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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

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802010966/bt6149sup1.cif
Contains datablocks MoOCl~4~H~2~O, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536802010966/bt6149Isup2.hkl
Contains datablock I

CCDC reference: 189876

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](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


Yellow Alert 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

Computing details top

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
C8H22Cl4MoNO2Dx = 1.687 Mg m3
Mr = 402.01Melting point: not measured K
Orthorhombic, PnmaMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2nCell parameters from 1886 reflections
a = 10.9913 (3) Åθ = 5.1–27.5°
b = 12.6073 (5) ŵ = 1.48 mm1
c = 11.4222 (3) ÅT = 293 K
V = 1582.78 Å3Block, bright green
Z = 40.15 × 0.15 × 0.15 mm
F(000) = 812.0
Data collection top
Nonius KappaCCD
diffractometer
1402 reflections with I > 3σ(I)
Graphite monochromatorRint = 0.022
2θ/ω scansθmax = 27.5°, θmin = 5.1°
Absorption correction: multi-scan
(DENZO/SCALEPACK; Otwinowski & Minor, 1997)
h = 1414
Tmin = 0.801, Tmax = 0.801k = 1616
10054 measured reflectionsl = 1414
1886 independent reflections
Refinement top
Refinement on FPrimary atom site location: Direct_Methods
Least-squares matrix: fullHydrogen site location: geometric
R[F2 > 2σ(F2)] = 0.031H 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 reflectionsΔρmax = 0.38 e Å3
100 parametersΔρmin = 0.49 e Å3
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Mo10.76702 (3)0.75000.40739 (3)0.0302
Cl10.84771 (8)0.88059 (7)0.27812 (7)0.0457
Cl20.64352 (9)0.61832 (8)0.49478 (9)0.0516
O10.8766 (3)0.75000.5049 (3)0.0486
O20.6062 (3)0.75000.2717 (3)0.0447
N10.7373 (3)0.25000.3888 (3)0.0305
C10.6180 (4)0.1094 (3)0.2799 (4)0.0584
C20.8575 (4)0.3890 (3)0.4980 (4)0.0567
C30.8522 (5)0.3191 (5)0.3856 (5)0.03900.5000
C40.7390 (5)0.3207 (5)0.4983 (5)0.03640.5000
C50.6250 (5)0.1783 (5)0.3924 (5)0.03580.5000
C60.7346 (5)0.1794 (5)0.2804 (5)0.04120.5000
H10.561 (3)0.695 (3)0.279 (3)0.0500*
H100.54430.06310.28340.0500*0.5000
H110.69250.06420.27400.0500*0.5000
H120.61270.15660.20970.0500*0.5000
H200.63010.13090.46240.0500*0.5000
H210.55030.22330.39800.0500*0.5000
H300.80800.13250.28050.0500*0.5000
H310.73540.22500.20880.0500*0.5000
H400.93240.43400.49600.0500*0.5000
H410.85970.34230.56880.0500*0.5000
H420.78390.43550.50140.0500*0.5000
H500.92580.27250.38220.0500*0.5000
H510.85000.36580.31490.0500*0.5000
H600.73710.27530.57010.0500*0.5000
H610.66630.36840.49780.0500*0.5000
H700.61770.06370.20830.0500*0.5000
H710.61700.06360.35130.0500*0.5000
H720.54440.15610.27960.0500*0.5000
H800.85910.43520.56920.0500*0.5000
H810.93010.34120.49850.0500*0.5000
H820.85930.43440.42620.0500*0.5000
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mo10.0244 (2)0.0388 (2)0.0289 (2)0.00000.0003 (1)0.0000
Cl10.0488 (5)0.0408 (5)0.0533 (5)0.0028 (4)0.0143 (4)0.0051 (4)
Cl20.0526 (5)0.0506 (5)0.0627 (6)0.0037 (4)0.0186 (4)0.0133 (5)
O10.036 (2)0.089 (3)0.038 (2)0.00000.009 (1)0.0000
O20.032 (2)0.061 (2)0.048 (2)0.00000.008 (2)0.0000
N10.026 (2)0.040 (2)0.027 (2)0.00000.004 (1)0.0000
C10.064 (2)0.047 (2)0.085 (3)0.001 (2)0.031 (2)0.012 (2)
C20.075 (3)0.039 (2)0.087 (3)0.009 (2)0.041 (2)0.002 (2)
C30.029 (3)0.050 (4)0.046 (4)0.008 (3)0.003 (3)0.010 (3)
C40.043 (3)0.042 (4)0.028 (3)0.004 (3)0.003 (3)0.005 (3)
C50.028 (3)0.040 (4)0.045 (4)0.008 (3)0.005 (3)0.002 (3)
C60.045 (3)0.051 (4)0.034 (3)0.007 (3)0.004 (3)0.010 (3)
Geometric parameters (Å, º) top
Mo1—Cl12.3827 (9)C1—H121.000 (4)
Mo1—Cl1i2.3827 (9)C1—H701.000 (4)
Mo1—Cl22.3654 (9)C1—H711.000 (4)
Mo1—Cl2i2.3654 (9)C1—H721.000 (4)
Mo1—O11.641 (3)C2—C31.559 (4)
Mo1—O22.351 (3)C2—C41.561 (4)
O2—H10.86 (3)C2—H401.000 (4)
O2—H1i0.86 (3)C2—H411.000 (4)
N1—C31.534 (6)C2—H421.000 (4)
N1—C3ii1.534 (6)C2—H801.000 (4)
N1—C41.537 (6)C2—H811.000 (4)
N1—C4ii1.537 (6)C2—H821.000 (4)
N1—C51.530 (6)C3—H501.000 (6)
N1—C5ii1.530 (6)C3—H511.000 (6)
N1—C61.524 (6)C4—H601.000 (6)
N1—C6ii1.524 (6)C4—H611.000 (6)
C1—C51.553 (4)C5—H201.000 (6)
C1—C61.556 (4)C5—H211.000 (6)
C1—H101.000 (4)C6—H301.000 (7)
C1—H111.000 (4)C6—H311.000 (6)
Cl1—Mo1—Cl1i87.41 (4)C5—C1—H12109.5 (4)
Cl1—Mo1—Cl2163.75 (4)H10—C1—H12109.5 (3)
Cl1i—Mo1—Cl289.44 (3)H11—C1—H12109.5 (4)
Cl1—Mo1—Cl2i89.44 (3)C6—C1—H70109.5 (4)
Cl1i—Mo1—Cl2i163.75 (4)C6—C1—H71109.5 (4)
Cl2—Mo1—Cl2i89.15 (5)C6—C1—H72109.5 (4)
Cl1—Mo1—O198.47 (9)H70—C1—H71109.5 (4)
Cl1i—Mo1—O198.47 (9)H70—C1—H72109.5 (3)
Cl2—Mo1—O197.75 (9)H71—C1—H72109.5 (4)
Cl2i—Mo1—O197.75 (9)C3—C2—H40109.5 (4)
Cl1—Mo1—O282.60 (7)C3—C2—H41109.5 (4)
Cl1i—Mo1—O282.60 (7)H40—C2—H41109.5 (3)
Cl2—Mo1—O281.19 (7)C3—C2—H42109.5 (4)
Cl2i—Mo1—O281.19 (7)H40—C2—H42109.5 (4)
O1—Mo1—O2178.5 (1)H41—C2—H42109.5 (4)
Mo1—O2—H1112 (3)C4—C2—H81109.5 (4)
Mo1—O2—H1i112 (3)C4—C2—H82109.5 (4)
H1—O2—H1i108 (5)H80—C2—H81109.5 (3)
C3—N1—C3ii69.2 (5)H80—C2—H82109.5 (4)
C3—N1—C471.3 (3)H81—C2—H82109.5 (4)
C3ii—N1—C4109.8 (4)N1—C3—C2109.4 (4)
C3—N1—C4ii109.8 (4)N1—C3—H50109.5 (5)
C3ii—N1—C4ii71.3 (3)C2—C3—H50109.5 (5)
C3ii—N1—C5109.2 (3)N1—C3—H51109.5 (5)
C4—N1—C5109.3 (3)C2—C3—H51109.5 (5)
C4ii—N1—C569.2 (3)H50—C3—H51109.5 (5)
C3—N1—C5ii109.2 (3)N1—C4—C2109.1 (4)
C3ii—N1—C5ii178.4 (4)N1—C4—H60109.6 (5)
C4—N1—C5ii69.2 (3)C2—C4—H60109.6 (5)
C4ii—N1—C5ii109.3 (3)N1—C4—H61109.6 (5)
C5—N1—C5ii72.4 (5)C2—C4—H61109.6 (5)
C3—N1—C6109.3 (3)H60—C4—H61109.5 (5)
C3ii—N1—C670.5 (3)N1—C5—C1110.4 (4)
C4—N1—C6179.5 (3)N1—C5—H20109.3 (4)
C4ii—N1—C6108.8 (3)C1—C5—H20109.3 (5)
C5—N1—C670.2 (3)N1—C5—H21109.2 (5)
C3—N1—C6ii70.5 (3)C1—C5—H21109.2 (5)
C3ii—N1—C6ii109.2 (3)H20—C5—H21109.5 (5)
C4—N1—C6ii108.8 (3)N1—C6—C1110.5 (4)
C5—N1—C6ii110.5 (4)N1—C6—H30109.2 (5)
C5ii—N1—C6110.5 (4)C1—C6—H30109.2 (5)
C5—C1—H10109.5 (4)N1—C6—H31109.2 (5)
C5—C1—H11109.5 (4)C1—C6—H31109.2 (5)
H10—C1—H11109.5 (3)H30—C6—H31109.5 (5)
Symmetry codes: (i) x, y+3/2, z; (ii) x, y+1/2, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O2—H1···Cl1iii0.86 (3)2.61 (3)3.332 (3)142 (1)
Symmetry code: (iii) x1/2, y+3/2, z+1/2.
 

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