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Mixed lithium/ammonium perchlorate, Li0.41(NH4)0.59ClO4, has been prepared by gel diffusion using agar agar gel as the medium of growth at ambient temperature. The Cl and mixed Li/N atoms are located on the 4a ({1 \over 2}{1 \over 2}{1 \over 2}) and 4b ({1 \over 2}, 0, {1 \over 4}) special positions, respectively, in the space group I\overline 42d. The structure features a twofold inter­penetrated three-dimensional entanglement architecture, in which single three-dimensional networks are constructed from tetra­hedral coordination based on [-(ClO4)-(Li/NH4)-(ClO4)-][infinity] diamondoid arrays. A com­parison of the crystal structures of Li0.41(NH4)0.59ClO4, LiClO4·3H2O, LiClO4 and NH4ClO4 is given.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270113005684/ov3020sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270113005684/ov3020Isup2.hkl
Contains datablock I

Computing details top

Data collection: APEX2 (Bruker, 2010); cell refinement: APEX2 (Bruker, 2010); data reduction: APEX2 (Bruker, 2010); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg, 1999); software used to prepare material for publication: WinGX (Farrugia, 2012) and publCIF (Westrip, 2010).

Lithium/ammonium perchlorate top
Crystal data top
Li0.41(NH4)0.59ClO4Dx = 1.774 Mg m3
Mr = 112.92Mo Kα radiation, λ = 0.71073 Å
Tetragonal, I42dCell parameters from 1503 reflections
Hall symbol: I -4 2bwθ = 3.8–33.6°
a = 7.4946 (2) ŵ = 0.78 mm1
c = 7.5457 (2) ÅT = 293 K
V = 423.83 (2) Å3Parallelepiped, colourless
Z = 40.23 × 0.23 × 0.18 mm
F(000) = 227
Data collection top
Bruker APEXII CCD area-detector
diffractometer
488 independent reflections
Radiation source: fine-focus sealed tube456 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.033
ω scansθmax = 35.4°, θmin = 3.8°
Absorption correction: multi-scan
(Blessing, 1995)
h = 1212
Tmin = 0.829, Tmax = 0.85k = 1212
4093 measured reflectionsl = 1012
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.035All H-atom parameters refined
wR(F2) = 0.139 w = 1/[σ2(Fo2) + (0.0794P)2 + 0.1679P]
where P = (Fo2 + 2Fc2)/3
S = 1.33(Δ/σ)max < 0.001
488 reflectionsΔρmax = 0.88 e Å3
18 parametersΔρmin = 0.56 e Å3
4 restraintsAbsolute structure: Flack (1983) and Hooft et al. (2008), with 3875 Bijvoet pairs
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.22 (17)
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*/UeqOcc. (<1)
Cl10.50000.50000.50000.0218 (2)
O10.4152 (2)0.3535 (2)0.3858 (2)0.0240 (4)
Li10.50000.00000.25000.0197 (11)0.41 (3)
N10.50000.00000.25000.0197 (11)0.59 (3)
H10.605 (2)0.018 (11)0.1733 (15)0.030*0.59 (3)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cl10.0190 (3)0.0190 (3)0.0275 (4)0.0000.0000.000
O10.0199 (7)0.0209 (6)0.0309 (7)0.0038 (5)0.0062 (6)0.0095 (6)
Li10.0230 (14)0.0230 (14)0.0130 (15)0.0000.0000.000
N10.0230 (14)0.0230 (14)0.0130 (15)0.0000.0000.000
Geometric parameters (Å, º) top
Cl1—O11.5339 (15)Cl1—O1ii1.5339 (15)
Cl1—O1i1.5339 (15)Cl1—O1iii1.5339 (15)
O1—Cl1—O1i108.41 (7)O1—Cl1—O1iii108.41 (7)
O1—Cl1—O1ii111.61 (14)O1i—Cl1—O1iii111.61 (14)
O1i—Cl1—O1ii108.41 (7)O1ii—Cl1—O1iii108.41 (7)
Symmetry codes: (i) y+1, x, z+1; (ii) x+1, y+1, z; (iii) y, x+1, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1···O1iv0.99 (2)1.98 (2)2.9108 (15)157 (2)
Symmetry code: (iv) y+1/2, x+1/2, z+1/2.
 

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