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Indium arsenate(V) monohydrate, InAsO4·H2O, (I), crystallizes in the structure type of MnMoO4·H2O. The structure is built of In2O8(H2O)2 dimers (mean In-O = 2.150 Å) corner-linked to slightly distorted AsO4 tetra­hedra (mean As-O = 1.686 Å). The linkage results in a three-dimensional framework, with small voids into which the apical water ligand of the InO5(H2O) octa­hedron points. The hydrogen bonds in (I) are of medium strength. Lead(II) indium arsenate(V) hydrogen arsenate(V), PbIn(AsO4)(AsO3OH), (II), represents the first reported lead indium arsenate. It is characterized by a framework structure of InO6 octa­hedra corner-linked to AsO4 and AsO3OH tetra­hedra. The resulting voids are occupied by Pb2O10(OH)2 dimers built of two edge-sharing highly distorted PbO6(OH) polyhedra (mean Pb-O = 2.623 Å). The compound is isotypic with PbFeIII(AsO4)(AsO3OH). The average In-O bond length in (II) is 2.157 Å. In both arsenates, all atoms are in general positions.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270105022894/iz1060sup1.cif
Contains datablocks global, I, II

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270105022894/iz1060Isup2.hkl
Contains datablock I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270105022894/iz1060IIsup3.hkl
Contains datablock II

Comment top

InAsO4·H2O, indium arsenate(V) monohydrate, (I), and PbIn(AsO4)(AsO3OH), lead(II) indium arsenate(V) hydrogen arsenate(V), (II), were obtained during an ongoing systematic study of the crystallography and crystal chemistry of metal–MIII arsenates (M = Al, Ga, In, Sc, Cr and Fe), which were synthesized by hydrothermal methods.

Compound (I) is a previously unknown indium arsenate compound. It has a triclinic crystal structure (space group P1) and is isotypic with its Sc analogue ScAsO4·H2O (Kolitsch & Schwendtner, 2004), its phosphate analogue InPO4·H2O (Tang & Lachgar, 1998), the vanadate schubnelite FeIIIVO4·H2O (Schindler & Hawthorne, 1999), and the molybdates and tungstates MIIXO4·H2O (M = Mg and Mn; X = Mo and W; Clearfield et al., 1985; Amberg et al., 1988).

Other known indium arsenates(V) are InAsO4·2H2O (Chen et al., 2002; Tang et al., 2002) and InAsO4. The former adopts the structure type of variscite (AlPO4·2H2O), and is also known in nature as the mineral yanomatite (Botelho et al., 1994). The crystal structure of InAsO4 appears to be unknown, although its unindexed X-ray powder diffraction pattern (Ezhova et al., 1977) suggests it may be isostructural with orthorhombic InPO4 (Mooney, 1956).

The asymmetric unit of (I) contains one crystallographically non-equivalent In atom, one As atom and five O atoms, all of which are located in general positions (Figs. 1 and 2). The O ligand OW5 represents a water molecule. The In atom is octahedrally coordinated to six O ligands (including OW5), with an average In—O bond length of 2.150 Å (Table 1). The somewhat distorted InO5(H2O) octahedron shares one O1—O1' edge with another crystallographically equivalent octahedron, thus forming an In2O8(H2O)2 dimer. As expected from In–In repulsion across the shared edge, this edge represents the shortest O—O distance within the dimeric unit. The In2O8(H2O)2 dimers are corner-linked to slightly distorted AsO4 tetrahedra (mean As—O = 1.686 Å). The linkage results in a three-dimensional framework with small voids into which the apical water ligand (OW5) of the InO5(H2O) octahedron points.

The positions of the H atoms in (I) are close to those in MgMoO4·H2O (Amberg et al., 1988). The hydrogen bonds are of medium strength (Table 2). The hydrogen-bonding schemes in isotypic InPO4·H2O (Tang & Lachgar, 1998) and ScAsO4·H2O (Kolitsch & Schwendtner, 2004) are practically identical to that in (I). Bond-valence sums for all atoms were calculated using the bond-valence parameters of Brese & O'Keeffe (1991). The bond-valence sums are 3.09 (In), 4.99 (As), 2.02 (O1), 1.80 (O2), 1.97 (O3), 1.81 (O4) and 0.49 v.u. (valence units) (OW5), and thus are all reasonably close to ideal valencies. The somewhat undersatured O2 and O4 ligands are acceptors of the two hydrogen bonds (Table 2).

Compound (I) represents the first inorganic compound containing an In2O8(H2O)2 dimer. A closely related, equally unique, In2O9(H2O)1 dimer is present in In2(HPO3)3(H2O) (Yi et al., 2005). In contrast, water-free In2O10 dimers have been reported in several indium compounds, such as α-LiIn(MoO4)2 (Velikodnyi et al., 1980), CaIn2(PO4)2(HPO4) (Tang & Lachgar, 1996), Na3In2(PO4)3 and Na3In2(AsO4)3 (Lii & Ye, 1997), and In2O(PO4) (Thauern & Glaum, 2004).

The unit-cell volume of (I) is slightly smaller than that of the Sc analogue ScAsO4·H2O [201.21 (6) Å3; Kolitsch & Schwendtner, 2004], which is not the result that would be expected from the slightly larger ionic radius of six-coordinate InIII [the average In—O bond length is 2.141 Å, while the average Sc—O bond is 2.105 Å (Baur, 1981)]. However, the change in the unit-cell parameters shows a fairly irregular behaviour. In (I), a and c are smaller than in ScAsO4·H2O, whereas b is larger; the three angles differ by only 0.2–0.3°. Apparently, the polyhedral connectivity in (I) results in a more efficient space-filling.

PbIn(AsO4)(AsO3OH), (II), is the first lead(II) indium arsenate(V) reported. Its monoclinc crystal structure (space group P21/n) is a three-dimensional framework (Figs. 3 and 4) based on the corner-linkage of distorted AsO4 and AsO3OH tetrahedra (mean As—O = 1.695 and 1.688 Å, respectively), with slightly distorted InO6 octahedra (mean In—O = 2.157 Å). Voids in the framework are occupied by Pb2O10(OH)2 dimers, which are built of two edge-sharing symmetrically equivalent PbO6(OH) polyhedra [Pb···Pb = 4.069 (1) Å]. The coordination number of the Pb atom is unambiguous; there are seven O ligands within 2.88 Å (mean Pb—O = 2.623 Å), whereas the eighth O neighbour is at a distance of 3.365 (9) Å. The PbO6(OH) polyhedron is highly distorted and the distinct tendency for a one-sided coordination environment indicates that the lone electron pair on the PbII cation is stereochemically active; the electron pair points toward the remaining void space within the framework. The Pb-containing voids in the framework are arranged to form channels parallel to [100] (Fig. 3). A view along the b axis (not shown) reveals a layer-like arrangement of tetrahedra and octahedra, as often encountered in mixed octahedral–tetrahedral framework structures. PbIn(AsO4)(AsO3OH) is isotypic with PbFeIII(AsO4)(AsO3OH) (Effenberger et al., 1996). The crystal structure of the phosphate analogue PbIn(PO4)(PO3OH) (Belokoneva et al., 2001) shows only weak relations to that of (II).

Interestingly, the structure type of PbMIII(AsO4)(AsO3OH) (M = Fe and In) is related to that of (H3O)Fe(HPO4)2 (Vencato et al., 1989). The latter has similar unit-cell parameters (a = 5.191 Å, b = 8.748 Å, c = 14.448 Å and β = 94.81°) and a similar topology, albeit a different space group (P21/c). The structure type of (H3O)Fe(HPO4)2 is adopted by several other acid phosphates and arsenates [see overview by Schwendtner & Kolitsch (2004)].

The very long As2—O8 bond in (II) (Table 3) confirms that atom O8 represents an OH group belonging to an AsO3OH tetrahedron (cf. Ferraris & Ivaldi, 1984). The hydrogen bonding is strong, as the distance between the donor O8 (OH) and the only possible acceptor atom (O2) is fairly short [2.614 (13) Å]. In isotypic PbFeIII(AsO4)(AsO3OH) (Effenberger et al., 1996), the corresponding O···O distance is slightly longer [2.648 (10) Å]. The hydrogen bonds serve to reinforce the walls of the voids hosting the Pb2O10(OH)2 dimers. Bond-valence sums for all atoms in (II) were calculated using the bond-valence parameters of Krivovichev & Brown (2001) for Pb—O bonds, and of Brese & O'Keeffe (1991) for the remaining bonds. The values obtained, 1.93 (Pb), 3.03 (In), 4.86 (As1), 4.96 (As2), 1.85 (O1), 1.74 (O2, the acceptor of a strong hydrogen bond), 2.04 (O3), 1.91 (O4), 1.97 (O5), 2.05 (O6), 1.97 (O7) and 1.26 v.u. (O8 = OH), are all close to ideal valencies.

Experimental top

The title compounds were prepared by a hydrothermal method (Teflon-lined stainless steel bombs, 493 K, 7 d, slow furnace cooling) from a mixture of distilled water, arsenic acid, In2O3 [for (I) and (II)], Li2CO3 [for (I)] and yellow PbO [for (II)]. The final pH values of the reacted solutions were about 1 and 2 for (I) and (II), respectively. Compound (I) formed tiny, colourless, pseudo-rhombohedral crystals. Compound (II) formed tiny, colourless, indistinct (grain-like) crystals, associated with very minor amounts of synthetic schultenite (PbHAsO4) as tiny rectangular platelets.

Refinement top

The atomic coordinates of ScAsO4·H2O (Kolitsch & Schwendtner, 2004) were used as starting parameters for the final refinement of (I). H atoms were freely refined (see Table 2 for refined O—H distances). The atomic coordinates of PbFeIII(AsO4)(AsO3OH) (Effenberger et al., 1996) were used as starting parameters for the final refinement of (II). The H atom could not be located. A total of 52 reflections were omitted from the data set of (II) because these were strongly affected by overlap with reflections from about two extremely small additional grains intergrown with the measured crystal grain. The highest electron-density peak in the difference map of (II) is 0.86 Å from the Pb site. The deepest hole is 0.77 Å from the Pb site.

Computing details top

For both compounds, data collection: COLLECT (Nonius, 2004); cell refinement: HKL SCALEPACK (Otwinowski et al., 2003); data reduction: HKL DENZO (Otwinowski et al., 2003) and SCALEPACK; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997). Molecular graphics: Diamond (Brandenburg, 2005) and ORTEP-3 for Windows (Farrugia, 1997) for (I); Diamond (Pennington, 1999) and ORTEP-3 for Windows (Farrugia, 1997) for (II). For both compounds, software used to prepare material for publication: SHELXL97.

Figures top
[Figure 1] Fig. 1. View of InAsO4·H2O along (a) [010] and (b) [001]. Slightly distorted AsO4 tetrahedra are corner-linked to In2O8(H2O)2 dimers, which are built of two edge-sharing InO5(H2O) octahedra. The medium-strong hydrogen bonds are shown as dashed lines. The unit cell is outlined.
[Figure 2] Fig. 2. Connectivity in InAsO4·H2O, showing the atom-labelling scheme and 70% probability displacement ellipsoids. H atoms are shown as small spheres of arbitrary radii. [Symmetry codes: (i) x, y, z − 1; (ii) −x, −y, −z; (iii) 1 − x, −y, −z; (iv) 1 − x, 1 − y, −z.]
[Figure 3] Fig. 3. View of PbIn(AsO4)(AsO3OH) along [100]. AsO4 and AsO3OH tetrahedra are corner-linked to InO6 octahedra. Voids in the resulting octahedral–tetrahedral framework are occupied by Pb2O10(OH)2 dimers, which are built of two edge-sharing, highly distorted, PbO6(OH) polyhedra [Pb···Pb = 4.069 (1) Å]. The unit cell is outlined.
[Figure 4] Fig. 4. Connectivity in PbIn(AsO4)(AsO3OH), showing the atom-labelling scheme and 50% probability displacement ellipsoids. [Symmetry codes: (i) 1 + x, y, z; (iv) 1 − x, 1 − y, −z, (v) 3/2 − x, 1/2 + y, 1/2 − z.]
(I) indium arsenate(V) monohydrate top
Crystal data top
InAsO4·H2OZ = 2
Mr = 271.76F(000) = 248
Triclinic, P1Dx = 4.598 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 5.500 (1) ÅCell parameters from 1409 reflections
b = 5.720 (1) Åθ = 2.0–32.5°
c = 6.685 (1) ŵ = 14.28 mm1
α = 98.90 (3)°T = 293 K
β = 94.60 (3)°Pseudo-rhombohedral, colourless
γ = 107.55 (3)°0.05 × 0.05 × 0.03 mm
V = 196.30 (7) Å3
Data collection top
Nonius KappaCCD
diffractometer
1427 independent reflections
Radiation source: fine-focus sealed tube1405 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.013
ϕ and ω scansθmax = 32.5°, θmin = 3.1°
Absorption correction: multi-scan
(HKL SCALEPACK; Otwinowski et al., 2003)
h = 88
Tmin = 0.535, Tmax = 0.674k = 88
2799 measured reflectionsl = 1010
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.013All H-atom parameters refined
wR(F2) = 0.033 w = 1/[σ2(Fo2) + (0.0067P)2 + 0.2212P]
where P = (Fo2 + 2Fc2)/3
S = 1.20(Δ/σ)max < 0.001
1427 reflectionsΔρmax = 0.91 e Å3
73 parametersΔρmin = 0.77 e Å3
0 restraintsExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0355 (12)
Crystal data top
InAsO4·H2Oγ = 107.55 (3)°
Mr = 271.76V = 196.30 (7) Å3
Triclinic, P1Z = 2
a = 5.500 (1) ÅMo Kα radiation
b = 5.720 (1) ŵ = 14.28 mm1
c = 6.685 (1) ÅT = 293 K
α = 98.90 (3)°0.05 × 0.05 × 0.03 mm
β = 94.60 (3)°
Data collection top
Nonius KappaCCD
diffractometer
1427 independent reflections
Absorption correction: multi-scan
(HKL SCALEPACK; Otwinowski et al., 2003)
1405 reflections with I > 2σ(I)
Tmin = 0.535, Tmax = 0.674Rint = 0.013
2799 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0130 restraints
wR(F2) = 0.033All H-atom parameters refined
S = 1.20Δρmax = 0.91 e Å3
1427 reflectionsΔρmin = 0.77 e Å3
73 parameters
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
In0.36738 (2)0.27146 (2)0.218959 (18)0.00643 (5)
As0.26452 (3)0.12140 (3)0.25584 (3)0.00472 (5)
O10.3540 (3)0.3488 (2)0.11118 (19)0.0076 (2)
O20.3210 (3)0.1381 (2)0.1445 (2)0.0092 (2)
O30.4449 (3)0.2396 (3)0.4814 (2)0.0109 (2)
O40.0534 (3)0.0638 (2)0.2615 (2)0.0103 (2)
OW50.0879 (3)0.4616 (3)0.2689 (3)0.0163 (3)
H10.101 (8)0.600 (8)0.260 (6)0.040 (10)*
H20.032 (7)0.413 (7)0.237 (6)0.037 (11)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
In0.00618 (7)0.00640 (7)0.00620 (7)0.00141 (5)0.00079 (4)0.00085 (4)
As0.00481 (9)0.00425 (8)0.00507 (9)0.00095 (6)0.00109 (6)0.00152 (6)
O10.0106 (6)0.0053 (5)0.0061 (5)0.0000 (4)0.0025 (4)0.0030 (4)
O20.0099 (6)0.0072 (5)0.0111 (6)0.0047 (5)0.0007 (5)0.0001 (4)
O30.0106 (6)0.0139 (6)0.0058 (5)0.0012 (5)0.0000 (4)0.0010 (4)
O40.0052 (6)0.0079 (5)0.0180 (7)0.0013 (5)0.0034 (5)0.0033 (5)
OW50.0095 (6)0.0105 (6)0.0313 (9)0.0045 (5)0.0045 (6)0.0075 (6)
Geometric parameters (Å, º) top
In—O3i2.0731 (14)As—O31.6600 (15)
In—O4ii2.1203 (16)As—O21.6816 (13)
In—O2iii2.1298 (14)As—O41.6834 (13)
In—OW52.1667 (16)As—O11.7173 (13)
In—O12.1945 (13)OW5—H10.76 (4)
In—O1iv2.2173 (16)OW5—H20.70 (4)
O3i—In—O4ii97.01 (7)O2iii—In—O1iv86.16 (5)
O3i—In—O2iii88.70 (6)OW5—In—O1iv85.34 (6)
O4ii—In—O2iii100.50 (5)O1—In—O1iv75.43 (6)
O3i—In—OW594.04 (7)O3—As—O2110.81 (7)
O4ii—In—OW587.39 (6)O3—As—O4114.63 (7)
O2iii—In—OW5171.29 (6)O2—As—O4110.00 (7)
O3i—In—O1170.09 (5)O3—As—O1105.57 (7)
O4ii—In—O192.24 (6)O2—As—O1109.81 (7)
O2iii—In—O186.13 (6)O4—As—O1105.75 (7)
OW5—In—O189.90 (6)In—OW5—H1132 (3)
O3i—In—O1iv95.81 (6)In—OW5—H2117 (3)
O4ii—In—O1iv165.67 (5)H1—OW5—H2102 (4)
Symmetry codes: (i) x, y, z1; (ii) x, y, z; (iii) x+1, y, z; (iv) x+1, y+1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
OW5—H1···O4v0.76 (4)2.02 (4)2.771 (2)167 (4)
OW5—H2···O2ii0.70 (4)2.08 (4)2.728 (2)154 (4)
Symmetry codes: (ii) x, y, z; (v) x, y+1, z.
(II) lead(II) indium arsenate(V) hydrogen arsenate(V) top
Crystal data top
PbIn(AsO4)(AsO3OH)F(000) = 1048
Mr = 600.86Dx = 5.911 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 2570 reflections
a = 4.955 (1) Åθ = 2.0–30.0°
b = 8.591 (2) ŵ = 38.05 mm1
c = 15.874 (3) ÅT = 293 K
β = 92.38 (3)°Irregular fragment, colourless
V = 675.2 (2) Å30.03 × 0.03 × 0.02 mm
Z = 4
Data collection top
Nonius KappaCCD
diffractometer
1903 independent reflections
Radiation source: fine-focus sealed tube1445 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.040
ϕ and ω scansθmax = 30.0°, θmin = 3.5°
Absorption correction: multi-scan
(HKL SCALEPACK; Otwinowski et al., 2003)
h = 66
Tmin = 0.357, Tmax = 0.467k = 1212
3677 measured reflectionsl = 2222
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.047H-atom parameters not defined
wR(F2) = 0.121 w = 1/[σ2(Fo2) + (0.07P)2 + 1P]
where P = (Fo2 + 2Fc2)/3
S = 1.01(Δ/σ)max < 0.001
1903 reflectionsΔρmax = 3.95 e Å3
109 parametersΔρmin = 1.91 e Å3
0 restraints
Crystal data top
PbIn(AsO4)(AsO3OH)V = 675.2 (2) Å3
Mr = 600.86Z = 4
Monoclinic, P21/nMo Kα radiation
a = 4.955 (1) ŵ = 38.05 mm1
b = 8.591 (2) ÅT = 293 K
c = 15.874 (3) Å0.03 × 0.03 × 0.02 mm
β = 92.38 (3)°
Data collection top
Nonius KappaCCD
diffractometer
1903 independent reflections
Absorption correction: multi-scan
(HKL SCALEPACK; Otwinowski et al., 2003)
1445 reflections with I > 2σ(I)
Tmin = 0.357, Tmax = 0.467Rint = 0.040
3677 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0470 restraints
wR(F2) = 0.121H-atom parameters not defined
S = 1.01Δρmax = 3.95 e Å3
1903 reflectionsΔρmin = 1.91 e Å3
109 parameters
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
Pb0.82765 (10)0.03180 (6)0.11282 (3)0.02153 (16)
In0.82989 (18)0.45566 (11)0.14541 (6)0.0169 (2)
As10.3138 (2)0.30485 (16)0.02208 (8)0.0160 (3)
As20.3323 (3)0.25861 (15)0.25775 (8)0.0166 (3)
O10.170 (2)0.4559 (11)0.0700 (6)0.024 (2)
O20.3384 (18)0.3443 (10)0.0820 (5)0.0186 (19)
O30.6321 (18)0.2845 (11)0.0664 (6)0.0203 (19)
O40.1791 (18)0.1241 (11)0.0288 (6)0.0204 (18)
O50.5031 (19)0.0911 (11)0.2511 (6)0.023 (2)
O60.0454 (18)0.2476 (10)0.2003 (6)0.020 (2)
O70.527 (2)0.4139 (11)0.2368 (6)0.022 (2)
O80.259 (2)0.2988 (12)0.3611 (6)0.023 (2)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pb0.0216 (3)0.0172 (3)0.0257 (3)0.0009 (2)0.00007 (18)0.0003 (2)
In0.0158 (4)0.0146 (4)0.0200 (4)0.0000 (3)0.0004 (3)0.0000 (3)
As10.0148 (6)0.0138 (6)0.0192 (6)0.0014 (5)0.0010 (4)0.0010 (5)
As20.0150 (6)0.0141 (6)0.0206 (6)0.0011 (4)0.0008 (5)0.0013 (5)
O10.030 (5)0.017 (5)0.026 (5)0.000 (4)0.008 (4)0.002 (4)
O20.020 (5)0.014 (4)0.021 (4)0.011 (4)0.001 (3)0.001 (4)
O30.014 (4)0.016 (4)0.030 (5)0.002 (3)0.007 (3)0.001 (4)
O40.018 (4)0.019 (5)0.024 (5)0.006 (4)0.000 (3)0.002 (4)
O50.021 (5)0.021 (5)0.026 (5)0.010 (4)0.003 (4)0.001 (4)
O60.013 (4)0.011 (4)0.037 (5)0.005 (3)0.000 (4)0.005 (4)
O70.032 (5)0.014 (4)0.020 (4)0.001 (4)0.009 (4)0.002 (4)
O80.027 (5)0.024 (5)0.019 (4)0.000 (4)0.010 (4)0.001 (4)
Geometric parameters (Å, º) top
Pb—O4i2.373 (9)In—O5v2.150 (9)
Pb—O32.477 (9)In—O72.161 (9)
Pb—O6i2.531 (9)In—O6i2.240 (9)
Pb—O4ii2.616 (9)As1—O11.679 (10)
Pb—O7iii2.664 (9)As1—O21.695 (9)
Pb—O52.821 (10)As1—O41.696 (9)
Pb—O8iii2.880 (10)As1—O31.710 (9)
Pb—O2ii3.365 (9)As2—O61.659 (9)
In—O1i2.105 (10)As2—O51.675 (9)
In—O2iv2.143 (8)As2—O71.688 (9)
In—O32.143 (9)As2—O81.730 (9)
O4i—Pb—O380.0 (3)O1i—In—O2iv92.1 (4)
O4i—Pb—O6i76.0 (3)O1i—In—O391.4 (4)
O3—Pb—O6i71.0 (3)O2iv—In—O396.6 (4)
O4i—Pb—O4ii70.8 (3)O1i—In—O5v98.2 (4)
O3—Pb—O4ii101.7 (3)O2iv—In—O5v93.2 (4)
O6i—Pb—O4ii146.8 (3)O3—In—O5v166.0 (4)
O4i—Pb—O7iii116.9 (3)O1i—In—O7167.4 (4)
O3—Pb—O7iii133.4 (3)O2iv—In—O7100.5 (4)
O6i—Pb—O7iii72.2 (3)O3—In—O788.0 (4)
O4ii—Pb—O7iii124.7 (3)O5v—In—O780.4 (4)
O4i—Pb—O5146.3 (3)O1i—In—O6i80.9 (4)
O3—Pb—O581.1 (3)O2iv—In—O6i173.0 (3)
O6i—Pb—O571.6 (3)O3—In—O6i83.0 (3)
O4ii—Pb—O5140.7 (3)O5v—In—O6i88.4 (4)
O7iii—Pb—O560.9 (3)O7—In—O6i86.5 (3)
O4i—Pb—O8iii77.2 (3)O1—As1—O2109.6 (4)
O3—Pb—O8iii156.7 (3)O1—As1—O4120.2 (5)
O6i—Pb—O8iii98.4 (3)O2—As1—O4106.8 (4)
O4ii—Pb—O8iii75.6 (3)O1—As1—O3107.2 (5)
O7iii—Pb—O8iii56.2 (3)O2—As1—O3108.6 (4)
O5—Pb—O8iii116.0 (3)O4—As1—O3103.8 (5)
O4i—Pb—O2ii114.8 (3)O6—As2—O5109.9 (5)
O3—Pb—O2ii135.1 (3)O6—As2—O7114.9 (5)
O6i—Pb—O2ii151.6 (3)O5—As2—O7111.8 (5)
O4ii—Pb—O2ii52.3 (3)O6—As2—O8109.0 (5)
O7iii—Pb—O2ii79.7 (2)O5—As2—O8110.9 (5)
O5—Pb—O2ii98.2 (3)O7—As2—O899.9 (5)
O8iii—Pb—O2ii61.4 (3)
Symmetry codes: (i) x+1, y, z; (ii) x+1, y, z; (iii) x+3/2, y1/2, z+1/2; (iv) x+1, y+1, z; (v) x+3/2, y+1/2, z+1/2.

Experimental details

(I)(II)
Crystal data
Chemical formulaInAsO4·H2OPbIn(AsO4)(AsO3OH)
Mr271.76600.86
Crystal system, space groupTriclinic, P1Monoclinic, P21/n
Temperature (K)293293
a, b, c (Å)5.500 (1), 5.720 (1), 6.685 (1)4.955 (1), 8.591 (2), 15.874 (3)
α, β, γ (°)98.90 (3), 94.60 (3), 107.55 (3)90, 92.38 (3), 90
V3)196.30 (7)675.2 (2)
Z24
Radiation typeMo KαMo Kα
µ (mm1)14.2838.05
Crystal size (mm)0.05 × 0.05 × 0.030.03 × 0.03 × 0.02
Data collection
DiffractometerNonius KappaCCD
diffractometer
Nonius KappaCCD
diffractometer
Absorption correctionMulti-scan
(HKL SCALEPACK; Otwinowski et al., 2003)
Multi-scan
(HKL SCALEPACK; Otwinowski et al., 2003)
Tmin, Tmax0.535, 0.6740.357, 0.467
No. of measured, independent and
observed [I > 2σ(I)] reflections
2799, 1427, 1405 3677, 1903, 1445
Rint0.0130.040
(sin θ/λ)max1)0.7570.704
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.013, 0.033, 1.20 0.047, 0.121, 1.01
No. of reflections14271903
No. of parameters73109
H-atom treatmentAll H-atom parameters refinedH-atom parameters not defined
Δρmax, Δρmin (e Å3)0.91, 0.773.95, 1.91

Computer programs: COLLECT (Nonius, 2004), HKL SCALEPACK (Otwinowski et al., 2003), HKL DENZO (Otwinowski et al., 2003) and SCALEPACK, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), Diamond (Brandenburg, 2005) and ORTEP-3 for Windows (Farrugia, 1997), Diamond (Pennington, 1999) and ORTEP-3 for Windows (Farrugia, 1997), SHELXL97.

Selected bond lengths (Å) for (I) top
In—O3i2.0731 (14)In—O1iv2.2173 (16)
In—O4ii2.1203 (16)As—O31.6600 (15)
In—O2iii2.1298 (14)As—O21.6816 (13)
In—OW52.1667 (16)As—O41.6834 (13)
In—O12.1945 (13)As—O11.7173 (13)
Symmetry codes: (i) x, y, z1; (ii) x, y, z; (iii) x+1, y, z; (iv) x+1, y+1, z.
Hydrogen-bond geometry (Å, º) for (I) top
D—H···AD—HH···AD···AD—H···A
OW5—H1···O4v0.76 (4)2.02 (4)2.771 (2)167 (4)
OW5—H2···O2ii0.70 (4)2.08 (4)2.728 (2)154 (4)
Symmetry codes: (ii) x, y, z; (v) x, y+1, z.
Selected bond lengths (Å) for (II) top
Pb—O4i2.373 (9)In—O5v2.150 (9)
Pb—O32.477 (9)In—O72.161 (9)
Pb—O6i2.531 (9)In—O6i2.240 (9)
Pb—O4ii2.616 (9)As1—O11.679 (10)
Pb—O7iii2.664 (9)As1—O21.695 (9)
Pb—O52.821 (10)As1—O41.696 (9)
Pb—O8iii2.880 (10)As1—O31.710 (9)
Pb—O2ii3.365 (9)As2—O61.659 (9)
In—O1i2.105 (10)As2—O51.675 (9)
In—O2iv2.143 (8)As2—O71.688 (9)
In—O32.143 (9)As2—O81.730 (9)
Symmetry codes: (i) x+1, y, z; (ii) x+1, y, z; (iii) x+3/2, y1/2, z+1/2; (iv) x+1, y+1, z; (v) x+3/2, y+1/2, z+1/2.
 

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