Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802013892/bt6175sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536802013892/bt6175Isup2.hkl |
CCDC reference: 197452
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (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
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.
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.
Fig. 1. A view of the structure of the title compound, showing 30% probability displacement ellipsoids. H atoms have been omitted for clarity. |
(C2H5N)[Mo3Cl6O(C2H3O2)3] | Z = 4 |
Mr = 823.90 | F(000) = 1616 |
Triclinic, P1 | Dx = 1.972 Mg m−3 |
a = 7.9356 (1) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 14.4258 (1) Å | Cell parameters from 6220 reflections |
c = 24.4415 (4) Å | θ = 0.8–25.1° |
α = 96.613 (1)° | µ = 1.95 mm−1 |
β = 92.518 (1)° | T = 293 K |
γ = 91.815 (1)° | Prism, black |
V = 2774.80 (6) Å3 | 0.84 × 0.20 × 0.02 mm |
Siemens SMART CCD diffractometer | 9771 independent reflections |
Radiation source: fine-focus sealed tube | 7292 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.041 |
ϕ and ω scans | θmax = 25.1°, θmin = 0.8° |
Absorption correction: empirical (using intensity measurements) (SADABS; Sheldrick, 1996) | h = −9→9 |
Tmin = 0.680, Tmax = 1.000 | k = −15→17 |
14579 measured reflections | l = −29→26 |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.071 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.157 | H-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 parameters | Δρmax = 0.80 e Å−3 |
0 restraints | Δρmin = −0.81 e Å−3 |
(C2H5N)[Mo3Cl6O(C2H3O2)3] | γ = 91.815 (1)° |
Mr = 823.90 | V = 2774.80 (6) Å3 |
Triclinic, P1 | Z = 4 |
a = 7.9356 (1) Å | Mo Kα radiation |
b = 14.4258 (1) Å | µ = 1.95 mm−1 |
c = 24.4415 (4) Å | T = 293 K |
α = 96.613 (1)° | 0.84 × 0.20 × 0.02 mm |
β = 92.518 (1)° |
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 = 1.000 | Rint = 0.041 |
14579 measured reflections |
R[F2 > 2σ(F2)] = 0.071 | 0 restraints |
wR(F2) = 0.157 | H-atom parameters constrained |
S = 1.07 | w = 1/[σ2(Fo2) + 55.1956P] where P = (Fo2 + 2Fc2)/3 |
9771 reflections | Δρmax = 0.80 e Å−3 |
559 parameters | Δρmin = −0.81 e Å−3 |
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. |
x | y | z | Uiso*/Ueq | ||
Mo6 | 0.69390 (12) | 0.11122 (7) | 0.39186 (4) | 0.0368 (2) | |
Mo2 | 0.22701 (13) | −0.12059 (7) | 0.10533 (4) | 0.0397 (2) | |
Mo3 | 0.36214 (13) | −0.26659 (7) | 0.13669 (4) | 0.0398 (2) | |
Mo5 | 0.73040 (12) | 0.25706 (7) | 0.46432 (4) | 0.0362 (2) | |
Mo1 | 0.23874 (12) | −0.27048 (7) | 0.03718 (4) | 0.0382 (2) | |
Mo4 | 0.82278 (13) | 0.26484 (7) | 0.36521 (4) | 0.0391 (2) | |
Cl8 | 0.4600 (4) | 0.1752 (2) | 0.44300 (13) | 0.0500 (7) | |
Cl7 | 0.6312 (4) | 0.3743 (2) | 0.40919 (12) | 0.0476 (7) | |
Cl9 | 0.5832 (4) | 0.1835 (2) | 0.31459 (13) | 0.0510 (8) | |
Cl1 | −0.0231 (4) | −0.1937 (2) | 0.05651 (13) | 0.0489 (7) | |
Cl3 | 0.1564 (4) | −0.3845 (2) | 0.09652 (13) | 0.0482 (7) | |
Cl11 | 0.6126 (4) | 0.3444 (2) | 0.54238 (13) | 0.0521 (8) | |
Cl4 | 0.0944 (4) | −0.3673 (2) | −0.03834 (13) | 0.0558 (8) | |
Cl2 | 0.1377 (4) | −0.1886 (2) | 0.18511 (12) | 0.0510 (7) | |
Cl6 | 0.3975 (5) | −0.3570 (2) | 0.21331 (14) | 0.0622 (9) | |
Cl10 | 0.8318 (5) | 0.3646 (2) | 0.29225 (13) | 0.0602 (9) | |
Cl12 | 0.5202 (4) | −0.0258 (2) | 0.35826 (14) | 0.0530 (8) | |
Cl5 | 0.0636 (4) | 0.0122 (2) | 0.13473 (15) | 0.0616 (9) | |
O14 | 0.9010 (8) | 0.1849 (5) | 0.4221 (3) | 0.0342 (16) | |
O13 | 0.4228 (9) | −0.1900 (5) | 0.0772 (3) | 0.0388 (17) | |
O10 | 0.7550 (10) | 0.0364 (5) | 0.4569 (3) | 0.0405 (18) | |
O5 | 0.5505 (9) | −0.3465 (6) | 0.1020 (3) | 0.046 (2) | |
O12 | 0.9833 (10) | 0.1812 (5) | 0.3191 (3) | 0.0439 (19) | |
O11 | 0.8755 (10) | 0.0473 (5) | 0.3432 (3) | 0.0396 (18) | |
O9 | 0.7905 (10) | 0.1633 (5) | 0.5195 (3) | 0.0410 (18) | |
O8 | 0.9480 (9) | 0.3402 (5) | 0.4881 (3) | 0.0414 (18) | |
O2 | 0.2718 (10) | −0.0505 (6) | 0.0375 (3) | 0.047 (2) | |
O3 | 0.4213 (11) | −0.0456 (6) | 0.1533 (3) | 0.052 (2) | |
O7 | 1.0235 (10) | 0.3480 (6) | 0.4019 (3) | 0.048 (2) | |
O4 | 0.5359 (10) | −0.1736 (6) | 0.1807 (3) | 0.050 (2) | |
O1 | 0.2837 (10) | −0.1805 (6) | −0.0217 (3) | 0.050 (2) | |
O6 | 0.4457 (10) | −0.3482 (6) | 0.0159 (3) | 0.048 (2) | |
C11 | 0.9857 (15) | 0.0940 (9) | 0.3200 (4) | 0.046 (3) | |
C1 | 0.2924 (15) | −0.0934 (10) | −0.0102 (5) | 0.051 (3) | |
C3 | 0.5353 (16) | −0.0858 (9) | 0.1790 (5) | 0.049 (3) | |
C5 | 0.5578 (15) | −0.3674 (8) | 0.0504 (5) | 0.045 (3) | |
C10 | 0.8372 (16) | 0.0139 (9) | 0.5491 (5) | 0.052 (3) | |
H10A | 0.8603 | 0.0517 | 0.5838 | 0.077* | |
H10B | 0.9359 | −0.0194 | 0.5388 | 0.077* | |
H10C | 0.7456 | −0.0298 | 0.5525 | 0.077* | |
C9 | 0.7898 (14) | 0.0757 (9) | 0.5056 (5) | 0.044 (3) | |
C6 | 0.7068 (16) | −0.4188 (10) | 0.0306 (6) | 0.061 (4) | |
H6A | 0.6983 | −0.4304 | −0.0089 | 0.091* | |
H6B | 0.7104 | −0.4771 | 0.0459 | 0.091* | |
H6C | 0.8079 | −0.3821 | 0.0420 | 0.091* | |
C12 | 1.1214 (17) | 0.0416 (10) | 0.2906 (6) | 0.061 (4) | |
H12A | 1.1079 | −0.0236 | 0.2946 | 0.092* | |
H12B | 1.2298 | 0.0648 | 0.3063 | 0.092* | |
H12C | 1.1136 | 0.0502 | 0.2523 | 0.092* | |
C7 | 1.0493 (16) | 0.3649 (8) | 0.4531 (5) | 0.045 (3) | |
C4 | 0.6768 (18) | −0.0276 (11) | 0.2088 (6) | 0.069 (4) | |
H4A | 0.6616 | 0.0369 | 0.2042 | 0.104* | |
H4B | 0.7819 | −0.0468 | 0.1940 | 0.104* | |
H4C | 0.6781 | −0.0354 | 0.2473 | 0.104* | |
C8 | 1.2075 (16) | 0.4187 (9) | 0.4754 (6) | 0.062 (4) | |
H8A | 1.2736 | 0.4332 | 0.4453 | 0.093* | |
H8B | 1.2718 | 0.3817 | 0.4984 | 0.093* | |
H8C | 1.1783 | 0.4755 | 0.4967 | 0.093* | |
C2 | 0.3262 (17) | −0.0345 (11) | −0.0559 (6) | 0.066 (4) | |
H2A | 0.3395 | −0.0743 | −0.0895 | 0.099* | |
H2B | 0.4276 | 0.0032 | −0.0466 | 0.099* | |
H2C | 0.2332 | 0.0053 | −0.0606 | 0.099* | |
C13 | 0.1502 (18) | 0.3095 (10) | 0.7284 (5) | 0.061 (4) | |
H13A | 0.0957 | 0.2535 | 0.7389 | 0.073* | |
H13B | 0.2696 | 0.3076 | 0.7383 | 0.073* | |
C18 | 0.2127 (19) | 0.2066 (10) | 0.5789 (6) | 0.066 (4) | |
H18A | 0.2680 | 0.1500 | 0.5673 | 0.099* | |
H18B | 0.2722 | 0.2585 | 0.5663 | 0.099* | |
H18C | 0.0988 | 0.2026 | 0.5636 | 0.099* | |
C20 | 0.3920 (19) | 0.4114 (10) | 0.6635 (6) | 0.068 (4) | |
H20A | 0.4322 | 0.4670 | 0.6493 | 0.102* | |
H20B | 0.4552 | 0.3593 | 0.6489 | 0.102* | |
H20C | 0.4061 | 0.4194 | 0.7030 | 0.102* | |
C17 | 0.211 (2) | 0.2206 (9) | 0.6416 (6) | 0.065 (4) | |
H17A | 0.1530 | 0.1670 | 0.6538 | 0.078* | |
H17B | 0.3266 | 0.2223 | 0.6565 | 0.078* | |
C19 | 0.2077 (19) | 0.3934 (9) | 0.6468 (6) | 0.062 (4) | |
H19A | 0.1461 | 0.4471 | 0.6613 | 0.075* | |
H19B | 0.1951 | 0.3882 | 0.6069 | 0.075* | |
C16 | −0.1645 (18) | 0.2270 (12) | 0.6631 (6) | 0.078 (5) | |
H16A | −0.2791 | 0.2331 | 0.6501 | 0.117* | |
H16B | −0.1599 | 0.2287 | 0.7025 | 0.117* | |
H16C | −0.1234 | 0.1687 | 0.6469 | 0.117* | |
C21 | 1.105 (2) | 0.3311 (11) | 0.1646 (6) | 0.072 (4) | |
H21A | 1.0794 | 0.3837 | 0.1910 | 0.086* | |
H21B | 1.0768 | 0.3479 | 0.1281 | 0.086* | |
C15 | −0.0565 (17) | 0.3063 (11) | 0.6471 (6) | 0.069 (4) | |
H15A | −0.1036 | 0.3646 | 0.6620 | 0.082* | |
H15B | −0.0640 | 0.3040 | 0.6072 | 0.082* | |
C23 | 1.342 (2) | 0.2272 (10) | 0.1351 (6) | 0.072 (4) | |
H23A | 1.2884 | 0.1750 | 0.1503 | 0.086* | |
H23B | 1.4628 | 0.2209 | 0.1392 | 0.086* | |
C24 | 1.293 (2) | 0.2195 (12) | 0.0744 (6) | 0.088 (5) | |
H24A | 1.3304 | 0.1615 | 0.0565 | 0.131* | |
H24B | 1.3449 | 0.2705 | 0.0586 | 0.131* | |
H24C | 1.1725 | 0.2214 | 0.0694 | 0.131* | |
C28 | 1.314 (2) | 0.3886 (13) | 0.2696 (7) | 0.095 (6) | |
H28A | 1.3522 | 0.3758 | 0.3057 | 0.142* | |
H28B | 1.1942 | 0.3975 | 0.2692 | 0.142* | |
H28C | 1.3709 | 0.4441 | 0.2607 | 0.142* | |
C25 | 1.379 (3) | 0.3995 (11) | 0.1495 (8) | 0.092 (6) | |
H25A | 1.3443 | 0.4548 | 0.1721 | 0.111* | |
H25B | 1.3367 | 0.4035 | 0.1121 | 0.111* | |
C14 | 0.079 (2) | 0.3933 (12) | 0.7609 (6) | 0.087 (5) | |
H14A | 0.0988 | 0.3895 | 0.7996 | 0.130* | |
H14B | −0.0397 | 0.3947 | 0.7524 | 0.130* | |
H14C | 0.1340 | 0.4492 | 0.7514 | 0.130* | |
C27 | 1.351 (2) | 0.3071 (12) | 0.2277 (6) | 0.088 (5) | |
H27A | 1.4714 | 0.2981 | 0.2294 | 0.105* | |
H27B | 1.2959 | 0.2513 | 0.2383 | 0.105* | |
C22 | 0.993 (2) | 0.2490 (13) | 0.1741 (8) | 0.099 (6) | |
H22A | 0.8772 | 0.2651 | 0.1704 | 0.148* | |
H22B | 1.0172 | 0.2326 | 0.2106 | 0.148* | |
H22C | 1.0141 | 0.1969 | 0.1475 | 0.148* | |
C26 | 1.569 (3) | 0.4016 (16) | 0.1502 (10) | 0.126 (8) | |
H26A | 1.6086 | 0.4572 | 0.1360 | 0.189* | |
H26B | 1.6053 | 0.3477 | 0.1277 | 0.189* | |
H26C | 1.6129 | 0.4014 | 0.1874 | 0.189* | |
N1 | 0.1278 (13) | 0.3082 (7) | 0.6656 (4) | 0.049 (3) | |
N2 | 1.2964 (15) | 0.3163 (7) | 0.1693 (4) | 0.058 (3) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Mo6 | 0.0367 (5) | 0.0361 (5) | 0.0373 (5) | 0.0032 (4) | −0.0019 (4) | 0.0037 (4) |
Mo2 | 0.0402 (6) | 0.0425 (6) | 0.0369 (5) | 0.0026 (4) | 0.0015 (4) | 0.0066 (4) |
Mo3 | 0.0399 (6) | 0.0457 (6) | 0.0341 (5) | 0.0017 (4) | −0.0034 (4) | 0.0081 (4) |
Mo5 | 0.0364 (5) | 0.0356 (5) | 0.0363 (5) | 0.0019 (4) | 0.0016 (4) | 0.0035 (4) |
Mo1 | 0.0360 (5) | 0.0463 (6) | 0.0323 (5) | 0.0059 (4) | −0.0017 (4) | 0.0050 (4) |
Mo4 | 0.0445 (6) | 0.0372 (5) | 0.0361 (5) | 0.0056 (4) | 0.0020 (4) | 0.0059 (4) |
Cl8 | 0.0404 (16) | 0.0472 (17) | 0.0606 (19) | 0.0016 (13) | 0.0040 (14) | −0.0021 (14) |
Cl7 | 0.0526 (18) | 0.0428 (16) | 0.0499 (17) | 0.0153 (14) | 0.0055 (14) | 0.0112 (13) |
Cl9 | 0.0553 (18) | 0.0499 (18) | 0.0472 (17) | 0.0063 (14) | −0.0110 (14) | 0.0078 (14) |
Cl1 | 0.0385 (15) | 0.0565 (18) | 0.0510 (18) | 0.0069 (13) | −0.0043 (13) | 0.0041 (14) |
Cl3 | 0.0484 (17) | 0.0458 (17) | 0.0506 (17) | −0.0053 (14) | −0.0023 (14) | 0.0101 (14) |
Cl11 | 0.0545 (18) | 0.0524 (18) | 0.0483 (17) | 0.0036 (15) | 0.0094 (14) | −0.0019 (14) |
Cl4 | 0.0507 (18) | 0.067 (2) | 0.0465 (18) | 0.0119 (16) | −0.0122 (14) | −0.0051 (15) |
Cl2 | 0.0588 (19) | 0.0577 (19) | 0.0377 (16) | 0.0017 (15) | 0.0114 (14) | 0.0077 (14) |
Cl6 | 0.075 (2) | 0.065 (2) | 0.0494 (19) | 0.0062 (18) | −0.0091 (17) | 0.0228 (16) |
Cl10 | 0.087 (3) | 0.0516 (19) | 0.0456 (18) | 0.0096 (17) | 0.0106 (17) | 0.0163 (15) |
Cl12 | 0.0469 (17) | 0.0489 (18) | 0.060 (2) | −0.0040 (14) | −0.0059 (15) | −0.0016 (15) |
Cl5 | 0.061 (2) | 0.054 (2) | 0.069 (2) | 0.0130 (16) | 0.0065 (17) | 0.0003 (16) |
O14 | 0.031 (4) | 0.038 (4) | 0.033 (4) | 0.003 (3) | −0.007 (3) | 0.004 (3) |
O13 | 0.038 (4) | 0.049 (5) | 0.030 (4) | 0.001 (4) | 0.003 (3) | 0.009 (3) |
O10 | 0.047 (5) | 0.034 (4) | 0.040 (5) | −0.001 (3) | 0.004 (4) | 0.003 (3) |
O5 | 0.036 (4) | 0.058 (5) | 0.047 (5) | 0.011 (4) | 0.000 (4) | 0.014 (4) |
O12 | 0.053 (5) | 0.041 (5) | 0.040 (4) | 0.007 (4) | 0.009 (4) | 0.008 (4) |
O11 | 0.046 (5) | 0.035 (4) | 0.037 (4) | 0.012 (4) | 0.000 (4) | −0.002 (3) |
O9 | 0.052 (5) | 0.039 (5) | 0.031 (4) | 0.000 (4) | −0.002 (3) | 0.001 (3) |
O8 | 0.040 (4) | 0.044 (5) | 0.038 (4) | −0.005 (4) | 0.007 (4) | −0.001 (4) |
O2 | 0.046 (5) | 0.052 (5) | 0.044 (5) | 0.001 (4) | 0.002 (4) | 0.015 (4) |
O3 | 0.058 (5) | 0.043 (5) | 0.053 (5) | 0.001 (4) | −0.003 (4) | 0.003 (4) |
O7 | 0.055 (5) | 0.049 (5) | 0.042 (5) | −0.003 (4) | 0.008 (4) | 0.014 (4) |
O4 | 0.043 (5) | 0.061 (6) | 0.041 (5) | −0.003 (4) | −0.016 (4) | −0.001 (4) |
O1 | 0.050 (5) | 0.061 (6) | 0.041 (5) | 0.008 (4) | 0.000 (4) | 0.014 (4) |
O6 | 0.041 (5) | 0.055 (5) | 0.047 (5) | 0.008 (4) | 0.002 (4) | 0.002 (4) |
C11 | 0.046 (7) | 0.062 (9) | 0.027 (6) | 0.005 (6) | −0.003 (5) | 0.004 (6) |
C1 | 0.037 (7) | 0.072 (10) | 0.045 (8) | −0.003 (6) | −0.005 (6) | 0.018 (7) |
C3 | 0.050 (8) | 0.055 (8) | 0.040 (7) | −0.003 (6) | 0.011 (6) | −0.002 (6) |
C5 | 0.048 (7) | 0.034 (6) | 0.057 (8) | 0.009 (5) | 0.004 (6) | 0.015 (6) |
C10 | 0.060 (8) | 0.053 (8) | 0.045 (7) | 0.007 (6) | 0.008 (6) | 0.019 (6) |
C9 | 0.031 (6) | 0.057 (8) | 0.044 (7) | −0.002 (5) | 0.009 (5) | 0.009 (6) |
C6 | 0.046 (8) | 0.067 (9) | 0.067 (9) | 0.018 (7) | −0.003 (7) | −0.005 (7) |
C12 | 0.055 (8) | 0.063 (9) | 0.067 (9) | 0.020 (7) | 0.011 (7) | 0.008 (7) |
C7 | 0.051 (7) | 0.034 (6) | 0.053 (8) | 0.009 (5) | 0.005 (6) | 0.010 (6) |
C4 | 0.063 (9) | 0.085 (11) | 0.054 (8) | −0.029 (8) | −0.013 (7) | −0.007 (8) |
C8 | 0.047 (8) | 0.057 (8) | 0.079 (10) | −0.015 (6) | −0.007 (7) | 0.000 (7) |
C2 | 0.057 (9) | 0.087 (11) | 0.060 (9) | −0.006 (8) | −0.002 (7) | 0.038 (8) |
C13 | 0.062 (9) | 0.072 (10) | 0.047 (8) | −0.010 (7) | −0.001 (7) | 0.003 (7) |
C18 | 0.077 (10) | 0.056 (9) | 0.064 (9) | 0.009 (7) | 0.015 (8) | −0.007 (7) |
C20 | 0.088 (11) | 0.068 (10) | 0.049 (8) | −0.008 (8) | 0.000 (8) | 0.015 (7) |
C17 | 0.088 (11) | 0.043 (8) | 0.065 (9) | 0.014 (7) | 0.004 (8) | 0.004 (7) |
C19 | 0.086 (11) | 0.051 (8) | 0.051 (8) | 0.001 (7) | −0.003 (7) | 0.012 (6) |
C16 | 0.058 (9) | 0.101 (13) | 0.068 (10) | −0.021 (9) | −0.006 (8) | −0.009 (9) |
C21 | 0.086 (11) | 0.073 (10) | 0.054 (9) | 0.031 (9) | −0.014 (8) | −0.004 (8) |
C15 | 0.053 (8) | 0.082 (11) | 0.069 (10) | 0.007 (8) | −0.005 (7) | −0.001 (8) |
C23 | 0.076 (10) | 0.060 (9) | 0.081 (11) | 0.012 (8) | 0.001 (8) | 0.009 (8) |
C24 | 0.104 (14) | 0.096 (13) | 0.063 (10) | 0.028 (11) | 0.012 (9) | −0.003 (9) |
C28 | 0.113 (15) | 0.108 (15) | 0.058 (10) | −0.002 (12) | −0.004 (10) | −0.002 (10) |
C25 | 0.135 (18) | 0.055 (10) | 0.091 (13) | 0.000 (10) | 0.006 (12) | 0.026 (9) |
C14 | 0.102 (14) | 0.094 (13) | 0.062 (10) | −0.014 (11) | 0.020 (9) | 0.002 (9) |
C27 | 0.101 (13) | 0.097 (13) | 0.068 (11) | 0.006 (10) | −0.030 (10) | 0.034 (10) |
C22 | 0.088 (13) | 0.099 (14) | 0.104 (15) | 0.018 (11) | 0.022 (11) | −0.021 (11) |
C26 | 0.113 (18) | 0.126 (19) | 0.15 (2) | −0.018 (15) | 0.030 (15) | 0.040 (16) |
N1 | 0.061 (7) | 0.039 (6) | 0.047 (6) | 0.011 (5) | 0.000 (5) | −0.001 (5) |
N2 | 0.078 (8) | 0.049 (6) | 0.046 (6) | 0.007 (6) | −0.009 (6) | 0.011 (5) |
Mo6—O14 | 1.995 (7) | Mo4—O7 | 2.070 (8) |
Mo6—O10 | 2.071 (7) | Mo4—Cl9 | 2.417 (3) |
Mo6—O11 | 2.079 (7) | Mo4—Cl10 | 2.419 (3) |
Mo6—Cl9 | 2.406 (3) | Mo4—Cl7 | 2.422 (3) |
Mo6—Cl12 | 2.415 (3) | O10—C9 | 1.272 (13) |
Mo6—Cl8 | 2.430 (3) | O5—C5 | 1.265 (14) |
Mo6—Mo4 | 2.5746 (14) | O12—C11 | 1.262 (14) |
Mo6—Mo5 | 2.5894 (14) | O11—C11 | 1.279 (14) |
Mo2—O13 | 1.981 (7) | O9—C9 | 1.269 (14) |
Mo2—O2 | 2.078 (8) | O8—C7 | 1.270 (14) |
Mo2—O3 | 2.089 (8) | O2—C1 | 1.274 (15) |
Mo2—Cl2 | 2.405 (3) | O3—C3 | 1.272 (15) |
Mo2—Cl5 | 2.406 (3) | O7—C7 | 1.255 (14) |
Mo2—Cl1 | 2.418 (3) | O4—C3 | 1.272 (15) |
Mo2—Mo3 | 2.5722 (14) | O1—C1 | 1.256 (15) |
Mo2—Mo1 | 2.5798 (14) | O6—C5 | 1.259 (14) |
Mo3—O13 | 1.992 (7) | C11—C12 | 1.496 (16) |
Mo3—O5 | 2.068 (8) | C1—C2 | 1.507 (17) |
Mo3—O4 | 2.068 (8) | C3—C4 | 1.491 (16) |
Mo3—Cl3 | 2.413 (3) | C5—C6 | 1.485 (16) |
Mo3—Cl6 | 2.414 (3) | C10—C9 | 1.508 (16) |
Mo3—Cl2 | 2.417 (3) | C7—C8 | 1.502 (16) |
Mo3—Mo1 | 2.5756 (13) | C13—C14 | 1.51 (2) |
Mo5—O14 | 1.986 (7) | C13—N1 | 1.536 (16) |
Mo5—O9 | 2.070 (7) | C18—C17 | 1.524 (18) |
Mo5—O8 | 2.092 (7) | C20—C19 | 1.508 (19) |
Mo5—Cl11 | 2.404 (3) | C17—N1 | 1.513 (15) |
Mo5—Cl7 | 2.411 (3) | C19—N1 | 1.493 (16) |
Mo5—Cl8 | 2.423 (3) | C16—C15 | 1.51 (2) |
Mo5—Mo4 | 2.5751 (14) | C21—C22 | 1.50 (2) |
Mo1—O13 | 1.985 (7) | C21—N2 | 1.542 (18) |
Mo1—O6 | 2.070 (8) | C15—N1 | 1.510 (16) |
Mo1—O1 | 2.080 (8) | C23—N2 | 1.511 (17) |
Mo1—Cl4 | 2.406 (3) | C23—C24 | 1.51 (2) |
Mo1—Cl3 | 2.409 (3) | C28—C27 | 1.51 (2) |
Mo1—Cl1 | 2.425 (3) | C25—N2 | 1.488 (18) |
Mo4—O14 | 1.997 (7) | C25—C26 | 1.50 (3) |
Mo4—O12 | 2.063 (8) | C27—N2 | 1.495 (17) |
O14—Mo6—O10 | 81.2 (3) | O13—Mo1—Cl4 | 157.7 (2) |
O14—Mo6—O11 | 79.2 (3) | O6—Mo1—Cl4 | 84.7 (2) |
O10—Mo6—O11 | 92.5 (3) | O1—Mo1—Cl4 | 84.3 (3) |
O14—Mo6—Cl9 | 107.6 (2) | O13—Mo1—Cl3 | 107.3 (2) |
O10—Mo6—Cl9 | 171.1 (2) | O6—Mo1—Cl3 | 89.5 (2) |
O11—Mo6—Cl9 | 90.5 (2) | O1—Mo1—Cl3 | 172.1 (2) |
O14—Mo6—Cl12 | 157.5 (2) | Cl4—Mo1—Cl3 | 88.18 (12) |
O10—Mo6—Cl12 | 84.1 (2) | O13—Mo1—Cl1 | 106.8 (2) |
O11—Mo6—Cl12 | 84.5 (2) | O6—Mo1—Cl1 | 173.5 (2) |
Cl9—Mo6—Cl12 | 87.87 (11) | O1—Mo1—Cl1 | 89.3 (2) |
O14—Mo6—Cl8 | 106.7 (2) | Cl4—Mo1—Cl1 | 89.26 (11) |
O10—Mo6—Cl8 | 88.8 (2) | Cl3—Mo1—Cl1 | 88.16 (11) |
O11—Mo6—Cl8 | 174.0 (2) | O13—Mo1—Mo3 | 49.8 (2) |
Cl9—Mo6—Cl8 | 87.41 (11) | O6—Mo1—Mo3 | 84.9 (2) |
Cl12—Mo6—Cl8 | 89.86 (11) | O1—Mo1—Mo3 | 130.1 (2) |
O14—Mo6—Mo4 | 49.9 (2) | Cl4—Mo1—Mo3 | 144.41 (10) |
O10—Mo6—Mo4 | 130.7 (2) | Cl3—Mo1—Mo3 | 57.80 (8) |
O11—Mo6—Mo4 | 85.0 (2) | Cl1—Mo1—Mo3 | 98.90 (8) |
Cl9—Mo6—Mo4 | 57.94 (8) | O13—Mo1—Mo2 | 49.3 (2) |
Cl12—Mo6—Mo4 | 144.06 (9) | O6—Mo1—Mo2 | 128.7 (2) |
Cl8—Mo6—Mo4 | 98.51 (8) | O1—Mo1—Mo2 | 85.4 (2) |
O14—Mo6—Mo5 | 49.3 (2) | Cl4—Mo1—Mo2 | 145.42 (9) |
O10—Mo6—Mo5 | 85.3 (2) | Cl3—Mo1—Mo2 | 99.56 (8) |
O11—Mo6—Mo5 | 128.3 (2) | Cl1—Mo1—Mo2 | 57.68 (8) |
Cl9—Mo6—Mo5 | 99.42 (8) | Mo3—Mo1—Mo2 | 59.86 (4) |
Cl12—Mo6—Mo5 | 145.94 (9) | O14—Mo4—O12 | 80.5 (3) |
Cl8—Mo6—Mo5 | 57.62 (8) | O14—Mo4—O7 | 80.4 (3) |
Mo4—Mo6—Mo5 | 59.82 (4) | O12—Mo4—O7 | 91.4 (3) |
O13—Mo2—O2 | 80.8 (3) | O14—Mo4—Cl9 | 107.1 (2) |
O13—Mo2—O3 | 80.4 (3) | O12—Mo4—Cl9 | 89.8 (2) |
O2—Mo2—O3 | 92.6 (3) | O7—Mo4—Cl9 | 172.5 (2) |
O13—Mo2—Cl2 | 107.6 (2) | O14—Mo4—Cl10 | 160.1 (2) |
O2—Mo2—Cl2 | 171.5 (2) | O12—Mo4—Cl10 | 85.9 (2) |
O3—Mo2—Cl2 | 90.0 (3) | O7—Mo4—Cl10 | 85.6 (2) |
O13—Mo2—Cl5 | 157.9 (2) | Cl9—Mo4—Cl10 | 87.16 (12) |
O2—Mo2—Cl5 | 84.5 (2) | O14—Mo4—Cl7 | 106.9 (2) |
O3—Mo2—Cl5 | 83.9 (2) | O12—Mo4—Cl7 | 172.6 (2) |
Cl2—Mo2—Cl5 | 87.75 (12) | O7—Mo4—Cl7 | 89.0 (2) |
O13—Mo2—Cl1 | 107.2 (2) | Cl9—Mo4—Cl7 | 88.79 (11) |
O2—Mo2—Cl1 | 88.9 (2) | Cl10—Mo4—Cl7 | 86.72 (11) |
O3—Mo2—Cl1 | 172.4 (2) | O14—Mo4—Mo6 | 49.8 (2) |
Cl2—Mo2—Cl1 | 87.40 (11) | O12—Mo4—Mo6 | 85.7 (2) |
Cl5—Mo2—Cl1 | 88.84 (12) | O7—Mo4—Mo6 | 129.9 (2) |
O13—Mo2—Mo3 | 49.8 (2) | Cl9—Mo4—Mo6 | 57.54 (8) |
O2—Mo2—Mo3 | 130.3 (2) | Cl10—Mo4—Mo6 | 143.66 (10) |
O3—Mo2—Mo3 | 85.5 (2) | Cl7—Mo4—Mo6 | 99.71 (8) |
Cl2—Mo2—Mo3 | 57.99 (8) | O14—Mo4—Mo5 | 49.5 (2) |
Cl5—Mo2—Mo3 | 144.07 (10) | O12—Mo4—Mo5 | 129.8 (2) |
Cl1—Mo2—Mo3 | 99.17 (8) | O7—Mo4—Mo5 | 85.3 (2) |
O13—Mo2—Mo1 | 49.5 (2) | Cl9—Mo4—Mo5 | 99.54 (9) |
O2—Mo2—Mo1 | 85.2 (2) | Cl10—Mo4—Mo5 | 143.23 (9) |
O3—Mo2—Mo1 | 129.6 (2) | Cl7—Mo4—Mo5 | 57.59 (8) |
Cl2—Mo2—Mo1 | 99.28 (9) | Mo6—Mo4—Mo5 | 60.37 (4) |
Cl5—Mo2—Mo1 | 145.34 (10) | Mo5—Cl8—Mo6 | 64.49 (8) |
Cl1—Mo2—Mo1 | 57.94 (8) | Mo5—Cl7—Mo4 | 64.39 (8) |
Mo3—Mo2—Mo1 | 59.99 (4) | Mo6—Cl9—Mo4 | 64.52 (8) |
O13—Mo3—O5 | 80.6 (3) | Mo2—Cl1—Mo1 | 64.38 (8) |
O13—Mo3—O4 | 80.7 (3) | Mo1—Cl3—Mo3 | 64.57 (8) |
O5—Mo3—O4 | 92.1 (3) | Mo2—Cl2—Mo3 | 64.47 (8) |
O13—Mo3—Cl3 | 106.9 (2) | Mo5—O14—Mo6 | 81.1 (3) |
O5—Mo3—Cl3 | 89.1 (2) | Mo5—O14—Mo4 | 80.5 (3) |
O4—Mo3—Cl3 | 172.4 (3) | Mo6—O14—Mo4 | 80.3 (2) |
O13—Mo3—Cl6 | 159.4 (2) | Mo2—O13—Mo1 | 81.2 (3) |
O5—Mo3—Cl6 | 85.2 (2) | Mo2—O13—Mo3 | 80.7 (3) |
O4—Mo3—Cl6 | 84.9 (3) | Mo1—O13—Mo3 | 80.7 (3) |
Cl3—Mo3—Cl6 | 87.68 (12) | C9—O10—Mo6 | 122.4 (7) |
O13—Mo3—Cl2 | 106.8 (2) | C5—O5—Mo3 | 122.5 (7) |
O5—Mo3—Cl2 | 172.6 (2) | C11—O12—Mo4 | 122.8 (8) |
O4—Mo3—Cl2 | 89.5 (3) | C11—O11—Mo6 | 122.4 (7) |
Cl3—Mo3—Cl2 | 88.42 (11) | C9—O9—Mo5 | 122.6 (7) |
Cl6—Mo3—Cl2 | 87.73 (12) | C7—O8—Mo5 | 122.0 (8) |
O13—Mo3—Mo2 | 49.5 (2) | C1—O2—Mo2 | 122.3 (8) |
O5—Mo3—Mo2 | 129.8 (2) | C3—O3—Mo2 | 122.1 (8) |
O4—Mo3—Mo2 | 85.4 (2) | C7—O7—Mo4 | 123.4 (8) |
Cl3—Mo3—Mo2 | 99.66 (8) | C3—O4—Mo3 | 123.3 (8) |
Cl6—Mo3—Mo2 | 143.94 (10) | C1—O1—Mo1 | 122.4 (8) |
Cl2—Mo3—Mo2 | 57.54 (8) | C5—O6—Mo1 | 123.2 (8) |
O13—Mo3—Mo1 | 49.5 (2) | O12—C11—O11 | 123.6 (11) |
O5—Mo3—Mo1 | 85.4 (2) | O12—C11—C12 | 118.3 (12) |
O4—Mo3—Mo1 | 130.0 (2) | O11—C11—C12 | 118.0 (12) |
Cl3—Mo3—Mo1 | 57.64 (8) | O1—C1—O2 | 124.6 (12) |
Cl6—Mo3—Mo1 | 144.14 (10) | O1—C1—C2 | 118.2 (12) |
Cl2—Mo3—Mo1 | 99.08 (8) | O2—C1—C2 | 117.1 (13) |
Mo2—Mo3—Mo1 | 60.15 (4) | O3—C3—O4 | 123.6 (11) |
O14—Mo5—O9 | 80.5 (3) | O3—C3—C4 | 118.7 (12) |
O14—Mo5—O8 | 79.6 (3) | O4—C3—C4 | 117.7 (12) |
O9—Mo5—O8 | 92.3 (3) | O6—C5—O5 | 123.7 (11) |
O14—Mo5—Cl11 | 157.4 (2) | O6—C5—C6 | 119.1 (12) |
O9—Mo5—Cl11 | 84.4 (2) | O5—C5—C6 | 117.2 (11) |
O8—Mo5—Cl11 | 84.3 (2) | O9—C9—O10 | 124.4 (11) |
O14—Mo5—Cl7 | 107.7 (2) | O9—C9—C10 | 118.1 (11) |
O9—Mo5—Cl7 | 171.8 (2) | O10—C9—C10 | 117.5 (11) |
O8—Mo5—Cl7 | 89.8 (2) | O7—C7—O8 | 123.9 (11) |
Cl11—Mo5—Cl7 | 87.89 (11) | O7—C7—C8 | 119.0 (12) |
O14—Mo5—Cl8 | 107.2 (2) | O8—C7—C8 | 117.1 (11) |
O9—Mo5—Cl8 | 89.6 (2) | C14—C13—N1 | 114.3 (12) |
O8—Mo5—Cl8 | 173.1 (2) | N1—C17—C18 | 114.9 (11) |
Cl11—Mo5—Cl8 | 89.34 (11) | N1—C19—C20 | 115.6 (11) |
Cl7—Mo5—Cl8 | 87.52 (11) | C22—C21—N2 | 115.7 (12) |
O14—Mo5—Mo4 | 49.9 (2) | C16—C15—N1 | 116.2 (12) |
O9—Mo5—Mo4 | 130.1 (2) | N2—C23—C24 | 116.2 (12) |
O8—Mo5—Mo4 | 85.2 (2) | N2—C25—C26 | 116.2 (15) |
Cl11—Mo5—Mo4 | 144.26 (9) | N2—C27—C28 | 115.8 (13) |
Cl7—Mo5—Mo4 | 58.02 (8) | C19—N1—C15 | 106.7 (10) |
Cl8—Mo5—Mo4 | 98.69 (9) | C19—N1—C17 | 111.3 (11) |
O14—Mo5—Mo6 | 49.6 (2) | C15—N1—C17 | 111.0 (11) |
O9—Mo5—Mo6 | 85.3 (2) | C19—N1—C13 | 111.2 (10) |
O8—Mo5—Mo6 | 128.8 (2) | C15—N1—C13 | 111.4 (10) |
Cl11—Mo5—Mo6 | 145.66 (9) | C17—N1—C13 | 105.3 (10) |
Cl7—Mo5—Mo6 | 99.60 (8) | C25—N2—C27 | 111.5 (13) |
Cl8—Mo5—Mo6 | 57.90 (8) | C25—N2—C23 | 111.3 (12) |
Mo4—Mo5—Mo6 | 59.80 (4) | C27—N2—C23 | 106.9 (11) |
O13—Mo1—O6 | 79.7 (3) | C25—N2—C21 | 105.9 (12) |
O13—Mo1—O1 | 80.6 (3) | C27—N2—C21 | 110.2 (12) |
O6—Mo1—O1 | 92.2 (3) | C23—N2—C21 | 111.1 (11) |
Experimental details
Crystal data | |
Chemical formula | (C2H5N)[Mo3Cl6O(C2H3O2)3] |
Mr | 823.90 |
Crystal system, space group | Triclinic, 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) |
V (Å3) | 2774.80 (6) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 1.95 |
Crystal size (mm) | 0.84 × 0.20 × 0.02 |
Data collection | |
Diffractometer | Siemens SMART CCD diffractometer |
Absorption correction | Empirical (using intensity measurements) (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.680, 1.000 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 14579, 9771, 7292 |
Rint | 0.041 |
(sin θ/λ)max (Å−1) | 0.598 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.071, 0.157, 1.07 |
No. of reflections | 9771 |
No. of parameters | 559 |
H-atom treatment | H-atom parameters constrained |
w = 1/[σ2(Fo2) + 55.1956P] where P = (Fo2 + 2Fc2)/3 | |
Δρmax, Δρmin (e Å−3) | 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.
Mo6—O14 | 1.995 (7) | Mo3—Cl2 | 2.417 (3) |
Mo6—O10 | 2.071 (7) | Mo3—Mo1 | 2.5756 (13) |
Mo6—O11 | 2.079 (7) | Mo5—O14 | 1.986 (7) |
Mo6—Cl9 | 2.406 (3) | Mo5—O9 | 2.070 (7) |
Mo6—Cl12 | 2.415 (3) | Mo5—O8 | 2.092 (7) |
Mo6—Cl8 | 2.430 (3) | Mo5—Cl11 | 2.404 (3) |
Mo6—Mo4 | 2.5746 (14) | Mo5—Cl7 | 2.411 (3) |
Mo6—Mo5 | 2.5894 (14) | Mo5—Cl8 | 2.423 (3) |
Mo2—O13 | 1.981 (7) | Mo5—Mo4 | 2.5751 (14) |
Mo2—O2 | 2.078 (8) | Mo1—O13 | 1.985 (7) |
Mo2—O3 | 2.089 (8) | Mo1—O6 | 2.070 (8) |
Mo2—Cl2 | 2.405 (3) | Mo1—O1 | 2.080 (8) |
Mo2—Cl5 | 2.406 (3) | Mo1—Cl4 | 2.406 (3) |
Mo2—Cl1 | 2.418 (3) | Mo1—Cl3 | 2.409 (3) |
Mo2—Mo3 | 2.5722 (14) | Mo1—Cl1 | 2.425 (3) |
Mo2—Mo1 | 2.5798 (14) | Mo4—O14 | 1.997 (7) |
Mo3—O13 | 1.992 (7) | Mo4—O12 | 2.063 (8) |
Mo3—O5 | 2.068 (8) | Mo4—O7 | 2.070 (8) |
Mo3—O4 | 2.068 (8) | Mo4—Cl9 | 2.417 (3) |
Mo3—Cl3 | 2.413 (3) | Mo4—Cl10 | 2.419 (3) |
Mo3—Cl6 | 2.414 (3) | Mo4—Cl7 | 2.422 (3) |
O14—Mo6—O10 | 81.2 (3) | O8—Mo5—Cl8 | 173.1 (2) |
O14—Mo6—O11 | 79.2 (3) | Cl11—Mo5—Cl8 | 89.34 (11) |
O10—Mo6—O11 | 92.5 (3) | Cl7—Mo5—Cl8 | 87.52 (11) |
O14—Mo6—Cl9 | 107.6 (2) | O14—Mo5—Mo4 | 49.9 (2) |
O10—Mo6—Cl9 | 171.1 (2) | O9—Mo5—Mo4 | 130.1 (2) |
O11—Mo6—Cl9 | 90.5 (2) | O8—Mo5—Mo4 | 85.2 (2) |
O14—Mo6—Cl12 | 157.5 (2) | Cl11—Mo5—Mo4 | 144.26 (9) |
O10—Mo6—Cl12 | 84.1 (2) | Cl7—Mo5—Mo4 | 58.02 (8) |
O11—Mo6—Cl12 | 84.5 (2) | Cl8—Mo5—Mo4 | 98.69 (9) |
Cl9—Mo6—Cl12 | 87.87 (11) | O14—Mo5—Mo6 | 49.6 (2) |
O14—Mo6—Cl8 | 106.7 (2) | O9—Mo5—Mo6 | 85.3 (2) |
O10—Mo6—Cl8 | 88.8 (2) | O8—Mo5—Mo6 | 128.8 (2) |
O11—Mo6—Cl8 | 174.0 (2) | Cl11—Mo5—Mo6 | 145.66 (9) |
Cl9—Mo6—Cl8 | 87.41 (11) | Cl7—Mo5—Mo6 | 99.60 (8) |
Cl12—Mo6—Cl8 | 89.86 (11) | Cl8—Mo5—Mo6 | 57.90 (8) |
O14—Mo6—Mo4 | 49.9 (2) | Mo4—Mo5—Mo6 | 59.80 (4) |
O10—Mo6—Mo4 | 130.7 (2) | O13—Mo1—O6 | 79.7 (3) |
O11—Mo6—Mo4 | 85.0 (2) | O13—Mo1—O1 | 80.6 (3) |
Cl9—Mo6—Mo4 | 57.94 (8) | O6—Mo1—O1 | 92.2 (3) |
Cl12—Mo6—Mo4 | 144.06 (9) | O13—Mo1—Cl4 | 157.7 (2) |
Cl8—Mo6—Mo4 | 98.51 (8) | O6—Mo1—Cl4 | 84.7 (2) |
O14—Mo6—Mo5 | 49.3 (2) | O1—Mo1—Cl4 | 84.3 (3) |
O10—Mo6—Mo5 | 85.3 (2) | O13—Mo1—Cl3 | 107.3 (2) |
O11—Mo6—Mo5 | 128.3 (2) | O6—Mo1—Cl3 | 89.5 (2) |
Cl9—Mo6—Mo5 | 99.42 (8) | O1—Mo1—Cl3 | 172.1 (2) |
Cl12—Mo6—Mo5 | 145.94 (9) | Cl4—Mo1—Cl3 | 88.18 (12) |
Cl8—Mo6—Mo5 | 57.62 (8) | O13—Mo1—Cl1 | 106.8 (2) |
Mo4—Mo6—Mo5 | 59.82 (4) | O6—Mo1—Cl1 | 173.5 (2) |
O13—Mo2—O2 | 80.8 (3) | O1—Mo1—Cl1 | 89.3 (2) |
O13—Mo2—O3 | 80.4 (3) | Cl4—Mo1—Cl1 | 89.26 (11) |
O2—Mo2—O3 | 92.6 (3) | Cl3—Mo1—Cl1 | 88.16 (11) |
O13—Mo2—Cl2 | 107.6 (2) | O13—Mo1—Mo3 | 49.8 (2) |
O2—Mo2—Cl2 | 171.5 (2) | O6—Mo1—Mo3 | 84.9 (2) |
O3—Mo2—Cl2 | 90.0 (3) | O1—Mo1—Mo3 | 130.1 (2) |
O13—Mo2—Cl5 | 157.9 (2) | Cl4—Mo1—Mo3 | 144.41 (10) |
O2—Mo2—Cl5 | 84.5 (2) | Cl3—Mo1—Mo3 | 57.80 (8) |
O3—Mo2—Cl5 | 83.9 (2) | Cl1—Mo1—Mo3 | 98.90 (8) |
Cl2—Mo2—Cl5 | 87.75 (12) | O13—Mo1—Mo2 | 49.3 (2) |
O13—Mo2—Cl1 | 107.2 (2) | O6—Mo1—Mo2 | 128.7 (2) |
O2—Mo2—Cl1 | 88.9 (2) | O1—Mo1—Mo2 | 85.4 (2) |
O3—Mo2—Cl1 | 172.4 (2) | Cl4—Mo1—Mo2 | 145.42 (9) |
Cl2—Mo2—Cl1 | 87.40 (11) | Cl3—Mo1—Mo2 | 99.56 (8) |
Cl5—Mo2—Cl1 | 88.84 (12) | Cl1—Mo1—Mo2 | 57.68 (8) |
O13—Mo2—Mo3 | 49.8 (2) | Mo3—Mo1—Mo2 | 59.86 (4) |
O2—Mo2—Mo3 | 130.3 (2) | O14—Mo4—O12 | 80.5 (3) |
O3—Mo2—Mo3 | 85.5 (2) | O14—Mo4—O7 | 80.4 (3) |
Cl2—Mo2—Mo3 | 57.99 (8) | O12—Mo4—O7 | 91.4 (3) |
Cl5—Mo2—Mo3 | 144.07 (10) | O14—Mo4—Cl9 | 107.1 (2) |
Cl1—Mo2—Mo3 | 99.17 (8) | O12—Mo4—Cl9 | 89.8 (2) |
O13—Mo2—Mo1 | 49.5 (2) | O7—Mo4—Cl9 | 172.5 (2) |
O2—Mo2—Mo1 | 85.2 (2) | O14—Mo4—Cl10 | 160.1 (2) |
O3—Mo2—Mo1 | 129.6 (2) | O12—Mo4—Cl10 | 85.9 (2) |
Cl2—Mo2—Mo1 | 99.28 (9) | O7—Mo4—Cl10 | 85.6 (2) |
Cl5—Mo2—Mo1 | 145.34 (10) | Cl9—Mo4—Cl10 | 87.16 (12) |
Cl1—Mo2—Mo1 | 57.94 (8) | O14—Mo4—Cl7 | 106.9 (2) |
Mo3—Mo2—Mo1 | 59.99 (4) | O12—Mo4—Cl7 | 172.6 (2) |
O13—Mo3—O5 | 80.6 (3) | O7—Mo4—Cl7 | 89.0 (2) |
O13—Mo3—O4 | 80.7 (3) | Cl9—Mo4—Cl7 | 88.79 (11) |
O5—Mo3—O4 | 92.1 (3) | Cl10—Mo4—Cl7 | 86.72 (11) |
O13—Mo3—Cl3 | 106.9 (2) | O14—Mo4—Mo6 | 49.8 (2) |
O5—Mo3—Cl3 | 89.1 (2) | O12—Mo4—Mo6 | 85.7 (2) |
O4—Mo3—Cl3 | 172.4 (3) | O7—Mo4—Mo6 | 129.9 (2) |
O13—Mo3—Cl6 | 159.4 (2) | Cl9—Mo4—Mo6 | 57.54 (8) |
O5—Mo3—Cl6 | 85.2 (2) | Cl10—Mo4—Mo6 | 143.66 (10) |
O4—Mo3—Cl6 | 84.9 (3) | Cl7—Mo4—Mo6 | 99.71 (8) |
Cl3—Mo3—Cl6 | 87.68 (12) | O14—Mo4—Mo5 | 49.5 (2) |
O13—Mo3—Cl2 | 106.8 (2) | O12—Mo4—Mo5 | 129.8 (2) |
O5—Mo3—Cl2 | 172.6 (2) | O7—Mo4—Mo5 | 85.3 (2) |
O4—Mo3—Cl2 | 89.5 (3) | Cl9—Mo4—Mo5 | 99.54 (9) |
Cl3—Mo3—Cl2 | 88.42 (11) | Cl10—Mo4—Mo5 | 143.23 (9) |
Cl6—Mo3—Cl2 | 87.73 (12) | Cl7—Mo4—Mo5 | 57.59 (8) |
O13—Mo3—Mo2 | 49.5 (2) | Mo6—Mo4—Mo5 | 60.37 (4) |
O5—Mo3—Mo2 | 129.8 (2) | Mo5—Cl8—Mo6 | 64.49 (8) |
O4—Mo3—Mo2 | 85.4 (2) | Mo5—Cl7—Mo4 | 64.39 (8) |
Cl3—Mo3—Mo2 | 99.66 (8) | Mo6—Cl9—Mo4 | 64.52 (8) |
Cl6—Mo3—Mo2 | 143.94 (10) | Mo2—Cl1—Mo1 | 64.38 (8) |
Cl2—Mo3—Mo2 | 57.54 (8) | Mo1—Cl3—Mo3 | 64.57 (8) |
O13—Mo3—Mo1 | 49.5 (2) | Mo2—Cl2—Mo3 | 64.47 (8) |
O5—Mo3—Mo1 | 85.4 (2) | Mo5—O14—Mo6 | 81.1 (3) |
O4—Mo3—Mo1 | 130.0 (2) | Mo5—O14—Mo4 | 80.5 (3) |
Cl3—Mo3—Mo1 | 57.64 (8) | Mo6—O14—Mo4 | 80.3 (2) |
Cl6—Mo3—Mo1 | 144.14 (10) | Mo2—O13—Mo1 | 81.2 (3) |
Cl2—Mo3—Mo1 | 99.08 (8) | Mo2—O13—Mo3 | 80.7 (3) |
Mo2—Mo3—Mo1 | 60.15 (4) | Mo1—O13—Mo3 | 80.7 (3) |
O14—Mo5—O9 | 80.5 (3) | C9—O10—Mo6 | 122.4 (7) |
O14—Mo5—O8 | 79.6 (3) | C5—O5—Mo3 | 122.5 (7) |
O9—Mo5—O8 | 92.3 (3) | C11—O12—Mo4 | 122.8 (8) |
O14—Mo5—Cl11 | 157.4 (2) | C11—O11—Mo6 | 122.4 (7) |
O9—Mo5—Cl11 | 84.4 (2) | C9—O9—Mo5 | 122.6 (7) |
O8—Mo5—Cl11 | 84.3 (2) | C7—O8—Mo5 | 122.0 (8) |
O14—Mo5—Cl7 | 107.7 (2) | C1—O2—Mo2 | 122.3 (8) |
O9—Mo5—Cl7 | 171.8 (2) | C3—O3—Mo2 | 122.1 (8) |
O8—Mo5—Cl7 | 89.8 (2) | C7—O7—Mo4 | 123.4 (8) |
Cl11—Mo5—Cl7 | 87.89 (11) | C3—O4—Mo3 | 123.3 (8) |
O14—Mo5—Cl8 | 107.2 (2) | C1—O1—Mo1 | 122.4 (8) |
O9—Mo5—Cl8 | 89.6 (2) | C5—O6—Mo1 | 123.2 (8) |
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A series of trinuclear Mo3 cluster compounds with the cluster anions {[Mo3(µ3-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.