MIn(HAsO4)2 (M = K, Rb, Cs): three new hydrogen­arsenates adopting two different structure types

Schwendtner, K.; Kolitsch, U.

doi:10.1107/S205698901701355X

research communications

CRYSTALLOGRAPHIC
COMMUNICATIONS

ISSN: 2056-9890

Volume 73| Part 10| October 2017| Pages 1580-1586

https://doi.org/10.1107/S205698901701355X

Open

access

MIn(HAsO₄)₂ (M = K, Rb, Cs): three new hydrogenarsenates adopting two different structure types

Karolina Schwendtner ^a ^* and Uwe Kolitsch ^b

^aInstitute for Chemical Technology and Analytics, Division of Structural Chemistry, TU Wien, Getreidemarkt 9/164-SC, 1060 Vienna, Austria, and ^bMineralogisch-Petrographische Abteilung, Naturhistorisches Museum Wien, Burgring 7, 1010 Wien, and Institut für Mineralogie und Kristallographie, Universität Wien, Althanstrasse 14, 1090 Wien, Austria
^*Correspondence e-mail: karolina.schwendtner@tuwien.ac.at

Edited by T. J. Prior, University of Hull, England (Received 12 September 2017; accepted 21 September 2017; online 29 September 2017)

Potassium indium bis[hydrogen arsenate(V)], KIn(HAsO₄)₂, rubidium indium bis[hydrogen arsenate(V)], RbIn(HAsO₄)₂, and caesium indium bis[hydrogen arsenate(V)], CsIn(HAsO₄)₂, were grown under mild hydrothermal conditions (T = 493 K, 7–8 d). KIn(HAsO₄)₂ adopts the KSc(HAsO₄)₂ structure type (space group C2/c), while RbIn(HAsO₄)₂ and CsIn(HAsO₄)₂ crystallize in the space group R-3c and are the first arsenate representatives of the RbFe(HPO₄)₂ structure type. All three compounds have tetrahedral–octahedral framework topologies. The M⁺ cations, located in voids of the respective framework, are slightly disordered in RbIn(HAsO₄)₂. In KIn(HAsO₄)₂, there is a second K-atom position with a very low occupancy, which may suggest that the K atom can easily move in the channels extending along [101].

Keywords: crystal structure; KIn(HAsO₄)₂; RbIn(HAsO₄)₂; CsIn(HAsO₄)₂; arsenate.

CCDC references: 1575921; 1575920; 1575919

1. Chemical context

Metal arsenates often form tetrahedral–octahedral framework structures that frequently show potentially interesting properties, such as ion conductivity, ion exchange and catalytic properties (Masquelier et al., 1990 , 1994a ,b , 1995 , 1996 , 1998 ; Mesa et al., 2000 ; Ouerfelli et al., 2007a ,b , 2008 ; Pintard-Scrépel et al., 1983 ; Rousse et al., 2013 ). In the course of a detailed study of the system M⁺–M³⁺–As–O–(H) by hydrothermal syntheses, a large variety of new arsenate(V) compounds and structure types were found (Kolitsch, 2004 ; Schwendtner, 2006 ; Schwendtner & Kolitsch, 2004a ,b , 2005 , 2007a ,b ,c ,d , 2017a ,b ,c ).

The three new title compounds belong to the family of hydrogenarsenate compounds with the general formula M⁺M³⁺(HAsO₄)₂. Including the three compounds reported here, nine compounds with this general formula are known. They crystallize in four different structure types. KIn(HAsO₄)₂ is a further representative of the KSc(HAsO₄)₂ structure type (Schwendtner & Kolitsch, 2004a), which is also adopted by AgGa(HAsO₄)₂ and AgAl(HAsO₄)₂ (Schwendtner & Kolitsch, 2017c). The (H₃O)Fe(HPO₄)₂ structure type (Vencato et al., 1989 ) is adopted by CsSc(HAsO₄)₂ (Schwendtner & Kolitsch, 2004b). Another modification of CsSc(HAsO₄)₂ crystallizes in the (NH₄)Fe(HPO₄)₂ type (Yakubovich, 1993 ), in which also (NH₄)Fe(HAsO₄)₂ crystallizes (Ouerfelli et al., 2014 ). The two new title compounds RbIn(HAsO₄)₂ and CsIn(HAsO₄)₂ adopt a structure type hitherto unknown among arsenates which is, however, known from the phosphates RbFe(HPO₄)₂ (Lii & Wu, 1994 ) and RbM³⁺(HPO₄)₂ (M = Al, Ga) (Lesage et al., 2007 ). All of these compounds consist of frameworks of singly protonated AsO₄ tetrahedra and M³⁺O₆ octahedra. The M⁺ cations occupy channels that extend along one or more directions in the framework.

A number of M⁺–In–arsenates have been reported in the literature. Among these are several diarsenates: NaInAs₂O₇ (Belam et al., 1997 ), KInAs₂O₇ (Schwendtner & Kolitsch, 2017b) and RbInAs₂O₇, TlInAs₂O₇ and (NH₄)InAs₂O₇ (Schwendtner, 2006), furthermore Na₃In₂(AsO₄)₃ (Lii & Ye, 1997 ; Khorari et al., 1997 ) and KIn(H₂O)(H_1.5AsO₄)₂(H₂AsO₄) (Schwendtner & Kolitsch, 2007c). There also exist indexed X-ray powder diffraction data of Li₃In₂(AsO₄)₃ (Winand et al., 1990 ) and unindexed powder patterns of KIn(HAsO₄)₂·xH₂O, RbIn(HAsO₄)₂·xH₂O, CsIn(HAsO₄)₂·xH₂O and CsInAs₂O₇ (Ezhova et al., 1977 ).

The hydrogenphosphates KIn(HPO₄)₂ and RbIn(HPO₄)₂ (Filaretov et al., 2002b ), which are the phosphate analogues of two of the title compounds, crystallize in the (NH₄)In(HPO₄)₂ structure type (P2₁/c; Filaretov et al., 2002a ; Mao et al., 2002 ), for which no arsenate members were known prior to the present work. CsIn(HPO₄)₂ (Huang et al., 2004 ; Lesage et al., 2007) is known as two modifications, the (NH₄)Fe(HPO₄)₂-type (P $[\overline{1}]$ ; Yakubovich, 1993) and the (H₃O)Fe(HPO₄)₂-type (P2₁/c; Vencato et al., 1989). Both structure types are common among hydrogenphosphates, with eleven and seven members, respectively, and both have one arsenate representative each, viz. α- and β-CsSc(HAsO₄)₂ (Schwendtner & Kolitsch, 2004). The (NH₄)Fe(HPO₄)₂-type CsIn(HPO₄)₂ is closely related to and basically a distorted variety of the RbFe(HPO₄)₂ type in which CsIn(HAsO₄)₂ crystallizes (see discussion in Lesage et al., 2007). According to Huang et al. (2004), a second variety of RbIn(HPO₄)₂ exists, which is also isotypic to (H₃O)Fe(HPO₄)₂.

2. Structural commentary

KIn(HAsO₄)₂ crystallizes in space group C2/c and is isotypic to KSc(HAsO₄)₂ (Schwendtner & Kolitsch, 2004a), AgGa(HAsO₄)₂ and AgAl(HAsO₄)₂ (Schwendtner & Kolitsch, 2017c). The asymmetric unit contains one K, one In, one As, one H and four O atoms (Fig. 1a). The slightly distorted InO₆ octahedra share corners with six HAsO₄ tetrahedra, thus forming a three-dimensional anionic framework with narrow channels parallel to [110] and [101] (Fig. 2a,b) which host the K atoms. There are two K-atom positions (K1 and K2), at a distance of 2.653 (15) Å from each other. The K1 position is located on an inversion centre and has a refined occupancy of 0.976 (2), while K2, which lies between two K1 positions, is located on a twofold axis (like the In atom) and has a refined occupancy of 0.024 (2). Both K-atom positions show a [4 + 4]-coordination with average K—O bond lengths of 2.949 and 3.016 Å for K1 and K2, respectively (Table 1). This is slightly longer than the reported average K—O bond length for ^[8]K atoms of 2.85 Å (Baur, 1981 ). However, bond-valence calculations after Gagné & Hawthorne (2015 ) show bond-valence sums (BVSs) of 0.99 valence units (v.u.) for K1 and 0.85 v.u. for K2, indicating an `underbonded' character of K2, and explaining the difference in site occupancies.

Table 1
Selected bond lengths (Å) for KIn(HAsO₄)

K1—O1ⁱ	2.6488 (17)	K2—O3^vii	3.20 (3)
K1—O1	2.6488 (17)	K2—O2	3.33 (3)
K1—O3ⁱⁱ	2.7788 (17)	K2—O2^vi	3.33 (3)
K1—O3ⁱⁱⁱ	2.7788 (17)	In—O1	2.1104 (17)
K1—O4^iv	3.112 (2)	In—O1^vi	2.1104 (17)
K1—O4^v	3.112 (2)	In—O3ⁱⁱ	2.1388 (16)
K1—O2	3.2553 (19)	In—O3^ix	2.1388 (16)
K1—O2ⁱ	3.2553 (19)	In—O2^x	2.1473 (16)
K2—O4	2.74 (4)	In—O2^v	2.1473 (16)
K2—O4^vi	2.74 (4)	As—O1	1.6574 (17)
K2—O1^vii	2.792 (18)	As—O3	1.6721 (17)
K2—O1^viii	2.792 (18)	As—O2	1.6762 (16)
K2—O3^viii	3.20 (3)	As—O4	1.7231 (19)
Symmetry codes: (i) $[-x+{\script{1\over 2}}, -y+{\script{1\over 2}}, -z]$ ; (ii) $[x-{\script{1\over 2}}, -y+{\script{1\over 2}}, z-{\script{1\over 2}}]$ ; (iii) $[-x+1, y, -z+{\script{1\over 2}}]$ ; (iv) $[x, -y+1, z-{\script{1\over 2}}]$ ; (v) $[-x+{\script{1\over 2}}, y-{\script{1\over 2}}, -z+{\script{1\over 2}}]$ ; (vi) $[-x, y, -z+{\script{1\over 2}}]$ ; (vii) $[-x+{\script{1\over 2}}, y+{\script{1\over 2}}, -z+{\script{1\over 2}}]$ ; (viii) $[x-{\script{1\over 2}}, y+{\script{1\over 2}}, z]$ ; (ix) $[-x+{\script{1\over 2}}, -y+{\script{1\over 2}}, -z+1]$ ; (x) $[x-{\script{1\over 2}}, y-{\script{1\over 2}}, z]$ .

Figure 1
The principal building units of (a) KIn(HAsO₄)₂ and (b) CsIn(HAsO₄)₂, shown as displacement ellipsoids at the 70% probability level. Symmetry codes: KIn(HAsO₄)₂: (i) −x + $[{1\over 2}]$ , −y + $[{1\over 2}]$ , −z; (ii) −x, −y + 1, −z; (iii) x + $[{1\over 2}]$ , y − $[{1\over 2}]$ , z; (iv) x − $[{1\over 2}]$ , −y + $[{1\over 2}]$ , z − $[{1\over 2}]$ ; (v) −x + 1, y, −z + $[{1\over 2}]$ ; (vi) x, −y + 1, z − $[{1\over 2}]$ ; (vii) −x + $[{1\over 2}]$ , y − $[{1\over 2}]$ , −z + $[{1\over 2}]$ ; (viii) −x, y, −z + $[{1\over 2}]$ ; (ix) −x + $[{1\over 2}]$ , y + $[{1\over 2}]$ , −z + $[{1\over 2}]$ ; (x) x − $[{1\over 2}]$ , y + $[{1\over 2}]$ , z; CsIn(HAsO₄)₂: (ii) −x, −x + y, −z + $[{3\over 2}]$ ; (iii) −x + y, −x, z; (iv) −y, x − y, z; (vii) y + $[{2\over 3}]$ , −x + y + $[{4\over 3}]$ , −z + $[{4\over 3}]$ ; (xi) x − y − $[{1\over 3}]$ , x + $[{1\over 3}]$ , −z + 4/3; (xv) −y, x − y + 1, z; (xvi) x + 1, y + 1, z; (xvii) x, y + 1, z; (xviii) −x + y+1, −x + 1, z; (xix) −x + $[{2\over 3}]$ , −y + $[{1\over 3}]$ , −z + $[{4\over 3}]$ ; (xx) x − 1, y, z.

Figure 2
The framework structure of KIn(HAsO₄)₂ in views parallel to (a) [101], (b) [110] and (c) [100]. The K atoms are located in channels of the framework (note that the K2 position has an occupancy of only 0.024 (2). Hydrogen bonds (dashed lines) reinforce the framework and extend roughly along c.

As expected, the protonated AsO₄ tetrahedron is strongly distorted as three vertices connect to neighbouring InO₆ octahedra, while O4 (OH) is a terminal vertex and only involved in a medium–strong hydrogen bond (Fig. 2b and 2c; Table 4).

Table 4
Hydrogen-bond geometry (Å, °) for KIn(HAsO₄)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O4—H⋯O2^xi	0.88 (2)	1.89 (3)	2.690 (3)	151 (4)
Symmetry code: (xi) $[x, -y+1, z+{\script{1\over 2}}]$ .

Calculated BVSs (Gagné & Hawthorne, 2015) of the framework atoms amount to 3.06 v.u. for In, 5.07 v.u. for As and 2.11/1.83/1.96/1.20 v.u. for O1–O4, respectively. Although these sums appear slightly too high for In and As, the average In—O and As—O bond lengths fit very well to published averages: the average As—O bond length in KIn(HAsO₄)₂ is 1.682 Å and the As—OH bond length is 1.723 Å, very close to the average of 704 analyzed AsO₄ groups in inorganic compounds [1.686 (10) Å; Schwendtner, 2008 ] and the average As—OH in 45 HAsO₄ groups [1.72 (3) Å; Schwendtner, 2008], respectively. The average In—O bond length (2.132 Å) is slightly shorter than the published average of 2.141 Å for inorganic compounds (Baur, 1981).

RbIn(HAsO₄)₂ and CsIn(HAsO₄)₂ crystallize in the space group R $[\overline{3}]$ c and are isotypic to RbFe(HPO₄)₂ (Lii & Wu, 1994) and RbM³⁺(HPO₄)₂ (M = Al, Ga) (Lesage et al., 2007). The asymmetric unit contains two M⁺, two In, one As, one H and four O positions and the structure is characterized by a long c axis in the hexagonal setting (Fig. 3). As in KIn(HAsO₄)₂, each InO₆ octahedron shares six vertices with six HAsO₄ tetrahedra, resulting in an InAs₆O₂₄ group. These groups are in turn connected via three corners to other InO₆ octahedra. The protonated apices of the HAsO₄ tetrahedra form a strong hydrogen bond (O—H⋯O = 2.62–2.63 Å) to the neighbouring InAs₆O₂₄ group. The InAs₆O₂₄ groups in RbIn(HAsO₄)₂ and CsIn(HAsO₄)₂ are arranged in layers normal to c, and the groups within these layers are interconnected by strong hydrogen bonds extending in directions [100] and [110] (Fig. 4a and 4b). The 12-coordinated Cs atoms are located in channels which extend along a and b. As in KIn(HAsO₄)₂, the average In—O bond lengths (2.138/2.131 and 2.139/2.133 Å for In1/In2 in the Rb and Cs compounds, respectively; Tables 2 and 3) are slightly smaller than the literature value (2.141 Å; Baur, 1981), while the average As—O bond lengths (1.683 and 1.687 Å) show good agreement with the literature value (see above). The calculated BVSs (Gagné & Hawthorne, 2015) amount to 1.05 (Rb1), 0.65 (Rb2), 3.02 (In1), 3.07 (In2), 5.07 (As) and 1.94/1.90/1.30/1.82 v.u. (O1–O4) for RbIn(HAsO₄)₂, and 0.92 (Cs1), 0.80 (Cs2), 3.02 (In1), 3.05 (In2), 5.01 (As) and 1.94/1.88/1.29/1.80 v.u. (O1–O4) for CsIn(HAsO₄)₂. These values are reasonably close to ideal valencies, although the fairly low value for Rb2 is noteworthy; apparently the Rb2-hosting cavity is too large for the Rb atom. In fact, both Rb atoms seem to `rattle' somewhat in their cavities and are characterized by rather large anisotropic displacement ellipsoids; therefore, they were modeled by split positions involving an additional, low-occupancy Rb position (Rb1B, Rb2B) in each case. The severely underbonded O3 atom is donor of the strong hydrogen bonds (Tables 5 and 6). As expected, the unit-cell volume of the isotypic phosphates is about 20% smaller than that of the arsenates. The stronger condensation due to the smaller stronger-bonded phosphate also leads to even stronger hydrogen bonds, with O—H⋯O distances ranging from 2.58 to 2.59 Å (Lii & Wu, 1994; Lesage et al., 2007).

Table 2
Selected bond lengths (Å) for RbIn(HAsO₄)

Rb1A—O3ⁱ	3.042 (2)	Rb2A—O4^xi	3.668 (5)
Rb1A—O3ⁱⁱ	3.042 (2)	Rb2A—O1^xii	3.830 (3)
Rb1A—O3ⁱⁱⁱ	3.042 (2)	Rb2A—O1^xiii	3.830 (3)
Rb1A—O3^iv	3.042 (2)	Rb2A—O1^xiv	3.830 (3)
Rb1A—O3^v	3.042 (2)	In1—O2^xv	2.1306 (17)
Rb1A—O3	3.042 (2)	In1—O2^v	2.1306 (17)
Rb1A—O2	3.3114 (19)	In1—O2^xvi	2.1306 (17)
Rb1A—O2^iv	3.3115 (19)	In1—O4^xvii	2.1457 (17)
Rb1A—O2ⁱⁱⁱ	3.3114 (19)	In1—O4ⁱⁱ	2.1457 (16)
Rb1A—O2^v	3.3114 (19)	In1—O4^xii	2.1457 (16)
Rb1A—O2ⁱ	3.3114 (18)	In2—O1^vii	2.1312 (19)
Rb1A—O2ⁱⁱ	3.3114 (18)	In2—O1^xviii	2.131 (2)
Rb2A—O3	3.006 (5)	In2—O1ⁱⁱ	2.1312 (19)
Rb2A—O3ⁱⁱ	3.006 (5)	In2—O1^xii	2.131 (2)
Rb2A—O3^v	3.006 (5)	In2—O1^xvii	2.1312 (19)
Rb2A—O1^vi	3.462 (3)	In2—O1^xix	2.1312 (19)
Rb2A—O1^vii	3.462 (3)	As—O1^xiii	1.6508 (18)
Rb2A—O1^viii	3.462 (3)	As—O2	1.6668 (17)
Rb2A—O4^ix	3.668 (5)	As—O4^iv	1.6736 (17)
Rb2A—O4^x	3.668 (5)	As—O3	1.7409 (19)
Symmetry codes: (i) $[x-y, -y, -z+{\script{3\over 2}}]$ ; (ii) -y, x-y, z; (iii) $[y, x, -z+{\script{3\over 2}}]$ ; (iv) $[-x, -x+y, -z+{\script{3\over 2}}]$ ; (v) -x+y, -x, z; (vi) $[-x+{\script{2\over 3}}, -y-{\script{2\over 3}}, -z+{\script{4\over 3}}]$ ; (vii) $[y+{\script{2\over 3}}, -x+y+{\script{4\over 3}}, -z+{\script{4\over 3}}]$ ; (viii) $[x-y-{\script{4\over 3}}, x-{\script{2\over 3}}, -z+{\script{4\over 3}}]$ ; (ix) $[x-{\script{1\over 3}}, x-y-{\script{2\over 3}}, z-{\script{1\over 6}}]$ ; (x) $[-y-{\script{1\over 3}}, -x+{\script{1\over 3}}, z-{\script{1\over 6}}]$ ; (xi) $[-x+y+{\script{2\over 3}}, y+{\script{1\over 3}}, z-{\script{1\over 6}}]$ ; (xii) -x+y+1, -x+1, z; (xiii) x-1, y, z; (xiv) -y, x-y-1, z; (xv) -y, x-y+1, z; (xvi) x+1, y+1, z; (xvii) x, y+1, z; (xviii) $[x-y-{\script{1\over 3}}, x+{\script{1\over 3}}, -z+{\script{4\over 3}}]$ ; (xix) $[-x+{\script{2\over 3}}, -y+{\script{1\over 3}}, -z+{\script{4\over 3}}]$ .

Table 3
Selected bond lengths (Å) for CsIn(HAsO₄)

Cs1—O3	3.280 (3)	Cs2—O3^xi	3.698 (3)
Cs1—O3ⁱ	3.280 (3)	Cs2—O4^xii	3.703 (2)
Cs1—O3ⁱⁱ	3.280 (3)	Cs2—O4^xiii	3.703 (2)
Cs1—O3ⁱⁱⁱ	3.280 (3)	Cs2—O4^xiv	3.703 (2)
Cs1—O3^iv	3.280 (3)	In1—O2^xv	2.127 (2)
Cs1—O3^v	3.280 (3)	In1—O2ⁱⁱⁱ	2.127 (2)
Cs1—O2	3.434 (2)	In1—O2^xvi	2.127 (2)
Cs1—O2ⁱⁱ	3.434 (2)	In1—O4^xvii	2.150 (2)
Cs1—O2^v	3.434 (2)	In1—O4^iv	2.150 (2)
Cs1—O2ⁱⁱⁱ	3.434 (2)	In1—O4^xviii	2.150 (2)
Cs1—O2ⁱ	3.434 (2)	In2—O1^vii	2.133 (2)
Cs1—O2^iv	3.434 (2)	In2—O1^xi	2.133 (3)
Cs2—O3^iv	3.121 (3)	In2—O1^xix	2.133 (2)
Cs2—O3ⁱⁱⁱ	3.121 (2)	In2—O1^iv	2.133 (2)
Cs2—O3	3.121 (3)	In2—O1^xviii	2.133 (3)
Cs2—O1^vi	3.419 (3)	In2—O1^xvii	2.133 (2)
Cs2—O1^vii	3.419 (3)	As—O1^xx	1.655 (2)
Cs2—O1^viii	3.419 (3)	As—O2	1.671 (2)
Cs2—O3^ix	3.698 (3)	As—O4ⁱⁱ	1.679 (2)
Cs2—O3^x	3.698 (3)	As—O3	1.743 (3)
Symmetry codes: (i) $[x-y, -y, -z+{\script{3\over 2}}]$ ; (ii) $[-x, -x+y, -z+{\script{3\over 2}}]$ ; (iii) -x+y, -x, z; (iv) -y, x-y, z; (v) $[y, x, -z+{\script{3\over 2}}]$ ; (vi) $[-x+{\script{2\over 3}}, -y-{\script{2\over 3}}, -z+{\script{4\over 3}}]$ ; (vii) $[y+{\script{2\over 3}}, -x+y+{\script{4\over 3}}, -z+{\script{4\over 3}}]$ ; (viii) $[x-y-{\script{4\over 3}}, x-{\script{2\over 3}}, -z+{\script{4\over 3}}]$ ; (ix) $[-x-{\script{1\over 3}}, -y-{\script{2\over 3}}, -z+{\script{4\over 3}}]$ ; (x) $[y+{\script{2\over 3}}, -x+y+{\script{1\over 3}}, -z+{\script{4\over 3}}]$ ; (xi) $[x-y-{\script{1\over 3}}, x+{\script{1\over 3}}, -z+{\script{4\over 3}}]$ ; (xii) $[x-{\script{1\over 3}}, x-y-{\script{2\over 3}}, z-{\script{1\over 6}}]$ ; (xiii) $[-y-{\script{1\over 3}}, -x+{\script{1\over 3}}, z-{\script{1\over 6}}]$ ; (xiv) $[-x+y+{\script{2\over 3}}, y+{\script{1\over 3}}, z-{\script{1\over 6}}]$ ; (xv) -y, x-y+1, z; (xvi) x+1, y+1, z; (xvii) x, y+1, z; (xviii) -x+y+1, -x+1, z; (xix) $[-x+{\script{2\over 3}}, -y+{\script{1\over 3}}, -z+{\script{4\over 3}}]$ ; (xx) x-1, y, z.

Table 5
Hydrogen-bond geometry (Å, °) for RbIn(HAsO₄)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O3—H⋯O4^xx	0.83 (3)	1.82 (3)	2.634 (2)	168 (4)
Symmetry code: (xx) $[y, x-1, -z+{\script{3\over 2}}]$ .

Table 6
Hydrogen-bond geometry (Å, °) for CsIn(HAsO₄)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O3—H⋯O4^xxi	0.83 (3)	1.80 (3)	2.621 (3)	170 (4)
Symmetry code: (xxi) $[y, x-1, -z+{\script{3\over 2}}]$ .

Figure 3
The framework structure of CsIn(HAsO₄)₂ in a view parallel to b. The unit cell (outlined) is characterized by a long c axis. Cs atoms occupy channels extending parallel to a and b. Hydrogen bonds are shown as dashed lines.

Figure 4
View along c of the two different layers involving the two different Cs atoms positions in the framework structure of CsIn(HAsO₄)₂. These layers are stacked along c (cf. Fig. 3

). Hydrogen bonds are shown as dashed lines.

3. Synthesis and crystallization

The compounds were grown by hydrothermal synthesis at 493 K (7–8 d, autogeneous pressure, slow furnace cooling) using Teflon-lined stainless steel autoclaves with an approximate filling volume of 2 cm³. Reagent-grade KOH/Rb₂CO₃/Cs₂CO₃, In₂O₃, α-Al₂O₃ (only in the case of the K–In–arsenate) and H₃AsO₄·0.5H₂O were used as starting reagents in approximate volume ratios of M⁺:M³⁺:As of 1:1:2. In the synthesis of KIn(HAsO₄)₂, the In₂O₃:α-Al₂O₃ ratio was 1:1. The vessels were filled with distilled water to about 70% of their inner volumes which led to final pH values of < 1 for all synthesis batches except KIn(HAsO₄)₂ (initial pH 4.5, final pH 3). The reaction products were washed thoroughly with distilled water, filtered and dried at room temperature. They are stable in air.

KIn(HAsO₄)₂ formed prismatic-bipyramidal crystals (Fig. 5a) that were accompanied by cubic crystals of synthetic pharmacoalumite [KAl₄(AsO₄)₃(OH)₄·6.5H₂O]. Thus, the Al and In present in the synthesis of these phases seemingly fractionate completely between the two phases KIn(HAsO₄)₂ and KAl₄(AsO₄)₃(OH)₄·6.5H₂O. RbIn(HAsO₄)₂ and CsIn(HAsO₄)₂ formed pseudo-octahedral crystals and platelets with pseudohexagonal outline (Fig. 5b and 5c, respectively). RbIn(HAsO₄)₂ was accompanied by crystals of RbInAs₂O₇ (Schwendtner, 2006), while the X-ray powder diffraction pattern of CsIn(HAsO₄)₂ showed a few peaks of an unidentified impurity.

Figure 5
SEM micrographs of hydrothermally synthesized crystals of (a) KIn(HAsO₄)₂, (b) RbIn(HAsO₄)₂ and (c) CsIn(HAsO₄)₂.

Measured X-ray powder diffraction diagrams of RbIn(HAsO₄)₂ and CsIn(HAsO₄)₂ were deposited at the International Centre for Diffraction Data under PDF number 56–1371 (Prem et al., 2005a ) for RbIn(HAsO₄)₂ and 56–1372 (Prem et al., 2005b ) for CsIn(HAsO₄)₂.

The chemical composition of the title compounds was checked by standard SEM–EDX analysis of several crystals of each compound; no impurities could be detected.

4. Refinement

Crystal data, data collection and structure refinement details are summarized in Table 7.

Table 7
Experimental details

	KIn(HAsO₄)₂	RbIn(HAsO₄)₂	CsIn(HAsO₄)₂
Crystal data
M_r	433.78	480.15	527.59
Crystal system, space group	Monoclinic, C2/c	Trigonal, R $[\overline{3}]$ c:H	Trigonal, R $[\overline{3}]$ c:H
Temperature (K)	293	293	293
a, b, c (Å)	8.340 (2), 10.657 (2), 9.197 (2)	8.512 (1), 8.512 (1), 56.434 (11)	8.629 (1), 8.629 (1), 56.986 (11)
α, β, γ (°)	90, 109.37 (3), 90	90, 90, 120	90, 90, 120
V (Å³)	771.2 (3)	3541.1 (11)	3674.7 (11)
Z	4	18	18
Radiation type	Mo Kα	Mo Kα	Mo Kα
μ (mm⁻¹)	12.13	17.50	15.34
Crystal size (mm)	0.19 × 0.02 × 0.02	0.05 × 0.05 × 0.02	0.06 × 0.06 × 0.04

Data collection
Diffractometer	Nonius KappaCCD single-crystal four-circle	Nonius KappaCCD single-crystal four-circle	Nonius KappaCCD single-crystal four-circle
Absorption correction	Multi-scan (SCALEPACK; Otwinowski et al., 2003 )	Multi-scan (SCALEPACK; Otwinowski et al., 2003)	Multi-scan (SCALEPACK; Otwinowski et al., 2003)
T_min, T_max	0.207, 0.794	0.475, 0.779	0.460, 0.579
No. of measured, independent and observed [I > 2σ(I)] reflections	2743, 1406, 1295	5262, 1443, 1255	4350, 1199, 1039
R_int	0.015	0.024	0.019
(sin θ/λ)_max (Å⁻¹)	0.758	0.757	0.704

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.019, 0.046, 1.09	0.018, 0.041, 1.12	0.022, 0.052, 1.07
No. of reflections	1406	1443	1199
No. of parameters	64	69	61
No. of restraints	1	3	1
H-atom treatment	All H-atom parameters refined	All H-atom parameters refined	All H-atom parameters refined
Δρ_max, Δρ_min (e Å⁻³)	1.18, −1.00	1.00, −0.86	2.09, −0.86
Computer programs: COLLECT (Nonius, 2003 ), DENZO and SCALEPACK (Otwinowski et al., 2003), SHELXS97 (Sheldrick, 2008 ), SHELXL2016 (Sheldrick, 2015 ), DIAMOND (Brandenburg, 2005 ) and publCIF (Westrip, 2010 ).

For all three refinements, the atomic coordinates of the first description of the respective structure types [KSc(HAsO₄)₂ (Schwendtner & Kolitsch, 2004a) and RbFe(HPO₄)₂ (Lii & Wu, 1994)] were used as initial parameters for better comparison. Hydrogen atoms and additional disordered positions were then located from difference-Fourier maps and added to the respective models.

The two K-atom positions in KIn(HAsO₄)₂ were restrained to give a total occupancy of one. Freely refined occupancies were 0.989 (4) (K1) and 0.029 (4) (K2), i.e. very close to the ideal bulk occupancy of 1.00. Also the anisotropic displacement parameters were restrained to the same values. The O—H bond lengths were restrained to 0.90 (4) (K compound) and 0.90 (2) Å (Rb and Cs compounds). Residual electron-density peaks of 1.02 and 1.03 e Å⁻³ were encountered close to the Rb1 and Rb2 positions. It seems that the Rb atoms, similarly to what was found for isotypic RbAl(HPO₄)₂ (Lesage et al., 2007), have irregular atomic displacement parameters; therefore, two further, low-occupancy Rb positions, Rb1B and Rb2B, were included in the refinement to model this positional disorder. The occupancies were accordingly restrained to give a total occupancy of 1.00 for Rb1 and Rb2 [Rb1a = 0.949 (3), 3 × Rb1b = 0.0170 (9), Rb2a = 0.567 (3), 3 × Rb2b = 0.1442 (9)]. The refined Rb1A—R1B, Rb1B—R1B′, Rb2A—R2B′ and Rb2B—Rb2B distances are 0.44 (3), 0.76 (5), 0.249 (8) and 0.423 (14) Å, respectively. The anisotropic displacement parameters of Rb1a and Rb1b, as well as Rb2a and Rb2b, were restrained to give the same value.

The highest residual electron densities are 2.03 e Å⁻³ in CsIn(HAsO₄)₂. They are located about 1.65 Å from As at the same z coordinate value. At first, it seemed sensible that this position is a `flipped' As position centring an alternative location of the AsO₄ tetrahedron. An unrestrained refinement of this position led to occupancy factors of 0.984 (2) for As and 0.015 (2) for the second position and R1 decreased from 2.17 to 1.99%. However, the isotropic displacement parameter of the second position refined to zero, which suggested that this position may be an artifact. The position can be generated by a mirror plane in (110) (Fig. 6). Since application of appropriate twin matrices to the original model did not improve the refinement and since O ligands for this second possible As position could not be detected, the position was omitted from the model.

Figure 6
Possible second As position (AsB) in CsIn(HAsO₄)₂, which could explain the residual electron densities. The AsB position can roughly be generated by a mirror plane in (110). See text for discussion.

The highest residual electron densities of RbIn(HAsO₄)₂ are at or below 1 e Å⁻³ and 1.43 Å from atom O4. The highest residual electron densities of KIn(HAsO₄)₂ are 1.18 e Å⁻³ and close to the As position.

Supporting information

CCDC references: 1575921; 1575920; 1575919

Crystal structure: contains datablocks KInHAsO42, RbInHAsO42, CsInHAsO42. DOI: https://doi.org/10.1107/S205698901701355X/pj2047sup1.cif

Structure factors: contains datablock KInHAsO42. DOI: https://doi.org/10.1107/S205698901701355X/pj2047KInHAsO42sup2.hkl

Structure factors: contains datablock RbInHAsO42. DOI: https://doi.org/10.1107/S205698901701355X/pj2047RbInHAsO42sup3.hkl

Structure factors: contains datablock CsInHAsO42. DOI: https://doi.org/10.1107/S205698901701355X/pj2047CsInHAsO42sup4.hkl

checkCIF report

Computing details top

For all structures, data collection: COLLECT (Nonius, 2003); cell refinement: SCALEPACK (Otwinowski et al., 2003); data reduction: DENZO and SCALEPACK (Otwinowski et al., 2003); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL2016 (Sheldrick, 2015); molecular graphics: DIAMOND (Brandenburg, 2005); software used to prepare material for publication: publCIF (Westrip, 2010).

Potassium indium bis[hydrogen arsenate(V)] (KInHAsO42) top

Crystal data top

KIn(HAsO₄)₂	F(000) = 800
M_r = 433.78	D_x = 3.736 Mg m⁻³
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
a = 8.340 (2) Å	Cell parameters from 1474 reflections
b = 10.657 (2) Å	θ = 3.4–32.6°
c = 9.197 (2) Å	µ = 12.13 mm⁻¹
β = 109.37 (3)°	T = 293 K
V = 771.2 (3) Å³	Small prisms, colourless
Z = 4	0.19 × 0.02 × 0.02 mm

Data collection top

Nonius KappaCCD single-crystal four-circle diffractometer	1295 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	R_int = 0.015
φ and ω scans	θ_max = 32.6°, θ_min = 3.4°
Absorption correction: multi-scan (SCALEPACK; Otwinowski et al., 2003)	h = −12→12
T_min = 0.207, T_max = 0.794	k = −16→16
2743 measured reflections	l = −13→13
1406 independent reflections

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: difference Fourier map
R[F² > 2σ(F²)] = 0.019	All H-atom parameters refined
wR(F²) = 0.046	w = 1/[σ²(F_o²) + (0.0227P)² + 1.2908P] where P = (F_o² + 2F_c²)/3
S = 1.09	(Δ/σ)_max = 0.001
1406 reflections	Δρ_max = 1.18 e Å⁻³
64 parameters	Δρ_min = −1.00 e Å⁻³
1 restraint	Extinction correction: SHELXL2016 (Sheldrick, 2015), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.00181 (17)

Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
K1	0.250000	0.250000	0.000000	0.0437 (3)	0.976 (2)
K2	0.000000	0.678 (5)	0.250000	0.0437 (3)	0.024 (2)
In	0.000000	0.13427 (2)	0.250000	0.00852 (7)
As	0.27607 (3)	0.39725 (2)	0.36013 (2)	0.00952 (7)
O1	0.1914 (2)	0.26806 (16)	0.26523 (19)	0.0186 (3)
O2	0.3114 (2)	0.49181 (17)	0.22827 (18)	0.0177 (3)
O3	0.4522 (2)	0.36289 (15)	0.50672 (18)	0.0139 (3)
O4	0.1329 (2)	0.4729 (2)	0.4285 (2)	0.0254 (4)
H	0.159 (6)	0.473 (5)	0.529 (2)	0.076 (16)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
K1	0.0550 (7)	0.0588 (7)	0.0301 (5)	−0.0355 (6)	0.0312 (5)	−0.0195 (5)
K2	0.0550 (7)	0.0588 (7)	0.0301 (5)	−0.0355 (6)	0.0312 (5)	−0.0195 (5)
In	0.00910 (10)	0.00802 (11)	0.00799 (10)	0.000	0.00224 (7)	0.000
As	0.01099 (11)	0.00995 (12)	0.00731 (10)	−0.00206 (7)	0.00262 (8)	−0.00008 (7)
O1	0.0243 (9)	0.0157 (8)	0.0181 (8)	−0.0108 (7)	0.0103 (7)	−0.0055 (6)
O2	0.0199 (8)	0.0178 (8)	0.0114 (7)	−0.0096 (6)	−0.0003 (6)	0.0062 (6)
O3	0.0138 (7)	0.0176 (8)	0.0087 (7)	0.0024 (6)	0.0015 (6)	−0.0005 (5)
O4	0.0192 (9)	0.0402 (12)	0.0152 (8)	0.0122 (8)	0.0035 (7)	−0.0053 (8)

Geometric parameters (Å, º) top

K1—O1ⁱ	2.6488 (17)	K2—O3^ix	3.20 (3)
K1—O1	2.6488 (17)	K2—O2	3.33 (3)
K1—K2ⁱⁱ	2.653 (15)	K2—O2^viii	3.33 (3)
K1—K2ⁱⁱⁱ	2.653 (15)	K2—As^ix	3.35 (4)
K1—O3^iv	2.7788 (17)	K2—As^x	3.35 (4)
K1—O3^v	2.7788 (17)	In—O1	2.1104 (17)
K1—O4^vi	3.112 (2)	In—O1^viii	2.1104 (17)
K1—O4^vii	3.112 (2)	In—O3^iv	2.1388 (16)
K1—O2	3.2553 (19)	In—O3^xi	2.1388 (16)
K1—O2ⁱ	3.2553 (19)	In—O2^xii	2.1473 (16)
K1—As	3.6059 (7)	In—O2^vii	2.1473 (16)
K1—Asⁱ	3.6059 (7)	As—O1	1.6574 (17)
K2—O4	2.74 (4)	As—O3	1.6721 (17)
K2—O4^viii	2.74 (4)	As—O2	1.6762 (16)
K2—O1^ix	2.792 (18)	As—O4	1.7231 (19)
K2—O1^x	2.792 (18)	O4—H	0.876 (19)
K2—O3^x	3.20 (3)

O1ⁱ—K1—O1	180.0	K1^ix—K2—As^ix	72.8 (8)
O1ⁱ—K1—K2ⁱⁱ	63.6 (3)	K1^x—K2—As^ix	83.9 (10)
O1—K1—K2ⁱⁱ	116.4 (3)	O4—K2—As^ix	125.63 (13)
O1ⁱ—K1—K2ⁱⁱⁱ	116.4 (3)	O4^viii—K2—As^ix	122.06 (11)
O1—K1—K2ⁱⁱⁱ	63.6 (3)	O1^ix—K2—As^ix	29.6 (4)
K2ⁱⁱ—K1—K2ⁱⁱⁱ	180 (2)	O1^x—K2—As^ix	113.1 (16)
O1ⁱ—K1—O3^iv	115.35 (5)	O3^x—K2—As^ix	90.8 (12)
O1—K1—O3^iv	64.65 (5)	O3^ix—K2—As^ix	29.5 (3)
K2ⁱⁱ—K1—O3^iv	72.1 (6)	O2—K2—As^ix	82.73 (9)
K2ⁱⁱⁱ—K1—O3^iv	107.9 (6)	O2^viii—K2—As^ix	163.5 (6)
O1ⁱ—K1—O3^v	64.65 (5)	K1^ix—K2—As^x	83.9 (10)
O1—K1—O3^v	115.35 (5)	K1^x—K2—As^x	72.8 (8)
K2ⁱⁱ—K1—O3^v	107.9 (6)	O4—K2—As^x	122.06 (11)
K2ⁱⁱⁱ—K1—O3^v	72.1 (6)	O4^viii—K2—As^x	125.63 (13)
O3^iv—K1—O3^v	180.00 (6)	O1^ix—K2—As^x	113.1 (16)
O1ⁱ—K1—O4^vi	90.87 (5)	O1^x—K2—As^x	29.6 (4)
O1—K1—O4^vi	89.13 (5)	O3^x—K2—As^x	29.5 (3)
K2ⁱⁱ—K1—O4^vi	56.1 (11)	O3^ix—K2—As^x	90.8 (12)
K2ⁱⁱⁱ—K1—O4^vi	123.9 (11)	O2—K2—As^x	163.5 (6)
O3^iv—K1—O4^vi	101.27 (5)	O2^viii—K2—As^x	82.73 (9)
O3^v—K1—O4^vi	78.73 (5)	As^ix—K2—As^x	91.7 (13)
O1ⁱ—K1—O4^vii	89.13 (5)	O1—In—O1^viii	94.99 (10)
O1—K1—O4^vii	90.87 (5)	O1—In—O3^iv	86.23 (7)
K2ⁱⁱ—K1—O4^vii	123.9 (11)	O1^viii—In—O3^iv	92.67 (7)
K2ⁱⁱⁱ—K1—O4^vii	56.1 (11)	O1—In—O3^xi	92.67 (7)
O3^iv—K1—O4^vii	78.73 (5)	O1^viii—In—O3^xi	86.23 (7)
O3^v—K1—O4^vii	101.27 (5)	O3^iv—In—O3^xi	178.38 (9)
O4^vi—K1—O4^vii	180.0	O1—In—O2^xii	177.02 (7)
O1ⁱ—K1—O2	127.87 (5)	O1^viii—In—O2^xii	87.52 (7)
O1—K1—O2	52.13 (5)	O3^iv—In—O2^xii	92.07 (6)
K2ⁱⁱ—K1—O2	104.0 (10)	O3^xi—In—O2^xii	89.08 (7)
K2ⁱⁱⁱ—K1—O2	76.0 (10)	O1—In—O2^vii	87.52 (7)
O3^iv—K1—O2	106.19 (5)	O1^viii—In—O2^vii	177.02 (7)
O3^v—K1—O2	73.81 (5)	O3^iv—In—O2^vii	89.08 (7)
O4^vi—K1—O2	49.92 (5)	O3^xi—In—O2^vii	92.07 (6)
O4^vii—K1—O2	130.08 (5)	O2^xii—In—O2^vii	90.01 (10)
O1ⁱ—K1—O2ⁱ	52.13 (5)	O1—In—K1^viii	107.25 (5)
O1—K1—O2ⁱ	127.87 (5)	O1^viii—In—K1^viii	42.55 (5)
K2ⁱⁱ—K1—O2ⁱ	76.0 (10)	O3^iv—In—K1^viii	132.97 (5)
K2ⁱⁱⁱ—K1—O2ⁱ	104.0 (10)	O3^xi—In—K1^viii	46.31 (5)
O3^iv—K1—O2ⁱ	73.80 (5)	O2^xii—In—K1^viii	75.69 (5)
O3^v—K1—O2ⁱ	106.20 (5)	O2^vii—In—K1^viii	135.06 (5)
O4^vi—K1—O2ⁱ	130.08 (5)	O1—In—K1	42.55 (5)
O4^vii—K1—O2ⁱ	49.92 (5)	O1^viii—In—K1	107.25 (5)
O2—K1—O2ⁱ	180.0	O3^iv—In—K1	46.31 (5)
O1ⁱ—K1—As	154.71 (4)	O3^xi—In—K1	132.97 (5)
O1—K1—As	25.29 (4)	O2^xii—In—K1	135.06 (5)
K2ⁱⁱ—K1—As	117.5 (7)	O2^vii—In—K1	75.69 (5)
K2ⁱⁱⁱ—K1—As	62.5 (7)	K1^viii—In—K1	141.977 (12)
O3^iv—K1—As	87.14 (4)	O1—In—K2ⁱⁱⁱ	36.3 (7)
O3^v—K1—As	92.86 (4)	O1^viii—In—K2ⁱⁱⁱ	130.9 (7)
O4^vi—K1—As	72.55 (4)	O3^iv—In—K2ⁱⁱⁱ	80.73 (5)
O4^vii—K1—As	107.45 (4)	O3^xi—In—K2ⁱⁱⁱ	99.09 (6)
O2—K1—As	27.68 (3)	O2^xii—In—K2ⁱⁱⁱ	140.9 (7)
O2ⁱ—K1—As	152.32 (3)	O2^vii—In—K2ⁱⁱⁱ	51.8 (7)
O1ⁱ—K1—Asⁱ	25.29 (4)	K1^viii—In—K2ⁱⁱⁱ	135.3 (4)
O1—K1—Asⁱ	154.71 (4)	K1—In—K2ⁱⁱⁱ	38.4 (3)
K2ⁱⁱ—K1—Asⁱ	62.5 (7)	O1—In—K2^xii	130.9 (7)
K2ⁱⁱⁱ—K1—Asⁱ	117.5 (7)	O1^viii—In—K2^xii	36.3 (7)
O3^iv—K1—Asⁱ	92.86 (4)	O3^iv—In—K2^xii	99.09 (6)
O3^v—K1—Asⁱ	87.14 (4)	O3^xi—In—K2^xii	80.73 (5)
O4^vi—K1—Asⁱ	107.45 (4)	O2^xii—In—K2^xii	51.8 (7)
O4^vii—K1—Asⁱ	72.55 (4)	O2^vii—In—K2^xii	140.9 (7)
O2—K1—Asⁱ	152.32 (3)	K1^viii—In—K2^xii	38.4 (3)
O2ⁱ—K1—Asⁱ	27.68 (3)	K1—In—K2^xii	135.3 (4)
As—K1—Asⁱ	180.0	K2ⁱⁱⁱ—In—K2^xii	167.1 (14)
K1^ix—K2—K1^x	147 (2)	O1—As—O3	110.45 (9)
K1^ix—K2—O4	70.4 (4)	O1—As—O2	105.35 (8)
K1^x—K2—O4	142.6 (17)	O3—As—O2	113.38 (8)
K1^ix—K2—O4^viii	142.6 (17)	O1—As—O4	110.80 (10)
K1^x—K2—O4^viii	70.4 (4)	O3—As—O4	109.76 (8)
O4—K2—O4^viii	73.9 (13)	O2—As—O4	106.99 (10)
K1^ix—K2—O1^ix	58.2 (4)	O1—As—K2ⁱⁱⁱ	56.3 (5)
K1^x—K2—O1^ix	109.3 (10)	O3—As—K2ⁱⁱⁱ	70.26 (6)
O4—K2—O1^ix	96.2 (5)	O2—As—K2ⁱⁱⁱ	87.2 (6)
O4^viii—K2—O1^ix	116.1 (8)	O4—As—K2ⁱⁱⁱ	163.7 (7)
K1^ix—K2—O1^x	109.3 (10)	O1—As—K1	43.06 (6)
K1^x—K2—O1^x	58.2 (4)	O3—As—K1	114.49 (6)
O4—K2—O1^x	116.1 (8)	O2—As—K1	64.44 (6)
O4^viii—K2—O1^x	96.2 (5)	O4—As—K1	134.49 (6)
O1^ix—K2—O1^x	140 (2)	K2ⁱⁱⁱ—As—K1	44.66 (8)
K1^ix—K2—O3^x	55.8 (6)	O1—As—K2	114.2 (5)
K1^x—K2—O3^x	102.0 (12)	O3—As—K2	134.2 (4)
O4—K2—O3^x	100.01 (14)	O2—As—K2	63.8 (2)
O4^viii—K2—O3^x	144.0 (5)	O4—As—K2	43.88 (15)
O1^ix—K2—O3^x	99.8 (12)	K2ⁱⁱⁱ—As—K2	146.9 (3)
O1^x—K2—O3^x	53.8 (5)	K1—As—K2	104.94 (19)
K1^ix—K2—O3^ix	102.0 (12)	As—O1—In	140.97 (10)
K1^x—K2—O3^ix	55.8 (6)	As—O1—K1	111.65 (8)
O4—K2—O3^ix	144.0 (5)	In—O1—K1	104.85 (7)
O4^viii—K2—O3^ix	100.01 (14)	As—O1—K2ⁱⁱⁱ	94.1 (9)
O1^ix—K2—O3^ix	53.8 (5)	In—O1—K2ⁱⁱⁱ	117.1 (10)
O1^x—K2—O3^ix	99.8 (12)	K1—O1—K2ⁱⁱⁱ	58.29 (14)
O3^x—K2—O3^ix	104.1 (15)	As—O2—In^xiii	131.05 (9)
K1^ix—K2—O2	79.6 (4)	As—O2—K1	87.88 (7)
K1^x—K2—O2	121.6 (6)	In^xiii—O2—K1	124.98 (7)
O4—K2—O2	52.4 (7)	As—O2—K2	89.3 (6)
O4^viii—K2—O2	69.8 (10)	In^xiii—O2—K2	97.7 (7)
O1^ix—K2—O2	56.7 (3)	K1—O2—K2	123.5 (5)
O1^x—K2—O2	163.3 (17)	As—O3—In^xi	130.50 (9)
O3^x—K2—O2	134.62 (5)	As—O3—K1^v	129.02 (8)
O3^ix—K2—O2	91.84 (5)	In^xi—O3—K1^v	99.88 (6)
K1^ix—K2—O2^viii	121.6 (6)	As—O3—K2ⁱⁱⁱ	80.2 (3)
K1^x—K2—O2^viii	79.6 (4)	In^xi—O3—K2ⁱⁱⁱ	139.1 (7)
O4—K2—O2^viii	69.8 (10)	K1^v—O3—K2ⁱⁱⁱ	52.13 (8)
O4^viii—K2—O2^viii	52.4 (7)	As—O4—K2	110.3 (2)
O1^ix—K2—O2^viii	163.3 (17)	As—O4—K1^ix	108.30 (10)
O1^x—K2—O2^viii	56.7 (3)	K2—O4—K1^ix	53.4 (7)
O3^x—K2—O2^viii	91.84 (5)	As—O4—H	115 (3)
O3^ix—K2—O2^viii	134.62 (5)	K2—O4—H	123 (3)
O2—K2—O2^viii	106.6 (15)	K1^ix—O4—H	80 (3)

Symmetry codes: (i) −x+1/2, −y+1/2, −z; (ii) −x, −y+1, −z; (iii) x+1/2, y−1/2, z; (iv) x−1/2, −y+1/2, z−1/2; (v) −x+1, y, −z+1/2; (vi) x, −y+1, z−1/2; (vii) −x+1/2, y−1/2, −z+1/2; (viii) −x, y, −z+1/2; (ix) −x+1/2, y+1/2, −z+1/2; (x) x−1/2, y+1/2, z; (xi) −x+1/2, −y+1/2, −z+1; (xii) x−1/2, y−1/2, z; (xiii) x+1/2, y+1/2, z.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O4—H···O2^xiv	0.88 (2)	1.89 (3)	2.690 (3)	151 (4)

Symmetry code: (xiv) x, −y+1, z+1/2.

Rubidium indium bis[hydrogen arsenate(V)] (RbInHAsO42) top

Crystal data top

RbIn(HAsO₄)₂	D_x = 4.053 Mg m⁻³
M_r = 480.15	Mo Kα radiation, λ = 0.71073 Å
Trigonal, R3c:H	Cell parameters from 2882 reflections
a = 8.512 (1) Å	θ = 2.9–32.6°
c = 56.434 (11) Å	µ = 17.50 mm⁻¹
V = 3541.1 (11) Å³	T = 293 K
Z = 18	Small hexagonal platelets, colourless
F(000) = 3924	0.05 × 0.05 × 0.02 mm

Data collection top

Nonius KappaCCD single-crystal four-circle diffractometer	1255 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	R_int = 0.024
φ and ω scans	θ_max = 32.6°, θ_min = 2.9°
Absorption correction: multi-scan (SCALEPACK; Otwinowski et al., 2003)	h = −12→12
T_min = 0.475, T_max = 0.779	k = −10→10
5262 measured reflections	l = −85→85
1443 independent reflections

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: difference Fourier map
R[F² > 2σ(F²)] = 0.018	All H-atom parameters refined
wR(F²) = 0.041	w = 1/[σ²(F_o²) + (0.014P)² + 16.3085P] where P = (F_o² + 2F_c²)/3
S = 1.12	(Δ/σ)_max = 0.006
1443 reflections	Δρ_max = 1.00 e Å⁻³
69 parameters	Δρ_min = −0.86 e Å⁻³
3 restraints	Extinction correction: SHELXL2016 (Sheldrick, 2015), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.000313 (12)

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
Rb1A	0.000000	0.000000	0.750000	0.0236 (2)	0.949 (3)
Rb1B	0.000000	−0.051 (4)	0.750000	0.0236 (2)	0.0170 (9)
Rb2A	0.000000	0.000000	0.66882 (10)	0.0423 (6)	0.567 (3)
Rb2B	−0.0304 (11)	−0.0266 (11)	0.66795 (15)	0.0423 (6)	0.1442 (9)
In1	0.333333	0.666667	0.75297 (2)	0.01028 (7)
In2	0.333333	0.666667	0.666667	0.01217 (8)
As	−0.39741 (3)	−0.36940 (3)	0.71279 (2)	0.01097 (7)
O1	0.5235 (3)	−0.3776 (3)	0.68584 (3)	0.0298 (5)
O2	−0.4271 (2)	−0.2389 (2)	0.73221 (3)	0.0171 (3)
O3	−0.1635 (2)	−0.2654 (3)	0.70899 (3)	0.0201 (4)
O4	0.4679 (2)	−0.1119 (2)	0.77738 (3)	0.0155 (3)
H	−0.131 (6)	−0.339 (5)	0.7128 (7)	0.051 (13)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Rb1A	0.0267 (3)	0.0267 (3)	0.0175 (3)	0.01335 (15)	0.000	0.000
Rb1B	0.0267 (3)	0.0267 (3)	0.0175 (3)	0.01335 (15)	0.000	0.000
Rb2A	0.0509 (8)	0.0509 (8)	0.0250 (4)	0.0254 (4)	0.000	0.000
Rb2B	0.0509 (8)	0.0509 (8)	0.0250 (4)	0.0254 (4)	0.000	0.000
In1	0.01052 (8)	0.01052 (8)	0.00981 (12)	0.00526 (4)	0.000	0.000
In2	0.01472 (11)	0.01472 (11)	0.00707 (16)	0.00736 (6)	0.000	0.000
As	0.01290 (11)	0.01207 (11)	0.01030 (10)	0.00802 (9)	0.00056 (8)	0.00086 (8)
O1	0.0399 (12)	0.0513 (14)	0.0129 (8)	0.0337 (12)	−0.0062 (8)	−0.0002 (8)
O2	0.0170 (8)	0.0122 (8)	0.0203 (8)	0.0060 (7)	0.0076 (7)	−0.0012 (6)
O3	0.0145 (8)	0.0163 (9)	0.0308 (10)	0.0087 (7)	0.0061 (7)	0.0072 (7)
O4	0.0137 (8)	0.0133 (8)	0.0217 (8)	0.0084 (6)	−0.0038 (6)	−0.0056 (6)

Geometric parameters (Å, º) top

Rb1A—Rb1Bⁱ	0.44 (3)	Rb2A—O1^vi	3.462 (3)
Rb1A—Rb1Bⁱⁱ	0.44 (3)	Rb2A—O1^vii	3.462 (3)
Rb1A—O3ⁱⁱⁱ	3.042 (2)	Rb2A—O1^viii	3.462 (3)
Rb1A—O3ⁱ	3.042 (2)	Rb2A—O4^ix	3.668 (5)
Rb1A—O3^iv	3.042 (2)	Rb2A—O4^x	3.668 (5)
Rb1A—O3^v	3.042 (2)	Rb2A—O4^xi	3.668 (5)
Rb1A—O3ⁱⁱ	3.042 (2)	Rb2A—O1^xii	3.830 (3)
Rb1A—O3	3.042 (2)	Rb2A—O1^xiii	3.830 (3)
Rb1A—O2	3.3114 (19)	Rb2A—O1^xiv	3.830 (3)
Rb1A—O2^v	3.3115 (19)	Rb2A—O3^xv	3.888 (4)
Rb1A—O2^iv	3.3114 (19)	Rb2B—Rb2Bⁱ	0.423 (14)
Rb1A—O2ⁱⁱ	3.3114 (19)	Rb2B—Rb2Bⁱⁱ	0.423 (14)
Rb1A—O2ⁱⁱⁱ	3.3114 (18)	Rb2B—O3	2.911 (9)
Rb1A—O2ⁱ	3.3114 (18)	Rb2B—O3ⁱⁱ	3.056 (9)
Rb1A—Asⁱⁱⁱ	3.8862 (5)	Rb2B—O3ⁱ	3.185 (8)
Rb1A—H	3.28 (4)	Rb2B—O1^viii	3.259 (8)
Rb1A—Hⁱ	3.28 (4)	Rb2B—O1^vi	3.436 (9)
Rb1A—Hⁱⁱ	3.28 (4)	Rb2B—O4^x	3.525 (8)
Rb1A—H^iv	3.28 (4)	Rb2B—O1^xiii	3.608 (9)
Rb1A—Hⁱⁱⁱ	3.28 (4)	Rb2B—As^xvi	3.781 (8)
Rb1A—H^v	3.28 (4)	Rb2B—As^xv	3.869 (8)
Rb1B—Rb1Bⁱ	0.76 (6)	Rb2B—As	3.945 (9)
Rb1B—Rb1Bⁱⁱ	0.76 (5)	In1—O2^xvii	2.1306 (17)
Rb1B—O3^v	2.842 (12)	In1—O2ⁱⁱ	2.1306 (17)
Rb1B—O3	2.842 (12)	In1—O2^xviii	2.1306 (17)
Rb1B—O2^iv	2.98 (2)	In1—O4^xix	2.1457 (17)
Rb1B—O2ⁱ	2.98 (2)	In1—O4ⁱ	2.1457 (16)
Rb1B—O3^iv	3.035 (3)	In1—O4^xii	2.1457 (16)
Rb1B—O3ⁱ	3.035 (3)	In2—O1^vii	2.1312 (19)
Rb1B—O2	3.312 (3)	In2—O1^xvi	2.131 (2)
Rb1B—O2^v	3.312 (3)	In2—O1ⁱ	2.1312 (19)
Rb1B—O3ⁱⁱⁱ	3.32 (2)	In2—O1^xii	2.131 (2)
Rb1B—O3ⁱⁱ	3.32 (2)	In2—O1^xix	2.1312 (19)
Rb1B—H	2.99 (4)	In2—O1^xx	2.1312 (19)
Rb1B—H^v	2.99 (4)	As—O1^xiii	1.6508 (18)
Rb2A—Rb2Bⁱⁱ	0.249 (8)	As—O2	1.6668 (17)
Rb2A—Rb2Bⁱ	0.249 (8)	As—O4^v	1.6736 (17)
Rb2A—O3	3.006 (5)	As—O3	1.7409 (19)
Rb2A—O3ⁱ	3.006 (5)	O3—H	0.83 (3)
Rb2A—O3ⁱⁱ	3.006 (5)

Rb1Bⁱ—Rb1A—Rb1Bⁱⁱ	120.00 (12)	O3—Rb2A—O1^xiv	76.69 (8)
Rb1Bⁱ—Rb1A—O3ⁱⁱⁱ	59.08 (4)	O3ⁱ—Rb2A—O1^xiv	44.11 (5)
Rb1Bⁱⁱ—Rb1A—O3ⁱⁱⁱ	85.05 (9)	O3ⁱⁱ—Rb2A—O1^xiv	112.37 (15)
Rb1Bⁱ—Rb1A—O3ⁱ	59.08 (4)	O1^vi—Rb2A—O1^xiv	45.46 (6)
Rb1Bⁱⁱ—Rb1A—O3ⁱ	126.88 (5)	O1^vii—Rb2A—O1^xiv	95.29 (5)
O3ⁱⁱⁱ—Rb1A—O3ⁱ	118.16 (8)	O1^viii—Rb2A—O1^xiv	150.55 (6)
Rb1Bⁱ—Rb1A—O3^iv	126.88 (4)	O4^ix—Rb2A—O1^xiv	78.40 (6)
Rb1Bⁱⁱ—Rb1A—O3^iv	59.08 (7)	O4^x—Rb2A—O1^xiv	120.81 (10)
O3ⁱⁱⁱ—Rb1A—O3^iv	68.39 (6)	O4^xi—Rb2A—O1^xiv	111.19 (9)
O3ⁱ—Rb1A—O3^iv	170.10 (7)	O1^xii—Rb2A—O1^xiv	113.93 (7)
Rb1Bⁱ—Rb1A—O3^v	85.05 (4)	O1^xiii—Rb2A—O1^xiv	113.93 (7)
Rb1Bⁱⁱ—Rb1A—O3^v	126.88 (5)	Rb2Bⁱⁱ—Rb2A—O3^xv	126 (3)
O3ⁱⁱⁱ—Rb1A—O3^v	68.39 (6)	Rb2Bⁱ—Rb2A—O3^xv	74 (3)
O3ⁱ—Rb1A—O3^v	106.24 (7)	O3—Rb2A—O3^xv	89.86 (5)
O3^iv—Rb1A—O3^v	68.39 (6)	O3ⁱ—Rb2A—O3^xv	129.48 (6)
Rb1Bⁱ—Rb1A—O3ⁱⁱ	85.05 (4)	O3ⁱⁱ—Rb2A—O3^xv	145.79 (7)
Rb1Bⁱⁱ—Rb1A—O3ⁱⁱ	59.08 (7)	O1^vi—Rb2A—O3^xv	42.24 (6)
O3ⁱⁱⁱ—Rb1A—O3ⁱⁱ	106.24 (7)	O1^vii—Rb2A—O3^xv	117.63 (15)
O3ⁱ—Rb1A—O3ⁱⁱ	68.39 (6)	O1^viii—Rb2A—O3^xv	66.65 (8)
O3^iv—Rb1A—O3ⁱⁱ	118.16 (7)	O4^ix—Rb2A—O3^xv	42.47 (6)
O3^v—Rb1A—O3ⁱⁱ	170.10 (8)	O4^x—Rb2A—O3^xv	40.66 (6)
Rb1Bⁱ—Rb1A—O3	126.88 (4)	O4^xi—Rb2A—O3^xv	76.43 (11)
Rb1Bⁱⁱ—Rb1A—O3	85.05 (9)	O1^xii—Rb2A—O3^xv	151.71 (14)
O3ⁱⁱⁱ—Rb1A—O3	170.10 (7)	O1^xiii—Rb2A—O3^xv	69.64 (5)
O3ⁱ—Rb1A—O3	68.38 (6)	O1^xiv—Rb2A—O3^xv	87.30 (5)
O3^iv—Rb1A—O3	106.24 (7)	Rb2Bⁱ—Rb2B—Rb2Bⁱⁱ	60.00 (6)
O3^v—Rb1A—O3	118.16 (7)	Rb2Bⁱ—Rb2B—O3	106.1 (12)
O3ⁱⁱ—Rb1A—O3	68.38 (6)	Rb2Bⁱⁱ—Rb2B—O3	127.22 (14)
Rb1Bⁱ—Rb1A—O2	148.87 (3)	Rb2Bⁱ—Rb2B—O3ⁱⁱ	104.1 (12)
Rb1Bⁱⁱ—Rb1A—O2	37.75 (11)	Rb2Bⁱⁱ—Rb2B—O3ⁱⁱ	66.3 (12)
O3ⁱⁱⁱ—Rb1A—O2	120.30 (5)	O3—Rb2B—O3ⁱⁱ	69.9 (2)
O3ⁱ—Rb1A—O2	112.03 (5)	Rb2Bⁱ—Rb2B—O3ⁱ	46.66 (16)
O3^iv—Rb1A—O2	67.27 (5)	Rb2Bⁱⁱ—Rb2B—O3ⁱ	68.5 (12)
O3^v—Rb1A—O2	125.02 (5)	O3—Rb2B—O3ⁱ	68.05 (19)
O3ⁱⁱ—Rb1A—O2	64.77 (5)	O3ⁱⁱ—Rb2B—O3ⁱ	66.39 (17)
O3—Rb1A—O2	50.13 (4)	Rb2Bⁱ—Rb2B—O1^viii	158.2 (7)
Rb1Bⁱ—Rb1A—O2^v	37.75 (3)	Rb2Bⁱⁱ—Rb2B—O1^viii	111 (2)
Rb1Bⁱⁱ—Rb1A—O2^v	148.87 (10)	O3—Rb2B—O1^viii	94.9 (2)
O3ⁱⁱⁱ—Rb1A—O2^v	64.77 (5)	O3ⁱⁱ—Rb2B—O1^viii	88.5 (2)
O3ⁱ—Rb1A—O2^v	67.27 (5)	O3ⁱ—Rb2B—O1^viii	153.0 (3)
O3^iv—Rb1A—O2^v	112.03 (5)	Rb2Bⁱ—Rb2B—O1^vi	62.0 (19)
O3^v—Rb1A—O2^v	50.13 (5)	Rb2Bⁱⁱ—Rb2B—O1^vi	118.2 (19)
O3ⁱⁱ—Rb1A—O2^v	120.30 (5)	O3—Rb2B—O1^vi	87.5 (2)
O3—Rb1A—O2^v	125.02 (5)	O3ⁱⁱ—Rb2B—O1^vi	149.7 (3)
O2—Rb1A—O2^v	172.51 (6)	O3ⁱ—Rb2B—O1^vi	86.8 (2)
Rb1Bⁱ—Rb1A—O2^iv	148.87 (3)	O1^viii—Rb2B—O1^vi	114.2 (2)
Rb1Bⁱⁱ—Rb1A—O2^iv	86.26 (12)	Rb2Bⁱ—Rb2B—O4^x	113.2 (3)
O3ⁱⁱⁱ—Rb1A—O2^iv	112.03 (5)	Rb2Bⁱⁱ—Rb2B—O4^x	105.2 (7)
O3ⁱ—Rb1A—O2^iv	120.30 (5)	O3—Rb2B—O4^x	125.4 (3)
O3^iv—Rb1A—O2^iv	50.13 (4)	O3ⁱⁱ—Rb2B—O4^x	130.1 (3)
O3^v—Rb1A—O2^iv	64.77 (5)	O3ⁱ—Rb2B—O4^x	159.7 (3)
O3ⁱⁱ—Rb1A—O2^iv	125.02 (5)	O1^viii—Rb2B—O4^x	47.08 (11)
O3—Rb1A—O2^iv	67.27 (5)	O1^vi—Rb2B—O4^x	79.33 (17)
O2—Rb1A—O2^iv	62.27 (6)	Rb2Bⁱ—Rb2B—O1^xiii	150.5 (18)
O2^v—Rb1A—O2^iv	111.23 (3)	Rb2Bⁱⁱ—Rb2B—O1^xiii	141.8 (19)
Rb1Bⁱ—Rb1A—O2ⁱⁱ	37.75 (3)	O3—Rb2B—O1^xiii	47.02 (14)
Rb1Bⁱⁱ—Rb1A—O2ⁱⁱ	86.26 (12)	O3ⁱⁱ—Rb2B—O1^xiii	79.7 (2)
O3ⁱⁱⁱ—Rb1A—O2ⁱⁱ	67.27 (5)	O3ⁱ—Rb2B—O1^xiii	113.9 (3)
O3ⁱ—Rb1A—O2ⁱⁱ	64.77 (5)	O1^viii—Rb2B—O1^xiii	48.49 (13)
O3^iv—Rb1A—O2ⁱⁱ	125.02 (5)	O1^vi—Rb2B—O1^xiii	99.9 (2)
O3^v—Rb1A—O2ⁱⁱ	120.30 (5)	O4^x—Rb2B—O1^xiii	83.29 (17)
O3ⁱⁱ—Rb1A—O2ⁱⁱ	50.13 (5)	Rb2Bⁱ—Rb2B—As^xvi	132.4 (6)
O3—Rb1A—O2ⁱⁱ	112.03 (5)	Rb2Bⁱⁱ—Rb2B—As^xvi	98.8 (15)
O2—Rb1A—O2ⁱⁱ	111.23 (3)	O3—Rb2B—As^xvi	119.4 (2)
O2^v—Rb1A—O2ⁱⁱ	75.50 (6)	O3ⁱⁱ—Rb2B—As^xvi	104.1 (2)
O2^iv—Rb1A—O2ⁱⁱ	172.51 (6)	O3ⁱ—Rb2B—As^xvi	166.2 (3)
Rb1Bⁱ—Rb1A—O2ⁱⁱⁱ	86.26 (3)	O1^viii—Rb2B—As^xvi	25.78 (7)
Rb1Bⁱⁱ—Rb1A—O2ⁱⁱⁱ	37.75 (11)	O1^vi—Rb2B—As^xvi	104.6 (2)
O3ⁱⁱⁱ—Rb1A—O2ⁱⁱⁱ	50.13 (4)	O4^x—Rb2B—As^xvi	26.18 (6)
O3ⁱ—Rb1A—O2ⁱⁱⁱ	125.02 (5)	O1^xiii—Rb2B—As^xvi	72.35 (15)
O3^iv—Rb1A—O2ⁱⁱⁱ	64.77 (5)	Rb2Bⁱ—Rb2B—As^xv	75.0 (15)
O3^v—Rb1A—O2ⁱⁱⁱ	112.03 (5)	Rb2Bⁱⁱ—Rb2B—As^xv	117.0 (13)
O3ⁱⁱ—Rb1A—O2ⁱⁱⁱ	67.27 (5)	O3—Rb2B—As^xv	105.0 (2)
O3—Rb1A—O2ⁱⁱⁱ	120.30 (5)	O3ⁱⁱ—Rb2B—As^xv	174.4 (3)
O2—Rb1A—O2ⁱⁱⁱ	75.50 (6)	O3ⁱ—Rb2B—As^xv	110.1 (2)
O2^v—Rb1A—O2ⁱⁱⁱ	111.23 (3)	O1^viii—Rb2B—As^xv	94.17 (18)
O2^iv—Rb1A—O2ⁱⁱⁱ	111.23 (3)	O1^vi—Rb2B—As^xv	25.24 (7)
O2ⁱⁱ—Rb1A—O2ⁱⁱⁱ	62.27 (6)	O4^x—Rb2B—As^xv	54.35 (12)
Rb1Bⁱ—Rb1A—O2ⁱ	86.26 (3)	O1^xiii—Rb2B—As^xv	98.42 (18)
Rb1Bⁱⁱ—Rb1A—O2ⁱ	148.87 (11)	As^xvi—Rb2B—As^xv	80.12 (15)
O3ⁱⁱⁱ—Rb1A—O2ⁱ	125.02 (5)	Rb2Bⁱ—Rb2B—As	129.9 (12)
O3ⁱ—Rb1A—O2ⁱ	50.13 (4)	Rb2Bⁱⁱ—Rb2B—As	133.2 (10)
O3^iv—Rb1A—O2ⁱ	120.30 (5)	O3—Rb2B—As	23.86 (9)
O3^v—Rb1A—O2ⁱ	67.27 (5)	O3ⁱⁱ—Rb2B—As	67.16 (17)
O3ⁱⁱ—Rb1A—O2ⁱ	112.03 (5)	O3ⁱ—Rb2B—As	89.1 (2)
O3—Rb1A—O2ⁱ	64.77 (5)	O1^viii—Rb2B—As	71.31 (17)
O2—Rb1A—O2ⁱ	111.23 (3)	O1^vi—Rb2B—As	100.0 (2)
O2^v—Rb1A—O2ⁱ	62.27 (6)	O4^x—Rb2B—As	107.7 (2)
O2^iv—Rb1A—O2ⁱ	75.50 (6)	O1^xiii—Rb2B—As	24.73 (7)
O2ⁱⁱ—Rb1A—O2ⁱ	111.23 (3)	As^xvi—Rb2B—As	96.34 (18)
O2ⁱⁱⁱ—Rb1A—O2ⁱ	172.51 (7)	As^xv—Rb2B—As	109.1 (2)
Rb1Bⁱ—Rb1A—Asⁱⁱⁱ	68.045 (6)	O2^xvii—In1—O2ⁱⁱ	92.65 (7)
Rb1Bⁱⁱ—Rb1A—Asⁱⁱⁱ	62.23 (10)	O2^xvii—In1—O2^xviii	92.65 (7)
O3ⁱⁱⁱ—Rb1A—Asⁱⁱⁱ	25.58 (3)	O2ⁱⁱ—In1—O2^xviii	92.65 (7)
O3ⁱ—Rb1A—Asⁱⁱⁱ	121.18 (4)	O2^xvii—In1—O4^xix	91.95 (7)
O3^iv—Rb1A—Asⁱⁱⁱ	68.11 (4)	O2ⁱⁱ—In1—O4^xix	173.42 (7)
O3^v—Rb1A—Asⁱⁱⁱ	92.38 (4)	O2^xviii—In1—O4^xix	91.82 (7)
O3ⁱⁱ—Rb1A—Asⁱⁱⁱ	83.92 (4)	O2^xvii—In1—O4ⁱ	91.82 (7)
O3—Rb1A—Asⁱⁱⁱ	145.24 (3)	O2ⁱⁱ—In1—O4ⁱ	91.95 (7)
O2—Rb1A—Asⁱⁱⁱ	99.68 (3)	O2^xviii—In1—O4ⁱ	173.42 (7)
O2^v—Rb1A—Asⁱⁱⁱ	86.65 (3)	O4^xix—In1—O4ⁱ	83.21 (7)
O2^iv—Rb1A—Asⁱⁱⁱ	118.16 (3)	O2^xvii—In1—O4^xii	173.42 (7)
O2ⁱⁱ—Rb1A—Asⁱⁱⁱ	57.81 (3)	O2ⁱⁱ—In1—O4^xii	91.82 (7)
O2ⁱⁱⁱ—Rb1A—Asⁱⁱⁱ	25.19 (3)	O2^xviii—In1—O4^xii	91.95 (7)
O2ⁱ—Rb1A—Asⁱⁱⁱ	148.88 (3)	O4^xix—In1—O4^xii	83.21 (7)
Rb1Bⁱ—Rb1A—H	127.6 (7)	O4ⁱ—In1—O4^xii	83.21 (7)
Rb1Bⁱⁱ—Rb1A—H	95.7 (8)	O2^xvii—In1—Rb2A^xxi	123.37 (5)
O3ⁱⁱⁱ—Rb1A—H	170.2 (6)	O2ⁱⁱ—In1—Rb2A^xxi	123.36 (5)
O3ⁱ—Rb1A—H	69.0 (7)	O2^xviii—In1—Rb2A^xxi	123.36 (5)
O3^iv—Rb1A—H	103.6 (7)	O4^xix—In1—Rb2A^xxi	50.06 (5)
O3^v—Rb1A—H	103.8 (6)	O4ⁱ—In1—Rb2A^xxi	50.06 (5)
O3ⁱⁱ—Rb1A—H	82.3 (6)	O4^xii—In1—Rb2A^xxi	50.06 (5)
O3—Rb1A—H	14.5 (6)	O2^xvii—In1—Rb1A^xix	32.08 (5)
O2—Rb1A—H	58.6 (7)	O2ⁱⁱ—In1—Rb1A^xix	107.92 (5)
O2^v—Rb1A—H	115.4 (7)	O2^xviii—In1—Rb1A^xix	118.90 (5)
O2^iv—Rb1A—H	58.4 (6)	O4^xix—In1—Rb1A^xix	73.96 (4)
O2ⁱⁱ—Rb1A—H	122.5 (6)	O4ⁱ—In1—Rb1A^xix	63.88 (4)
O2ⁱⁱⁱ—Rb1A—H	132.7 (7)	O4^xii—In1—Rb1A^xix	141.47 (5)
O2ⁱ—Rb1A—H	53.3 (7)	Rb2A^xxi—In1—Rb1A^xix	91.955 (3)
Asⁱⁱⁱ—Rb1A—H	157.8 (7)	O2^xvii—In1—Rb1A	118.90 (5)
Rb1Bⁱ—Rb1A—Hⁱ	44.8 (6)	O2ⁱⁱ—In1—Rb1A	32.08 (5)
Rb1Bⁱⁱ—Rb1A—Hⁱ	127.6 (8)	O2^xviii—In1—Rb1A	107.92 (5)
O3ⁱⁱⁱ—Rb1A—Hⁱ	103.8 (6)	O4^xix—In1—Rb1A	141.47 (5)
O3ⁱ—Rb1A—Hⁱ	14.5 (6)	O4ⁱ—In1—Rb1A	73.96 (4)
O3^iv—Rb1A—Hⁱ	170.2 (6)	O4^xii—In1—Rb1A	63.88 (5)
O3^v—Rb1A—Hⁱ	103.6 (7)	Rb2A^xxi—In1—Rb1A	91.954 (3)
O3ⁱⁱ—Rb1A—Hⁱ	69.0 (7)	Rb1A^xix—In1—Rb1A	119.9
O3—Rb1A—Hⁱ	82.3 (6)	O2^xvii—In1—Rb1A^xviii	107.92 (5)
O2—Rb1A—Hⁱ	122.5 (6)	O2ⁱⁱ—In1—Rb1A^xviii	118.90 (5)
O2^v—Rb1A—Hⁱ	58.4 (6)	O2^xviii—In1—Rb1A^xviii	32.08 (5)
O2^iv—Rb1A—Hⁱ	132.7 (7)	O4^xix—In1—Rb1A^xviii	63.88 (5)
O2ⁱⁱ—Rb1A—Hⁱ	53.3 (7)	O4ⁱ—In1—Rb1A^xviii	141.47 (5)
O2ⁱⁱⁱ—Rb1A—Hⁱ	115.4 (7)	O4^xii—In1—Rb1A^xviii	73.96 (5)
O2ⁱ—Rb1A—Hⁱ	58.6 (7)	Rb2A^xxi—In1—Rb1A^xviii	91.954 (3)
Asⁱⁱⁱ—Rb1A—Hⁱ	107.6 (7)	Rb1A^xix—In1—Rb1A^xviii	119.9
H—Rb1A—Hⁱ	83.5 (9)	Rb1A—In1—Rb1A^xviii	119.9
Rb1Bⁱ—Rb1A—Hⁱⁱ	95.7 (7)	O1^vii—In2—O1^xvi	96.52 (7)
Rb1Bⁱⁱ—Rb1A—Hⁱⁱ	44.8 (6)	O1^vii—In2—O1ⁱ	180.0
O3ⁱⁱⁱ—Rb1A—Hⁱⁱ	103.6 (7)	O1^xvi—In2—O1ⁱ	83.48 (7)
O3ⁱ—Rb1A—Hⁱⁱ	82.3 (6)	O1^vii—In2—O1^xii	83.48 (7)
O3^iv—Rb1A—Hⁱⁱ	103.8 (6)	O1^xvi—In2—O1^xii	180.0
O3^v—Rb1A—Hⁱⁱ	170.2 (6)	O1ⁱ—In2—O1^xii	96.52 (7)
O3ⁱⁱ—Rb1A—Hⁱⁱ	14.5 (6)	O1^vii—In2—O1^xix	83.48 (7)
O3—Rb1A—Hⁱⁱ	69.0 (7)	O1^xvi—In2—O1^xix	83.48 (7)
O2—Rb1A—Hⁱⁱ	53.3 (7)	O1ⁱ—In2—O1^xix	96.52 (7)
O2^v—Rb1A—Hⁱⁱ	132.7 (7)	O1^xii—In2—O1^xix	96.52 (7)
O2^iv—Rb1A—Hⁱⁱ	115.4 (8)	O1^vii—In2—O1^xx	96.52 (7)
O2ⁱⁱ—Rb1A—Hⁱⁱ	58.6 (7)	O1^xvi—In2—O1^xx	96.52 (7)
O2ⁱⁱⁱ—Rb1A—Hⁱⁱ	58.4 (6)	O1ⁱ—In2—O1^xx	83.48 (7)
O2ⁱ—Rb1A—Hⁱⁱ	122.5 (6)	O1^xii—In2—O1^xx	83.48 (7)
Asⁱⁱⁱ—Rb1A—Hⁱⁱ	78.9 (7)	O1^xix—In2—O1^xx	180.0
H—Rb1A—Hⁱⁱ	83.5 (9)	O1^vii—In2—Rb2A^xx	47.93 (8)
Hⁱ—Rb1A—Hⁱⁱ	83.5 (9)	O1^xvi—In2—Rb2A^xx	80.47 (7)
Rb1Bⁱ—Rb1A—H^iv	127.6 (7)	O1ⁱ—In2—Rb2A^xx	132.07 (8)
Rb1Bⁱⁱ—Rb1A—H^iv	44.8 (6)	O1^xii—In2—Rb2A^xx	99.53 (7)
O3ⁱⁱⁱ—Rb1A—H^iv	69.0 (7)	O1^xix—In2—Rb2A^xx	37.05 (8)
O3ⁱ—Rb1A—H^iv	170.2 (6)	O1^xx—In2—Rb2A^xx	142.95 (8)
O3^iv—Rb1A—H^iv	14.5 (6)	O1^vii—In2—Rb2A^xix	132.07 (8)
O3^v—Rb1A—H^iv	82.3 (6)	O1^xvi—In2—Rb2A^xix	99.53 (7)
O3ⁱⁱ—Rb1A—H^iv	103.8 (6)	O1ⁱ—In2—Rb2A^xix	47.93 (8)
O3—Rb1A—H^iv	103.6 (7)	O1^xii—In2—Rb2A^xix	80.47 (7)
O2—Rb1A—H^iv	58.4 (6)	O1^xix—In2—Rb2A^xix	142.95 (8)
O2^v—Rb1A—H^iv	122.5 (6)	O1^xx—In2—Rb2A^xix	37.05 (8)
O2^iv—Rb1A—H^iv	58.6 (7)	Rb2A^xx—In2—Rb2A^xix	180.0
O2ⁱⁱ—Rb1A—H^iv	115.4 (7)	O1^vii—In2—Rb2A	37.05 (8)
O2ⁱⁱⁱ—Rb1A—H^iv	53.3 (7)	O1^xvi—In2—Rb2A	132.07 (8)
O2ⁱ—Rb1A—H^iv	132.7 (7)	O1ⁱ—In2—Rb2A	142.95 (8)
Asⁱⁱⁱ—Rb1A—H^iv	62.0 (7)	O1^xii—In2—Rb2A	47.93 (8)
H—Rb1A—H^iv	104.8 (15)	O1^xix—In2—Rb2A	80.47 (7)
Hⁱ—Rb1A—H^iv	168.6 (14)	O1^xx—In2—Rb2A	99.53 (7)
Hⁱⁱ—Rb1A—H^iv	89.6 (11)	Rb2A^xx—In2—Rb2A	60.060 (6)
Rb1Bⁱ—Rb1A—Hⁱⁱⁱ	44.8 (6)	Rb2A^xix—In2—Rb2A	119.940 (6)
Rb1Bⁱⁱ—Rb1A—Hⁱⁱⁱ	95.7 (8)	O1^vii—In2—Rb2A^xviii	99.53 (7)
O3ⁱⁱⁱ—Rb1A—Hⁱⁱⁱ	14.5 (6)	O1^xvi—In2—Rb2A^xviii	37.05 (8)
O3ⁱ—Rb1A—Hⁱⁱⁱ	103.8 (6)	O1ⁱ—In2—Rb2A^xviii	80.47 (7)
O3^iv—Rb1A—Hⁱⁱⁱ	82.3 (6)	O1^xii—In2—Rb2A^xviii	142.95 (8)
O3^v—Rb1A—Hⁱⁱⁱ	69.0 (7)	O1^xix—In2—Rb2A^xviii	47.93 (8)
O3ⁱⁱ—Rb1A—Hⁱⁱⁱ	103.6 (7)	O1^xx—In2—Rb2A^xviii	132.07 (8)
O3—Rb1A—Hⁱⁱⁱ	170.2 (6)	Rb2A^xx—In2—Rb2A^xviii	60.060 (6)
O2—Rb1A—Hⁱⁱⁱ	132.7 (7)	Rb2A^xix—In2—Rb2A^xviii	119.940 (7)
O2^v—Rb1A—Hⁱⁱⁱ	53.3 (7)	Rb2A—In2—Rb2A^xviii	119.940 (6)
O2^iv—Rb1A—Hⁱⁱⁱ	122.5 (6)	O1^vii—In2—Rb2A^xxii	80.47 (7)
O2ⁱⁱ—Rb1A—Hⁱⁱⁱ	58.4 (6)	O1^xvi—In2—Rb2A^xxii	142.95 (8)
O2ⁱⁱⁱ—Rb1A—Hⁱⁱⁱ	58.6 (7)	O1ⁱ—In2—Rb2A^xxii	99.53 (7)
O2ⁱ—Rb1A—Hⁱⁱⁱ	115.4 (7)	O1^xii—In2—Rb2A^xxii	37.05 (8)
Asⁱⁱⁱ—Rb1A—Hⁱⁱⁱ	33.5 (7)	O1^xix—In2—Rb2A^xxii	132.07 (8)
H—Rb1A—Hⁱⁱⁱ	168.6 (14)	O1^xx—In2—Rb2A^xxii	47.93 (8)
Hⁱ—Rb1A—Hⁱⁱⁱ	89.6 (12)	Rb2A^xx—In2—Rb2A^xxii	119.940 (6)
Hⁱⁱ—Rb1A—Hⁱⁱⁱ	104.8 (15)	Rb2A^xix—In2—Rb2A^xxii	60.060 (6)
H^iv—Rb1A—Hⁱⁱⁱ	83.5 (9)	Rb2A—In2—Rb2A^xxii	60.061 (6)
Rb1Bⁱ—Rb1A—H^v	95.7 (7)	Rb2A^xviii—In2—Rb2A^xxii	180.0
Rb1Bⁱⁱ—Rb1A—H^v	127.6 (8)	O1^vii—In2—Rb2A^xxiii	142.95 (8)
O3ⁱⁱⁱ—Rb1A—H^v	82.3 (6)	O1^xvi—In2—Rb2A^xxiii	47.93 (8)
O3ⁱ—Rb1A—H^v	103.6 (7)	O1ⁱ—In2—Rb2A^xxiii	37.05 (8)
O3^iv—Rb1A—H^v	69.0 (7)	O1^xii—In2—Rb2A^xxiii	132.07 (8)
O3^v—Rb1A—H^v	14.5 (6)	O1^xix—In2—Rb2A^xxiii	99.53 (7)
O3ⁱⁱ—Rb1A—H^v	170.2 (6)	O1^xx—In2—Rb2A^xxiii	80.47 (7)
O3—Rb1A—H^v	103.8 (6)	Rb2A^xx—In2—Rb2A^xxiii	119.940 (7)
O2—Rb1A—H^v	115.4 (8)	Rb2A^xix—In2—Rb2A^xxiii	60.060 (6)
O2^v—Rb1A—H^v	58.6 (7)	Rb2A—In2—Rb2A^xxiii	180.0
O2^iv—Rb1A—H^v	53.3 (7)	Rb2A^xviii—In2—Rb2A^xxiii	60.061 (6)
O2ⁱⁱ—Rb1A—H^v	132.7 (7)	Rb2A^xxii—In2—Rb2A^xxiii	119.939 (6)
O2ⁱⁱⁱ—Rb1A—H^v	122.5 (6)	O1^xiii—As—O2	116.08 (10)
O2ⁱ—Rb1A—H^v	58.4 (6)	O1^xiii—As—O4^v	109.85 (10)
Asⁱⁱⁱ—Rb1A—H^v	105.4 (6)	O2—As—O4^v	113.73 (8)
H—Rb1A—H^v	89.6 (11)	O1^xiii—As—O3	104.27 (10)
Hⁱ—Rb1A—H^v	104.8 (14)	O2—As—O3	104.94 (9)
Hⁱⁱ—Rb1A—H^v	168.6 (15)	O4^v—As—O3	106.99 (8)
H^iv—Rb1A—H^v	83.5 (9)	O1^xiii—As—Rb1Bⁱⁱ	133.87 (15)
Hⁱⁱⁱ—Rb1A—H^v	83.5 (9)	O2—As—Rb1Bⁱⁱ	51.9 (5)
Rb1Bⁱ—Rb1B—Rb1Bⁱⁱ	60.00 (3)	O4^v—As—Rb1Bⁱⁱ	115.4 (2)
Rb1Bⁱ—Rb1B—O3^v	97.5 (5)	O3—As—Rb1Bⁱⁱ	54.3 (4)
Rb1Bⁱⁱ—Rb1B—O3^v	123.7 (5)	O1^xiii—As—Rb1B	138.5 (3)
Rb1Bⁱ—Rb1B—O3	123.7 (5)	O2—As—Rb1B	62.1 (4)
Rb1Bⁱⁱ—Rb1B—O3	97.5 (6)	O4^v—As—Rb1B	107.4 (4)
O3^v—Rb1B—O3	133.3 (11)	O3—As—Rb1B	46.49 (19)
Rb1Bⁱ—Rb1B—O2^iv	158.5 (3)	Rb1Bⁱⁱ—As—Rb1B	11.6 (9)
Rb1Bⁱⁱ—Rb1B—O2^iv	109.8 (5)	O1^xiii—As—Rb2B^xxiv	59.16 (16)
O3^v—Rb1B—O2^iv	71.7 (5)	O2—As—Rb2B^xxiv	175.06 (16)
O3—Rb1B—O2^iv	74.5 (5)	O4^v—As—Rb2B^xxiv	68.35 (14)
Rb1Bⁱ—Rb1B—O2ⁱ	109.8 (4)	O3—As—Rb2B^xxiv	78.23 (14)
Rb1Bⁱⁱ—Rb1B—O2ⁱ	158.5 (3)	Rb1Bⁱⁱ—As—Rb2B^xxiv	131.9 (5)
O3^v—Rb1B—O2ⁱ	74.5 (5)	Rb1B—As—Rb2B^xxiv	122.0 (3)
O3—Rb1B—O2ⁱ	71.7 (5)	O1^xiii—As—Rb2B^xv	62.57 (15)
O2^iv—Rb1B—O2ⁱ	85.8 (8)	O2—As—Rb2B^xv	175.80 (17)
Rb1Bⁱ—Rb1B—O3^iv	105.8 (5)	O4^v—As—Rb2B^xv	70.24 (15)
Rb1Bⁱⁱ—Rb1B—O3^iv	68.2 (6)	O3—As—Rb2B^xv	72.08 (14)
O3^v—Rb1B—O3^iv	71.05 (15)	Rb1Bⁱⁱ—As—Rb2B^xv	125.7 (4)
O3—Rb1B—O3^iv	111.7 (3)	Rb1B—As—Rb2B^xv	115.9 (3)
O2^iv—Rb1B—O3^iv	53.4 (2)	Rb2B^xxiv—As—Rb2B^xv	6.2 (2)
O2ⁱ—Rb1B—O3^iv	132.8 (9)	O1^xiii—As—Rb1A	134.73 (9)
Rb1Bⁱ—Rb1B—O3ⁱ	68.2 (5)	O2—As—Rb1A	57.74 (6)
Rb1Bⁱⁱ—Rb1B—O3ⁱ	105.8 (5)	O4^v—As—Rb1A	112.84 (6)
O3^v—Rb1B—O3ⁱ	111.7 (3)	O3—As—Rb1A	48.98 (7)
O3—Rb1B—O3ⁱ	71.04 (15)	Rb1Bⁱⁱ—As—Rb1A	6.0 (4)
O2^iv—Rb1B—O3ⁱ	132.8 (9)	Rb1B—As—Rb1A	6.2 (5)
O2ⁱ—Rb1B—O3ⁱ	53.4 (2)	Rb2B^xxiv—As—Rb1A	126.16 (13)
O3^iv—Rb1B—O3ⁱ	173.4 (12)	Rb2B^xv—As—Rb1A	119.97 (12)
Rb1Bⁱ—Rb1B—O2	114.7 (5)	O1^xiii—As—Rb2A^xv	61.31 (9)
Rb1Bⁱⁱ—Rb1B—O2	57.8 (6)	O2—As—Rb2A^xv	177.30 (9)
O3^v—Rb1B—O2	132.6 (4)	O4^v—As—Rb2A^xv	68.43 (8)
O3—Rb1B—O2	51.41 (7)	O3—As—Rb2A^xv	75.58 (7)
O2^iv—Rb1B—O2	65.7 (2)	Rb1Bⁱⁱ—As—Rb2A^xv	129.1 (4)
O2ⁱ—Rb1B—O2	120.6 (6)	Rb1B—As—Rb2A^xv	119.2 (3)
O3^iv—Rb1B—O2	67.34 (7)	Rb2B^xxiv—As—Rb2A^xv	2.88 (15)
O3ⁱ—Rb1B—O2	112.19 (11)	Rb2B^xv—As—Rb2A^xv	3.52 (13)
Rb1Bⁱ—Rb1B—O2^v	57.8 (5)	Rb1A—As—Rb2A^xv	123.340 (18)
Rb1Bⁱⁱ—Rb1B—O2^v	114.7 (4)	O1^xiii—As—Rb2B	66.15 (14)
O3^v—Rb1B—O2^v	51.41 (7)	O2—As—Rb2B	104.87 (14)
O3—Rb1B—O2^v	132.6 (4)	O4^v—As—Rb2B	137.04 (14)
O2^iv—Rb1B—O2^v	120.6 (6)	O3—As—Rb2B	42.56 (14)
O2ⁱ—Rb1B—O2^v	65.7 (2)	Rb1Bⁱⁱ—As—Rb2B	74.7 (2)
O3^iv—Rb1B—O2^v	112.19 (11)	Rb1B—As—Rb2B	74.33 (18)
O3ⁱ—Rb1B—O2^v	67.34 (7)	Rb2B^xxiv—As—Rb2B	74.78 (3)
O2—Rb1B—O2^v	172.4 (11)	Rb2B^xv—As—Rb2B	70.9 (2)
Rb1Bⁱ—Rb1B—O3ⁱⁱⁱ	45.4 (3)	Rb1A—As—Rb2B	72.61 (11)
Rb1Bⁱⁱ—Rb1B—O3ⁱⁱⁱ	61.5 (3)	Rb2A^xv—As—Rb2B	73.66 (14)
O3^v—Rb1B—O3ⁱⁱⁱ	66.84 (19)	O1^xiii—As—Rb2B^xxv	63.55 (13)
O3—Rb1B—O3ⁱⁱⁱ	158.9 (9)	O2—As—Rb2B^xxv	178.70 (16)
O2^iv—Rb1B—O3ⁱⁱⁱ	113.43 (5)	O4^v—As—Rb2B^xxv	65.54 (13)
O2ⁱ—Rb1B—O3ⁱⁱⁱ	126.87 (6)	O3—As—Rb2B^xxv	76.36 (14)
O3^iv—Rb1B—O3ⁱⁱⁱ	64.9 (3)	Rb1Bⁱⁱ—As—Rb2B^xxv	129.3 (5)
O3ⁱ—Rb1B—O3ⁱⁱⁱ	110.3 (6)	Rb1B—As—Rb2B^xxv	119.0 (4)
O2—Rb1B—O3ⁱⁱⁱ	112.4 (6)	Rb2B^xxiv—As—Rb2B^xxv	4.39 (15)
O2^v—Rb1B—O3ⁱⁱⁱ	61.9 (2)	Rb2B^xv—As—Rb2B^xxv	5.30 (19)
Rb1Bⁱ—Rb1B—O3ⁱⁱ	61.5 (3)	Rb1A—As—Rb2B^xxv	123.48 (12)
Rb1Bⁱⁱ—Rb1B—O3ⁱⁱ	45.4 (3)	Rb2A^xv—As—Rb2B^xxv	2.94 (15)
O3^v—Rb1B—O3ⁱⁱ	158.9 (9)	Rb2B—As—Rb2B^xxv	76.18 (18)
O3—Rb1B—O3ⁱⁱ	66.84 (19)	As^xxvi—O1—In2^xxvii	142.20 (12)
O2^iv—Rb1B—O3ⁱⁱ	126.87 (6)	As^xxvi—O1—Rb2B^xxviii	95.06 (18)
O2ⁱ—Rb1B—O3ⁱⁱ	113.43 (5)	In2^xxvii—O1—Rb2B^xxviii	119.53 (18)
O3^iv—Rb1B—O3ⁱⁱ	110.3 (6)	As^xxvi—O1—Rb2B^vi	92.19 (16)
O3ⁱ—Rb1B—O3ⁱⁱ	64.9 (3)	In2^xxvii—O1—Rb2B^vi	123.76 (15)
O2—Rb1B—O3ⁱⁱ	61.9 (2)	Rb2B^xxviii—O1—Rb2B^vi	6.6 (3)
O2^v—Rb1B—O3ⁱⁱ	112.4 (6)	As^xxvi—O1—Rb2A^vi	93.97 (12)
O3ⁱⁱⁱ—Rb1B—O3ⁱⁱ	94.2 (8)	In2^xxvii—O1—Rb2A^vi	121.16 (11)
Rb1Bⁱ—Rb1B—H	135.3 (8)	Rb2B^xxviii—O1—Rb2A^vi	2.47 (17)
Rb1Bⁱⁱ—Rb1B—H	112.7 (9)	Rb2B^vi—O1—Rb2A^vi	4.12 (14)
O3^v—Rb1B—H	117.3 (12)	As^xxvi—O1—Rb2B^xxvi	89.12 (16)
O3—Rb1B—H	16.1 (6)	In2^xxvii—O1—Rb2B^xxvi	106.82 (16)
O2^iv—Rb1B—H	65.2 (9)	Rb2B^xxviii—O1—Rb2B^xxvi	86.07 (7)
O2ⁱ—Rb1B—H	59.4 (9)	Rb2B^vi—O1—Rb2B^xxvi	80.1 (2)
O3^iv—Rb1B—H	111.3 (10)	Rb2A^vi—O1—Rb2B^xxvi	83.83 (15)
O3ⁱ—Rb1B—H	73.1 (8)	As^xxvi—O1—Rb2A^xxvi	87.55 (12)
O2—Rb1B—H	61.4 (8)	In2^xxvii—O1—Rb2A^xxvi	107.67 (9)
O2^v—Rb1B—H	124.3 (10)	Rb2B^xxviii—O1—Rb2A^xxvi	86.97 (17)
O3ⁱⁱⁱ—Rb1B—H	173.7 (9)	Rb2B^vi—O1—Rb2A^xxvi	80.92 (17)
O3ⁱⁱ—Rb1B—H	82.4 (6)	Rb2A^vi—O1—Rb2A^xxvi	84.71 (5)
Rb1Bⁱ—Rb1B—H^v	112.7 (9)	Rb2B^xxvi—O1—Rb2A^xxvi	1.7 (2)
Rb1Bⁱⁱ—Rb1B—H^v	135.3 (7)	As^xxvi—O1—Rb2A^xxvii	110.41 (11)
O3^v—Rb1B—H^v	16.1 (6)	In2^xxvii—O1—Rb2A^xxvii	74.80 (7)
O3—Rb1B—H^v	117.3 (12)	Rb2B^xxviii—O1—Rb2A^xxvii	65.58 (17)
O2^iv—Rb1B—H^v	59.4 (9)	Rb2B^vi—O1—Rb2A^xxvii	72.13 (14)
O2ⁱ—Rb1B—H^v	65.2 (9)	Rb2A^vi—O1—Rb2A^xxvii	68.03 (4)
O3^iv—Rb1B—H^v	73.1 (8)	Rb2B^xxvi—O1—Rb2A^xxvii	146.21 (11)
O3ⁱ—Rb1B—H^v	111.3 (9)	Rb2A^xxvi—O1—Rb2A^xxvii	147.76 (12)
O2—Rb1B—H^v	124.3 (11)	As—O2—In1^xxix	123.06 (9)
O2^v—Rb1B—H^v	61.4 (8)	As—O2—Rb1Bⁱⁱ	102.0 (4)
O3ⁱⁱⁱ—Rb1B—H^v	82.4 (6)	In1^xxix—O2—Rb1Bⁱⁱ	124.8 (3)
O3ⁱⁱ—Rb1B—H^v	173.7 (10)	As—O2—Rb1A	97.07 (7)
H—Rb1B—H^v	101.4 (15)	In1^xxix—O2—Rb1A	127.94 (7)
Rb2Bⁱⁱ—Rb2A—Rb2Bⁱ	116 (2)	Rb1Bⁱⁱ—O2—Rb1A	5.1 (4)
Rb2Bⁱⁱ—Rb2A—O3	134 (3)	As—O2—Rb1B	91.5 (4)
Rb2Bⁱ—Rb2A—O3	99 (3)	In1^xxix—O2—Rb1B	128.91 (9)
Rb2Bⁱⁱ—Rb2A—O3ⁱ	99 (3)	Rb1Bⁱⁱ—O2—Rb1B	12.4 (9)
Rb2Bⁱ—Rb2A—O3ⁱ	65 (3)	Rb1A—O2—Rb1B	7.5 (5)
O3—Rb2A—O3ⁱ	69.31 (13)	As—O2—Rb2A	56.91 (5)
Rb2Bⁱⁱ—Rb2A—O3ⁱⁱ	65 (3)	In1^xxix—O2—Rb2A	162.73 (8)
Rb2Bⁱ—Rb2A—O3ⁱⁱ	134 (3)	Rb1Bⁱⁱ—O2—Rb2A	68.43 (19)
O3—Rb2A—O3ⁱⁱ	69.31 (13)	Rb1A—O2—Rb2A	66.24 (6)
O3ⁱ—Rb2A—O3ⁱⁱ	69.31 (13)	Rb1B—O2—Rb2A	66.61 (7)
Rb2Bⁱⁱ—Rb2A—O1^vi	140 (3)	As—O3—Rb1B	107.13 (15)
Rb2Bⁱ—Rb2A—O1^vi	34 (2)	As—O3—Rb2B	113.58 (18)
O3—Rb2A—O1^vi	85.60 (6)	Rb1B—O3—Rb2B	107.8 (5)
O3ⁱ—Rb2A—O1^vi	89.21 (6)	As—O3—Rb2A	117.21 (9)
O3ⁱⁱ—Rb2A—O1^vi	151.25 (17)	Rb1B—O3—Rb2A	103.8 (4)
Rb2Bⁱⁱ—Rb2A—O1^vii	34 (2)	Rb2B—O3—Rb2A	4.46 (18)
Rb2Bⁱ—Rb2A—O1^vii	82 (2)	As—O3—Rb1Bⁱⁱ	98.0 (5)
O3—Rb2A—O1^vii	151.25 (17)	Rb1B—O3—Rb1Bⁱⁱ	14.3 (10)
O3ⁱ—Rb2A—O1^vii	85.60 (6)	Rb2B—O3—Rb1Bⁱⁱ	102.66 (17)
O3ⁱⁱ—Rb2A—O1^vii	89.21 (6)	Rb2A—O3—Rb1Bⁱⁱ	99.24 (11)
O1^vi—Rb2A—O1^vii	108.60 (10)	As—O3—Rb1A	105.44 (8)
Rb2Bⁱⁱ—Rb2A—O1^viii	82 (2)	Rb1B—O3—Rb1A	7.6 (6)
Rb2Bⁱ—Rb2A—O1^viii	140 (3)	Rb2B—O3—Rb1A	102.30 (16)
O3—Rb2A—O1^viii	89.21 (6)	Rb2A—O3—Rb1A	98.50 (9)
O3ⁱ—Rb2A—O1^viii	151.25 (17)	Rb1Bⁱⁱ—O3—Rb1A	8.2 (6)
O3ⁱⁱ—Rb2A—O1^viii	85.60 (6)	As—O3—Rb2Bⁱ	121.23 (19)
O1^vi—Rb2A—O1^viii	108.60 (10)	Rb1B—O3—Rb2Bⁱ	103.8 (4)
O1^vii—Rb2A—O1^viii	108.59 (10)	Rb2B—O3—Rb2Bⁱ	7.6 (3)
Rb2Bⁱⁱ—Rb2A—O4^ix	98 (3)	Rb2A—O3—Rb2Bⁱ	4.62 (15)
Rb2Bⁱ—Rb2A—O4^ix	53 (3)	Rb1Bⁱⁱ—O3—Rb2Bⁱ	100.4 (2)
O3—Rb2A—O4^ix	126.63 (6)	Rb1A—O3—Rb2Bⁱ	99.01 (18)
O3ⁱ—Rb2A—O4^ix	117.83 (6)	As—O3—Rb2Bⁱⁱ	115.94 (17)
O3ⁱⁱ—Rb2A—O4^ix	163.52 (11)	Rb1B—O3—Rb2Bⁱⁱ	101.7 (5)
O1^vi—Rb2A—O4^ix	44.75 (6)	Rb2B—O3—Rb2Bⁱⁱ	6.1 (2)
O1^vii—Rb2A—O4^ix	77.05 (10)	Rb2A—O3—Rb2Bⁱⁱ	3.2 (2)
O1^viii—Rb2A—O4^ix	90.14 (12)	Rb1Bⁱⁱ—O3—Rb2Bⁱⁱ	96.67 (18)
Rb2Bⁱⁱ—Rb2A—O4^x	86 (3)	Rb1A—O3—Rb2Bⁱⁱ	96.23 (18)
Rb2Bⁱ—Rb2A—O4^x	98 (3)	Rb2Bⁱ—O3—Rb2Bⁱⁱ	7.4 (2)
O3—Rb2A—O4^x	117.83 (6)	As—O3—Rb1Bⁱ	110.6 (3)
O3ⁱ—Rb2A—O4^x	163.52 (11)	Rb1B—O3—Rb1Bⁱ	10.9 (8)
O3ⁱⁱ—Rb2A—O4^x	126.63 (6)	Rb2B—O3—Rb1Bⁱ	97.1 (4)
O1^vi—Rb2A—O4^x	77.05 (10)	Rb2A—O3—Rb1Bⁱ	93.2 (4)
O1^vii—Rb2A—O4^x	90.14 (12)	Rb1Bⁱⁱ—O3—Rb1Bⁱ	12.6 (9)
O1^viii—Rb2A—O4^x	44.75 (6)	Rb1A—O3—Rb1Bⁱ	6.0 (4)
O4^ix—Rb2A—O4^x	45.71 (8)	Rb2Bⁱ—O3—Rb1Bⁱ	93.5 (4)
Rb2Bⁱⁱ—Rb2A—O4^xi	53 (3)	Rb2Bⁱⁱ—O3—Rb1Bⁱ	91.0 (4)
Rb2Bⁱ—Rb2A—O4^xi	86 (3)	As—O3—Rb2A^xv	78.72 (7)
O3—Rb2A—O4^xi	163.52 (11)	Rb1B—O3—Rb2A^xv	159.5 (6)
O3ⁱ—Rb2A—O4^xi	126.63 (6)	Rb2B—O3—Rb2A^xv	86.8 (2)
O3ⁱⁱ—Rb2A—O4^xi	117.83 (6)	Rb2A—O3—Rb2A^xv	90.14 (5)
O1^vi—Rb2A—O4^xi	90.14 (12)	Rb1Bⁱⁱ—O3—Rb2A^xv	170.52 (10)
O1^vii—Rb2A—O4^xi	44.75 (6)	Rb1A—O3—Rb2A^xv	167.05 (8)
O1^viii—Rb2A—O4^xi	77.05 (10)	Rb2Bⁱ—O3—Rb2A^xv	88.8 (2)
O4^ix—Rb2A—O4^xi	45.71 (8)	Rb2Bⁱⁱ—O3—Rb2A^xv	92.8 (2)
O4^x—Rb2A—O4^xi	45.71 (8)	Rb1Bⁱ—O3—Rb2A^xv	167.03 (11)
Rb2Bⁱⁱ—Rb2A—O1^xii	26 (3)	As—O3—H	108 (3)
Rb2Bⁱ—Rb2A—O1^xii	117 (2)	Rb1B—O3—H	92 (3)
O3—Rb2A—O1^xii	112.37 (15)	Rb2B—O3—H	125 (3)
O3ⁱ—Rb2A—O1^xii	76.69 (8)	Rb2A—O3—H	124 (3)
O3ⁱⁱ—Rb2A—O1^xii	44.11 (5)	Rb1Bⁱⁱ—O3—H	105 (3)
O1^vi—Rb2A—O1^xii	150.55 (6)	Rb1A—O3—H	99 (3)
O1^vii—Rb2A—O1^xii	45.46 (6)	Rb2Bⁱ—O3—H	120 (3)
O1^viii—Rb2A—O1^xii	95.29 (5)	Rb2Bⁱⁱ—O3—H	127 (3)
O4^ix—Rb2A—O1^xii	120.81 (10)	Rb1Bⁱ—O3—H	100 (3)
O4^x—Rb2A—O1^xii	111.19 (9)	Rb2A^xv—O3—H	68 (3)
O4^xi—Rb2A—O1^xii	78.40 (6)	As^v—O4—In1^xxvii	127.87 (9)
Rb2Bⁱⁱ—Rb2A—O1^xiii	117 (2)	As^v—O4—Rb2B^xxx	85.47 (16)
Rb2Bⁱ—Rb2A—O1^xiii	126 (2)	In1^xxvii—O4—Rb2B^xxx	106.35 (17)
O3—Rb2A—O1^xiii	44.11 (5)	As^v—O4—Rb2A^xxx	86.47 (7)
O3ⁱ—Rb2A—O1^xiii	112.37 (15)	In1^xxvii—O4—Rb2A^xxx	103.30 (7)
O3ⁱⁱ—Rb2A—O1^xiii	76.69 (8)	Rb2B^xxx—O4—Rb2A^xxx	3.25 (18)
O1^vi—Rb2A—O1^xiii	95.29 (5)	As^v—O4—Rb1A^xxvi	131.05 (7)
O1^vii—Rb2A—O1^xiii	150.54 (6)	In1^xxvii—O4—Rb1A^xxvi	90.25 (5)
O1^viii—Rb2A—O1^xiii	45.46 (6)	Rb2B^xxx—O4—Rb1A^xxvi	115.02 (15)
O4^ix—Rb2A—O1^xiii	111.19 (9)	Rb2A^xxx—O4—Rb1A^xxvi	116.54 (4)
O4^x—Rb2A—O1^xiii	78.40 (6)	As^v—O4—Rb1A	48.38 (5)
O4^xi—Rb2A—O1^xiii	120.81 (10)	In1^xxvii—O4—Rb1A	80.54 (5)
O1^xii—Rb2A—O1^xiii	113.93 (7)	Rb2B^xxx—O4—Rb1A	109.65 (15)
Rb2Bⁱⁱ—Rb2A—O1^xiv	126 (2)	Rb2A^xxx—O4—Rb1A	108.26 (4)
Rb2Bⁱ—Rb2A—O1^xiv	26 (3)	Rb1A^xxvi—O4—Rb1A	135.18 (4)

Symmetry codes: (i) −y, x−y, z; (ii) −x+y, −x, z; (iii) x−y, −y, −z+3/2; (iv) y, x, −z+3/2; (v) −x, −x+y, −z+3/2; (vi) −x+2/3, −y−2/3, −z+4/3; (vii) y+2/3, −x+y+4/3, −z+4/3; (viii) x−y−4/3, x−2/3, −z+4/3; (ix) x−1/3, x−y−2/3, z−1/6; (x) −y−1/3, −x+1/3, z−1/6; (xi) −x+y+2/3, y+1/3, z−1/6; (xii) −x+y+1, −x+1, z; (xiii) x−1, y, z; (xiv) −y, x−y−1, z; (xv) −x−1/3, −y−2/3, −z+4/3; (xvi) x−y−1/3, x+1/3, −z+4/3; (xvii) −y, x−y+1, z; (xviii) x+1, y+1, z; (xix) x, y+1, z; (xx) −x+2/3, −y+1/3, −z+4/3; (xxi) −y+1/3, −x+2/3, z+1/6; (xxii) −x−1/3, −y+1/3, −z+4/3; (xxiii) −x+2/3, −y+4/3, −z+4/3; (xxiv) y−1/3, −x+y−2/3, −z+4/3; (xxv) x−y−1/3, x−2/3, −z+4/3; (xxvi) x+1, y, z; (xxvii) x, y−1, z; (xxviii) y+2/3, −x+y−2/3, −z+4/3; (xxix) x−1, y−1, z; (xxx) −y+1/3, −x−1/3, z+1/6.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O3—H···O4^xxxi	0.83 (3)	1.82 (3)	2.634 (2)	168 (4)

Symmetry code: (xxxi) y, x−1, −z+3/2.

Caesium indium bis[hydrogen arsenate(V)] (CsInHAsO42) top

Crystal data top

CsIn(HAsO₄)₂	D_x = 4.291 Mg m⁻³
M_r = 527.59	Mo Kα radiation, λ = 0.71073 Å
Trigonal, R3c:H	Cell parameters from 2985 reflections
a = 8.629 (1) Å	θ = 3.1–30.0°
c = 56.986 (11) Å	µ = 15.34 mm⁻¹
V = 3674.7 (11) Å³	T = 293 K
Z = 18	Small pseudooctahedra, colourless
F(000) = 4248	0.06 × 0.06 × 0.04 mm

Data collection top

Nonius KappaCCD single-crystal four-circle diffractometer	1039 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	R_int = 0.019
φ and ω scans	θ_max = 30.0°, θ_min = 3.1°
Absorption correction: multi-scan (SCALEPACK; Otwinowski et al., 2003)	h = −12→12
T_min = 0.460, T_max = 0.579	k = −9→9
4350 measured reflections	l = −79→79
1199 independent reflections

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: difference Fourier map
R[F² > 2σ(F²)] = 0.022	All H-atom parameters refined
wR(F²) = 0.052	w = 1/[σ²(F_o²) + (0.0234P)² + 28.1228P] where P = (F_o² + 2F_c²)/3
S = 1.07	(Δ/σ)_max = 0.004
1199 reflections	Δρ_max = 2.09 e Å⁻³
61 parameters	Δρ_min = −0.86 e Å⁻³
1 restraint	Extinction correction: SHELXL2016 (Sheldrick, 2015), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.000028 (7)

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Cs1	0.000000	0.000000	0.750000	0.02557 (14)
Cs2	0.000000	0.000000	0.66740 (2)	0.02940 (12)
In1	0.333333	0.666667	0.75230 (2)	0.00967 (10)
In2	0.333333	0.666667	0.666667	0.01033 (12)
As	−0.41576 (4)	−0.38822 (4)	0.71249 (2)	0.01182 (10)
O1	0.4878 (4)	−0.4176 (4)	0.68649 (4)	0.0247 (6)
O2	−0.4350 (3)	−0.2496 (3)	0.73117 (4)	0.0154 (5)
O3	−0.1870 (3)	−0.2856 (3)	0.70680 (5)	0.0217 (5)
O4	0.4768 (3)	−0.1133 (3)	0.77606 (4)	0.0147 (5)
H	−0.152 (5)	−0.354 (4)	0.7115 (6)	0.013 (10)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Cs1	0.0283 (2)	0.0283 (2)	0.0201 (3)	0.01415 (10)	0.000	0.000
Cs2	0.03461 (17)	0.03461 (17)	0.0190 (2)	0.01730 (8)	0.000	0.000
In1	0.01027 (13)	0.01027 (13)	0.00848 (17)	0.00513 (6)	0.000	0.000
In2	0.01173 (16)	0.01173 (16)	0.0075 (2)	0.00587 (8)	0.000	0.000
As	0.01466 (17)	0.01309 (17)	0.01022 (15)	0.00882 (14)	0.00082 (12)	0.00125 (11)
O1	0.0366 (15)	0.0361 (15)	0.0126 (11)	0.0265 (13)	−0.0067 (11)	−0.0014 (10)
O2	0.0155 (11)	0.0154 (11)	0.0157 (11)	0.0079 (9)	0.0056 (9)	−0.0020 (9)
O3	0.0174 (12)	0.0216 (13)	0.0290 (13)	0.0120 (11)	0.0083 (10)	0.0115 (11)
O4	0.0154 (11)	0.0126 (11)	0.0183 (11)	0.0086 (9)	−0.0032 (9)	−0.0057 (9)

Geometric parameters (Å, º) top

Cs1—O3	3.280 (3)	Cs2—O4^xii	3.703 (2)
Cs1—O3ⁱ	3.280 (3)	Cs2—O4^xiii	3.703 (2)
Cs1—O3ⁱⁱ	3.280 (3)	Cs2—O4^xiv	3.703 (2)
Cs1—O3ⁱⁱⁱ	3.280 (3)	Cs2—As^xi	3.8762 (6)
Cs1—O3^iv	3.280 (3)	Cs2—As^ix	3.8762 (6)
Cs1—O3^v	3.280 (3)	Cs2—As^x	3.8762 (6)
Cs1—O2	3.434 (2)	In1—O2^xv	2.127 (2)
Cs1—O2ⁱⁱ	3.434 (2)	In1—O2ⁱⁱⁱ	2.127 (2)
Cs1—O2^v	3.434 (2)	In1—O2^xvi	2.127 (2)
Cs1—O2ⁱⁱⁱ	3.434 (2)	In1—O4^xvii	2.150 (2)
Cs1—O2ⁱ	3.434 (2)	In1—O4^iv	2.150 (2)
Cs1—O2^iv	3.434 (2)	In1—O4^xviii	2.150 (2)
Cs1—H	3.44 (4)	In2—O1^vii	2.133 (2)
Cs1—H^iv	3.44 (4)	In2—O1^xi	2.133 (3)
Cs1—Hⁱⁱⁱ	3.44 (4)	In2—O1^xix	2.133 (2)
Cs2—O3^iv	3.121 (3)	In2—O1^iv	2.133 (2)
Cs2—O3ⁱⁱⁱ	3.121 (2)	In2—O1^xviii	2.133 (3)
Cs2—O3	3.121 (3)	In2—O1^xvii	2.133 (2)
Cs2—O1^vi	3.419 (3)	As—O1^xx	1.655 (2)
Cs2—O1^vii	3.419 (3)	As—O2	1.671 (2)
Cs2—O1^viii	3.419 (3)	As—O4ⁱⁱ	1.679 (2)
Cs2—O3^ix	3.698 (3)	As—O3	1.743 (3)
Cs2—O3^x	3.698 (3)	O3—H	0.83 (3)
Cs2—O3^xi	3.698 (3)

O3—Cs1—O3ⁱ	166.65 (9)	O1^vi—Cs2—As^xi	102.94 (4)
O3—Cs1—O3ⁱⁱ	119.30 (9)	O1^vii—Cs2—As^xi	88.69 (5)
O3ⁱ—Cs1—O3ⁱⁱ	69.82 (7)	O1^viii—Cs2—As^xi	25.24 (4)
O3—Cs1—O3ⁱⁱⁱ	69.82 (7)	O3^ix—Cs2—As^xi	61.32 (4)
O3ⁱ—Cs1—O3ⁱⁱⁱ	103.15 (9)	O3^x—Cs2—As^xi	94.72 (4)
O3ⁱⁱ—Cs1—O3ⁱⁱⁱ	166.65 (10)	O3^xi—Cs2—As^xi	26.48 (4)
O3—Cs1—O3^iv	69.82 (7)	O4^xii—Cs2—As^xi	70.49 (4)
O3ⁱ—Cs1—O3^iv	119.30 (10)	O4^xiii—Cs2—As^xi	25.47 (3)
O3ⁱⁱ—Cs1—O3^iv	103.15 (9)	O4^xiv—Cs2—As^xi	53.44 (4)
O3ⁱⁱⁱ—Cs1—O3^iv	69.82 (7)	O3^iv—Cs2—As^ix	107.26 (5)
O3—Cs1—O3^v	103.15 (9)	O3ⁱⁱⁱ—Cs2—As^ix	174.10 (5)
O3ⁱ—Cs1—O3^v	69.82 (7)	O3—Cs2—As^ix	100.69 (5)
O3ⁱⁱ—Cs1—O3^v	69.82 (7)	O1^vi—Cs2—As^ix	25.24 (4)
O3ⁱⁱⁱ—Cs1—O3^v	119.30 (9)	O1^vii—Cs2—As^ix	102.94 (4)
O3^iv—Cs1—O3^v	166.65 (9)	O1^viii—Cs2—As^ix	88.69 (5)
O3—Cs1—O2	47.28 (6)	O3^ix—Cs2—As^ix	26.48 (4)
O3ⁱ—Cs1—O2	119.81 (6)	O3^x—Cs2—As^ix	61.32 (4)
O3ⁱⁱ—Cs1—O2	126.64 (6)	O3^xi—Cs2—As^ix	94.72 (4)
O3ⁱⁱⁱ—Cs1—O2	66.62 (6)	O4^xii—Cs2—As^ix	25.47 (3)
O3^iv—Cs1—O2	111.83 (6)	O4^xiii—Cs2—As^ix	53.44 (4)
O3^v—Cs1—O2	67.00 (6)	O4^xiv—Cs2—As^ix	70.49 (4)
O3—Cs1—O2ⁱⁱ	126.65 (6)	As^xi—Cs2—As^ix	78.314 (13)
O3ⁱ—Cs1—O2ⁱⁱ	66.61 (6)	O3^iv—Cs2—As^x	100.69 (5)
O3ⁱⁱ—Cs1—O2ⁱⁱ	47.28 (6)	O3ⁱⁱⁱ—Cs2—As^x	107.26 (5)
O3ⁱⁱⁱ—Cs1—O2ⁱⁱ	119.81 (6)	O3—Cs2—As^x	174.10 (5)
O3^iv—Cs1—O2ⁱⁱ	67.01 (6)	O1^vi—Cs2—As^x	88.69 (5)
O3^v—Cs1—O2ⁱⁱ	111.83 (6)	O1^vii—Cs2—As^x	25.24 (4)
O2—Cs1—O2ⁱⁱ	170.75 (8)	O1^viii—Cs2—As^x	102.94 (4)
O3—Cs1—O2^v	67.01 (6)	O3^ix—Cs2—As^x	94.72 (4)
O3ⁱ—Cs1—O2^v	111.83 (6)	O3^x—Cs2—As^x	26.48 (4)
O3ⁱⁱ—Cs1—O2^v	66.61 (6)	O3^xi—Cs2—As^x	61.32 (4)
O3ⁱⁱⁱ—Cs1—O2^v	126.65 (6)	O4^xii—Cs2—As^x	53.44 (4)
O3^iv—Cs1—O2^v	119.81 (6)	O4^xiii—Cs2—As^x	70.49 (4)
O3^v—Cs1—O2^v	47.28 (6)	O4^xiv—Cs2—As^x	25.47 (4)
O2—Cs1—O2^v	61.36 (8)	As^xi—Cs2—As^x	78.314 (13)
O2ⁱⁱ—Cs1—O2^v	110.71 (3)	As^ix—Cs2—As^x	78.314 (13)
O3—Cs1—O2ⁱⁱⁱ	111.83 (6)	O2^xv—In1—O2ⁱⁱⁱ	91.11 (9)
O3ⁱ—Cs1—O2ⁱⁱⁱ	67.01 (6)	O2^xv—In1—O2^xvi	91.11 (9)
O3ⁱⁱ—Cs1—O2ⁱⁱⁱ	119.81 (6)	O2ⁱⁱⁱ—In1—O2^xvi	91.11 (9)
O3ⁱⁱⁱ—Cs1—O2ⁱⁱⁱ	47.28 (6)	O2^xv—In1—O4^xvii	92.57 (9)
O3^iv—Cs1—O2ⁱⁱⁱ	66.61 (6)	O2ⁱⁱⁱ—In1—O4^xvii	175.38 (9)
O3^v—Cs1—O2ⁱⁱⁱ	126.65 (6)	O2^xvi—In1—O4^xvii	91.61 (9)
O2—Cs1—O2ⁱⁱⁱ	110.71 (3)	O2^xv—In1—O4^iv	91.61 (8)
O2ⁱⁱ—Cs1—O2ⁱⁱⁱ	77.59 (7)	O2ⁱⁱⁱ—In1—O4^iv	92.57 (9)
O2^v—Cs1—O2ⁱⁱⁱ	170.75 (8)	O2^xvi—In1—O4^iv	175.38 (9)
O3—Cs1—O2ⁱ	119.82 (6)	O4^xvii—In1—O4^iv	84.54 (9)
O3ⁱ—Cs1—O2ⁱ	47.28 (6)	O2^xv—In1—O4^xviii	175.38 (9)
O3ⁱⁱ—Cs1—O2ⁱ	111.83 (6)	O2ⁱⁱⁱ—In1—O4^xviii	91.61 (9)
O3ⁱⁱⁱ—Cs1—O2ⁱ	67.01 (6)	O2^xvi—In1—O4^xviii	92.57 (9)
O3^iv—Cs1—O2ⁱ	126.65 (6)	O4^xvii—In1—O4^xviii	84.54 (9)
O3^v—Cs1—O2ⁱ	66.61 (6)	O4^iv—In1—O4^xviii	84.54 (9)
O2—Cs1—O2ⁱ	77.59 (7)	O2^xv—In1—Cs2^xxi	124.48 (6)
O2ⁱⁱ—Cs1—O2ⁱ	110.71 (3)	O2ⁱⁱⁱ—In1—Cs2^xxi	124.48 (6)
O2^v—Cs1—O2ⁱ	110.71 (3)	O2^xvi—In1—Cs2^xxi	124.48 (6)
O2ⁱⁱⁱ—Cs1—O2ⁱ	61.36 (8)	O4^xvii—In1—Cs2^xxi	50.96 (6)
O3—Cs1—O2^iv	66.61 (6)	O4^iv—In1—Cs2^xxi	50.96 (6)
O3ⁱ—Cs1—O2^iv	126.65 (6)	O4^xviii—In1—Cs2^xxi	50.96 (6)
O3ⁱⁱ—Cs1—O2^iv	67.01 (6)	O1^vii—In2—O1^xi	94.56 (9)
O3ⁱⁱⁱ—Cs1—O2^iv	111.83 (6)	O1^vii—In2—O1^xix	94.55 (9)
O3^iv—Cs1—O2^iv	47.28 (6)	O1^xi—In2—O1^xix	94.55 (9)
O3^v—Cs1—O2^iv	119.81 (6)	O1^vii—In2—O1^iv	180.0
O2—Cs1—O2^iv	110.71 (3)	O1^xi—In2—O1^iv	85.45 (9)
O2ⁱⁱ—Cs1—O2^iv	61.36 (8)	O1^xix—In2—O1^iv	85.45 (9)
O2^v—Cs1—O2^iv	77.59 (7)	O1^vii—In2—O1^xviii	85.45 (9)
O2ⁱⁱⁱ—Cs1—O2^iv	110.71 (3)	O1^xi—In2—O1^xviii	180.0
O2ⁱ—Cs1—O2^iv	170.75 (8)	O1^xix—In2—O1^xviii	85.45 (9)
O3—Cs1—H	13.9 (5)	O1^iv—In2—O1^xviii	94.55 (9)
O3ⁱ—Cs1—H	170.1 (7)	O1^vii—In2—O1^xvii	85.45 (9)
O3ⁱⁱ—Cs1—H	105.5 (5)	O1^xi—In2—O1^xvii	85.45 (9)
O3ⁱⁱⁱ—Cs1—H	83.1 (5)	O1^xix—In2—O1^xvii	180.0
O3^iv—Cs1—H	69.8 (6)	O1^iv—In2—O1^xvii	94.55 (9)
O3^v—Cs1—H	100.5 (7)	O1^xviii—In2—O1^xvii	94.55 (9)
O2—Cs1—H	55.4 (6)	O1^vii—In2—Cs2^xix	56.94 (8)
O2ⁱⁱ—Cs1—H	117.1 (6)	O1^xi—In2—Cs2^xix	72.56 (8)
O2^v—Cs1—H	58.5 (6)	O1^xix—In2—Cs2^xix	146.29 (7)
O2ⁱⁱⁱ—Cs1—H	122.2 (6)	O1^iv—In2—Cs2^xix	123.06 (8)
O2ⁱ—Cs1—H	131.7 (6)	O1^xviii—In2—Cs2^xix	107.44 (8)
O2^iv—Cs1—H	55.8 (6)	O1^xvii—In2—Cs2^xix	33.71 (7)
O3—Cs1—H^iv	83.1 (5)	O1^vii—In2—Cs2^xvii	123.06 (8)
O3ⁱ—Cs1—H^iv	105.5 (6)	O1^xi—In2—Cs2^xvii	107.44 (8)
O3ⁱⁱ—Cs1—H^iv	100.5 (6)	O1^xix—In2—Cs2^xvii	33.71 (7)
O3ⁱⁱⁱ—Cs1—H^iv	69.8 (6)	O1^iv—In2—Cs2^xvii	56.94 (8)
O3^iv—Cs1—H^iv	13.9 (5)	O1^xviii—In2—Cs2^xvii	72.56 (8)
O3^v—Cs1—H^iv	170.2 (6)	O1^xvii—In2—Cs2^xvii	146.29 (7)
O2—Cs1—H^iv	122.2 (6)	Cs2^xix—In2—Cs2^xvii	180.0
O2ⁱⁱ—Cs1—H^iv	58.5 (6)	O1^vii—In2—Cs2	33.71 (7)
O2^v—Cs1—H^iv	131.7 (6)	O1^xi—In2—Cs2	123.06 (8)
O2ⁱⁱⁱ—Cs1—H^iv	55.8 (6)	O1^xix—In2—Cs2	107.44 (8)
O2ⁱ—Cs1—H^iv	117.1 (6)	O1^iv—In2—Cs2	146.29 (7)
O2^iv—Cs1—H^iv	55.4 (6)	O1^xviii—In2—Cs2	56.94 (8)
H—Cs1—H^iv	83.7 (8)	O1^xvii—In2—Cs2	72.56 (8)
O3—Cs1—Hⁱⁱⁱ	69.8 (6)	Cs2^xix—In2—Cs2	60.0
O3ⁱ—Cs1—Hⁱⁱⁱ	100.5 (6)	Cs2^xvii—In2—Cs2	120.0
O3ⁱⁱ—Cs1—Hⁱⁱⁱ	170.2 (6)	O1^vii—In2—Cs2^xvi	107.44 (8)
O3ⁱⁱⁱ—Cs1—Hⁱⁱⁱ	13.9 (5)	O1^xi—In2—Cs2^xvi	33.71 (7)
O3^iv—Cs1—Hⁱⁱⁱ	83.1 (5)	O1^xix—In2—Cs2^xvi	123.06 (8)
O3^v—Cs1—Hⁱⁱⁱ	105.5 (5)	O1^iv—In2—Cs2^xvi	72.56 (8)
O2—Cs1—Hⁱⁱⁱ	55.8 (6)	O1^xviii—In2—Cs2^xvi	146.29 (7)
O2ⁱⁱ—Cs1—Hⁱⁱⁱ	131.7 (6)	O1^xvii—In2—Cs2^xvi	56.94 (8)
O2^v—Cs1—Hⁱⁱⁱ	117.1 (7)	Cs2^xix—In2—Cs2^xvi	60.0
O2ⁱⁱⁱ—Cs1—Hⁱⁱⁱ	55.4 (6)	Cs2^xvii—In2—Cs2^xvi	120.0
O2ⁱ—Cs1—Hⁱⁱⁱ	58.5 (6)	Cs2—In2—Cs2^xvi	120.0
O2^iv—Cs1—Hⁱⁱⁱ	122.2 (6)	O1^vii—In2—Cs2^xxii	72.56 (8)
H—Cs1—Hⁱⁱⁱ	83.7 (8)	O1^xi—In2—Cs2^xxii	146.29 (7)
H^iv—Cs1—Hⁱⁱⁱ	83.7 (8)	O1^xix—In2—Cs2^xxii	56.94 (8)
O3^iv—Cs2—O3ⁱⁱⁱ	73.97 (8)	O1^iv—In2—Cs2^xxii	107.44 (8)
O3^iv—Cs2—O3	73.97 (8)	O1^xviii—In2—Cs2^xxii	33.71 (7)
O3ⁱⁱⁱ—Cs2—O3	73.97 (8)	O1^xvii—In2—Cs2^xxii	123.06 (8)
O3^iv—Cs2—O1^vi	82.81 (6)	Cs2^xix—In2—Cs2^xxii	120.0
O3ⁱⁱⁱ—Cs2—O1^vi	153.75 (6)	Cs2^xvii—In2—Cs2^xxii	60.0
O3—Cs2—O1^vi	88.16 (7)	Cs2—In2—Cs2^xxii	60.0
O3^iv—Cs2—O1^vii	88.16 (7)	Cs2^xvi—In2—Cs2^xxii	180.0
O3ⁱⁱⁱ—Cs2—O1^vii	82.80 (7)	O1^vii—In2—Cs2^xxiii	146.29 (7)
O3—Cs2—O1^vii	153.75 (7)	O1^xi—In2—Cs2^xxiii	56.94 (8)
O1^vi—Cs2—O1^vii	108.90 (4)	O1^xix—In2—Cs2^xxiii	72.56 (8)
O3^iv—Cs2—O1^viii	153.75 (7)	O1^iv—In2—Cs2^xxiii	33.71 (7)
O3ⁱⁱⁱ—Cs2—O1^viii	88.16 (7)	O1^xviii—In2—Cs2^xxiii	123.06 (8)
O3—Cs2—O1^viii	82.81 (6)	O1^xvii—In2—Cs2^xxiii	107.44 (8)
O1^vi—Cs2—O1^viii	108.90 (4)	Cs2^xix—In2—Cs2^xxiii	120.0
O1^vii—Cs2—O1^viii	108.90 (4)	Cs2^xvii—In2—Cs2^xxiii	60.0
O3^iv—Cs2—O3^ix	124.57 (9)	Cs2—In2—Cs2^xxiii	180.0
O3ⁱⁱⁱ—Cs2—O3^ix	148.48 (9)	Cs2^xvi—In2—Cs2^xxiii	60.0
O3—Cs2—O3^ix	86.50 (7)	Cs2^xxii—In2—Cs2^xxiii	120.0
O1^vi—Cs2—O3^ix	44.45 (6)	O1^xx—As—O2	117.25 (12)
O1^vii—Cs2—O3^ix	119.69 (6)	O1^xx—As—O4ⁱⁱ	108.41 (12)
O1^viii—Cs2—O3^ix	64.61 (6)	O2—As—O4ⁱⁱ	113.77 (11)
O3^iv—Cs2—O3^x	86.50 (7)	O1^xx—As—O3	105.44 (13)
O3ⁱⁱⁱ—Cs2—O3^x	124.56 (9)	O2—As—O3	104.33 (12)
O3—Cs2—O3^x	148.48 (8)	O4ⁱⁱ—As—O3	106.72 (11)
O1^vi—Cs2—O3^x	64.61 (6)	O1^xx—As—Cs2^ix	61.74 (9)
O1^vii—Cs2—O3^x	44.45 (6)	O2—As—Cs2^ix	174.14 (8)
O1^viii—Cs2—O3^x	119.69 (6)	O4ⁱⁱ—As—Cs2^ix	71.50 (8)
O3^ix—Cs2—O3^x	84.57 (6)	O3—As—Cs2^ix	71.06 (9)
O3^iv—Cs2—O3^xi	148.48 (9)	O1^xx—As—Cs1	139.73 (11)
O3ⁱⁱⁱ—Cs2—O3^xi	86.50 (7)	O2—As—Cs1	55.91 (8)
O3—Cs2—O3^xi	124.57 (9)	O4ⁱⁱ—As—Cs1	109.82 (8)
O1^vi—Cs2—O3^xi	119.69 (6)	O3—As—Cs1	51.15 (9)
O1^vii—Cs2—O3^xi	64.61 (6)	Cs2^ix—As—Cs1	120.598 (10)
O1^viii—Cs2—O3^xi	44.45 (6)	O1^xx—As—Cs2	75.26 (11)
O3^ix—Cs2—O3^xi	84.57 (6)	O2—As—Cs2	99.50 (8)
O3^x—Cs2—O3^xi	84.57 (6)	O4ⁱⁱ—As—Cs2	138.02 (8)
O3^iv—Cs2—O4^xii	113.69 (6)	O3—As—Cs2	37.36 (8)
O3ⁱⁱⁱ—Cs2—O4^xii	159.43 (6)	Cs2^ix—As—Cs2	74.638 (9)
O3—Cs2—O4^xii	126.02 (6)	Cs1—As—Cs2	68.078 (14)
O1^vi—Cs2—O4^xii	44.41 (5)	As^xxiv—O1—In2^xxv	140.67 (15)
O1^vii—Cs2—O4^xii	78.54 (5)	As^xxiv—O1—Cs2^vi	93.02 (10)
O1^viii—Cs2—O4^xii	89.74 (5)	In2^xxv—O1—Cs2^vi	126.03 (9)
O3^ix—Cs2—O4^xii	43.56 (5)	As^xxiv—O1—Cs2^xxiv	82.42 (10)
O3^x—Cs2—O4^xii	41.47 (5)	In2^xxv—O1—Cs2^xxiv	97.96 (9)
O3^xi—Cs2—O4^xii	77.76 (5)	Cs2^vi—O1—Cs2^xxiv	80.74 (5)
O3^iv—Cs2—O4^xiii	159.43 (6)	As^xxiv—O1—Cs2^xxv	118.31 (12)
O3ⁱⁱⁱ—Cs2—O4^xiii	126.02 (6)	In2^xxv—O1—Cs2^xxv	82.33 (8)
O3—Cs2—O4^xiii	113.70 (7)	Cs2^vi—O1—Cs2^xxv	72.50 (5)
O1^vi—Cs2—O4^xiii	78.54 (5)	Cs2^xxiv—O1—Cs2^xxv	146.39 (6)
O1^vii—Cs2—O4^xiii	89.74 (6)	As—O2—In1^xxvi	122.05 (12)
O1^viii—Cs2—O4^xiii	44.41 (5)	As—O2—Cs1	100.33 (9)
O3^ix—Cs2—O4^xiii	41.47 (5)	In1^xxvi—O2—Cs1	125.68 (9)
O3^x—Cs2—O4^xiii	77.76 (5)	As—O2—Cs2	60.78 (7)
O3^xi—Cs2—O4^xiii	43.56 (5)	In1^xxvi—O2—Cs2	162.87 (9)
O4^xii—Cs2—O4^xiii	45.97 (6)	Cs1—O2—Cs2	66.29 (4)
O3^iv—Cs2—O4^xiv	126.02 (6)	As—O3—Cs2	122.83 (12)
O3ⁱⁱⁱ—Cs2—O4^xiv	113.69 (6)	As—O3—Cs1	104.40 (11)
O3—Cs2—O4^xiv	159.43 (6)	Cs2—O3—Cs1	94.64 (7)
O1^vi—Cs2—O4^xiv	89.74 (5)	As—O3—Cs2^ix	82.46 (10)
O1^vii—Cs2—O4^xiv	44.41 (5)	Cs2—O3—Cs2^ix	93.50 (7)
O1^viii—Cs2—O4^xiv	78.53 (5)	Cs1—O3—Cs2^ix	164.05 (8)
O3^ix—Cs2—O4^xiv	77.76 (5)	As—O3—H	107 (3)
O3^x—Cs2—O4^xiv	43.56 (5)	Cs2—O3—H	124 (3)
O3^xi—Cs2—O4^xiv	41.47 (5)	Cs1—O3—H	94 (3)
O4^xii—Cs2—O4^xiv	45.97 (6)	Cs2^ix—O3—H	70 (3)
O4^xiii—Cs2—O4^xiv	45.97 (6)	Asⁱⁱ—O4—In1^xxv	129.32 (12)
O3^iv—Cs2—As^xi	174.10 (5)	Asⁱⁱ—O4—Cs2^xxvii	83.03 (8)
O3ⁱⁱⁱ—Cs2—As^xi	100.69 (5)	In1^xxv—O4—Cs2^xxvii	102.24 (8)
O3—Cs2—As^xi	107.26 (5)

Symmetry codes: (i) x−y, −y, −z+3/2; (ii) −x, −x+y, −z+3/2; (iii) −x+y, −x, z; (iv) −y, x−y, z; (v) y, x, −z+3/2; (vi) −x+2/3, −y−2/3, −z+4/3; (vii) y+2/3, −x+y+4/3, −z+4/3; (viii) x−y−4/3, x−2/3, −z+4/3; (ix) −x−1/3, −y−2/3, −z+4/3; (x) y+2/3, −x+y+1/3, −z+4/3; (xi) x−y−1/3, x+1/3, −z+4/3; (xii) x−1/3, x−y−2/3, z−1/6; (xiii) −y−1/3, −x+1/3, z−1/6; (xiv) −x+y+2/3, y+1/3, z−1/6; (xv) −y, x−y+1, z; (xvi) x+1, y+1, z; (xvii) x, y+1, z; (xviii) −x+y+1, −x+1, z; (xix) −x+2/3, −y+1/3, −z+4/3; (xx) x−1, y, z; (xxi) −y+1/3, −x+2/3, z+1/6; (xxii) −x−1/3, −y+1/3, −z+4/3; (xxiii) −x+2/3, −y+4/3, −z+4/3; (xxiv) x+1, y, z; (xxv) x, y−1, z; (xxvi) x−1, y−1, z; (xxvii) −y+1/3, −x−1/3, z+1/6.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O3—H···O4^xxviii	0.83 (3)	1.80 (3)	2.621 (3)	170 (4)

Symmetry code: (xxviii) y, x−1, −z+3/2.

Acknowledgements

The authors acknowledge the TU Wien University Library for financial support through its Open Access Funding Program.

Funding information

Funding for this research was provided by: Austrian Academy of Sciences, Doc-fForte Fellowship to K. Schwendtner.

References

Baur, W. H. (1981). Structure and Bonding in Crystals, edited by M. O'Keeffe & A. Navrotsky, pp. 31–52. New York: Academic Press.
Belam, W., Driss, A. & Jouini, T. (1997). Acta Cryst. C53, 5–7. CrossRef CAS Web of Science IUCr Journals
Brandenburg, K. (2005). DIAMOND. Crystal Impact GbR, Bonn, Germany.
Ezhova, Z. A., Deichman, E. N. & Tananaev, I. V. (1977). Zh. Neorg. Khim. 22, 2696–2703. CAS
Filaretov, A. A., Zhizhin, M. G., Komissarova, L. N., Danilov, V. P., Chernyshev, V. V. & Lazoryak, B. I. (2002a). J. Solid State Chem. 166, 362–368. CrossRef CAS
Filaretov, A. A., Zhizhin, M. G., Olenev, A. V., Gurkin, A. A., Bobylev, A. P., Lazoryak, B. I., Danilov, V. P. & Komissarova, L. N. (2002b). Zh. Neorg. Khim. 47, 1930–1946. CAS
Gagné, O. C. & Hawthorne, F. C. (2015). Acta Cryst. B71, 562–578. Web of Science CrossRef IUCr Journals
Huang, Y.-X., Li, M.-R., Mi, J.-X., Mao, S.-Y., Chen, H.-H. & Zhao, J.-T. (2004). Wuji Huaxue Xuebao, 20, 1191–1196. CAS
Khorari, S., Rulmont, A. & Tarte, P. (1997). J. Solid State Chem. 134, 31–37. Web of Science CrossRef CAS
Kolitsch, U. (2004). Z. Kristallogr. New Cryst. Struct. 219, 207–208. CAS
Lesage, J., Adam, L., Guesdon, A. & Raveau, B. (2007). J. Solid State Chem. 180, 1799–1808. Web of Science CrossRef CAS
Lii, K.-H. & Wu, L.-S. (1994). J. Chem. Soc. A, 10, 1577–1580.
Lii, K.-H. & Ye, J. (1997). J. Solid State Chem. 131, 131–137. CrossRef CAS Web of Science
Mao, S.-Y., Li, M.-R., Mi, J.-X., Chen, H.-H., Deng, J.-F. & Zhao, J.-T. (2002). Z. Kristallogr. New Cryst. Struct. 217, 311–312. CAS
Masquelier, C., d'Yvoire, F., Bretey, E., Berthet, P. & Peytour-Chansac, C. (1994a). Solid State Ionics, 67, 183–189. CrossRef CAS Web of Science
Masquelier, C., d'Yvoire, F. & Collin, G. (1994b). Solid State Ionic Materials, Proceedings of the 4th Asian Conference on Solid State Ionics, Kuala Lumpur, Malaysia, 2–6 August 1994, edited by B. V. R. Chowdari, M. Yahaya, I. A. Talib & M. M. Salleh, pp. 167–172. Singapore: World Scientific.
Masquelier, C., d'Yvoire, F. & Collin, G. (1995). J. Solid State Chem. 118, 33–42. CrossRef CAS Web of Science
Masquelier, C., d'Yvoire, F. & Rodier, N. (1990). Acta Cryst. C46, 1584–1587. CrossRef CAS Web of Science IUCr Journals
Masquelier, C., Padhi, A. K., Nanjundaswamy, K. S. & Goodenough, J. B. (1998). J. Solid State Chem. 135, 228–234. Web of Science CrossRef CAS
Masquelier, C., Padhi, A. K., Nanjundaswamy, K. S., Okada, S. & Goodenough, J. B. (1996). Proceedings of the 37th Power Sources Conference, Cherry Hill, New Jersey, June 17–20, 1996, pp. 188–191. Fort Monmouth, NJ: US Army Research Laboratory.
Mesa, J. L., Goñi, A., Brandl, A. L., Moreno, N. O., Barberis, G. E. & Rojo, T. (2000). J. Mater. Chem. 10, 2779–2785. Web of Science CrossRef CAS
Nonius (2003). KappaCCD Server Software and COLLECT. Nonius BV, Delft, The Netherlands.
Otwinowski, Z., Borek, D., Majewski, W. & Minor, W. (2003). Acta Cryst. A59, 228–234. Web of Science CrossRef CAS IUCr Journals
Ouerfelli, N., Guesmi, A., Mazza, D., Madani, A., Zid, M. F. & Driss, A. (2007a). J. Solid State Chem. 180, 1224–1229. Web of Science CrossRef CAS
Ouerfelli, N., Guesmi, A., Mazza, D., Zid, M. F. & Driss, A. (2008). Acta Cryst. C64, i41–i44. Web of Science CrossRef IUCr Journals
Ouerfelli, N., Guesmi, A., Molinié, P., Mazza, D., Zid, M. F. & Driss, A. (2007b). J. Solid State Chem. 180, 2942–2949. Web of Science CrossRef CAS
Ouerfelli, N., Souilem, A., Zid, M. F. & Driss, A. (2014). Acta Cryst. E70, i21–i22. CSD CrossRef IUCr Journals
Pintard-Scrépel, M., d'Yvoire, F. & Durand, J. (1983). Acta Cryst. C39, 9–12. CrossRef IUCr Journals
Prem, M., Lengauer, C. & Tillmanns, E. (2005a). University of Vienna, Austria. ICDD Grant-in-Aid.
Prem, M., Lengauer, C. & Tillmanns, E. (2005b). University of Vienna, Austria. ICDD Grant-in-Aid.
Rousse, G., Rodríguez-Carvajal, J., Wurm, C. & Masquelier, C. (2013). Phys. Rev. B, 88, 214433214431–214433/214439. CrossRef
Schwendtner, K. (2006). J. Alloys Compd. 421, 57–63. Web of Science CrossRef CAS
Schwendtner, K. (2008). PhD thesis, Universität Wien, Austria.
Schwendtner, K. & Kolitsch, U. (2004a). Acta Cryst. C60, i79–i83. Web of Science CrossRef CAS IUCr Journals
Schwendtner, K. & Kolitsch, U. (2004b). Acta Cryst. C60, i84–i88. Web of Science CrossRef CAS IUCr Journals
Schwendtner, K. & Kolitsch, U. (2005). Acta Cryst. C61, i90–i93. Web of Science CrossRef CAS IUCr Journals
Schwendtner, K. & Kolitsch, U. (2007a). Acta Cryst. B63, 205–215. Web of Science CrossRef IUCr Journals
Schwendtner, K. & Kolitsch, U. (2007b). Acta Cryst. C63, i17–i20. Web of Science CrossRef IUCr Journals
Schwendtner, K. & Kolitsch, U. (2007c). Eur. J. Mineral. 19, 399–409. Web of Science CrossRef CAS
Schwendtner, K. & Kolitsch, U. (2007d). Mineral. Mag. 71, 249–263. Web of Science CrossRef CAS
Schwendtner, K. & Kolitsch, U. (2017a). Acta Cryst. C73, 600–608. Web of Science CSD CrossRef IUCr Journals
Schwendtner, K. & Kolitsch, U. (2017b). Acta Cryst. E73, 1294–1297. CrossRef IUCr Journals
Schwendtner, K. & Kolitsch, U. (2017c). Acta Cryst. E73, 785–790. CrossRef IUCr Journals
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals
Sheldrick, G. M. (2015). Acta Cryst. C71, 3–8. Web of Science CrossRef IUCr Journals
Vencato, I., Mattievich, E., Moreira, L. F. & Mascarenhas, Y. P. (1989). Acta Cryst. C45, 367–371. CrossRef CAS IUCr Journals
Westrip, S. P. (2010). J. Appl. Cryst. 43, 920–925. Web of Science CrossRef CAS IUCr Journals
Winand, J. M., Rulmont, A. & Tarte, P. (1990). J. Solid State Chem. 87, 83–94. CrossRef CAS
Yakubovich, O. V. (1993). Kristallografiya, 38, 43–48. CAS

This is an open-access article distributed under the terms of the Creative Commons Attribution (CC-BY) Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.

CRYSTALLOGRAPHIC
COMMUNICATIONS

ISSN: 2056-9890

Volume 73| Part 10| October 2017| Pages 1580-1586

https://doi.org/10.1107/S205698901701355X

Open

access

Format		BIBTeX
		EndNote
		RefMan
		Refer
		Medline
		CIF
		SGML
		Plain Text
		Text

Format		BIBTeX
		EndNote
		RefMan
		Refer
		Medline
		CIF
		SGML
		Plain Text
		Text

Search IUCr Journals		doi		Advanced search
Author		volume	page

research communications\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)