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The single-crystal synchrotron study of the high-pressure modification of aluminium oxide hydroxide, δ-AlOOH, confirms the previous structure determination in the space group P21nm, which was based on X-ray powder data [Suzuki, Ohtani & Kamada (2000). Phys. Chem. Miner. 27, 689–693]. The present study includes the determination of the H-atom parameters, which revealed a strong asymmetric hydrogen bond with an O...O distance of 2.5479 (12) Å. The δ-AlOOH structure is isotypic with that of β-CrOOH and may be considered as a distorted rutile type with all atoms located on mirror planes.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680603916X/wm2048sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S160053680603916X/wm2048Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal synchrotron study
  • T = 297 K
  • Mean [sigma](l-O) = 0.001 Å
  • R factor = 0.014
  • wR factor = 0.041
  • Data-to-parameter ratio = 11.9

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT115_ALERT_5_B ADDSYM Detects Noncrystallographic Inversion ... 100 PerFi
Alert level C PLAT128_ALERT_4_C Non-standard setting of Space group Pmn21 .... P21nm
Alert level G ABSMU_01 Radiation type not identified. Calculation of _exptl_absorpt_correction_mu not performed. REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is correct. If it is not, please give the correct count in the _publ_section_exptl_refinement section of the submitted CIF. From the CIF: _diffrn_reflns_theta_max 42.48 From the CIF: _reflns_number_total 262 Count of symmetry unique reflns 262 Completeness (_total/calc) 100.00% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 0 Fraction of Friedel pairs measured 0.000 Are heavy atom types Z>Si present no
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 1 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 0 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 2 ALERT type 4 Improvement, methodology, query or suggestion 1 ALERT type 5 Informative message, check

Computing details top

Data collection: 10A.EXE (Tanaka & Sasaki, 1993); cell refinement: MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1991); data reduction: TEXSAN (Molecular Structure Corporation, 1999); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: VESTA (Momma & Izumi, 2006); software used to prepare material for publication: SHELXL97.

Aluminium oxide hydroxide top
Crystal data top
AlO(OH)F(000) = 60
Mr = 59.99Dx = 3.536 Mg m3
Orthorhombic, P21nmSynchrotron radiation, λ = 0.7007 (1) Å
Hall symbol: P -2 2acCell parameters from 56 reflections
a = 4.7128 (11) Åθ = 6.4–14.8°
b = 4.2221 (15) ŵ = 1.05 mm1
c = 2.8315 (7) ÅT = 297 K
V = 56.34 (3) Å3Prism, colourless
Z = 20.04 × 0.04 × 0.04 mm
Data collection top
Tsukuba-BL-10A
diffractometer
θmax = 42.5°, θmin = 4.8°
Radiation source: synchrotronh = 99
ω/2θ scansk = 88
1633 measured reflectionsl = 55
262 independent reflections3 standard reflections every 50 reflections
262 reflections with I > 2σ(I) intensity decay: none
Rint = 0.034
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.014All H-atom parameters refined
wR(F2) = 0.041 w = 1/[σ2(Fo2) + (0.0183P)2 + 0.0106P]
where P = (Fo2 + 2Fc2)/3
S = 1.33(Δ/σ)max < 0.001
262 reflectionsΔρmax = 0.33 e Å3
22 parametersΔρmin = 0.35 e Å3
0 restraintsExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 1.01 (12)
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
xyzUiso*/Ueq
Al10.00000.27452 (7)0.00000.00298 (9)
O10.3420 (2)0.49850 (17)0.00000.00329 (12)
O20.64559 (19)0.00084 (17)0.00000.00356 (13)
H10.547 (13)0.157 (8)0.00000.034 (10)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Al10.00333 (13)0.00324 (12)0.00238 (12)0.00001 (15)0.0000.000
O10.0033 (3)0.0035 (2)0.0031 (2)0.00084 (19)0.0000.000
O20.0037 (3)0.0030 (2)0.0040 (2)0.00001 (19)0.0000.000
Geometric parameters (Å, º) top
Al1—O1i1.8647 (6)Al1—Al1vii2.8315 (7)
Al1—O1ii1.8647 (6)O1—Al1viii1.8647 (6)
Al1—O11.8688 (10)O1—Al1ix1.8647 (6)
Al1—O2iii1.9520 (7)O2—Al1x1.9520 (7)
Al1—O2iv1.9520 (7)O2—Al1xi1.9520 (7)
Al1—O2v2.0351 (10)O2—Al1xii2.0351 (10)
Al1—Al1vi2.8315 (7)
O1i—Al1—O1ii98.79 (4)O1—Al1—Al1vi90.0
O1i—Al1—O194.84 (2)O2iii—Al1—Al1vi136.49 (2)
O1ii—Al1—O194.84 (2)O2iv—Al1—Al1vi43.51 (2)
O1i—Al1—O2iii174.41 (4)O2v—Al1—Al1vi90.0
O1ii—Al1—O2iii83.91 (3)O1i—Al1—Al1vii139.40 (2)
O1—Al1—O2iii89.79 (4)O1ii—Al1—Al1vii40.60 (2)
O1i—Al1—O2iv83.91 (3)O1—Al1—Al1vii90.0
O1ii—Al1—O2iv174.41 (4)O2iii—Al1—Al1vii43.51 (2)
O1—Al1—O2iv89.79 (4)O2iv—Al1—Al1vii136.49 (2)
O2iii—Al1—O2iv92.98 (4)O2v—Al1—Al1vii90.0
O1i—Al1—O2v88.05 (4)Al1vi—Al1—Al1vii180.000 (12)
O1ii—Al1—O2v88.05 (4)Al1viii—O1—Al1ix98.79 (4)
O1—Al1—O2v175.56 (4)Al1viii—O1—Al1127.19 (3)
O2iii—Al1—O2v87.15 (2)Al1ix—O1—Al1127.19 (3)
O2iv—Al1—O2v87.15 (2)Al1x—O2—Al1xi92.98 (4)
O1i—Al1—Al1vi40.60 (2)Al1x—O2—Al1xii128.81 (3)
O1ii—Al1—Al1vi139.40 (2)Al1xi—O2—Al1xii128.81 (3)
Symmetry codes: (i) x1/2, y+1, z+1/2; (ii) x1/2, y+1, z1/2; (iii) x1/2, y, z1/2; (iv) x1/2, y, z+1/2; (v) x1, y, z; (vi) x, y, z+1; (vii) x, y, z1; (viii) x+1/2, y+1, z+1/2; (ix) x+1/2, y+1, z1/2; (x) x+1/2, y, z1/2; (xi) x+1/2, y, z+1/2; (xii) x+1, y, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O2—H1···O10.81 (4)1.74 (4)2.5479 (12)179 (6)
 

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