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The six Mo atoms in the title compound, (C
4H
12N)
2[Mo
6O
19].H
2O, form a standard octahedral cage through bridging O atoms. The [Mo
6O
19]
2- anion as a whole has O
h symmetry with three crystallographic fourfold axes aligned along Mo-O-Mo. There exist weak O
O hydrogen bonds (O100
O3 2.951 Å) between the terminal O3 atoms of the anions and O100 atoms of the solvate hydrates in the unit cell.
Supporting information
CCDC reference: 142936
The title compound was obtained in an attempt to synthesize new polyoxomolybdates in both reaction systems of Na2MoO4·2H2O (2.0 g, 8.3 mmol), (CHO)2 (3 ml), 3.5% HCl (1 ml), NH4VO3 (1.0 g, 8.6 mmol), [(CH3)4N]Br (1.0 g, 6.5 mmol) and H2O (60 ml), or of Na2MoO4·2H2O (2.15 g, 8.9 mmol), NH4VO3 (0.5 g, 4.3 mmol), [(CH3)4N]Cl (2.0 g, 18.2 mmol), NH2OH·HCl (3.14 g, 45.2 mmol), Al2O3 (234.51 mg, 2.3 mmol) and H2O (110 ml).
The H atom on C1 was located and refined isotropically. The water H atoms were not located.
Data collection: Enraf-Nonius CONTROL software; cell refinement: MolEN/VAX (Fair, 1990); data reduction: MolEN/VAX (Fair, 1990); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); software used to prepare material for publication: SHELXL97 (Sheldrick, 1997).
Bis(tetramethylammonium)Nonadecaoxohexamolybdenum(VI) Solvate Hydrate
top
Crystal data top
(C4H12N)2[Mo6O19]·H2O | Dx = 2.635 Mg m−3 |
Mr = 1043.93 | Mo Kα radiation, λ = 0.71073 Å |
Cubic, Fm3m | Cell parameters from 25 reflections |
Hall symbol: -F 4 2 3 | θ = 15.4–16.6° |
a = 13.8148 (16) Å | µ = 2.85 mm−1 |
V = 2636.5 (5) Å3 | T = 293 K |
Z = 4 | Octahedron, orange–red |
F(000) = 2000 | 0.53 × 0.48 × 0.45 mm |
Data collection top
Enraf-Nonius CAD-4 II diffractometer | Rint = 0.047 |
Radiation source: fine-focus sealed tube | θmax = 25.9°, θmin = 2.6° |
Graphite monochromator | h = −9→16 |
ω–2θ scans | k = −15→12 |
1396 measured reflections | l = −16→9 |
167 independent reflections | 3 standard reflections every 300 reflections |
149 reflections with I > 2σ(I) | intensity decay: none |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.034 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.095 | w = 1/[σ2(Fo2) + (0.0431P)2 + 29.6855P] where P = (Fo2 + 2Fc2)/3 |
S = 1.33 | (Δ/σ)max < 0.001 |
167 reflections | Δρmax = 0.70 e Å−3 |
21 parameters | Δρmin = −0.40 e Å−3 |
4 restraints | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0013 (2) |
Crystal data top
(C4H12N)2[Mo6O19]·H2O | Z = 4 |
Mr = 1043.93 | Mo Kα radiation |
Cubic, Fm3m | µ = 2.85 mm−1 |
a = 13.8148 (16) Å | T = 293 K |
V = 2636.5 (5) Å3 | 0.53 × 0.48 × 0.45 mm |
Data collection top
Enraf-Nonius CAD-4 II diffractometer | Rint = 0.047 |
1396 measured reflections | 3 standard reflections every 300 reflections |
167 independent reflections | intensity decay: none |
149 reflections with I > 2σ(I) | |
Refinement top
R[F2 > 2σ(F2)] = 0.034 | 4 restraints |
wR(F2) = 0.095 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.33 | w = 1/[σ2(Fo2) + (0.0431P)2 + 29.6855P] where P = (Fo2 + 2Fc2)/3 |
167 reflections | Δρmax = 0.70 e Å−3 |
21 parameters | Δρmin = −0.40 e Å−3 |
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 | x | y | z | Uiso*/Ueq | |
Mo1 | 0 | 0.66666 (8) | 0.5000 | 0.0387 (7) | |
N1 | 0.2500 | 0.7500 | 0.2500 | 0.032 (4) | |
C1 | 0.1884 (7) | 0.8116 (7) | 0.3116 (7) | 0.061 (4) | |
H1 | 0.1481 (7) | 0.766 (2) | 0.3519 (7) | 0.06 (2)* | |
O1 | 0 | 0.5000 | 0.5000 | 0.025 (4) | |
O2 | 0 | 0.6351 (3) | 0.6351 (3) | 0.0366 (15) | |
O3 | 0 | 0.7864 (7) | 0.5000 | 0.048 (3) | |
O100 | 0 | 1 | 0.5000 | 0.047 (6) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Mo1 | 0.0432 (7) | 0.0295 (9) | 0.0432 (7) | 0.000 | 0.000 | 0.000 |
N1 | 0.032 (4) | 0.032 (4) | 0.032 (4) | 0.000 | 0.000 | 0.000 |
C1 | 0.061 (4) | 0.061 (4) | 0.061 (4) | 0.011 (4) | 0.011 (4) | −0.011 (4) |
O1 | 0.025 (4) | 0.025 (4) | 0.025 (4) | 0.000 | 0.000 | 0.000 |
O2 | 0.047 (4) | 0.031 (2) | 0.031 (2) | 0.000 | 0.000 | −0.004 (3) |
O3 | 0.058 (4) | 0.028 (5) | 0.058 (4) | 0.000 | 0.000 | 0.000 |
O100 | 0.047 (6) | 0.047 (6) | 0.047 (6) | 0.000 | 0.000 | 0.000 |
Geometric parameters (Å, º) top
Mo1—O3 | 1.654 (10) | N1—C1vi | 1.474 (16) |
Mo1—O2 | 1.916 (3) | N1—C1 | 1.474 (16) |
Mo1—O2i | 1.916 (3) | O1—Mo1vii | 2.3023 (12) |
Mo1—O2ii | 1.916 (3) | O1—Mo1viii | 2.3023 (12) |
Mo1—O2iii | 1.916 (3) | O1—Mo1ix | 2.3023 (12) |
Mo1—O1 | 2.3023 (12) | O1—Mo1x | 2.3023 (12) |
N1—C1iv | 1.474 (16) | O1—Mo1iii | 2.3023 (12) |
N1—C1v | 1.474 (16) | O2—Mo1ix | 1.916 (3) |
| | | |
O3—Mo1—O2 | 103.17 (17) | C1v—N1—C1 | 109.471 (1) |
O3—Mo1—O2i | 103.17 (17) | C1vi—N1—C1 | 109.5 |
O2—Mo1—O2i | 153.7 (3) | Mo1—O1—Mo1vii | 90.0 |
O3—Mo1—O2ii | 103.17 (17) | Mo1—O1—Mo1viii | 180.0 |
O2—Mo1—O2ii | 87.02 (8) | Mo1vii—O1—Mo1viii | 90.0 |
O2i—Mo1—O2ii | 87.02 (8) | Mo1—O1—Mo1ix | 90.0 |
O3—Mo1—O2iii | 103.17 (17) | Mo1vii—O1—Mo1ix | 90.0 |
O2—Mo1—O2iii | 87.02 (8) | Mo1viii—O1—Mo1ix | 90.0 |
O2i—Mo1—O2iii | 87.02 (8) | Mo1—O1—Mo1x | 90.0 |
O2ii—Mo1—O2iii | 153.7 (3) | Mo1vii—O1—Mo1x | 90.0 |
O3—Mo1—O1 | 180.000 (2) | Mo1viii—O1—Mo1x | 90.0 |
O2—Mo1—O1 | 76.83 (17) | Mo1ix—O1—Mo1x | 180.0 |
O2i—Mo1—O1 | 76.83 (17) | Mo1—O1—Mo1iii | 90.0 |
O2ii—Mo1—O1 | 76.83 (17) | Mo1vii—O1—Mo1iii | 180.0 |
O2iii—Mo1—O1 | 76.83 (17) | Mo1viii—O1—Mo1iii | 90.0 |
C1iv—N1—C1v | 109.471 (2) | Mo1ix—O1—Mo1iii | 90.0 |
C1iv—N1—C1vi | 109.471 (1) | Mo1x—O1—Mo1iii | 90.0 |
C1v—N1—C1vi | 109.471 (5) | Mo1—O2—Mo1ix | 116.3 (3) |
C1iv—N1—C1 | 109.471 (1) | | |
Symmetry codes: (i) x, y, −z+1; (ii) −y+1/2, z, −x+1/2; (iii) y−1/2, z, x+1/2; (iv) x, −y+3/2, −z+1/2; (v) −x+1/2, y, −z+1/2; (vi) −x+1/2, −y+3/2, z; (vii) −y+1/2, −z+1, −x+1/2; (viii) −x, −y+1, −z+1; (ix) z−1/2, x+1/2, y; (x) −z+1/2, −x+1/2, −y+1. |
Experimental details
Crystal data |
Chemical formula | (C4H12N)2[Mo6O19]·H2O |
Mr | 1043.93 |
Crystal system, space group | Cubic, Fm3m |
Temperature (K) | 293 |
a (Å) | 13.8148 (16) |
V (Å3) | 2636.5 (5) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 2.85 |
Crystal size (mm) | 0.53 × 0.48 × 0.45 |
|
Data collection |
Diffractometer | Enraf-Nonius CAD-4 II diffractometer |
Absorption correction | – |
No. of measured, independent and observed [I > 2σ(I)] reflections | 1396, 167, 149 |
Rint | 0.047 |
(sin θ/λ)max (Å−1) | 0.614 |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | 0.034, 0.095, 1.33 |
No. of reflections | 167 |
No. of parameters | 21 |
No. of restraints | 4 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
| w = 1/[σ2(Fo2) + (0.0431P)2 + 29.6855P] where P = (Fo2 + 2Fc2)/3 |
Δρmax, Δρmin (e Å−3) | 0.70, −0.40 |
Selected geometric parameters (Å, º) topMo1—O3 | 1.654 (10) | Mo1—O1 | 2.3023 (12) |
Mo1—O2 | 1.916 (3) | | |
| | | |
O3—Mo1—O2 | 103.17 (17) | O2—Mo1—O1 | 76.83 (17) |
O3—Mo1—O1 | 180.000 (2) | | |
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The title compound has the same anion as the following compounds: C12H37N9P3+ (Allcock et al., 1973), C20H40MoN4S8+ (Garner et al., 1978), C12H24O6K+·H2O (Nagano & Sasaki, 1979), Ph4As+ (Clegg et al., 1982), C16H36N+ (Dahlstrom et al., 1982; Rheingold et al., 1993; Boyle et al., 1998), C22H22O2P+ and C22H22P+ (Arzoumanian et al., 1985), C12H24O6·H3O+ (Shoemaker et al., 1986), C39H33Mo2O4P2+ (Riera et al., 1988), C14H21ClN2Rh+ (Zhang et al., 1989), C10H8S8+ (Triki et al., 1991), C6H4S4+ (Attanasio et al., 1991; Triki et al., 1992), C20H30N10Re24+ (Bernstein & Dunbar, 1992), C15H35C11FeN5O52+ (Lu et al., 1992), C20H16S4+ (Triki et al., 1994), C8H20N+ (Liu et al., 1995), C14H20FeN+ (Veya & Kochi, 1995), C16H19N2+ (Xu et al., 1995), C20H21N2+ (Xu et al., 1995), C23H17O+ (Xu et al., 1996), C20H28NaO8+ (Lu et al., 1996), C16H16N2S2+ (Bellec et al., 1997), C72H60AgP4+ (Long et al., 1997) and C36H30NP2+ (Hoppe et al., 1997).