The title compound contains [MoOCl4(H2O)]- distorted octahedral anions with a short Mo-O bond of length 1.641 (3) Å trans to the H2O group. These units are linked by hydrogen bonds between the H2O group and chlorines of neighbouring anions to form infinite chains. Charge balance is achieved by [Et4N]+ cations which exhibit twofold disorder.
Supporting information
CCDC reference: 189876
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (Mo-O) = 0.003 Å
- Disorder in solvent or counterion
- R factor = 0.031
- wR factor = 0.028
- Data-to-parameter ratio = 14.0
checkCIF results
No syntax errors found
ADDSYM reports no extra symmetry
Alert Level C:
CRYSC_01 Alert C The word below has not been recognised as a standard
identifier.
bright
PLAT_302 Alert C Anion/Solvent Disorder ....................... 20.00 Perc.
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
2 Alert Level C = Please check
Data collection: COLLECT (Nonius, 1997); cell refinement: DENZO/SCALEPACK (Otwinowski and Minor, 1996); data reduction: DENZO/SCALEPACK (Otwinowski & Minor, 1997); program(s) used to solve structure: SIR92 (Altomare et al., 1992); program(s) used to refine structure: CRYSTALS (Watkin et al., 1996); molecular graphics: ATOMS (Shape Software, 1998); software used to prepare material for publication: CRYSTALS.
Tetraethylammonium aquatetrachlorooxomolybdenum(V)
top
Crystal data top
C8H22Cl4MoNO2 | Dx = 1.687 Mg m−3 |
Mr = 402.01 | Melting point: not measured K |
Orthorhombic, Pnma | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ac 2n | Cell parameters from 1886 reflections |
a = 10.9913 (3) Å | θ = 5.1–27.5° |
b = 12.6073 (5) Å | µ = 1.48 mm−1 |
c = 11.4222 (3) Å | T = 293 K |
V = 1582.78 Å3 | Block, bright green |
Z = 4 | 0.15 × 0.15 × 0.15 mm |
F(000) = 812.0 | |
Data collection top
Nonius KappaCCD diffractometer | 1402 reflections with I > 3σ(I) |
Graphite monochromator | Rint = 0.022 |
2θ/ω scans | θmax = 27.5°, θmin = 5.1° |
Absorption correction: multi-scan (DENZO/SCALEPACK; Otwinowski & Minor, 1997) | h = −14→14 |
Tmin = 0.801, Tmax = 0.801 | k = −16→16 |
10054 measured reflections | l = −14→14 |
1886 independent reflections | |
Refinement top
Refinement on F | Primary atom site location: Direct_Methods |
Least-squares matrix: full | Hydrogen site location: geometric |
R[F2 > 2σ(F2)] = 0.031 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.028 | Chebychev polynomial with 3 parameters (Carruthers & Watkin, 1979),
0.213, 0.0203 and -0.0593 |
S = 1.15 | (Δ/σ)max = 0.000343 |
1402 reflections | Δρmax = 0.38 e Å−3 |
100 parameters | Δρmin = −0.49 e Å−3 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Mo1 | 0.76702 (3) | 0.7500 | 0.40739 (3) | 0.0302 | |
Cl1 | 0.84771 (8) | 0.88059 (7) | 0.27812 (7) | 0.0457 | |
Cl2 | 0.64352 (9) | 0.61832 (8) | 0.49478 (9) | 0.0516 | |
O1 | 0.8766 (3) | 0.7500 | 0.5049 (3) | 0.0486 | |
O2 | 0.6062 (3) | 0.7500 | 0.2717 (3) | 0.0447 | |
N1 | 0.7373 (3) | 0.2500 | 0.3888 (3) | 0.0305 | |
C1 | 0.6180 (4) | 0.1094 (3) | 0.2799 (4) | 0.0584 | |
C2 | 0.8575 (4) | 0.3890 (3) | 0.4980 (4) | 0.0567 | |
C3 | 0.8522 (5) | 0.3191 (5) | 0.3856 (5) | 0.0390 | 0.5000 |
C4 | 0.7390 (5) | 0.3207 (5) | 0.4983 (5) | 0.0364 | 0.5000 |
C5 | 0.6250 (5) | 0.1783 (5) | 0.3924 (5) | 0.0358 | 0.5000 |
C6 | 0.7346 (5) | 0.1794 (5) | 0.2804 (5) | 0.0412 | 0.5000 |
H1 | 0.561 (3) | 0.695 (3) | 0.279 (3) | 0.0500* | |
H10 | 0.5443 | 0.0631 | 0.2834 | 0.0500* | 0.5000 |
H11 | 0.6925 | 0.0642 | 0.2740 | 0.0500* | 0.5000 |
H12 | 0.6127 | 0.1566 | 0.2097 | 0.0500* | 0.5000 |
H20 | 0.6301 | 0.1309 | 0.4624 | 0.0500* | 0.5000 |
H21 | 0.5503 | 0.2233 | 0.3980 | 0.0500* | 0.5000 |
H30 | 0.8080 | 0.1325 | 0.2805 | 0.0500* | 0.5000 |
H31 | 0.7354 | 0.2250 | 0.2088 | 0.0500* | 0.5000 |
H40 | 0.9324 | 0.4340 | 0.4960 | 0.0500* | 0.5000 |
H41 | 0.8597 | 0.3423 | 0.5688 | 0.0500* | 0.5000 |
H42 | 0.7839 | 0.4355 | 0.5014 | 0.0500* | 0.5000 |
H50 | 0.9258 | 0.2725 | 0.3822 | 0.0500* | 0.5000 |
H51 | 0.8500 | 0.3658 | 0.3149 | 0.0500* | 0.5000 |
H60 | 0.7371 | 0.2753 | 0.5701 | 0.0500* | 0.5000 |
H61 | 0.6663 | 0.3684 | 0.4978 | 0.0500* | 0.5000 |
H70 | 0.6177 | 0.0637 | 0.2083 | 0.0500* | 0.5000 |
H71 | 0.6170 | 0.0636 | 0.3513 | 0.0500* | 0.5000 |
H72 | 0.5444 | 0.1561 | 0.2796 | 0.0500* | 0.5000 |
H80 | 0.8591 | 0.4352 | 0.5692 | 0.0500* | 0.5000 |
H81 | 0.9301 | 0.3412 | 0.4985 | 0.0500* | 0.5000 |
H82 | 0.8593 | 0.4344 | 0.4262 | 0.0500* | 0.5000 |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Mo1 | 0.0244 (2) | 0.0388 (2) | 0.0289 (2) | 0.0000 | 0.0003 (1) | 0.0000 |
Cl1 | 0.0488 (5) | 0.0408 (5) | 0.0533 (5) | −0.0028 (4) | 0.0143 (4) | 0.0051 (4) |
Cl2 | 0.0526 (5) | 0.0506 (5) | 0.0627 (6) | −0.0037 (4) | 0.0186 (4) | 0.0133 (5) |
O1 | 0.036 (2) | 0.089 (3) | 0.038 (2) | 0.0000 | −0.009 (1) | 0.0000 |
O2 | 0.032 (2) | 0.061 (2) | 0.048 (2) | 0.0000 | −0.008 (2) | 0.0000 |
N1 | 0.026 (2) | 0.040 (2) | 0.027 (2) | 0.0000 | 0.004 (1) | 0.0000 |
C1 | 0.064 (2) | 0.047 (2) | 0.085 (3) | −0.001 (2) | −0.031 (2) | −0.012 (2) |
C2 | 0.075 (3) | 0.039 (2) | 0.087 (3) | −0.009 (2) | −0.041 (2) | −0.002 (2) |
C3 | 0.029 (3) | 0.050 (4) | 0.046 (4) | −0.008 (3) | 0.003 (3) | 0.010 (3) |
C4 | 0.043 (3) | 0.042 (4) | 0.028 (3) | 0.004 (3) | 0.003 (3) | −0.005 (3) |
C5 | 0.028 (3) | 0.040 (4) | 0.045 (4) | −0.008 (3) | 0.005 (3) | 0.002 (3) |
C6 | 0.045 (3) | 0.051 (4) | 0.034 (3) | 0.007 (3) | −0.004 (3) | −0.010 (3) |
Geometric parameters (Å, º) top
Mo1—Cl1 | 2.3827 (9) | C1—H12 | 1.000 (4) |
Mo1—Cl1i | 2.3827 (9) | C1—H70 | 1.000 (4) |
Mo1—Cl2 | 2.3654 (9) | C1—H71 | 1.000 (4) |
Mo1—Cl2i | 2.3654 (9) | C1—H72 | 1.000 (4) |
Mo1—O1 | 1.641 (3) | C2—C3 | 1.559 (4) |
Mo1—O2 | 2.351 (3) | C2—C4 | 1.561 (4) |
O2—H1 | 0.86 (3) | C2—H40 | 1.000 (4) |
O2—H1i | 0.86 (3) | C2—H41 | 1.000 (4) |
N1—C3 | 1.534 (6) | C2—H42 | 1.000 (4) |
N1—C3ii | 1.534 (6) | C2—H80 | 1.000 (4) |
N1—C4 | 1.537 (6) | C2—H81 | 1.000 (4) |
N1—C4ii | 1.537 (6) | C2—H82 | 1.000 (4) |
N1—C5 | 1.530 (6) | C3—H50 | 1.000 (6) |
N1—C5ii | 1.530 (6) | C3—H51 | 1.000 (6) |
N1—C6 | 1.524 (6) | C4—H60 | 1.000 (6) |
N1—C6ii | 1.524 (6) | C4—H61 | 1.000 (6) |
C1—C5 | 1.553 (4) | C5—H20 | 1.000 (6) |
C1—C6 | 1.556 (4) | C5—H21 | 1.000 (6) |
C1—H10 | 1.000 (4) | C6—H30 | 1.000 (7) |
C1—H11 | 1.000 (4) | C6—H31 | 1.000 (6) |
| | | |
Cl1—Mo1—Cl1i | 87.41 (4) | C5—C1—H12 | 109.5 (4) |
Cl1—Mo1—Cl2 | 163.75 (4) | H10—C1—H12 | 109.5 (3) |
Cl1i—Mo1—Cl2 | 89.44 (3) | H11—C1—H12 | 109.5 (4) |
Cl1—Mo1—Cl2i | 89.44 (3) | C6—C1—H70 | 109.5 (4) |
Cl1i—Mo1—Cl2i | 163.75 (4) | C6—C1—H71 | 109.5 (4) |
Cl2—Mo1—Cl2i | 89.15 (5) | C6—C1—H72 | 109.5 (4) |
Cl1—Mo1—O1 | 98.47 (9) | H70—C1—H71 | 109.5 (4) |
Cl1i—Mo1—O1 | 98.47 (9) | H70—C1—H72 | 109.5 (3) |
Cl2—Mo1—O1 | 97.75 (9) | H71—C1—H72 | 109.5 (4) |
Cl2i—Mo1—O1 | 97.75 (9) | C3—C2—H40 | 109.5 (4) |
Cl1—Mo1—O2 | 82.60 (7) | C3—C2—H41 | 109.5 (4) |
Cl1i—Mo1—O2 | 82.60 (7) | H40—C2—H41 | 109.5 (3) |
Cl2—Mo1—O2 | 81.19 (7) | C3—C2—H42 | 109.5 (4) |
Cl2i—Mo1—O2 | 81.19 (7) | H40—C2—H42 | 109.5 (4) |
O1—Mo1—O2 | 178.5 (1) | H41—C2—H42 | 109.5 (4) |
Mo1—O2—H1 | 112 (3) | C4—C2—H81 | 109.5 (4) |
Mo1—O2—H1i | 112 (3) | C4—C2—H82 | 109.5 (4) |
H1—O2—H1i | 108 (5) | H80—C2—H81 | 109.5 (3) |
C3—N1—C3ii | 69.2 (5) | H80—C2—H82 | 109.5 (4) |
C3—N1—C4 | 71.3 (3) | H81—C2—H82 | 109.5 (4) |
C3ii—N1—C4 | 109.8 (4) | N1—C3—C2 | 109.4 (4) |
C3—N1—C4ii | 109.8 (4) | N1—C3—H50 | 109.5 (5) |
C3ii—N1—C4ii | 71.3 (3) | C2—C3—H50 | 109.5 (5) |
C3ii—N1—C5 | 109.2 (3) | N1—C3—H51 | 109.5 (5) |
C4—N1—C5 | 109.3 (3) | C2—C3—H51 | 109.5 (5) |
C4ii—N1—C5 | 69.2 (3) | H50—C3—H51 | 109.5 (5) |
C3—N1—C5ii | 109.2 (3) | N1—C4—C2 | 109.1 (4) |
C3ii—N1—C5ii | 178.4 (4) | N1—C4—H60 | 109.6 (5) |
C4—N1—C5ii | 69.2 (3) | C2—C4—H60 | 109.6 (5) |
C4ii—N1—C5ii | 109.3 (3) | N1—C4—H61 | 109.6 (5) |
C5—N1—C5ii | 72.4 (5) | C2—C4—H61 | 109.6 (5) |
C3—N1—C6 | 109.3 (3) | H60—C4—H61 | 109.5 (5) |
C3ii—N1—C6 | 70.5 (3) | N1—C5—C1 | 110.4 (4) |
C4—N1—C6 | 179.5 (3) | N1—C5—H20 | 109.3 (4) |
C4ii—N1—C6 | 108.8 (3) | C1—C5—H20 | 109.3 (5) |
C5—N1—C6 | 70.2 (3) | N1—C5—H21 | 109.2 (5) |
C3—N1—C6ii | 70.5 (3) | C1—C5—H21 | 109.2 (5) |
C3ii—N1—C6ii | 109.2 (3) | H20—C5—H21 | 109.5 (5) |
C4—N1—C6ii | 108.8 (3) | N1—C6—C1 | 110.5 (4) |
C5—N1—C6ii | 110.5 (4) | N1—C6—H30 | 109.2 (5) |
C5ii—N1—C6 | 110.5 (4) | C1—C6—H30 | 109.2 (5) |
C5—C1—H10 | 109.5 (4) | N1—C6—H31 | 109.2 (5) |
C5—C1—H11 | 109.5 (4) | C1—C6—H31 | 109.2 (5) |
H10—C1—H11 | 109.5 (3) | H30—C6—H31 | 109.5 (5) |
Symmetry codes: (i) x, −y+3/2, z; (ii) x, −y+1/2, z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O2—H1···Cl1iii | 0.86 (3) | 2.61 (3) | 3.332 (3) | 142 (1) |
Symmetry code: (iii) x−1/2, −y+3/2, −z+1/2. |