The crystal structure of Ba3(AlO4)H is isotypic with Ba3SiS5 and contains AlO45- and H- anions. The hydride and oxide anions are coordinated by six Ba and five Ba/one Al atoms in an octahedral geometry. The hydrogen content was examined by MAS-NMR experiments of the deuterated compound.
Supporting information
Data collection: SMART (Bruker, 1999); cell refinement: SAINT (Bruker, 1999); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP (Johnson, 1968) and DRAWxtl (Finger & Kroeker, 1999); software used to prepare material for publication: SHELXL97.
barium oxo-aluminate hydride
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Crystal data top
Ba3[AlO4][H] | F(000) = 856 |
Mr = 504.01 | Dx = 5.406 Mg m−3 |
Orthorhombic, Pnma | Mo Kα radiation, λ = 0.71070 Å |
Hall symbol: -P 2ac 2n | Cell parameters from 2363 reflections |
a = 10.4889 (8) Å | θ = 6.3–56.5° |
b = 8.1503 (9) Å | µ = 18.93 mm−1 |
c = 7.2440 (12) Å | T = 293 K |
V = 619.27 (13) Å3 | Irregular, clear_light_red |
Z = 4 | 0.17 × 0.12 × 0.10 mm |
Data collection top
Bruker AXS, CCD diffractometer | 810 independent reflections |
Radiation source: fine-focus sealed tube | 752 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.029 |
ω scans | θmax = 28.3°, θmin = 3.4° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −13→13 |
Tmin = 0.467, Tmax = 1.0 | k = −6→10 |
3661 measured reflections | l = −9→8 |
Refinement top
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)] = 0.023 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.054 | All H-atom parameters refined |
S = 1.13 | w = 1/[σ2(Fo2) + (0.0328P)2] where P = (Fo2 + 2Fc2)/3 |
810 reflections | (Δ/σ)max = 0.025 |
46 parameters | Δρmax = 1.05 e Å−3 |
0 restraints | Δρmin = −2.26 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 | |
Ba1 | 0.33491 (2) | 0.02502 (3) | 0.10190 (4) | 0.01025 (11) | |
Ba2 | 0.46337 (3) | 0.2500 | 0.59881 (5) | 0.00871 (12) | |
Al1 | 0.10373 (15) | 0.2500 | 0.3110 (3) | 0.0072 (3) | |
O1 | 0.0725 (3) | 0.0660 (4) | 0.1951 (5) | 0.0137 (6) | |
O2 | 0.0113 (4) | 0.2500 | 0.5170 (7) | 0.0112 (8) | |
O3 | 0.2678 (4) | 0.2500 | 0.3706 (6) | 0.0126 (9) | |
H1 | 0.224 (7) | 0.2500 | 0.822 (13) | 0.07 (2)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ba1 | 0.01116 (17) | 0.00649 (17) | 0.01310 (17) | 0.00021 (8) | 0.00083 (9) | −0.00146 (8) |
Ba2 | 0.01006 (19) | 0.00640 (19) | 0.0097 (2) | 0.000 | −0.00052 (12) | 0.000 |
Al1 | 0.0094 (8) | 0.0041 (7) | 0.0080 (8) | 0.000 | −0.0013 (7) | 0.000 |
O1 | 0.0165 (15) | 0.0075 (14) | 0.0173 (16) | −0.0019 (11) | 0.0025 (13) | −0.0031 (13) |
O2 | 0.012 (2) | 0.0094 (18) | 0.012 (2) | 0.000 | 0.0045 (17) | 0.000 |
O3 | 0.0105 (19) | 0.015 (2) | 0.012 (2) | 0.000 | −0.0024 (17) | 0.000 |
Bond lengths (Å) top
Ba1—O2i | 2.744 (3) | H1—Ba1vii | 2.82 (5) |
Ba1—O3 | 2.766 (3) | H1—Ba1xi | 2.97 (7) |
Ba1—H1ii | 2.82 (5) | H1—Ba1xii | 2.97 (7) |
Ba1—O2ii | 2.829 (3) | H1—Ba2 | 2.98 (8) |
Ba1—O1 | 2.854 (3) | O1—Al1 | 1.750 (3) |
Ba1—O1iii | 2.913 (3) | O1—Ba2ii | 2.694 (3) |
Ba1—H1iv | 2.97 (7) | O1—Ba2xiii | 2.844 (3) |
Ba1—O3ii | 2.998 (3) | O1—Ba1 | 2.854 (3) |
Ba1—O1v | 3.191 (3) | O1—Ba1xiv | 2.913 (3) |
Ba2—O3 | 2.635 (4) | O1—Ba1vii | 3.191 (3) |
Ba2—O1vi | 2.694 (3) | O2—Al1 | 1.780 (5) |
Ba2—O1vii | 2.694 (3) | O2—Ba1xiii | 2.744 (3) |
Ba2—H1viii | 2.80 (7) | O2—Ba1xiv | 2.744 (3) |
Ba2—O2viii | 2.828 (5) | O2—Ba2x | 2.828 (5) |
Ba2—O1i | 2.844 (3) | O2—Ba1vi | 2.829 (3) |
Ba2—O1iii | 2.844 (3) | O2—Ba1vii | 2.829 (3) |
Ba2—H1 | 2.98 (8) | O3—Al1 | 1.774 (5) |
Al1—O1ix | 1.750 (3) | O3—Ba2 | 2.635 (4) |
Al1—O1 | 1.750 (3) | O3—Ba1 | 2.766 (3) |
Al1—O3 | 1.774 (5) | O3—Ba1ix | 2.766 (3) |
Al1—O2 | 1.780 (5) | O3—Ba1vi | 2.998 (3) |
H1—Ba2x | 2.80 (7) | O3—Ba1vii | 2.998 (3) |
H1—Ba1vi | 2.82 (5) | | |
Symmetry codes: (i) x+1/2, −y+1/2, −z+1/2; (ii) −x+1/2, y−1/2, z−1/2; (iii) x+1/2, y, −z+1/2; (iv) x, y, z−1; (v) −x+1/2, −y, z−1/2; (vi) −x+1/2, y+1/2, z+1/2; (vii) −x+1/2, −y, z+1/2; (viii) x+1/2, −y+1/2, −z+3/2; (ix) x, −y+1/2, z; (x) x−1/2, −y+1/2, −z+3/2; (xi) x, −y+1/2, z+1; (xii) x, y, z+1; (xiii) x−1/2, −y+1/2, −z+1/2; (xiv) x−1/2, y, −z+1/2. |