MIn(HAsO4)2 (M = K, Rb, Cs): three new hydrogen-arsenates adopting two different structure types.

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 hydro-thermal 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 tetra-hedral-octa-hedral 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].

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 +–M 3+–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 + M 3+(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, 2004 ▸b). 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 RbM 3+(HPO4)2 (M = Al, Ga) (Lesage et al., 2007 ▸). All of these compounds consist of frameworks of singly protonated AsO4 tetra­hedra and M 3+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)(H1.5AsO4)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 ; 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.

Structural commentary

KIn(HAsO4)2 crystallizes in space group C2/c and is isotypic to KSc(HAsO4)2 (Schwendtner & Kolitsch, 2004 ▸ a), 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. 1 ▸ a). 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. 2 ▸ a,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.

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 + , −y + , −z; (ii) −x, −y + 1, −z; (iii) x + , y − , z; (iv) x − , −y + , z − ; (v) −x + 1, y, −z + ; (vi) x, −y + 1, z − ; (vii) −x + , y − , −z + ; (viii) −x, y, −z + ; (ix) −x + , y + , −z + ; (x) x − , y + , z; CsIn(HAsO4)2: (ii) −x, −x + y, −z + ; (iii) −x + y, −x, z; (iv) −y, x − y, z; (vii) y + , −x + y + , −z + ; (xi) x − y − , x + , −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 + , −y + , −z + ; (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.

Table 1

Selected bond lengths (Å) for KIn(HAsO4)

K1—O1i	2.6488 (17)	K2—O3vii	3.20 (3)
K1—O1	2.6488 (17)	K2—O2	3.33 (3)
K1—O3ii	2.7788 (17)	K2—O2vi	3.33 (3)
K1—O3iii	2.7788 (17)	In—O1	2.1104 (17)
K1—O4iv	3.112 (2)	In—O1vi	2.1104 (17)
K1—O4v	3.112 (2)	In—O3ii	2.1388 (16)
K1—O2	3.2553 (19)	In—O3ix	2.1388 (16)
K1—O2i	3.2553 (19)	In—O2x	2.1473 (16)
K2—O4	2.74 (4)	In—O2v	2.1473 (16)
K2—O4vi	2.74 (4)	As—O1	1.6574 (17)
K2—O1vii	2.792 (18)	As—O3	1.6721 (17)
K2—O1viii	2.792 (18)	As—O2	1.6762 (16)
K2—O3viii	3.20 (3)	As—O4	1.7231 (19)

Symmetry codes: (i) ; (ii) ; (iii) ; (iv) ; (v) ; (vi) ; (vii) ; (viii) ; (ix) ; (x) .

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. 2 ▸ b 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⋯O2xi	0.88 (2)	1.89 (3)	2.690 (3)	151 (4)

Symmetry code: (xi) .

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 c and are isotypic to RbFe(HPO4)2 (Lii & Wu, 1994 ▸) and RbM 3+(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. 4 ▸ a 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 ▸).

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.

Table 2

Selected bond lengths (Å) for RbIn(HAsO4)

Rb1A—O3i	3.042 (2)	Rb2A—O4xi	3.668 (5)
Rb1A—O3ii	3.042 (2)	Rb2A—O1xii	3.830 (3)
Rb1A—O3iii	3.042 (2)	Rb2A—O1xiii	3.830 (3)
Rb1A—O3iv	3.042 (2)	Rb2A—O1xiv	3.830 (3)
Rb1A—O3v	3.042 (2)	In1—O2xv	2.1306 (17)
Rb1A—O3	3.042 (2)	In1—O2v	2.1306 (17)
Rb1A—O2	3.3114 (19)	In1—O2xvi	2.1306 (17)
Rb1A—O2iv	3.3115 (19)	In1—O4xvii	2.1457 (17)
Rb1A—O2iii	3.3114 (19)	In1—O4ii	2.1457 (16)
Rb1A—O2v	3.3114 (19)	In1—O4xii	2.1457 (16)
Rb1A—O2i	3.3114 (18)	In2—O1vii	2.1312 (19)
Rb1A—O2ii	3.3114 (18)	In2—O1xviii	2.131 (2)
Rb2A—O3	3.006 (5)	In2—O1ii	2.1312 (19)
Rb2A—O3ii	3.006 (5)	In2—O1xii	2.131 (2)
Rb2A—O3v	3.006 (5)	In2—O1xvii	2.1312 (19)
Rb2A—O1vi	3.462 (3)	In2—O1xix	2.1312 (19)
Rb2A—O1vii	3.462 (3)	As—O1xiii	1.6508 (18)
Rb2A—O1viii	3.462 (3)	As—O2	1.6668 (17)
Rb2A—O4ix	3.668 (5)	As—O4iv	1.6736 (17)
Rb2A—O4x	3.668 (5)	As—O3	1.7409 (19)

Symmetry codes: (i) ; (ii) ; (iii) ; (iv) ; (v) ; (vi) ; (vii) ; (viii) ; (ix) ; (x) ; (xi) ; (xii) ; (xiii) ; (xiv) ; (xv) ; (xvi) ; (xvii) ; (xviii) ; (xix) .

Table 3

Selected bond lengths (Å) for CsIn(HAsO4)

Cs1—O3	3.280 (3)	Cs2—O3xi	3.698 (3)
Cs1—O3i	3.280 (3)	Cs2—O4xii	3.703 (2)
Cs1—O3ii	3.280 (3)	Cs2—O4xiii	3.703 (2)
Cs1—O3iii	3.280 (3)	Cs2—O4xiv	3.703 (2)
Cs1—O3iv	3.280 (3)	In1—O2xv	2.127 (2)
Cs1—O3v	3.280 (3)	In1—O2iii	2.127 (2)
Cs1—O2	3.434 (2)	In1—O2xvi	2.127 (2)
Cs1—O2ii	3.434 (2)	In1—O4xvii	2.150 (2)
Cs1—O2v	3.434 (2)	In1—O4iv	2.150 (2)
Cs1—O2iii	3.434 (2)	In1—O4xviii	2.150 (2)
Cs1—O2i	3.434 (2)	In2—O1vii	2.133 (2)
Cs1—O2iv	3.434 (2)	In2—O1xi	2.133 (3)
Cs2—O3iv	3.121 (3)	In2—O1xix	2.133 (2)
Cs2—O3iii	3.121 (2)	In2—O1iv	2.133 (2)
Cs2—O3	3.121 (3)	In2—O1xviii	2.133 (3)
Cs2—O1vi	3.419 (3)	In2—O1xvii	2.133 (2)
Cs2—O1vii	3.419 (3)	As—O1xx	1.655 (2)
Cs2—O1viii	3.419 (3)	As—O2	1.671 (2)
Cs2—O3ix	3.698 (3)	As—O4ii	1.679 (2)
Cs2—O3x	3.698 (3)	As—O3	1.743 (3)

Symmetry codes: (i) ; (ii) ; (iii) ; (iv) ; (v) ; (vi) ; (vii) ; (viii) ; (ix) ; (x) ; (xi) ; (xii) ; (xiii) ; (xiv) ; (xv) ; (xvi) ; (xvii) ; (xviii) ; (xix) ; (xx) .

Table 5

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

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O3—H⋯O4xx	0.83 (3)	1.82 (3)	2.634 (2)	168 (4)

Symmetry code: (xx) .

Table 6

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

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O3—H⋯O4xxi	0.83 (3)	1.80 (3)	2.621 (3)	170 (4)

Symmetry code: (xxi) .

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 +:M 3+: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. 5 ▸ a) 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. 5 ▸ b 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.

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 c:H	Trigonal, R 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[F 2 > 2σ(F 2)], wR(F 2), 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
Δρmax, Δρmin (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.

Crystal structure: contains datablock(s) KInHAsO42, RbInHAsO42, CsInHAsO42. DOI: 10.1107/S205698901701355X/pj2047sup1.cif

Structure factors: contains datablock(s) KInHAsO42. DOI: 10.1107/S205698901701355X/pj2047KInHAsO42sup2.hkl

Structure factors: contains datablock(s) RbInHAsO42. DOI: 10.1107/S205698901701355X/pj2047RbInHAsO42sup3.hkl

Structure factors: contains datablock(s) CsInHAsO42. DOI: 10.1107/S205698901701355X/pj2047CsInHAsO42sup4.hkl

CCDC references: 1575921, 1575920, 1575919

Additional supporting information: crystallographic information; 3D view; checkCIF report

KIn(HAsO4)2	F(000) = 800
Mr = 433.78	Dx = 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

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

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(Fo2) + (0.0227P)2 + 1.2908P] where P = (Fo2 + 2Fc2)/3
S = 1.09	(Δ/σ)max = 0.001
1406 reflections	Δρmax = 1.18 e Å−3
64 parameters	Δρmin = −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)

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.

	x	y	z	Uiso*/Ueq	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)*

	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)

K1—O1i	2.6488 (17)	K2—O3ix	3.20 (3)
K1—O1	2.6488 (17)	K2—O2	3.33 (3)
K1—K2ii	2.653 (15)	K2—O2viii	3.33 (3)
K1—K2iii	2.653 (15)	K2—Asix	3.35 (4)
K1—O3iv	2.7788 (17)	K2—Asx	3.35 (4)
K1—O3v	2.7788 (17)	In—O1	2.1104 (17)
K1—O4vi	3.112 (2)	In—O1viii	2.1104 (17)
K1—O4vii	3.112 (2)	In—O3iv	2.1388 (16)
K1—O2	3.2553 (19)	In—O3xi	2.1388 (16)
K1—O2i	3.2553 (19)	In—O2xii	2.1473 (16)
K1—As	3.6059 (7)	In—O2vii	2.1473 (16)
K1—Asi	3.6059 (7)	As—O1	1.6574 (17)
K2—O4	2.74 (4)	As—O3	1.6721 (17)
K2—O4viii	2.74 (4)	As—O2	1.6762 (16)
K2—O1ix	2.792 (18)	As—O4	1.7231 (19)
K2—O1x	2.792 (18)	O4—H	0.876 (19)
K2—O3x	3.20 (3)
O1i—K1—O1	180.0	K1ix—K2—Asix	72.8 (8)
O1i—K1—K2ii	63.6 (3)	K1x—K2—Asix	83.9 (10)
O1—K1—K2ii	116.4 (3)	O4—K2—Asix	125.63 (13)
O1i—K1—K2iii	116.4 (3)	O4viii—K2—Asix	122.06 (11)
O1—K1—K2iii	63.6 (3)	O1ix—K2—Asix	29.6 (4)
K2ii—K1—K2iii	180 (2)	O1x—K2—Asix	113.1 (16)
O1i—K1—O3iv	115.35 (5)	O3x—K2—Asix	90.8 (12)
O1—K1—O3iv	64.65 (5)	O3ix—K2—Asix	29.5 (3)
K2ii—K1—O3iv	72.1 (6)	O2—K2—Asix	82.73 (9)
K2iii—K1—O3iv	107.9 (6)	O2viii—K2—Asix	163.5 (6)
O1i—K1—O3v	64.65 (5)	K1ix—K2—Asx	83.9 (10)
O1—K1—O3v	115.35 (5)	K1x—K2—Asx	72.8 (8)
K2ii—K1—O3v	107.9 (6)	O4—K2—Asx	122.06 (11)
K2iii—K1—O3v	72.1 (6)	O4viii—K2—Asx	125.63 (13)
O3iv—K1—O3v	180.00 (6)	O1ix—K2—Asx	113.1 (16)
O1i—K1—O4vi	90.87 (5)	O1x—K2—Asx	29.6 (4)
O1—K1—O4vi	89.13 (5)	O3x—K2—Asx	29.5 (3)
K2ii—K1—O4vi	56.1 (11)	O3ix—K2—Asx	90.8 (12)
K2iii—K1—O4vi	123.9 (11)	O2—K2—Asx	163.5 (6)
O3iv—K1—O4vi	101.27 (5)	O2viii—K2—Asx	82.73 (9)
O3v—K1—O4vi	78.73 (5)	Asix—K2—Asx	91.7 (13)
O1i—K1—O4vii	89.13 (5)	O1—In—O1viii	94.99 (10)
O1—K1—O4vii	90.87 (5)	O1—In—O3iv	86.23 (7)
K2ii—K1—O4vii	123.9 (11)	O1viii—In—O3iv	92.67 (7)
K2iii—K1—O4vii	56.1 (11)	O1—In—O3xi	92.67 (7)
O3iv—K1—O4vii	78.73 (5)	O1viii—In—O3xi	86.23 (7)
O3v—K1—O4vii	101.27 (5)	O3iv—In—O3xi	178.38 (9)
O4vi—K1—O4vii	180.0	O1—In—O2xii	177.02 (7)
O1i—K1—O2	127.87 (5)	O1viii—In—O2xii	87.52 (7)
O1—K1—O2	52.13 (5)	O3iv—In—O2xii	92.07 (6)
K2ii—K1—O2	104.0 (10)	O3xi—In—O2xii	89.08 (7)
K2iii—K1—O2	76.0 (10)	O1—In—O2vii	87.52 (7)
O3iv—K1—O2	106.19 (5)	O1viii—In—O2vii	177.02 (7)
O3v—K1—O2	73.81 (5)	O3iv—In—O2vii	89.08 (7)
O4vi—K1—O2	49.92 (5)	O3xi—In—O2vii	92.07 (6)
O4vii—K1—O2	130.08 (5)	O2xii—In—O2vii	90.01 (10)
O1i—K1—O2i	52.13 (5)	O1—In—K1viii	107.25 (5)
O1—K1—O2i	127.87 (5)	O1viii—In—K1viii	42.55 (5)
K2ii—K1—O2i	76.0 (10)	O3iv—In—K1viii	132.97 (5)
K2iii—K1—O2i	104.0 (10)	O3xi—In—K1viii	46.31 (5)
O3iv—K1—O2i	73.80 (5)	O2xii—In—K1viii	75.69 (5)
O3v—K1—O2i	106.20 (5)	O2vii—In—K1viii	135.06 (5)
O4vi—K1—O2i	130.08 (5)	O1—In—K1	42.55 (5)
O4vii—K1—O2i	49.92 (5)	O1viii—In—K1	107.25 (5)
O2—K1—O2i	180.0	O3iv—In—K1	46.31 (5)
O1i—K1—As	154.71 (4)	O3xi—In—K1	132.97 (5)
O1—K1—As	25.29 (4)	O2xii—In—K1	135.06 (5)
K2ii—K1—As	117.5 (7)	O2vii—In—K1	75.69 (5)
K2iii—K1—As	62.5 (7)	K1viii—In—K1	141.977 (12)
O3iv—K1—As	87.14 (4)	O1—In—K2iii	36.3 (7)
O3v—K1—As	92.86 (4)	O1viii—In—K2iii	130.9 (7)
O4vi—K1—As	72.55 (4)	O3iv—In—K2iii	80.73 (5)
O4vii—K1—As	107.45 (4)	O3xi—In—K2iii	99.09 (6)
O2—K1—As	27.68 (3)	O2xii—In—K2iii	140.9 (7)
O2i—K1—As	152.32 (3)	O2vii—In—K2iii	51.8 (7)
O1i—K1—Asi	25.29 (4)	K1viii—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—K2xii	130.9 (7)
K2iii—K1—Asi	117.5 (7)	O1viii—In—K2xii	36.3 (7)
O3iv—K1—Asi	92.86 (4)	O3iv—In—K2xii	99.09 (6)
O3v—K1—Asi	87.14 (4)	O3xi—In—K2xii	80.73 (5)
O4vi—K1—Asi	107.45 (4)	O2xii—In—K2xii	51.8 (7)
O4vii—K1—Asi	72.55 (4)	O2vii—In—K2xii	140.9 (7)
O2—K1—Asi	152.32 (3)	K1viii—In—K2xii	38.4 (3)
O2i—K1—Asi	27.68 (3)	K1—In—K2xii	135.3 (4)
As—K1—Asi	180.0	K2iii—In—K2xii	167.1 (14)
K1ix—K2—K1x	147 (2)	O1—As—O3	110.45 (9)
K1ix—K2—O4	70.4 (4)	O1—As—O2	105.35 (8)
K1x—K2—O4	142.6 (17)	O3—As—O2	113.38 (8)
K1ix—K2—O4viii	142.6 (17)	O1—As—O4	110.80 (10)
K1x—K2—O4viii	70.4 (4)	O3—As—O4	109.76 (8)
O4—K2—O4viii	73.9 (13)	O2—As—O4	106.99 (10)
K1ix—K2—O1ix	58.2 (4)	O1—As—K2iii	56.3 (5)
K1x—K2—O1ix	109.3 (10)	O3—As—K2iii	70.26 (6)
O4—K2—O1ix	96.2 (5)	O2—As—K2iii	87.2 (6)
O4viii—K2—O1ix	116.1 (8)	O4—As—K2iii	163.7 (7)
K1ix—K2—O1x	109.3 (10)	O1—As—K1	43.06 (6)
K1x—K2—O1x	58.2 (4)	O3—As—K1	114.49 (6)
O4—K2—O1x	116.1 (8)	O2—As—K1	64.44 (6)
O4viii—K2—O1x	96.2 (5)	O4—As—K1	134.49 (6)
O1ix—K2—O1x	140 (2)	K2iii—As—K1	44.66 (8)
K1ix—K2—O3x	55.8 (6)	O1—As—K2	114.2 (5)
K1x—K2—O3x	102.0 (12)	O3—As—K2	134.2 (4)
O4—K2—O3x	100.01 (14)	O2—As—K2	63.8 (2)
O4viii—K2—O3x	144.0 (5)	O4—As—K2	43.88 (15)
O1ix—K2—O3x	99.8 (12)	K2iii—As—K2	146.9 (3)
O1x—K2—O3x	53.8 (5)	K1—As—K2	104.94 (19)
K1ix—K2—O3ix	102.0 (12)	As—O1—In	140.97 (10)
K1x—K2—O3ix	55.8 (6)	As—O1—K1	111.65 (8)
O4—K2—O3ix	144.0 (5)	In—O1—K1	104.85 (7)
O4viii—K2—O3ix	100.01 (14)	As—O1—K2iii	94.1 (9)
O1ix—K2—O3ix	53.8 (5)	In—O1—K2iii	117.1 (10)
O1x—K2—O3ix	99.8 (12)	K1—O1—K2iii	58.29 (14)
O3x—K2—O3ix	104.1 (15)	As—O2—Inxiii	131.05 (9)
K1ix—K2—O2	79.6 (4)	As—O2—K1	87.88 (7)
K1x—K2—O2	121.6 (6)	Inxiii—O2—K1	124.98 (7)
O4—K2—O2	52.4 (7)	As—O2—K2	89.3 (6)
O4viii—K2—O2	69.8 (10)	Inxiii—O2—K2	97.7 (7)
O1ix—K2—O2	56.7 (3)	K1—O2—K2	123.5 (5)
O1x—K2—O2	163.3 (17)	As—O3—Inxi	130.50 (9)
O3x—K2—O2	134.62 (5)	As—O3—K1v	129.02 (8)
O3ix—K2—O2	91.84 (5)	Inxi—O3—K1v	99.88 (6)
K1ix—K2—O2viii	121.6 (6)	As—O3—K2iii	80.2 (3)
K1x—K2—O2viii	79.6 (4)	Inxi—O3—K2iii	139.1 (7)
O4—K2—O2viii	69.8 (10)	K1v—O3—K2iii	52.13 (8)
O4viii—K2—O2viii	52.4 (7)	As—O4—K2	110.3 (2)
O1ix—K2—O2viii	163.3 (17)	As—O4—K1ix	108.30 (10)
O1x—K2—O2viii	56.7 (3)	K2—O4—K1ix	53.4 (7)
O3x—K2—O2viii	91.84 (5)	As—O4—H	115 (3)
O3ix—K2—O2viii	134.62 (5)	K2—O4—H	123 (3)
O2—K2—O2viii	106.6 (15)	K1ix—O4—H	80 (3)

D—H···A	D—H	H···A	D···A	D—H···A
O4—H···O2xiv	0.88 (2)	1.89 (3)	2.690 (3)	151 (4)

RbIn(HAsO4)2	Dx = 4.053 Mg m−3
Mr = 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

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

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(Fo2) + (0.014P)2 + 16.3085P] where P = (Fo2 + 2Fc2)/3
S = 1.12	(Δ/σ)max = 0.006
1443 reflections	Δρmax = 1.00 e Å−3
69 parameters	Δρmin = −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)

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.

	x	y	z	Uiso*/Ueq	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)*

	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)

Rb1A—Rb1Bi	0.44 (3)	Rb2A—O1vi	3.462 (3)
Rb1A—Rb1Bii	0.44 (3)	Rb2A—O1vii	3.462 (3)
Rb1A—O3iii	3.042 (2)	Rb2A—O1viii	3.462 (3)
Rb1A—O3i	3.042 (2)	Rb2A—O4ix	3.668 (5)
Rb1A—O3iv	3.042 (2)	Rb2A—O4x	3.668 (5)
Rb1A—O3v	3.042 (2)	Rb2A—O4xi	3.668 (5)
Rb1A—O3ii	3.042 (2)	Rb2A—O1xii	3.830 (3)
Rb1A—O3	3.042 (2)	Rb2A—O1xiii	3.830 (3)
Rb1A—O2	3.3114 (19)	Rb2A—O1xiv	3.830 (3)
Rb1A—O2v	3.3115 (19)	Rb2A—O3xv	3.888 (4)
Rb1A—O2iv	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—O1viii	3.259 (8)
Rb1A—Hi	3.28 (4)	Rb2B—O1vi	3.436 (9)
Rb1A—Hii	3.28 (4)	Rb2B—O4x	3.525 (8)
Rb1A—Hiv	3.28 (4)	Rb2B—O1xiii	3.608 (9)
Rb1A—Hiii	3.28 (4)	Rb2B—Asxvi	3.781 (8)
Rb1A—Hv	3.28 (4)	Rb2B—Asxv	3.869 (8)
Rb1B—Rb1Bi	0.76 (6)	Rb2B—As	3.945 (9)
Rb1B—Rb1Bii	0.76 (5)	In1—O2xvii	2.1306 (17)
Rb1B—O3v	2.842 (12)	In1—O2ii	2.1306 (17)
Rb1B—O3	2.842 (12)	In1—O2xviii	2.1306 (17)
Rb1B—O2iv	2.98 (2)	In1—O4xix	2.1457 (17)
Rb1B—O2i	2.98 (2)	In1—O4i	2.1457 (16)
Rb1B—O3iv	3.035 (3)	In1—O4xii	2.1457 (16)
Rb1B—O3i	3.035 (3)	In2—O1vii	2.1312 (19)
Rb1B—O2	3.312 (3)	In2—O1xvi	2.131 (2)
Rb1B—O2v	3.312 (3)	In2—O1i	2.1312 (19)
Rb1B—O3iii	3.32 (2)	In2—O1xii	2.131 (2)
Rb1B—O3ii	3.32 (2)	In2—O1xix	2.1312 (19)
Rb1B—H	2.99 (4)	In2—O1xx	2.1312 (19)
Rb1B—Hv	2.99 (4)	As—O1xiii	1.6508 (18)
Rb2A—Rb2Bii	0.249 (8)	As—O2	1.6668 (17)
Rb2A—Rb2Bi	0.249 (8)	As—O4v	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—O1xiv	76.69 (8)
Rb1Bi—Rb1A—O3iii	59.08 (4)	O3i—Rb2A—O1xiv	44.11 (5)
Rb1Bii—Rb1A—O3iii	85.05 (9)	O3ii—Rb2A—O1xiv	112.37 (15)
Rb1Bi—Rb1A—O3i	59.08 (4)	O1vi—Rb2A—O1xiv	45.46 (6)
Rb1Bii—Rb1A—O3i	126.88 (5)	O1vii—Rb2A—O1xiv	95.29 (5)
O3iii—Rb1A—O3i	118.16 (8)	O1viii—Rb2A—O1xiv	150.55 (6)
Rb1Bi—Rb1A—O3iv	126.88 (4)	O4ix—Rb2A—O1xiv	78.40 (6)
Rb1Bii—Rb1A—O3iv	59.08 (7)	O4x—Rb2A—O1xiv	120.81 (10)
O3iii—Rb1A—O3iv	68.39 (6)	O4xi—Rb2A—O1xiv	111.19 (9)
O3i—Rb1A—O3iv	170.10 (7)	O1xii—Rb2A—O1xiv	113.93 (7)
Rb1Bi—Rb1A—O3v	85.05 (4)	O1xiii—Rb2A—O1xiv	113.93 (7)
Rb1Bii—Rb1A—O3v	126.88 (5)	Rb2Bii—Rb2A—O3xv	126 (3)
O3iii—Rb1A—O3v	68.39 (6)	Rb2Bi—Rb2A—O3xv	74 (3)
O3i—Rb1A—O3v	106.24 (7)	O3—Rb2A—O3xv	89.86 (5)
O3iv—Rb1A—O3v	68.39 (6)	O3i—Rb2A—O3xv	129.48 (6)
Rb1Bi—Rb1A—O3ii	85.05 (4)	O3ii—Rb2A—O3xv	145.79 (7)
Rb1Bii—Rb1A—O3ii	59.08 (7)	O1vi—Rb2A—O3xv	42.24 (6)
O3iii—Rb1A—O3ii	106.24 (7)	O1vii—Rb2A—O3xv	117.63 (15)
O3i—Rb1A—O3ii	68.39 (6)	O1viii—Rb2A—O3xv	66.65 (8)
O3iv—Rb1A—O3ii	118.16 (7)	O4ix—Rb2A—O3xv	42.47 (6)
O3v—Rb1A—O3ii	170.10 (8)	O4x—Rb2A—O3xv	40.66 (6)
Rb1Bi—Rb1A—O3	126.88 (4)	O4xi—Rb2A—O3xv	76.43 (11)
Rb1Bii—Rb1A—O3	85.05 (9)	O1xii—Rb2A—O3xv	151.71 (14)
O3iii—Rb1A—O3	170.10 (7)	O1xiii—Rb2A—O3xv	69.64 (5)
O3i—Rb1A—O3	68.38 (6)	O1xiv—Rb2A—O3xv	87.30 (5)
O3iv—Rb1A—O3	106.24 (7)	Rb2Bi—Rb2B—Rb2Bii	60.00 (6)
O3v—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)
O3iv—Rb1A—O2	67.27 (5)	Rb2Bii—Rb2B—O3i	68.5 (12)
O3v—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—O1viii	158.2 (7)
Rb1Bi—Rb1A—O2v	37.75 (3)	Rb2Bii—Rb2B—O1viii	111 (2)
Rb1Bii—Rb1A—O2v	148.87 (10)	O3—Rb2B—O1viii	94.9 (2)
O3iii—Rb1A—O2v	64.77 (5)	O3ii—Rb2B—O1viii	88.5 (2)
O3i—Rb1A—O2v	67.27 (5)	O3i—Rb2B—O1viii	153.0 (3)
O3iv—Rb1A—O2v	112.03 (5)	Rb2Bi—Rb2B—O1vi	62.0 (19)
O3v—Rb1A—O2v	50.13 (5)	Rb2Bii—Rb2B—O1vi	118.2 (19)
O3ii—Rb1A—O2v	120.30 (5)	O3—Rb2B—O1vi	87.5 (2)
O3—Rb1A—O2v	125.02 (5)	O3ii—Rb2B—O1vi	149.7 (3)
O2—Rb1A—O2v	172.51 (6)	O3i—Rb2B—O1vi	86.8 (2)
Rb1Bi—Rb1A—O2iv	148.87 (3)	O1viii—Rb2B—O1vi	114.2 (2)
Rb1Bii—Rb1A—O2iv	86.26 (12)	Rb2Bi—Rb2B—O4x	113.2 (3)
O3iii—Rb1A—O2iv	112.03 (5)	Rb2Bii—Rb2B—O4x	105.2 (7)
O3i—Rb1A—O2iv	120.30 (5)	O3—Rb2B—O4x	125.4 (3)
O3iv—Rb1A—O2iv	50.13 (4)	O3ii—Rb2B—O4x	130.1 (3)
O3v—Rb1A—O2iv	64.77 (5)	O3i—Rb2B—O4x	159.7 (3)
O3ii—Rb1A—O2iv	125.02 (5)	O1viii—Rb2B—O4x	47.08 (11)
O3—Rb1A—O2iv	67.27 (5)	O1vi—Rb2B—O4x	79.33 (17)
O2—Rb1A—O2iv	62.27 (6)	Rb2Bi—Rb2B—O1xiii	150.5 (18)
O2v—Rb1A—O2iv	111.23 (3)	Rb2Bii—Rb2B—O1xiii	141.8 (19)
Rb1Bi—Rb1A—O2ii	37.75 (3)	O3—Rb2B—O1xiii	47.02 (14)
Rb1Bii—Rb1A—O2ii	86.26 (12)	O3ii—Rb2B—O1xiii	79.7 (2)
O3iii—Rb1A—O2ii	67.27 (5)	O3i—Rb2B—O1xiii	113.9 (3)
O3i—Rb1A—O2ii	64.77 (5)	O1viii—Rb2B—O1xiii	48.49 (13)
O3iv—Rb1A—O2ii	125.02 (5)	O1vi—Rb2B—O1xiii	99.9 (2)
O3v—Rb1A—O2ii	120.30 (5)	O4x—Rb2B—O1xiii	83.29 (17)
O3ii—Rb1A—O2ii	50.13 (5)	Rb2Bi—Rb2B—Asxvi	132.4 (6)
O3—Rb1A—O2ii	112.03 (5)	Rb2Bii—Rb2B—Asxvi	98.8 (15)
O2—Rb1A—O2ii	111.23 (3)	O3—Rb2B—Asxvi	119.4 (2)
O2v—Rb1A—O2ii	75.50 (6)	O3ii—Rb2B—Asxvi	104.1 (2)
O2iv—Rb1A—O2ii	172.51 (6)	O3i—Rb2B—Asxvi	166.2 (3)
Rb1Bi—Rb1A—O2iii	86.26 (3)	O1viii—Rb2B—Asxvi	25.78 (7)
Rb1Bii—Rb1A—O2iii	37.75 (11)	O1vi—Rb2B—Asxvi	104.6 (2)
O3iii—Rb1A—O2iii	50.13 (4)	O4x—Rb2B—Asxvi	26.18 (6)
O3i—Rb1A—O2iii	125.02 (5)	O1xiii—Rb2B—Asxvi	72.35 (15)
O3iv—Rb1A—O2iii	64.77 (5)	Rb2Bi—Rb2B—Asxv	75.0 (15)
O3v—Rb1A—O2iii	112.03 (5)	Rb2Bii—Rb2B—Asxv	117.0 (13)
O3ii—Rb1A—O2iii	67.27 (5)	O3—Rb2B—Asxv	105.0 (2)
O3—Rb1A—O2iii	120.30 (5)	O3ii—Rb2B—Asxv	174.4 (3)
O2—Rb1A—O2iii	75.50 (6)	O3i—Rb2B—Asxv	110.1 (2)
O2v—Rb1A—O2iii	111.23 (3)	O1viii—Rb2B—Asxv	94.17 (18)
O2iv—Rb1A—O2iii	111.23 (3)	O1vi—Rb2B—Asxv	25.24 (7)
O2ii—Rb1A—O2iii	62.27 (6)	O4x—Rb2B—Asxv	54.35 (12)
Rb1Bi—Rb1A—O2i	86.26 (3)	O1xiii—Rb2B—Asxv	98.42 (18)
Rb1Bii—Rb1A—O2i	148.87 (11)	Asxvi—Rb2B—Asxv	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)
O3iv—Rb1A—O2i	120.30 (5)	O3—Rb2B—As	23.86 (9)
O3v—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)	O1viii—Rb2B—As	71.31 (17)
O2—Rb1A—O2i	111.23 (3)	O1vi—Rb2B—As	100.0 (2)
O2v—Rb1A—O2i	62.27 (6)	O4x—Rb2B—As	107.7 (2)
O2iv—Rb1A—O2i	75.50 (6)	O1xiii—Rb2B—As	24.73 (7)
O2ii—Rb1A—O2i	111.23 (3)	Asxvi—Rb2B—As	96.34 (18)
O2iii—Rb1A—O2i	172.51 (7)	Asxv—Rb2B—As	109.1 (2)
Rb1Bi—Rb1A—Asiii	68.045 (6)	O2xvii—In1—O2ii	92.65 (7)
Rb1Bii—Rb1A—Asiii	62.23 (10)	O2xvii—In1—O2xviii	92.65 (7)
O3iii—Rb1A—Asiii	25.58 (3)	O2ii—In1—O2xviii	92.65 (7)
O3i—Rb1A—Asiii	121.18 (4)	O2xvii—In1—O4xix	91.95 (7)
O3iv—Rb1A—Asiii	68.11 (4)	O2ii—In1—O4xix	173.42 (7)
O3v—Rb1A—Asiii	92.38 (4)	O2xviii—In1—O4xix	91.82 (7)
O3ii—Rb1A—Asiii	83.92 (4)	O2xvii—In1—O4i	91.82 (7)
O3—Rb1A—Asiii	145.24 (3)	O2ii—In1—O4i	91.95 (7)
O2—Rb1A—Asiii	99.68 (3)	O2xviii—In1—O4i	173.42 (7)
O2v—Rb1A—Asiii	86.65 (3)	O4xix—In1—O4i	83.21 (7)
O2iv—Rb1A—Asiii	118.16 (3)	O2xvii—In1—O4xii	173.42 (7)
O2ii—Rb1A—Asiii	57.81 (3)	O2ii—In1—O4xii	91.82 (7)
O2iii—Rb1A—Asiii	25.19 (3)	O2xviii—In1—O4xii	91.95 (7)
O2i—Rb1A—Asiii	148.88 (3)	O4xix—In1—O4xii	83.21 (7)
Rb1Bi—Rb1A—H	127.6 (7)	O4i—In1—O4xii	83.21 (7)
Rb1Bii—Rb1A—H	95.7 (8)	O2xvii—In1—Rb2Axxi	123.37 (5)
O3iii—Rb1A—H	170.2 (6)	O2ii—In1—Rb2Axxi	123.36 (5)
O3i—Rb1A—H	69.0 (7)	O2xviii—In1—Rb2Axxi	123.36 (5)
O3iv—Rb1A—H	103.6 (7)	O4xix—In1—Rb2Axxi	50.06 (5)
O3v—Rb1A—H	103.8 (6)	O4i—In1—Rb2Axxi	50.06 (5)
O3ii—Rb1A—H	82.3 (6)	O4xii—In1—Rb2Axxi	50.06 (5)
O3—Rb1A—H	14.5 (6)	O2xvii—In1—Rb1Axix	32.08 (5)
O2—Rb1A—H	58.6 (7)	O2ii—In1—Rb1Axix	107.92 (5)
O2v—Rb1A—H	115.4 (7)	O2xviii—In1—Rb1Axix	118.90 (5)
O2iv—Rb1A—H	58.4 (6)	O4xix—In1—Rb1Axix	73.96 (4)
O2ii—Rb1A—H	122.5 (6)	O4i—In1—Rb1Axix	63.88 (4)
O2iii—Rb1A—H	132.7 (7)	O4xii—In1—Rb1Axix	141.47 (5)
O2i—Rb1A—H	53.3 (7)	Rb2Axxi—In1—Rb1Axix	91.955 (3)
Asiii—Rb1A—H	157.8 (7)	O2xvii—In1—Rb1A	118.90 (5)
Rb1Bi—Rb1A—Hi	44.8 (6)	O2ii—In1—Rb1A	32.08 (5)
Rb1Bii—Rb1A—Hi	127.6 (8)	O2xviii—In1—Rb1A	107.92 (5)
O3iii—Rb1A—Hi	103.8 (6)	O4xix—In1—Rb1A	141.47 (5)
O3i—Rb1A—Hi	14.5 (6)	O4i—In1—Rb1A	73.96 (4)
O3iv—Rb1A—Hi	170.2 (6)	O4xii—In1—Rb1A	63.88 (5)
O3v—Rb1A—Hi	103.6 (7)	Rb2Axxi—In1—Rb1A	91.954 (3)
O3ii—Rb1A—Hi	69.0 (7)	Rb1Axix—In1—Rb1A	119.9
O3—Rb1A—Hi	82.3 (6)	O2xvii—In1—Rb1Axviii	107.92 (5)
O2—Rb1A—Hi	122.5 (6)	O2ii—In1—Rb1Axviii	118.90 (5)
O2v—Rb1A—Hi	58.4 (6)	O2xviii—In1—Rb1Axviii	32.08 (5)
O2iv—Rb1A—Hi	132.7 (7)	O4xix—In1—Rb1Axviii	63.88 (5)
O2ii—Rb1A—Hi	53.3 (7)	O4i—In1—Rb1Axviii	141.47 (5)
O2iii—Rb1A—Hi	115.4 (7)	O4xii—In1—Rb1Axviii	73.96 (5)
O2i—Rb1A—Hi	58.6 (7)	Rb2Axxi—In1—Rb1Axviii	91.954 (3)
Asiii—Rb1A—Hi	107.6 (7)	Rb1Axix—In1—Rb1Axviii	119.9
H—Rb1A—Hi	83.5 (9)	Rb1A—In1—Rb1Axviii	119.9
Rb1Bi—Rb1A—Hii	95.7 (7)	O1vii—In2—O1xvi	96.52 (7)
Rb1Bii—Rb1A—Hii	44.8 (6)	O1vii—In2—O1i	180.0
O3iii—Rb1A—Hii	103.6 (7)	O1xvi—In2—O1i	83.48 (7)
O3i—Rb1A—Hii	82.3 (6)	O1vii—In2—O1xii	83.48 (7)
O3iv—Rb1A—Hii	103.8 (6)	O1xvi—In2—O1xii	180.0
O3v—Rb1A—Hii	170.2 (6)	O1i—In2—O1xii	96.52 (7)
O3ii—Rb1A—Hii	14.5 (6)	O1vii—In2—O1xix	83.48 (7)
O3—Rb1A—Hii	69.0 (7)	O1xvi—In2—O1xix	83.48 (7)
O2—Rb1A—Hii	53.3 (7)	O1i—In2—O1xix	96.52 (7)
O2v—Rb1A—Hii	132.7 (7)	O1xii—In2—O1xix	96.52 (7)
O2iv—Rb1A—Hii	115.4 (8)	O1vii—In2—O1xx	96.52 (7)
O2ii—Rb1A—Hii	58.6 (7)	O1xvi—In2—O1xx	96.52 (7)
O2iii—Rb1A—Hii	58.4 (6)	O1i—In2—O1xx	83.48 (7)
O2i—Rb1A—Hii	122.5 (6)	O1xii—In2—O1xx	83.48 (7)
Asiii—Rb1A—Hii	78.9 (7)	O1xix—In2—O1xx	180.0
H—Rb1A—Hii	83.5 (9)	O1vii—In2—Rb2Axx	47.93 (8)
Hi—Rb1A—Hii	83.5 (9)	O1xvi—In2—Rb2Axx	80.47 (7)
Rb1Bi—Rb1A—Hiv	127.6 (7)	O1i—In2—Rb2Axx	132.07 (8)
Rb1Bii—Rb1A—Hiv	44.8 (6)	O1xii—In2—Rb2Axx	99.53 (7)
O3iii—Rb1A—Hiv	69.0 (7)	O1xix—In2—Rb2Axx	37.05 (8)
O3i—Rb1A—Hiv	170.2 (6)	O1xx—In2—Rb2Axx	142.95 (8)
O3iv—Rb1A—Hiv	14.5 (6)	O1vii—In2—Rb2Axix	132.07 (8)
O3v—Rb1A—Hiv	82.3 (6)	O1xvi—In2—Rb2Axix	99.53 (7)
O3ii—Rb1A—Hiv	103.8 (6)	O1i—In2—Rb2Axix	47.93 (8)
O3—Rb1A—Hiv	103.6 (7)	O1xii—In2—Rb2Axix	80.47 (7)
O2—Rb1A—Hiv	58.4 (6)	O1xix—In2—Rb2Axix	142.95 (8)
O2v—Rb1A—Hiv	122.5 (6)	O1xx—In2—Rb2Axix	37.05 (8)
O2iv—Rb1A—Hiv	58.6 (7)	Rb2Axx—In2—Rb2Axix	180.0
O2ii—Rb1A—Hiv	115.4 (7)	O1vii—In2—Rb2A	37.05 (8)
O2iii—Rb1A—Hiv	53.3 (7)	O1xvi—In2—Rb2A	132.07 (8)
O2i—Rb1A—Hiv	132.7 (7)	O1i—In2—Rb2A	142.95 (8)
Asiii—Rb1A—Hiv	62.0 (7)	O1xii—In2—Rb2A	47.93 (8)
H—Rb1A—Hiv	104.8 (15)	O1xix—In2—Rb2A	80.47 (7)
Hi—Rb1A—Hiv	168.6 (14)	O1xx—In2—Rb2A	99.53 (7)
Hii—Rb1A—Hiv	89.6 (11)	Rb2Axx—In2—Rb2A	60.060 (6)
Rb1Bi—Rb1A—Hiii	44.8 (6)	Rb2Axix—In2—Rb2A	119.940 (6)
Rb1Bii—Rb1A—Hiii	95.7 (8)	O1vii—In2—Rb2Axviii	99.53 (7)
O3iii—Rb1A—Hiii	14.5 (6)	O1xvi—In2—Rb2Axviii	37.05 (8)
O3i—Rb1A—Hiii	103.8 (6)	O1i—In2—Rb2Axviii	80.47 (7)
O3iv—Rb1A—Hiii	82.3 (6)	O1xii—In2—Rb2Axviii	142.95 (8)
O3v—Rb1A—Hiii	69.0 (7)	O1xix—In2—Rb2Axviii	47.93 (8)
O3ii—Rb1A—Hiii	103.6 (7)	O1xx—In2—Rb2Axviii	132.07 (8)
O3—Rb1A—Hiii	170.2 (6)	Rb2Axx—In2—Rb2Axviii	60.060 (6)
O2—Rb1A—Hiii	132.7 (7)	Rb2Axix—In2—Rb2Axviii	119.940 (7)
O2v—Rb1A—Hiii	53.3 (7)	Rb2A—In2—Rb2Axviii	119.940 (6)
O2iv—Rb1A—Hiii	122.5 (6)	O1vii—In2—Rb2Axxii	80.47 (7)
O2ii—Rb1A—Hiii	58.4 (6)	O1xvi—In2—Rb2Axxii	142.95 (8)
O2iii—Rb1A—Hiii	58.6 (7)	O1i—In2—Rb2Axxii	99.53 (7)
O2i—Rb1A—Hiii	115.4 (7)	O1xii—In2—Rb2Axxii	37.05 (8)
Asiii—Rb1A—Hiii	33.5 (7)	O1xix—In2—Rb2Axxii	132.07 (8)
H—Rb1A—Hiii	168.6 (14)	O1xx—In2—Rb2Axxii	47.93 (8)
Hi—Rb1A—Hiii	89.6 (12)	Rb2Axx—In2—Rb2Axxii	119.940 (6)
Hii—Rb1A—Hiii	104.8 (15)	Rb2Axix—In2—Rb2Axxii	60.060 (6)
Hiv—Rb1A—Hiii	83.5 (9)	Rb2A—In2—Rb2Axxii	60.061 (6)
Rb1Bi—Rb1A—Hv	95.7 (7)	Rb2Axviii—In2—Rb2Axxii	180.0
Rb1Bii—Rb1A—Hv	127.6 (8)	O1vii—In2—Rb2Axxiii	142.95 (8)
O3iii—Rb1A—Hv	82.3 (6)	O1xvi—In2—Rb2Axxiii	47.93 (8)
O3i—Rb1A—Hv	103.6 (7)	O1i—In2—Rb2Axxiii	37.05 (8)
O3iv—Rb1A—Hv	69.0 (7)	O1xii—In2—Rb2Axxiii	132.07 (8)
O3v—Rb1A—Hv	14.5 (6)	O1xix—In2—Rb2Axxiii	99.53 (7)
O3ii—Rb1A—Hv	170.2 (6)	O1xx—In2—Rb2Axxiii	80.47 (7)
O3—Rb1A—Hv	103.8 (6)	Rb2Axx—In2—Rb2Axxiii	119.940 (7)
O2—Rb1A—Hv	115.4 (8)	Rb2Axix—In2—Rb2Axxiii	60.060 (6)
O2v—Rb1A—Hv	58.6 (7)	Rb2A—In2—Rb2Axxiii	180.0
O2iv—Rb1A—Hv	53.3 (7)	Rb2Axviii—In2—Rb2Axxiii	60.061 (6)
O2ii—Rb1A—Hv	132.7 (7)	Rb2Axxii—In2—Rb2Axxiii	119.939 (6)
O2iii—Rb1A—Hv	122.5 (6)	O1xiii—As—O2	116.08 (10)
O2i—Rb1A—Hv	58.4 (6)	O1xiii—As—O4v	109.85 (10)
Asiii—Rb1A—Hv	105.4 (6)	O2—As—O4v	113.73 (8)
H—Rb1A—Hv	89.6 (11)	O1xiii—As—O3	104.27 (10)
Hi—Rb1A—Hv	104.8 (14)	O2—As—O3	104.94 (9)
Hii—Rb1A—Hv	168.6 (15)	O4v—As—O3	106.99 (8)
Hiv—Rb1A—Hv	83.5 (9)	O1xiii—As—Rb1Bii	133.87 (15)
Hiii—Rb1A—Hv	83.5 (9)	O2—As—Rb1Bii	51.9 (5)
Rb1Bi—Rb1B—Rb1Bii	60.00 (3)	O4v—As—Rb1Bii	115.4 (2)
Rb1Bi—Rb1B—O3v	97.5 (5)	O3—As—Rb1Bii	54.3 (4)
Rb1Bii—Rb1B—O3v	123.7 (5)	O1xiii—As—Rb1B	138.5 (3)
Rb1Bi—Rb1B—O3	123.7 (5)	O2—As—Rb1B	62.1 (4)
Rb1Bii—Rb1B—O3	97.5 (6)	O4v—As—Rb1B	107.4 (4)
O3v—Rb1B—O3	133.3 (11)	O3—As—Rb1B	46.49 (19)
Rb1Bi—Rb1B—O2iv	158.5 (3)	Rb1Bii—As—Rb1B	11.6 (9)
Rb1Bii—Rb1B—O2iv	109.8 (5)	O1xiii—As—Rb2Bxxiv	59.16 (16)
O3v—Rb1B—O2iv	71.7 (5)	O2—As—Rb2Bxxiv	175.06 (16)
O3—Rb1B—O2iv	74.5 (5)	O4v—As—Rb2Bxxiv	68.35 (14)
Rb1Bi—Rb1B—O2i	109.8 (4)	O3—As—Rb2Bxxiv	78.23 (14)
Rb1Bii—Rb1B—O2i	158.5 (3)	Rb1Bii—As—Rb2Bxxiv	131.9 (5)
O3v—Rb1B—O2i	74.5 (5)	Rb1B—As—Rb2Bxxiv	122.0 (3)
O3—Rb1B—O2i	71.7 (5)	O1xiii—As—Rb2Bxv	62.57 (15)
O2iv—Rb1B—O2i	85.8 (8)	O2—As—Rb2Bxv	175.80 (17)
Rb1Bi—Rb1B—O3iv	105.8 (5)	O4v—As—Rb2Bxv	70.24 (15)
Rb1Bii—Rb1B—O3iv	68.2 (6)	O3—As—Rb2Bxv	72.08 (14)
O3v—Rb1B—O3iv	71.05 (15)	Rb1Bii—As—Rb2Bxv	125.7 (4)
O3—Rb1B—O3iv	111.7 (3)	Rb1B—As—Rb2Bxv	115.9 (3)
O2iv—Rb1B—O3iv	53.4 (2)	Rb2Bxxiv—As—Rb2Bxv	6.2 (2)
O2i—Rb1B—O3iv	132.8 (9)	O1xiii—As—Rb1A	134.73 (9)
Rb1Bi—Rb1B—O3i	68.2 (5)	O2—As—Rb1A	57.74 (6)
Rb1Bii—Rb1B—O3i	105.8 (5)	O4v—As—Rb1A	112.84 (6)
O3v—Rb1B—O3i	111.7 (3)	O3—As—Rb1A	48.98 (7)
O3—Rb1B—O3i	71.04 (15)	Rb1Bii—As—Rb1A	6.0 (4)
O2iv—Rb1B—O3i	132.8 (9)	Rb1B—As—Rb1A	6.2 (5)
O2i—Rb1B—O3i	53.4 (2)	Rb2Bxxiv—As—Rb1A	126.16 (13)
O3iv—Rb1B—O3i	173.4 (12)	Rb2Bxv—As—Rb1A	119.97 (12)
Rb1Bi—Rb1B—O2	114.7 (5)	O1xiii—As—Rb2Axv	61.31 (9)
Rb1Bii—Rb1B—O2	57.8 (6)	O2—As—Rb2Axv	177.30 (9)
O3v—Rb1B—O2	132.6 (4)	O4v—As—Rb2Axv	68.43 (8)
O3—Rb1B—O2	51.41 (7)	O3—As—Rb2Axv	75.58 (7)
O2iv—Rb1B—O2	65.7 (2)	Rb1Bii—As—Rb2Axv	129.1 (4)
O2i—Rb1B—O2	120.6 (6)	Rb1B—As—Rb2Axv	119.2 (3)
O3iv—Rb1B—O2	67.34 (7)	Rb2Bxxiv—As—Rb2Axv	2.88 (15)
O3i—Rb1B—O2	112.19 (11)	Rb2Bxv—As—Rb2Axv	3.52 (13)
Rb1Bi—Rb1B—O2v	57.8 (5)	Rb1A—As—Rb2Axv	123.340 (18)
Rb1Bii—Rb1B—O2v	114.7 (4)	O1xiii—As—Rb2B	66.15 (14)
O3v—Rb1B—O2v	51.41 (7)	O2—As—Rb2B	104.87 (14)
O3—Rb1B—O2v	132.6 (4)	O4v—As—Rb2B	137.04 (14)
O2iv—Rb1B—O2v	120.6 (6)	O3—As—Rb2B	42.56 (14)
O2i—Rb1B—O2v	65.7 (2)	Rb1Bii—As—Rb2B	74.7 (2)
O3iv—Rb1B—O2v	112.19 (11)	Rb1B—As—Rb2B	74.33 (18)
O3i—Rb1B—O2v	67.34 (7)	Rb2Bxxiv—As—Rb2B	74.78 (3)
O2—Rb1B—O2v	172.4 (11)	Rb2Bxv—As—Rb2B	70.9 (2)
Rb1Bi—Rb1B—O3iii	45.4 (3)	Rb1A—As—Rb2B	72.61 (11)
Rb1Bii—Rb1B—O3iii	61.5 (3)	Rb2Axv—As—Rb2B	73.66 (14)
O3v—Rb1B—O3iii	66.84 (19)	O1xiii—As—Rb2Bxxv	63.55 (13)
O3—Rb1B—O3iii	158.9 (9)	O2—As—Rb2Bxxv	178.70 (16)
O2iv—Rb1B—O3iii	113.43 (5)	O4v—As—Rb2Bxxv	65.54 (13)
O2i—Rb1B—O3iii	126.87 (6)	O3—As—Rb2Bxxv	76.36 (14)
O3iv—Rb1B—O3iii	64.9 (3)	Rb1Bii—As—Rb2Bxxv	129.3 (5)
O3i—Rb1B—O3iii	110.3 (6)	Rb1B—As—Rb2Bxxv	119.0 (4)
O2—Rb1B—O3iii	112.4 (6)	Rb2Bxxiv—As—Rb2Bxxv	4.39 (15)
O2v—Rb1B—O3iii	61.9 (2)	Rb2Bxv—As—Rb2Bxxv	5.30 (19)
Rb1Bi—Rb1B—O3ii	61.5 (3)	Rb1A—As—Rb2Bxxv	123.48 (12)
Rb1Bii—Rb1B—O3ii	45.4 (3)	Rb2Axv—As—Rb2Bxxv	2.94 (15)
O3v—Rb1B—O3ii	158.9 (9)	Rb2B—As—Rb2Bxxv	76.18 (18)
O3—Rb1B—O3ii	66.84 (19)	Asxxvi—O1—In2xxvii	142.20 (12)
O2iv—Rb1B—O3ii	126.87 (6)	Asxxvi—O1—Rb2Bxxviii	95.06 (18)
O2i—Rb1B—O3ii	113.43 (5)	In2xxvii—O1—Rb2Bxxviii	119.53 (18)
O3iv—Rb1B—O3ii	110.3 (6)	Asxxvi—O1—Rb2Bvi	92.19 (16)
O3i—Rb1B—O3ii	64.9 (3)	In2xxvii—O1—Rb2Bvi	123.76 (15)
O2—Rb1B—O3ii	61.9 (2)	Rb2Bxxviii—O1—Rb2Bvi	6.6 (3)
O2v—Rb1B—O3ii	112.4 (6)	Asxxvi—O1—Rb2Avi	93.97 (12)
O3iii—Rb1B—O3ii	94.2 (8)	In2xxvii—O1—Rb2Avi	121.16 (11)
Rb1Bi—Rb1B—H	135.3 (8)	Rb2Bxxviii—O1—Rb2Avi	2.47 (17)
Rb1Bii—Rb1B—H	112.7 (9)	Rb2Bvi—O1—Rb2Avi	4.12 (14)
O3v—Rb1B—H	117.3 (12)	Asxxvi—O1—Rb2Bxxvi	89.12 (16)
O3—Rb1B—H	16.1 (6)	In2xxvii—O1—Rb2Bxxvi	106.82 (16)
O2iv—Rb1B—H	65.2 (9)	Rb2Bxxviii—O1—Rb2Bxxvi	86.07 (7)
O2i—Rb1B—H	59.4 (9)	Rb2Bvi—O1—Rb2Bxxvi	80.1 (2)
O3iv—Rb1B—H	111.3 (10)	Rb2Avi—O1—Rb2Bxxvi	83.83 (15)
O3i—Rb1B—H	73.1 (8)	Asxxvi—O1—Rb2Axxvi	87.55 (12)
O2—Rb1B—H	61.4 (8)	In2xxvii—O1—Rb2Axxvi	107.67 (9)
O2v—Rb1B—H	124.3 (10)	Rb2Bxxviii—O1—Rb2Axxvi	86.97 (17)
O3iii—Rb1B—H	173.7 (9)	Rb2Bvi—O1—Rb2Axxvi	80.92 (17)
O3ii—Rb1B—H	82.4 (6)	Rb2Avi—O1—Rb2Axxvi	84.71 (5)
Rb1Bi—Rb1B—Hv	112.7 (9)	Rb2Bxxvi—O1—Rb2Axxvi	1.7 (2)
Rb1Bii—Rb1B—Hv	135.3 (7)	Asxxvi—O1—Rb2Axxvii	110.41 (11)
O3v—Rb1B—Hv	16.1 (6)	In2xxvii—O1—Rb2Axxvii	74.80 (7)
O3—Rb1B—Hv	117.3 (12)	Rb2Bxxviii—O1—Rb2Axxvii	65.58 (17)
O2iv—Rb1B—Hv	59.4 (9)	Rb2Bvi—O1—Rb2Axxvii	72.13 (14)
O2i—Rb1B—Hv	65.2 (9)	Rb2Avi—O1—Rb2Axxvii	68.03 (4)
O3iv—Rb1B—Hv	73.1 (8)	Rb2Bxxvi—O1—Rb2Axxvii	146.21 (11)
O3i—Rb1B—Hv	111.3 (9)	Rb2Axxvi—O1—Rb2Axxvii	147.76 (12)
O2—Rb1B—Hv	124.3 (11)	As—O2—In1xxix	123.06 (9)
O2v—Rb1B—Hv	61.4 (8)	As—O2—Rb1Bii	102.0 (4)
O3iii—Rb1B—Hv	82.4 (6)	In1xxix—O2—Rb1Bii	124.8 (3)
O3ii—Rb1B—Hv	173.7 (10)	As—O2—Rb1A	97.07 (7)
H—Rb1B—Hv	101.4 (15)	In1xxix—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)	In1xxix—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)	In1xxix—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—O1vi	140 (3)	As—O3—Rb1B	107.13 (15)
Rb2Bi—Rb2A—O1vi	34 (2)	As—O3—Rb2B	113.58 (18)
O3—Rb2A—O1vi	85.60 (6)	Rb1B—O3—Rb2B	107.8 (5)
O3i—Rb2A—O1vi	89.21 (6)	As—O3—Rb2A	117.21 (9)
O3ii—Rb2A—O1vi	151.25 (17)	Rb1B—O3—Rb2A	103.8 (4)
Rb2Bii—Rb2A—O1vii	34 (2)	Rb2B—O3—Rb2A	4.46 (18)
Rb2Bi—Rb2A—O1vii	82 (2)	As—O3—Rb1Bii	98.0 (5)
O3—Rb2A—O1vii	151.25 (17)	Rb1B—O3—Rb1Bii	14.3 (10)
O3i—Rb2A—O1vii	85.60 (6)	Rb2B—O3—Rb1Bii	102.66 (17)
O3ii—Rb2A—O1vii	89.21 (6)	Rb2A—O3—Rb1Bii	99.24 (11)
O1vi—Rb2A—O1vii	108.60 (10)	As—O3—Rb1A	105.44 (8)
Rb2Bii—Rb2A—O1viii	82 (2)	Rb1B—O3—Rb1A	7.6 (6)
Rb2Bi—Rb2A—O1viii	140 (3)	Rb2B—O3—Rb1A	102.30 (16)
O3—Rb2A—O1viii	89.21 (6)	Rb2A—O3—Rb1A	98.50 (9)
O3i—Rb2A—O1viii	151.25 (17)	Rb1Bii—O3—Rb1A	8.2 (6)
O3ii—Rb2A—O1viii	85.60 (6)	As—O3—Rb2Bi	121.23 (19)
O1vi—Rb2A—O1viii	108.60 (10)	Rb1B—O3—Rb2Bi	103.8 (4)
O1vii—Rb2A—O1viii	108.59 (10)	Rb2B—O3—Rb2Bi	7.6 (3)
Rb2Bii—Rb2A—O4ix	98 (3)	Rb2A—O3—Rb2Bi	4.62 (15)
Rb2Bi—Rb2A—O4ix	53 (3)	Rb1Bii—O3—Rb2Bi	100.4 (2)
O3—Rb2A—O4ix	126.63 (6)	Rb1A—O3—Rb2Bi	99.01 (18)
O3i—Rb2A—O4ix	117.83 (6)	As—O3—Rb2Bii	115.94 (17)
O3ii—Rb2A—O4ix	163.52 (11)	Rb1B—O3—Rb2Bii	101.7 (5)
O1vi—Rb2A—O4ix	44.75 (6)	Rb2B—O3—Rb2Bii	6.1 (2)
O1vii—Rb2A—O4ix	77.05 (10)	Rb2A—O3—Rb2Bii	3.2 (2)
O1viii—Rb2A—O4ix	90.14 (12)	Rb1Bii—O3—Rb2Bii	96.67 (18)
Rb2Bii—Rb2A—O4x	86 (3)	Rb1A—O3—Rb2Bii	96.23 (18)
Rb2Bi—Rb2A—O4x	98 (3)	Rb2Bi—O3—Rb2Bii	7.4 (2)
O3—Rb2A—O4x	117.83 (6)	As—O3—Rb1Bi	110.6 (3)
O3i—Rb2A—O4x	163.52 (11)	Rb1B—O3—Rb1Bi	10.9 (8)
O3ii—Rb2A—O4x	126.63 (6)	Rb2B—O3—Rb1Bi	97.1 (4)
O1vi—Rb2A—O4x	77.05 (10)	Rb2A—O3—Rb1Bi	93.2 (4)
O1vii—Rb2A—O4x	90.14 (12)	Rb1Bii—O3—Rb1Bi	12.6 (9)
O1viii—Rb2A—O4x	44.75 (6)	Rb1A—O3—Rb1Bi	6.0 (4)
O4ix—Rb2A—O4x	45.71 (8)	Rb2Bi—O3—Rb1Bi	93.5 (4)
Rb2Bii—Rb2A—O4xi	53 (3)	Rb2Bii—O3—Rb1Bi	91.0 (4)
Rb2Bi—Rb2A—O4xi	86 (3)	As—O3—Rb2Axv	78.72 (7)
O3—Rb2A—O4xi	163.52 (11)	Rb1B—O3—Rb2Axv	159.5 (6)
O3i—Rb2A—O4xi	126.63 (6)	Rb2B—O3—Rb2Axv	86.8 (2)
O3ii—Rb2A—O4xi	117.83 (6)	Rb2A—O3—Rb2Axv	90.14 (5)
O1vi—Rb2A—O4xi	90.14 (12)	Rb1Bii—O3—Rb2Axv	170.52 (10)
O1vii—Rb2A—O4xi	44.75 (6)	Rb1A—O3—Rb2Axv	167.05 (8)
O1viii—Rb2A—O4xi	77.05 (10)	Rb2Bi—O3—Rb2Axv	88.8 (2)
O4ix—Rb2A—O4xi	45.71 (8)	Rb2Bii—O3—Rb2Axv	92.8 (2)
O4x—Rb2A—O4xi	45.71 (8)	Rb1Bi—O3—Rb2Axv	167.03 (11)
Rb2Bii—Rb2A—O1xii	26 (3)	As—O3—H	108 (3)
Rb2Bi—Rb2A—O1xii	117 (2)	Rb1B—O3—H	92 (3)
O3—Rb2A—O1xii	112.37 (15)	Rb2B—O3—H	125 (3)
O3i—Rb2A—O1xii	76.69 (8)	Rb2A—O3—H	124 (3)
O3ii—Rb2A—O1xii	44.11 (5)	Rb1Bii—O3—H	105 (3)
O1vi—Rb2A—O1xii	150.55 (6)	Rb1A—O3—H	99 (3)
O1vii—Rb2A—O1xii	45.46 (6)	Rb2Bi—O3—H	120 (3)
O1viii—Rb2A—O1xii	95.29 (5)	Rb2Bii—O3—H	127 (3)
O4ix—Rb2A—O1xii	120.81 (10)	Rb1Bi—O3—H	100 (3)
O4x—Rb2A—O1xii	111.19 (9)	Rb2Axv—O3—H	68 (3)
O4xi—Rb2A—O1xii	78.40 (6)	Asv—O4—In1xxvii	127.87 (9)
Rb2Bii—Rb2A—O1xiii	117 (2)	Asv—O4—Rb2Bxxx	85.47 (16)
Rb2Bi—Rb2A—O1xiii	126 (2)	In1xxvii—O4—Rb2Bxxx	106.35 (17)
O3—Rb2A—O1xiii	44.11 (5)	Asv—O4—Rb2Axxx	86.47 (7)
O3i—Rb2A—O1xiii	112.37 (15)	In1xxvii—O4—Rb2Axxx	103.30 (7)
O3ii—Rb2A—O1xiii	76.69 (8)	Rb2Bxxx—O4—Rb2Axxx	3.25 (18)
O1vi—Rb2A—O1xiii	95.29 (5)	Asv—O4—Rb1Axxvi	131.05 (7)
O1vii—Rb2A—O1xiii	150.54 (6)	In1xxvii—O4—Rb1Axxvi	90.25 (5)
O1viii—Rb2A—O1xiii	45.46 (6)	Rb2Bxxx—O4—Rb1Axxvi	115.02 (15)
O4ix—Rb2A—O1xiii	111.19 (9)	Rb2Axxx—O4—Rb1Axxvi	116.54 (4)
O4x—Rb2A—O1xiii	78.40 (6)	Asv—O4—Rb1A	48.38 (5)
O4xi—Rb2A—O1xiii	120.81 (10)	In1xxvii—O4—Rb1A	80.54 (5)
O1xii—Rb2A—O1xiii	113.93 (7)	Rb2Bxxx—O4—Rb1A	109.65 (15)
Rb2Bii—Rb2A—O1xiv	126 (2)	Rb2Axxx—O4—Rb1A	108.26 (4)
Rb2Bi—Rb2A—O1xiv	26 (3)	Rb1Axxvi—O4—Rb1A	135.18 (4)

D—H···A	D—H	H···A	D···A	D—H···A
O3—H···O4xxxi	0.83 (3)	1.82 (3)	2.634 (2)	168 (4)

CsIn(HAsO4)2	Dx = 4.291 Mg m−3
Mr = 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

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

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(Fo2) + (0.0234P)2 + 28.1228P] where P = (Fo2 + 2Fc2)/3
S = 1.07	(Δ/σ)max = 0.004
1199 reflections	Δρmax = 2.09 e Å−3
61 parameters	Δρmin = −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)

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.

	x	y	z	Uiso*/Ueq
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)*

	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)

Cs1—O3	3.280 (3)	Cs2—O4xii	3.703 (2)
Cs1—O3i	3.280 (3)	Cs2—O4xiii	3.703 (2)
Cs1—O3ii	3.280 (3)	Cs2—O4xiv	3.703 (2)
Cs1—O3iii	3.280 (3)	Cs2—Asxi	3.8762 (6)
Cs1—O3iv	3.280 (3)	Cs2—Asix	3.8762 (6)
Cs1—O3v	3.280 (3)	Cs2—Asx	3.8762 (6)
Cs1—O2	3.434 (2)	In1—O2xv	2.127 (2)
Cs1—O2ii	3.434 (2)	In1—O2iii	2.127 (2)
Cs1—O2v	3.434 (2)	In1—O2xvi	2.127 (2)
Cs1—O2iii	3.434 (2)	In1—O4xvii	2.150 (2)
Cs1—O2i	3.434 (2)	In1—O4iv	2.150 (2)
Cs1—O2iv	3.434 (2)	In1—O4xviii	2.150 (2)
Cs1—H	3.44 (4)	In2—O1vii	2.133 (2)
Cs1—Hiv	3.44 (4)	In2—O1xi	2.133 (3)
Cs1—Hiii	3.44 (4)	In2—O1xix	2.133 (2)
Cs2—O3iv	3.121 (3)	In2—O1iv	2.133 (2)
Cs2—O3iii	3.121 (2)	In2—O1xviii	2.133 (3)
Cs2—O3	3.121 (3)	In2—O1xvii	2.133 (2)
Cs2—O1vi	3.419 (3)	As—O1xx	1.655 (2)
Cs2—O1vii	3.419 (3)	As—O2	1.671 (2)
Cs2—O1viii	3.419 (3)	As—O4ii	1.679 (2)
Cs2—O3ix	3.698 (3)	As—O3	1.743 (3)
Cs2—O3x	3.698 (3)	O3—H	0.83 (3)
Cs2—O3xi	3.698 (3)
O3—Cs1—O3i	166.65 (9)	O1vi—Cs2—Asxi	102.94 (4)
O3—Cs1—O3ii	119.30 (9)	O1vii—Cs2—Asxi	88.69 (5)
O3i—Cs1—O3ii	69.82 (7)	O1viii—Cs2—Asxi	25.24 (4)
O3—Cs1—O3iii	69.82 (7)	O3ix—Cs2—Asxi	61.32 (4)
O3i—Cs1—O3iii	103.15 (9)	O3x—Cs2—Asxi	94.72 (4)
O3ii—Cs1—O3iii	166.65 (10)	O3xi—Cs2—Asxi	26.48 (4)
O3—Cs1—O3iv	69.82 (7)	O4xii—Cs2—Asxi	70.49 (4)
O3i—Cs1—O3iv	119.30 (10)	O4xiii—Cs2—Asxi	25.47 (3)
O3ii—Cs1—O3iv	103.15 (9)	O4xiv—Cs2—Asxi	53.44 (4)
O3iii—Cs1—O3iv	69.82 (7)	O3iv—Cs2—Asix	107.26 (5)
O3—Cs1—O3v	103.15 (9)	O3iii—Cs2—Asix	174.10 (5)
O3i—Cs1—O3v	69.82 (7)	O3—Cs2—Asix	100.69 (5)
O3ii—Cs1—O3v	69.82 (7)	O1vi—Cs2—Asix	25.24 (4)
O3iii—Cs1—O3v	119.30 (9)	O1vii—Cs2—Asix	102.94 (4)
O3iv—Cs1—O3v	166.65 (9)	O1viii—Cs2—Asix	88.69 (5)
O3—Cs1—O2	47.28 (6)	O3ix—Cs2—Asix	26.48 (4)
O3i—Cs1—O2	119.81 (6)	O3x—Cs2—Asix	61.32 (4)
O3ii—Cs1—O2	126.64 (6)	O3xi—Cs2—Asix	94.72 (4)
O3iii—Cs1—O2	66.62 (6)	O4xii—Cs2—Asix	25.47 (3)
O3iv—Cs1—O2	111.83 (6)	O4xiii—Cs2—Asix	53.44 (4)
O3v—Cs1—O2	67.00 (6)	O4xiv—Cs2—Asix	70.49 (4)
O3—Cs1—O2ii	126.65 (6)	Asxi—Cs2—Asix	78.314 (13)
O3i—Cs1—O2ii	66.61 (6)	O3iv—Cs2—Asx	100.69 (5)
O3ii—Cs1—O2ii	47.28 (6)	O3iii—Cs2—Asx	107.26 (5)
O3iii—Cs1—O2ii	119.81 (6)	O3—Cs2—Asx	174.10 (5)
O3iv—Cs1—O2ii	67.01 (6)	O1vi—Cs2—Asx	88.69 (5)
O3v—Cs1—O2ii	111.83 (6)	O1vii—Cs2—Asx	25.24 (4)
O2—Cs1—O2ii	170.75 (8)	O1viii—Cs2—Asx	102.94 (4)
O3—Cs1—O2v	67.01 (6)	O3ix—Cs2—Asx	94.72 (4)
O3i—Cs1—O2v	111.83 (6)	O3x—Cs2—Asx	26.48 (4)
O3ii—Cs1—O2v	66.61 (6)	O3xi—Cs2—Asx	61.32 (4)
O3iii—Cs1—O2v	126.65 (6)	O4xii—Cs2—Asx	53.44 (4)
O3iv—Cs1—O2v	119.81 (6)	O4xiii—Cs2—Asx	70.49 (4)
O3v—Cs1—O2v	47.28 (6)	O4xiv—Cs2—Asx	25.47 (4)
O2—Cs1—O2v	61.36 (8)	Asxi—Cs2—Asx	78.314 (13)
O2ii—Cs1—O2v	110.71 (3)	Asix—Cs2—Asx	78.314 (13)
O3—Cs1—O2iii	111.83 (6)	O2xv—In1—O2iii	91.11 (9)
O3i—Cs1—O2iii	67.01 (6)	O2xv—In1—O2xvi	91.11 (9)
O3ii—Cs1—O2iii	119.81 (6)	O2iii—In1—O2xvi	91.11 (9)
O3iii—Cs1—O2iii	47.28 (6)	O2xv—In1—O4xvii	92.57 (9)
O3iv—Cs1—O2iii	66.61 (6)	O2iii—In1—O4xvii	175.38 (9)
O3v—Cs1—O2iii	126.65 (6)	O2xvi—In1—O4xvii	91.61 (9)
O2—Cs1—O2iii	110.71 (3)	O2xv—In1—O4iv	91.61 (8)
O2ii—Cs1—O2iii	77.59 (7)	O2iii—In1—O4iv	92.57 (9)
O2v—Cs1—O2iii	170.75 (8)	O2xvi—In1—O4iv	175.38 (9)
O3—Cs1—O2i	119.82 (6)	O4xvii—In1—O4iv	84.54 (9)
O3i—Cs1—O2i	47.28 (6)	O2xv—In1—O4xviii	175.38 (9)
O3ii—Cs1—O2i	111.83 (6)	O2iii—In1—O4xviii	91.61 (9)
O3iii—Cs1—O2i	67.01 (6)	O2xvi—In1—O4xviii	92.57 (9)
O3iv—Cs1—O2i	126.65 (6)	O4xvii—In1—O4xviii	84.54 (9)
O3v—Cs1—O2i	66.61 (6)	O4iv—In1—O4xviii	84.54 (9)
O2—Cs1—O2i	77.59 (7)	O2xv—In1—Cs2xxi	124.48 (6)
O2ii—Cs1—O2i	110.71 (3)	O2iii—In1—Cs2xxi	124.48 (6)
O2v—Cs1—O2i	110.71 (3)	O2xvi—In1—Cs2xxi	124.48 (6)
O2iii—Cs1—O2i	61.36 (8)	O4xvii—In1—Cs2xxi	50.96 (6)
O3—Cs1—O2iv	66.61 (6)	O4iv—In1—Cs2xxi	50.96 (6)
O3i—Cs1—O2iv	126.65 (6)	O4xviii—In1—Cs2xxi	50.96 (6)
O3ii—Cs1—O2iv	67.01 (6)	O1vii—In2—O1xi	94.56 (9)
O3iii—Cs1—O2iv	111.83 (6)	O1vii—In2—O1xix	94.55 (9)
O3iv—Cs1—O2iv	47.28 (6)	O1xi—In2—O1xix	94.55 (9)
O3v—Cs1—O2iv	119.81 (6)	O1vii—In2—O1iv	180.0
O2—Cs1—O2iv	110.71 (3)	O1xi—In2—O1iv	85.45 (9)
O2ii—Cs1—O2iv	61.36 (8)	O1xix—In2—O1iv	85.45 (9)
O2v—Cs1—O2iv	77.59 (7)	O1vii—In2—O1xviii	85.45 (9)
O2iii—Cs1—O2iv	110.71 (3)	O1xi—In2—O1xviii	180.0
O2i—Cs1—O2iv	170.75 (8)	O1xix—In2—O1xviii	85.45 (9)
O3—Cs1—H	13.9 (5)	O1iv—In2—O1xviii	94.55 (9)
O3i—Cs1—H	170.1 (7)	O1vii—In2—O1xvii	85.45 (9)
O3ii—Cs1—H	105.5 (5)	O1xi—In2—O1xvii	85.45 (9)
O3iii—Cs1—H	83.1 (5)	O1xix—In2—O1xvii	180.0
O3iv—Cs1—H	69.8 (6)	O1iv—In2—O1xvii	94.55 (9)
O3v—Cs1—H	100.5 (7)	O1xviii—In2—O1xvii	94.55 (9)
O2—Cs1—H	55.4 (6)	O1vii—In2—Cs2xix	56.94 (8)
O2ii—Cs1—H	117.1 (6)	O1xi—In2—Cs2xix	72.56 (8)
O2v—Cs1—H	58.5 (6)	O1xix—In2—Cs2xix	146.29 (7)
O2iii—Cs1—H	122.2 (6)	O1iv—In2—Cs2xix	123.06 (8)
O2i—Cs1—H	131.7 (6)	O1xviii—In2—Cs2xix	107.44 (8)
O2iv—Cs1—H	55.8 (6)	O1xvii—In2—Cs2xix	33.71 (7)
O3—Cs1—Hiv	83.1 (5)	O1vii—In2—Cs2xvii	123.06 (8)
O3i—Cs1—Hiv	105.5 (6)	O1xi—In2—Cs2xvii	107.44 (8)
O3ii—Cs1—Hiv	100.5 (6)	O1xix—In2—Cs2xvii	33.71 (7)
O3iii—Cs1—Hiv	69.8 (6)	O1iv—In2—Cs2xvii	56.94 (8)
O3iv—Cs1—Hiv	13.9 (5)	O1xviii—In2—Cs2xvii	72.56 (8)
O3v—Cs1—Hiv	170.2 (6)	O1xvii—In2—Cs2xvii	146.29 (7)
O2—Cs1—Hiv	122.2 (6)	Cs2xix—In2—Cs2xvii	180.0
O2ii—Cs1—Hiv	58.5 (6)	O1vii—In2—Cs2	33.71 (7)
O2v—Cs1—Hiv	131.7 (6)	O1xi—In2—Cs2	123.06 (8)
O2iii—Cs1—Hiv	55.8 (6)	O1xix—In2—Cs2	107.44 (8)
O2i—Cs1—Hiv	117.1 (6)	O1iv—In2—Cs2	146.29 (7)
O2iv—Cs1—Hiv	55.4 (6)	O1xviii—In2—Cs2	56.94 (8)
H—Cs1—Hiv	83.7 (8)	O1xvii—In2—Cs2	72.56 (8)
O3—Cs1—Hiii	69.8 (6)	Cs2xix—In2—Cs2	60.0
O3i—Cs1—Hiii	100.5 (6)	Cs2xvii—In2—Cs2	120.0
O3ii—Cs1—Hiii	170.2 (6)	O1vii—In2—Cs2xvi	107.44 (8)
O3iii—Cs1—Hiii	13.9 (5)	O1xi—In2—Cs2xvi	33.71 (7)
O3iv—Cs1—Hiii	83.1 (5)	O1xix—In2—Cs2xvi	123.06 (8)
O3v—Cs1—Hiii	105.5 (5)	O1iv—In2—Cs2xvi	72.56 (8)
O2—Cs1—Hiii	55.8 (6)	O1xviii—In2—Cs2xvi	146.29 (7)
O2ii—Cs1—Hiii	131.7 (6)	O1xvii—In2—Cs2xvi	56.94 (8)
O2v—Cs1—Hiii	117.1 (7)	Cs2xix—In2—Cs2xvi	60.0
O2iii—Cs1—Hiii	55.4 (6)	Cs2xvii—In2—Cs2xvi	120.0
O2i—Cs1—Hiii	58.5 (6)	Cs2—In2—Cs2xvi	120.0
O2iv—Cs1—Hiii	122.2 (6)	O1vii—In2—Cs2xxii	72.56 (8)
H—Cs1—Hiii	83.7 (8)	O1xi—In2—Cs2xxii	146.29 (7)
Hiv—Cs1—Hiii	83.7 (8)	O1xix—In2—Cs2xxii	56.94 (8)
O3iv—Cs2—O3iii	73.97 (8)	O1iv—In2—Cs2xxii	107.44 (8)
O3iv—Cs2—O3	73.97 (8)	O1xviii—In2—Cs2xxii	33.71 (7)
O3iii—Cs2—O3	73.97 (8)	O1xvii—In2—Cs2xxii	123.06 (8)
O3iv—Cs2—O1vi	82.81 (6)	Cs2xix—In2—Cs2xxii	120.0
O3iii—Cs2—O1vi	153.75 (6)	Cs2xvii—In2—Cs2xxii	60.0
O3—Cs2—O1vi	88.16 (7)	Cs2—In2—Cs2xxii	60.0
O3iv—Cs2—O1vii	88.16 (7)	Cs2xvi—In2—Cs2xxii	180.0
O3iii—Cs2—O1vii	82.80 (7)	O1vii—In2—Cs2xxiii	146.29 (7)
O3—Cs2—O1vii	153.75 (7)	O1xi—In2—Cs2xxiii	56.94 (8)
O1vi—Cs2—O1vii	108.90 (4)	O1xix—In2—Cs2xxiii	72.56 (8)
O3iv—Cs2—O1viii	153.75 (7)	O1iv—In2—Cs2xxiii	33.71 (7)
O3iii—Cs2—O1viii	88.16 (7)	O1xviii—In2—Cs2xxiii	123.06 (8)
O3—Cs2—O1viii	82.81 (6)	O1xvii—In2—Cs2xxiii	107.44 (8)
O1vi—Cs2—O1viii	108.90 (4)	Cs2xix—In2—Cs2xxiii	120.0
O1vii—Cs2—O1viii	108.90 (4)	Cs2xvii—In2—Cs2xxiii	60.0
O3iv—Cs2—O3ix	124.57 (9)	Cs2—In2—Cs2xxiii	180.0
O3iii—Cs2—O3ix	148.48 (9)	Cs2xvi—In2—Cs2xxiii	60.0
O3—Cs2—O3ix	86.50 (7)	Cs2xxii—In2—Cs2xxiii	120.0
O1vi—Cs2—O3ix	44.45 (6)	O1xx—As—O2	117.25 (12)
O1vii—Cs2—O3ix	119.69 (6)	O1xx—As—O4ii	108.41 (12)
O1viii—Cs2—O3ix	64.61 (6)	O2—As—O4ii	113.77 (11)
O3iv—Cs2—O3x	86.50 (7)	O1xx—As—O3	105.44 (13)
O3iii—Cs2—O3x	124.56 (9)	O2—As—O3	104.33 (12)
O3—Cs2—O3x	148.48 (8)	O4ii—As—O3	106.72 (11)
O1vi—Cs2—O3x	64.61 (6)	O1xx—As—Cs2ix	61.74 (9)
O1vii—Cs2—O3x	44.45 (6)	O2—As—Cs2ix	174.14 (8)
O1viii—Cs2—O3x	119.69 (6)	O4ii—As—Cs2ix	71.50 (8)
O3ix—Cs2—O3x	84.57 (6)	O3—As—Cs2ix	71.06 (9)
O3iv—Cs2—O3xi	148.48 (9)	O1xx—As—Cs1	139.73 (11)
O3iii—Cs2—O3xi	86.50 (7)	O2—As—Cs1	55.91 (8)
O3—Cs2—O3xi	124.57 (9)	O4ii—As—Cs1	109.82 (8)
O1vi—Cs2—O3xi	119.69 (6)	O3—As—Cs1	51.15 (9)
O1vii—Cs2—O3xi	64.61 (6)	Cs2ix—As—Cs1	120.598 (10)
O1viii—Cs2—O3xi	44.45 (6)	O1xx—As—Cs2	75.26 (11)
O3ix—Cs2—O3xi	84.57 (6)	O2—As—Cs2	99.50 (8)
O3x—Cs2—O3xi	84.57 (6)	O4ii—As—Cs2	138.02 (8)
O3iv—Cs2—O4xii	113.69 (6)	O3—As—Cs2	37.36 (8)
O3iii—Cs2—O4xii	159.43 (6)	Cs2ix—As—Cs2	74.638 (9)
O3—Cs2—O4xii	126.02 (6)	Cs1—As—Cs2	68.078 (14)
O1vi—Cs2—O4xii	44.41 (5)	Asxxiv—O1—In2xxv	140.67 (15)
O1vii—Cs2—O4xii	78.54 (5)	Asxxiv—O1—Cs2vi	93.02 (10)
O1viii—Cs2—O4xii	89.74 (5)	In2xxv—O1—Cs2vi	126.03 (9)
O3ix—Cs2—O4xii	43.56 (5)	Asxxiv—O1—Cs2xxiv	82.42 (10)
O3x—Cs2—O4xii	41.47 (5)	In2xxv—O1—Cs2xxiv	97.96 (9)
O3xi—Cs2—O4xii	77.76 (5)	Cs2vi—O1—Cs2xxiv	80.74 (5)
O3iv—Cs2—O4xiii	159.43 (6)	Asxxiv—O1—Cs2xxv	118.31 (12)
O3iii—Cs2—O4xiii	126.02 (6)	In2xxv—O1—Cs2xxv	82.33 (8)
O3—Cs2—O4xiii	113.70 (7)	Cs2vi—O1—Cs2xxv	72.50 (5)
O1vi—Cs2—O4xiii	78.54 (5)	Cs2xxiv—O1—Cs2xxv	146.39 (6)
O1vii—Cs2—O4xiii	89.74 (6)	As—O2—In1xxvi	122.05 (12)
O1viii—Cs2—O4xiii	44.41 (5)	As—O2—Cs1	100.33 (9)
O3ix—Cs2—O4xiii	41.47 (5)	In1xxvi—O2—Cs1	125.68 (9)
O3x—Cs2—O4xiii	77.76 (5)	As—O2—Cs2	60.78 (7)
O3xi—Cs2—O4xiii	43.56 (5)	In1xxvi—O2—Cs2	162.87 (9)
O4xii—Cs2—O4xiii	45.97 (6)	Cs1—O2—Cs2	66.29 (4)
O3iv—Cs2—O4xiv	126.02 (6)	As—O3—Cs2	122.83 (12)
O3iii—Cs2—O4xiv	113.69 (6)	As—O3—Cs1	104.40 (11)
O3—Cs2—O4xiv	159.43 (6)	Cs2—O3—Cs1	94.64 (7)
O1vi—Cs2—O4xiv	89.74 (5)	As—O3—Cs2ix	82.46 (10)
O1vii—Cs2—O4xiv	44.41 (5)	Cs2—O3—Cs2ix	93.50 (7)
O1viii—Cs2—O4xiv	78.53 (5)	Cs1—O3—Cs2ix	164.05 (8)
O3ix—Cs2—O4xiv	77.76 (5)	As—O3—H	107 (3)
O3x—Cs2—O4xiv	43.56 (5)	Cs2—O3—H	124 (3)
O3xi—Cs2—O4xiv	41.47 (5)	Cs1—O3—H	94 (3)
O4xii—Cs2—O4xiv	45.97 (6)	Cs2ix—O3—H	70 (3)
O4xiii—Cs2—O4xiv	45.97 (6)	Asii—O4—In1xxv	129.32 (12)
O3iv—Cs2—Asxi	174.10 (5)	Asii—O4—Cs2xxvii	83.03 (8)
O3iii—Cs2—Asxi	100.69 (5)	In1xxv—O4—Cs2xxvii	102.24 (8)
O3—Cs2—Asxi	107.26 (5)

D—H···A	D—H	H···A	D···A	D—H···A
O3—H···O4xxviii	0.83 (3)	1.80 (3)	2.621 (3)	170 (4)