)O9—Mo5—Mo4130.1 (2)
O11—Mo6—Cl990.5 (2)O8—Mo5—Mo485.2 (2)
O14—Mo6—Cl12157.5 (2)Cl11—Mo5—Mo4144.26 (9)
O10—Mo6—Cl1284.1 (2)Cl7—Mo5—Mo458.02 (8)
O11—Mo6—Cl1284.5 (2)Cl8—Mo5—Mo498.69 (9)
Cl9—Mo6—Cl1287.87 (11)O14—Mo5—Mo649.6 (2)
O14—Mo6—Cl8106.7 (2)O9—Mo5—Mo685.3 (2)
O10—Mo6—Cl888.8 (2)O8—Mo5—Mo6128.8 (2)
O11—Mo6—Cl8174.0 (2)Cl11—Mo5—Mo6145.66 (9)
Cl9—Mo6—Cl887.41 (11)Cl7—Mo5—Mo699.60 (8)
Cl12—Mo6—Cl889.86 (11)Cl8—Mo5—Mo657.90 (8)
O14—Mo6—Mo449.9 (2)Mo4—Mo5—Mo659.80 (4)
O10—Mo6—Mo4130.7 (2)O13—Mo1—O679.7 (3)
O11—Mo6—Mo485.0 (2)O13—Mo1—O180.6 (3)
Cl9—Mo6—Mo457.94 (8)O6—Mo1—O192.2 (3)
Cl12—Mo6—Mo4144.06 (9)O13—Mo1—Cl4157.7 (2)
Cl8—Mo6—Mo498.51 (8)O6—Mo1—Cl484.7 (2)
O14—Mo6—Mo549.3 (2)O1—Mo1—Cl484.3 (3)
O10—Mo6—Mo585.3 (2)O13—Mo1—Cl3107.3 (2)
O11—Mo6—Mo5128.3 (2)O6—Mo1—Cl389.5 (2)
Cl9—Mo6—Mo599.42 (8)O1—Mo1—Cl3172.1 (2)
Cl12—Mo6—Mo5145.94 (9)Cl4—Mo1—Cl388.18 (12)
Cl8—Mo6—Mo557.62 (8)O13—Mo1—Cl1106.8 (2)
Mo4—Mo6—Mo559.82 (4)O6—Mo1—Cl1173.5 (2)
O13—Mo2—O280.8 (3)O1—Mo1—Cl189.3 (2)
O13—Mo2—O380.4 (3)Cl4—Mo1—Cl189.26 (11)
O2—Mo2—O392.6 (3)Cl3—Mo1—Cl188.16 (11)
O13—Mo2—Cl2107.6 (2)O13—Mo1—Mo349.8 (2)
O2—Mo2—Cl2171.5 (2)O6—Mo1—Mo384.9 (2)
O3—Mo2—Cl290.0 (3)O1—Mo1—Mo3130.1 (2)
O13—Mo2—Cl5157.9 (2)Cl4—Mo1—Mo3144.41 (10)
O2—Mo2—Cl584.5 (2)Cl3—Mo1—Mo357.80 (8)
O3—Mo2—Cl583.9 (2)Cl1—Mo1—Mo398.90 (8)
Cl2—Mo2—Cl587.75 (12)O13—Mo1—Mo249.3 (2)
O13—Mo2—Cl1107.2 (2)O6—Mo1—Mo2128.7 (2)
O2—Mo2—Cl188.9 (2)O1—Mo1—Mo285.4 (2)
O3—Mo2—Cl1172.4 (2)Cl4—Mo1—Mo2145.42 (9)
Cl2—Mo2—Cl187.40 (11)Cl3—Mo1—Mo299.56 (8)
Cl5—Mo2—Cl188.84 (12)Cl1—Mo1—Mo257.68 (8)
O13—Mo2—Mo349.8 (2)Mo3—Mo1—Mo259.86 (4)
O2—Mo2—Mo3130.3 (2)O14—Mo4—O1280.5 (3)
O3—Mo2—Mo385.5 (2)O14—Mo4—O780.4 (3)
Cl2—Mo2—Mo357.99 (8)O12—Mo4—O791.4 (3)
Cl5—Mo2—Mo3144.07 (10)O14—Mo4—Cl9107.1 (2)
Cl1—Mo2—Mo399.17 (8)O12—Mo4—Cl989.8 (2)
O13—Mo2—Mo149.5 (2)O7—Mo4—Cl9172.5 (2)
O2—Mo2—Mo185.2 (2)O14—Mo4—Cl10160.1 (2)
O3—Mo2—Mo1129.6 (2)O12—Mo4—Cl1085.9 (2)
Cl2—Mo2—Mo199.28 (9)O7—Mo4—Cl1085.6 (2)
Cl5—Mo2—Mo1145.34 (10)Cl9—Mo4—Cl1087.16 (12)
Cl1—Mo2—Mo157.94 (8)O14—Mo4—Cl7106.9 (2)
Mo3—Mo2—Mo159.99 (4)O12—Mo4—Cl7172.6 (2)
O13—Mo3—O580.6 (3)O7—Mo4—Cl789.0 (2)
O13—Mo3—O480.7 (3)Cl9—Mo4—Cl788.79 (11)
O5—Mo3—O492.1 (3)Cl10—Mo4—Cl786.72 (11)
O13—Mo3—Cl3106.9 (2)O14—Mo4—Mo649.8 (2)
O5—Mo3—Cl389.1 (2)O12—Mo4—Mo685.7 (2)
O4—Mo3—Cl3172.4 (3)O7—Mo4—Mo6129.9 (2)
O13—Mo3—Cl6159.4 (2)Cl9—Mo4—Mo657.54 (8)
O5—Mo3—Cl685.2 (2)Cl10—Mo4—Mo6143.66 (10)
O4—Mo3—Cl684.9 (3)Cl7—Mo4—Mo699.71 (8)
Cl3—Mo3—Cl687.68 (12)O14—Mo4—Mo549.5 (2)
O13—Mo3—Cl2106.8 (2)O12—Mo4—Mo5129.8 (2)
O5—Mo3—Cl2172.6 (2)O7—Mo4—Mo585.3 (2)
O4—Mo3—Cl289.5 (3)Cl9—Mo4—Mo599.54 (9)
Cl3—Mo3—Cl288.42 (11)Cl10—Mo4—Mo5143.23 (9)
Cl6—Mo3—Cl287.73 (12)Cl7—Mo4—Mo557.59 (8)
O13—Mo3—Mo249.5 (2)Mo6—Mo4—Mo560.37 (4)
O5—Mo3—Mo2129.8 (2)Mo5—Cl8—Mo664.49 (8)
O4—Mo3—Mo285.4 (2)Mo5—Cl7—Mo464.39 (8)
Cl3—Mo3—Mo299.66 (8)Mo6—Cl9—Mo464.52 (8)
Cl6—Mo3—Mo2143.94 (10)Mo2—Cl1—Mo164.38 (8)
Cl2—Mo3—Mo257.54 (8)Mo1—Cl3—Mo364.57 (8)
O13—Mo3—Mo149.5 (2)Mo2—Cl2—Mo364.47 (8)
O5—Mo3—Mo185.4 (2)Mo5—O14—Mo681.1 (3)
O4—Mo3—Mo1130.0 (2)Mo5—O14—Mo480.5 (3)
Cl3—Mo3—Mo157.64 (8)Mo6—O14—Mo480.3 (2)
Cl6—Mo3—Mo1144.14 (10)Mo2—O13—Mo181.2 (3)
Cl2—Mo3—Mo199.08 (8)Mo2—O13—Mo380.7 (3)
Mo2—Mo3—Mo160.15 (4)Mo1—O13—Mo380.7 (3)
O14—Mo5—O980.5 (3)C9—O10—Mo6122.4 (7)
O14—Mo5—O879.6 (3)C5—O5—Mo3122.5 (7)
O9—Mo5—O892.3 (3)C11—O12—Mo4122.8 (8)
O14—Mo5—Cl11157.4 (2)C11—O11—Mo6122.4 (7)
O9—Mo5—Cl1184.4 (2)C9—O9—Mo5122.6 (7)
O8—Mo5—Cl1184.3 (2)C7—O8—Mo5122.0 (8)
O14—Mo5—Cl7107.7 (2)C1—O2—Mo2122.3 (8)
O9—Mo5—Cl7171.8 (2)C3—O3—Mo2122.1 (8)
O8—Mo5—Cl789.8 (2)C7—O7—Mo4123.4 (8)
Cl11—Mo5—Cl787.89 (11)C3—O4—Mo3123.3 (8)
O14—Mo5—Cl8107.2 (2)C1—O1—Mo1122.4 (8)
O9—Mo5—Cl889.6 (2)C5—O6—Mo1123.2 (8)
 

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