Two new Rb–Ga arsenates: RbGa(HAsO4)2 and RbGa2As(HAsO4)6

Schwendtner, K.; Kolitsch, U.

doi:10.1107/S2056989018011180

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Volume 74| Part 9| September 2018| Pages 1244-1249

https://doi.org/10.1107/S2056989018011180

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Two new Rb–Ga arsenates: RbGa(HAsO₄)₂ and RbGa₂As(HAsO₄)₆

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 ^bNaturhistorisches 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 K. Fejfarova, Institute of Biotechnology CAS, Czech Republic (Received 27 June 2018; accepted 6 August 2018; online 14 August 2018)

The crystal structures of hydrothermally synthesized (T = 493 K, 7–9 d) rubidium gallium bis[hydrogenarsenate(V)], RbGa(HAsO₄)₂, and rubidium digallium arsenic(V) hexa[hydrogenarsenate(V)], RbGa₂As(HAsO₄)₆, were solved by single-crystal X-ray diffraction. Both compounds have tetrahedral–octahedral framework topologies. The M⁺ cations are located in channels of the respective framework. RbGa(HAsO₄)₂ crystallizes in the RbFe(HPO₄)₂ structure type (R $[\overline{3}]$ c), while RbGa₂As(HAsO₄)₆ adopts the structure type of RbAl₂As(HAsO₄)₆ (R $[\overline{3}]$ c), which represents a modification of the RbFe(HPO₄)₂ structure type. In this modification, one third of the M³⁺O₆ octahedra are replaced by AsO₆ octahedra, and two thirds of the voids in the structure, which are usually filled by M⁺ cations, remain empty to achieve charge balance.

Keywords: RbGa(HAsO₄)₂; RbGa₂As(HAsO₄)₆; AsO₆; arsenate; hydrogenarsenate; AsO₆ octahedra; crystal structure.

CCDC references: 1860366; 1860365

1. Chemical context

Compounds with mixed tetrahedral–octahedral (T–O) framework structures feature a broad range of different atomic arrangements, resulting in topologies with various interesting properties, such as ion exchange (Masquelier et al., 1996 ) and ion conductivity (Chouchene et al., 2017 ), as well as unusual piezoelectric (Ren et al., 2015 ), magnetic (Ouerfelli et al., 2007 ) or nonlinear optical features (frequency doubling) (Sun et al., 2017 ). In order to further increase the insufficient knowledge about the crystal chemistry and structure types of arsenates, a comprehensive study of the system M⁺–M³⁺–O–(H)–As⁵⁺ (M⁺ = Li, Na, K, Rb, Cs, Ag, Tl, NH₄; M³⁺ = Al, Ga, In, Sc, Fe, Cr, Tl) was undertaken, which led to a large number of new compounds, most of which have been published (Schwendtner & Kolitsch, 2007 , 2017 , 2018a ,b , and references therein).

Among the many different structure types found during our study, one atomic arrangement, i.e. the RbFe(HPO₄)₂ type (Lii & Wu, 1994 ; rhombohedral, R $[\overline{3}]$ c), was found to show a large crystal–chemical flexibility which allows the incorporation of a wide variety of cations. A total of nine representatives of this structure type are presently known among M⁺M³⁺(HTO₄)₂ (T = P, As) compounds containing Rb or Cs as the M⁺ cation and Al, Ga, Fe or In as the M³⁺ cation (Lesage et al., 2007 ; Lii & Wu, 1994; Schwendtner & Kolitsch, 2017, 2018a,b), including RbGa(HPO₄)₂ (Lesage et al., 2007). One of the title compounds, RbGa(HAsO₄)₂, is another new representative of the RbFe(HPO₄)₂ structure type. The second title compound, RbGa₂As(HAsO₄)₆, is the third representative of a recently described variation of the RbFe(HPO₄)₂ type, the RbAl₂As(HAsO₄)₆ type. It also crystallizes in R $[\overline{3}]$ c and up to now members with RbAl and CsFe as M⁺M³⁺ cation combinations are known (Schwendtner & Kolitsch, 2018b). Interestingly, all presently known M⁺M³⁺ combinations adopting this new structure type also have representatives adopting the RbFe(HPO₄)₂ type. It thus seems likely that more of the known RbFe(HPO₄)₂-type arsenates would also adopt the new RbAl₂As(HAsO₄)₆-type atomic arrangement under formally `dry' synthesis conditions (see §3). RbGa₂As(HAsO₄)₆ is a rare example of a compound containing AsO₆ octahedra. Out of all reported arsenates(V), only about 3% contain AsO₆ polyhedra, according to our earlier review paper (Schwendtner & Kolitsch, 2007), which provides an overview of all known compounds containing AsO₆ groups and their bond-length statistics. At present, 37 compounds containing As in an octahedral coordination are known (Schwendtner & Kolitsch, 2018b); RbGa₂As(HAsO₄)₆ represents the 38^th member of this class of compounds. While 12 Rb- and Ga-containing phosphates are contained in the ICSD (FIZ, 2018 ), only one Rb–Ga arsenate, i.e. RbGaF₃(H₂AsO₄) (Marshall et al., 2015 ), is known so far. Since submitting this paper, another paper dealing with isotypic M⁺M³⁺₂As(HAsO₄)₆ compounds (M⁺M³⁺ = TlGa, CsGa, CsAl) has been published (Schwendtner & Kolitsch, 2018c ).

2. Structural commentary

The two title compounds are very closely related to each other and are modifications of a basic tetrahedral–octahedral framework structure featuring interpenetrating channels, which host the M⁺ cations (Fig. 1). The two structure types, first reported for RbFe(HPO₄)₂ (R $[\overline{3}]$ c; Lii & Wu, 1994) and RbAl₂As(HAsO₄)₆ (R $[\overline{3}]$ c; Schwendtner & Kolitsch, 2018b), are also related to the triclinic (NH₄)Fe(HPO₄)₂ type (P $[\overline{1}]$ ; Yakubovich, 1993 ) and the RbAl(HAsO₄)₂ type (R32; Schwendtner & Kolitsch, 2018b). The fundamental building unit in all these structure types contains M³⁺O₆ octahedra which are connected via their six corners to six protonated AsO₄ tetrahedra, thereby forming an M³⁺As₆O₂₄ unit. These units are in turn connected via three corners to other M³⁺O₆ octahedra. The free protonated corner of each AsO₄ tetrahedron forms a hydrogen bond to the neighbouring M³⁺As₆O₂₄ group (Fig. 2). The M³⁺As₆O₂₄ units are arranged in layers perpendicular to the c_hex axis (Fig. 1). The units within these layers are held together by medium–strong hydrogen bonds (Tables 1 and 2). Both title compounds invariably show a very similar crystal habit: strongly pseudohexagonal to pseudo-octahedral (cf. Fig. 3).

Table 1
Hydrogen-bond geometry (Å, °) for RbGa(HAsO₄)₂

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O3—H⋯O4^xxi	0.85 (3)	1.76 (3)	2.598 (2)	168 (4)
Symmetry code: (xxi) $[y, x-1, -z+{\script{3\over 2}}]$ .

Table 2
Hydrogen-bond geometry (Å, °) for RbGa₂As(HAsO₄)₆

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O3—H⋯O4^xiv	0.80 (3)	1.98 (3)	2.7314 (17)	158 (3)
Symmetry code: (xiv) $[y, x-1, -z+{\script{3\over 2}}]$ .

Figure 1
Crystal structure drawings of (a) RbGa₂As(HAsO₄)₆ and (b) RbGa(HAsO₄)₂ in views along the b axis. A part of the GaO₆ octahedra is replaced by AsO₆ octahedra in RbGa₂As(HAsO₄)₆; the corresponding layers (see Figs. 2

and 3

) are compressed along c and the corresponding void remains vacant of Rb atoms.

Figure 2
Crystal structure drawings of (a) RbGa(HAsO₄)₂ and (b) RbGa₂As(HAsO₄)₆ inequal layers, viewed along the c axis. In this layer, the GaO₆ octahedra are replaced by AsO₆ octahedra in RbGa₂As(HAsO₄)₆ (b). Since the unit-cell dimensions in directions a and b are slightly longer in RbGa₂As(HAsO₄)₆ and the AsO₆ octahedra are smaller than the corresponding GaO₆ octahedra, the (Ga/As)As₆O₂₄ units within this layer move further apart – leading to longer D—H⋯A distances and a compressed (along c) void that is too small for Rb atoms (compare Fig. 1

Figure 3
SEM micrograph of the pseudohexagonal tabular crystals of RbGa(HAsO₄)₂.

The new compound RbGa₂As(HAsO₄)₆ could only be grown by `dry' hydrothermal techniques (without the addition of water). The extreme abundance of As during the synthesis and the formation of a melt of arsenic acid promotes the formation of this novel structure type and endorses the octahedral coordination of As. The substitution of one third of all Ga³⁺ cations by As⁵⁺ requires that two thirds of all Rb⁺ cations are omitted to achieve charge balance (compare Figs. 1a, 1b, 2a and 2b). This substitution also has an effect on the unit-cell parameters (Table 3) and the pore diameter. Since GaO₆ is only replaced by AsO₆ in every second layer (perpendicular to the c axis), the a axis must remain long enough to still be able to house the GaO₆ in the layers between. The effect of the smaller AsO₆ octahedra is therefore mainly reflected by a strong compression of about 5% along the c axis, while the a axis becomes even slightly longer compared to RbGa(HAsO₄)₂. Due to the comparatively smaller AsO₆ octahedra, the (Ga/As)As₆O₂₄ units are further apart in RbGa₂As(HAsO₄)₆ and the encased void is compressed along c, making it too small to house Rb⁺ cations (Figs. 1 and 2). This effect is also reflected by the considerably elongated hydrogen bond in RbGa₂As(HAsO₄)₆. While these bonds, which connect neighbouring (Ga/As)As₆O₂₄ groups, are very strong in RbGa(HAsO₄)₂ [D—H⋯A = 2.598 (2) Å], they are much longer in RbGa₂As(HAsO₄)₆ [2.7314 (17) Å; compare Tables 1 and 2]. The second layer, in contrast, remains practically identical in both compounds and contains Rb atoms with a slight positional disorder (Fig. 4). In both compounds, the Rb atoms are 12-coordinated (Figs. 2 and 3), and the average Rb—O bond lengths in RbGa₂As(HAsO₄)₆ (3.433 Å) are longer than the longest average bond length in RbO₁₂ polyhedra of 3.410 Å reported so far (Gagné & Hawthorne, 2016 ), thus leading to rather low bond-valence sums (BVSs; Gagné & Hawthorne, 2015 ) of only 0.59 valence units (v.u.), whereas the corresponding BVSs are 0.82 and 0.84 v.u. for RbGa(HAsO₄)_2. These loose bondings lead to considerable positional disorder of the Rb⁺ cations in these voids, which were modelled with two Rb positions, between 0.41 (2) and 0.42 (4) Å apart. While position Rb1A in the centre of the large framework void in RbGa₂As(HAsO₄)₆ has only 77% occupancy compared to the off-centre position Rb1B (with occupancy 23%), in RbGa(HAsO₄)₂, the central position Rb1A has 91% occupancy. Similar behaviour was observed for the isotypic CsFe and RbAl compounds (Schwendtner & Kolitsch, 2018b), as well as isotypic phosphates (Lesage et al., 2007).

Table 3
Experimental details

	RbGa(HAsO₄)₂	RbGa₂As(HAsO₄)₆
Crystal data
Chemical formula	RbGa(HAsO₄)₂	RbGa₂As(HAsO₄)₆
M_r	435.05	1139.40
Crystal system, space group	Trigonal, R $[\overline{3}]$ c:H	Trigonal, R $[\overline{3}]$ c:H
Temperature (K)	293	293
a, c (Å)	8.385 (1), 53.880 (11)	8.491 (1), 50.697 (11)
V (Å³)	3280.7 (10)	3165.4 (10)
Z	18	6
Radiation type	Mo Kα	Mo Kα
μ (mm⁻¹)	19.42	15.85
Crystal size (mm)	0.07 × 0.07 × 0.02	0.13 × 0.12 × 0.12

Data collection
Diffractometer	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)
T_min, T_max	0.343, 0.697	0.232, 0.252
No. of measured, independent and observed [I > 2σ(I)] reflections	3896, 1079, 1027	4684, 1287, 1196
R_int	0.016	0.016
(sin θ/λ)_max (Å⁻¹)	0.704	0.757

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.016, 0.040, 1.11	0.014, 0.034, 1.13
No. of reflections	1079	1287
No. of parameters	68	65
No. of restraints	2	2
H-atom treatment	All H-atom parameters refined	All H-atom parameters refined
Δρ_max, Δρ_min (e Å⁻³)	0.79, −0.53	0.75, −0.84
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 ).

Figure 4
Crystal structure drawing of (a) RbGa(HAsO₄)₂ and (b) RbGa₂As(HAsO₄)₆ equal layers, viewed along the a axis. In these topologically equivalent layers, there are no visible differences between the two structure types apart from very minor changes in the hydrogen-bond geometries. The Rb atoms in both compounds show a slight positional disorder and are 12-coordinated.

A further indirect effect of the substituting AsO₆ octahedra is a distinct change in the As—O distances of the AsO₄ tetrahedra. The average As—O distance in the protonated AsO₄ tetrahedra, with values between 1.688 and 1.689 Å, is in both compounds very close to the statistical average of 1.686 (10) Å (Schwendtner, 2008 ). Also the BVSs (Gagné & Hawthorne, 2015) are close to ideal values (4.98–5.00 v.u.). In RbGa(HAsO₄)₂, the HAsO₄ tetrahedra show a typical distortion, with three short As—O distances to attached GaO₆ octahedra and one elongated As—O bond length for the protonated O atom involved in the O—H bond. That bond length (Table 4) in RbGa(HAsO₄)₂ is slightly longer [1.7417 (17) Å] than the average distance of As—O⋯H bonds in HAsO₄ groups [1.72 (3) Å; Schwendtner, 2008]. In contrast, RbGa₂As(HAsO₄)₆ has two short ^[4]As—O bond lengths to neighbouring GaO₆ octahedra, but the ^[4]As—O bond length of the O atom shared with the AsO₆ octahedra is also elongated [1.7100 (11) Å] due to ^[4]As—O—^[6]As repulsion. The ^[4]As—OH bond is therefore shortened to 1.7122 (13) Å (Table 5). The average As—O distances in the AsO₆ octahedra are the shortest average distances of AsO₆ octahedra found so far, i.e. 1.807 Å, leading to rather high BVSs of 5.33 v.u. (after Gagné & Hawthorne, 2015). The grand mean As—O bond distance in AsO₆ octahedra in inorganic compounds is 1.830 (2) Å according to Schwendtner & Kolitsch (2007a); this value was determined on 33 AsO₆ octahedra of 31 compounds. Gagné & Hawthorne (2018 ) determined an identical, but less precise, value of 1.830 (28) Å, based on only 13 AsO₆ octahedra in AsO₆-containing compounds meeting all selection criteria as defined in Gagné & Hawthorne (2016). However, a larger number of compounds meeting these criteria were not used by Gagné & Hawthorne (2018) for unknown reasons. The average Ga—O bond lengths of the octahedrally coordinated Ga cations (1.962–1.964 Å) are slightly shorter than the grand mean average of 1.978 (17) Å (Gagné & Hawthorne, 2018), explaining the corresponding BVSs of 3.10 to 3.11 v.u.

Table 4
Selected bond lengths (Å) for RbGa(HAsO₄)₂

Rb1A—O3ⁱ	3.197 (2)	Rb2—O4^xi	3.4960 (16)
Rb1A—O3ⁱⁱ	3.197 (2)	Rb2—O3^xii	3.5327 (19)
Rb1A—O3ⁱⁱⁱ	3.197 (2)	Rb2—O3^xiii	3.533 (2)
Rb1A—O3^iv	3.197 (2)	Rb2—O3^xiv	3.5328 (19)
Rb1A—O3^v	3.197 (2)	Ga1—O2^xv	1.9596 (14)
Rb1A—O3	3.197 (2)	Ga1—O2ⁱⁱⁱ	1.9597 (15)
Rb1A—O2ⁱⁱ	3.3698 (16)	Ga1—O2^xvi	1.9597 (15)
Rb1A—O2ⁱⁱⁱ	3.3698 (16)	Ga1—O4^xvii	1.9690 (15)
Rb1A—O2^v	3.3699 (16)	Ga1—O4^iv	1.9690 (15)
Rb1A—O2	3.3699 (16)	Ga1—O4^xviii	1.9690 (15)
Rb1A—O2ⁱ	3.3699 (15)	Ga2—O1^viii	1.9625 (15)
Rb1A—O2^iv	3.3699 (15)	Ga2—O1^xiv	1.9625 (16)
Rb2—O3	2.9346 (17)	Ga2—O1^xix	1.9625 (15)
Rb2—O3^iv	2.9347 (17)	Ga2—O1^iv	1.9626 (15)
Rb2—O3ⁱⁱⁱ	2.9347 (17)	Ga2—O1^xviii	1.9626 (16)
Rb2—O1^vi	3.3714 (16)	Ga2—O1^xvii	1.9626 (15)
Rb2—O1^vii	3.3715 (16)	As—O1^xx	1.6576 (15)
Rb2—O1^viii	3.3715 (17)	As—O2	1.6724 (15)
Rb2—O4^ix	3.4960 (16)	As—O4ⁱⁱ	1.6805 (15)
Rb2—O4^x	3.4960 (17)	As—O3	1.7417 (17)
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) $[x-y-{\script{4\over 3}}, x-{\script{2\over 3}}, -z+{\script{4\over 3}}]$ ; (viii) $[y+{\script{2\over 3}}, -x+y+{\script{4\over 3}}, -z+{\script{4\over 3}}]$ ; (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) $[-x-{\script{1\over 3}}, -y-{\script{2\over 3}}, -z+{\script{4\over 3}}]$ ; (xiii) $[y+{\script{2\over 3}}, -x+y+{\script{1\over 3}}, -z+{\script{4\over 3}}]$ ; (xiv) $[x-y-{\script{1\over 3}}, x+{\script{1\over 3}}, -z+{\script{4\over 3}}]$ ; (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) $[-x+{\script{2\over 3}}, -y+{\script{1\over 3}}, -z+{\script{4\over 3}}]$ ; (xx) x-1, y, z.

Table 5
Selected bond lengths (Å) for RbGa₂As(HAsO₄)₆

Rb1A—O3ⁱ	3.4212 (16)	Ga1—O4^vii	1.9623 (11)
Rb1A—O3ⁱⁱ	3.4212 (16)	Ga1—O2^viii	1.9625 (11)
Rb1A—O3ⁱⁱⁱ	3.4212 (15)	Ga1—O2ⁱⁱⁱ	1.9625 (11)
Rb1A—O3^iv	3.4212 (16)	Ga1—O2^ix	1.9625 (11)
Rb1A—O3^v	3.4212 (15)	As1—O1^x	1.8067 (11)
Rb1A—O3	3.4213 (16)	As1—O1^xi	1.8068 (11)
Rb1A—O2ⁱⁱ	3.4438 (12)	As1—O1^xii	1.8068 (11)
Rb1A—O2ⁱⁱⁱ	3.4438 (12)	As1—O1^v	1.8068 (11)
Rb1A—O2	3.4438 (12)	As1—O1^vii	1.8068 (11)
Rb1A—O2^iv	3.4438 (12)	As1—O1^vi	1.8068 (11)
Rb1A—O2ⁱ	3.4438 (12)	As2—O2	1.6658 (11)
Rb1A—O2^v	3.4438 (12)	As2—O4ⁱⁱ	1.6670 (11)
Ga1—O4^vi	1.9623 (12)	As2—O1^xiii	1.7100 (11)
Ga1—O4^v	1.9623 (11)	As2—O3	1.7122 (13)
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) $[y, x, -z+{\script{3\over 2}}]$ ; (v) -y, x-y, z; (vi) x, y+1, z; (vii) -x+y+1, -x+1, z; (viii) -y, x-y+1, z; (ix) x+1, y+1, z; (x) $[x-y-{\script{1\over 3}}, x+{\script{1\over 3}}, -z+{\script{4\over 3}}]$ ; (xi) $[y+{\script{2\over 3}}, -x+y+{\script{4\over 3}}, -z+{\script{4\over 3}}]$ ; (xii) $[-x+{\script{2\over 3}}, -y+{\script{1\over 3}}, -z+{\script{4\over 3}}]$ ; (xiii) x-1, y, z.

3. Synthesis and crystallization

The compounds were grown by hydrothermal synthesis at 493 K (7 d, autogeneous pressure, slow furnace cooling) using Teflon-lined stainless steel autoclaves with an approximate filling volume of 2 ml. Reagent-grade Rb₂CO₃, Ga₂O₃ and H₃AsO₄·0.5H₂O were used as starting reagents in approximate volume ratios of Rb:Ga:As of 1:1:3 for both synthesis batches. For RbGa(HAsO₄)₂ the vessels were filled with distilled water to about 70% of their inner volumes, which led to initial and final pH values of 1.5. The reaction product was washed thoroughly with distilled water, filtered and dried at room temperature. RbGa(HAsO₄)₂ formed colourless pseudohexagonal platelets (Fig. 3) and is stable in air.

For RbGa₂As(HAsO₄)₆, which contains As in both tetrahedral and octahedral coordination, no additional water was added and arsenic acid was present in excess to promote the growth of crystals from a melt or even vapour of arsenic acid under extremely acidic conditions. RbGa₂As(HAsO₄)₆ formed large colourless pseudo-octahedral crystals accompanied by small colourless twinned crystals of RbH₃As₄O₁₂ (Schwendtner & Kolitsch, 2007). The crystals of RbGa₂As(HAsO₄)₆ were extracted mechanically and not further washed; they are hygroscopic and decompose slowly over a period of several years to an amorphous gel and a new, strongly protonated diarsenate containing Rb and Ga (P321, publication in preparation). This slow partial alteration is illustrated in an X-ray powder diffraction pattern (Fig. 5).

Figure 5
Graph of the Rietveld refinement (TOPAS; Bruker, 2009

) of RbGa₂As(HAsO₄)₆, showing the partial alteration of the pseudo-octahedral crystals after an 11-year storage in air. The crystals were hygroscopic and had partly transformed to an amorphous mass. The presence of the relics of the unaltered primary crystals are still visible (pink curve), but a newly crystallized overgrowth of extremely fine fibrous crystals could be attributed to a new strongly protonated Rb–Ga diarsenate with space group P321 (dark-red curve), which will be the subject of a future publication.

A measured X-ray powder diffraction diagram of RbGa(HAsO₄)₂ was deposited at the International Centre for Diffraction Data under PDF number 00-057-0239 (Wohlschlaeger et al., 2006 ).

4. Experimental and refinement

Crystal data, data collection and structure refinement are given in Table 3. For the refinement of RbGa(HAsO₄)₂, the coordinates of RbFe(HPO₄)₂ (Lii & Wu, 1994) were used for the final refinement steps. H atoms were then located from difference Fourier maps and added to the model. For the refinement of RbGa₂As(HAsO₄)₆, the model for RbAl₂As(HAsO₄)₆ (Schwendtner & Kolitsch, 2018b) was used as a starting point. In both compounds, O—H bonds were restrained to 0.9±0.04 Å. During the last refinement steps, residual electron-density peaks of up to 3.83 and 1.16 e Å⁻³ were located 0.63 and 0.68 Å from the Rb sites in RbGa₂As(HAsO₄)₆ and RbGa(HAsO₄)₂, respectively, suggesting irregular displacement parameters and split positions, similar to what was found for RbFe(HPO₄)₂-type RbAl(HPO₄)₂ (Lesage et al., 2007). Therefore, a further position, Rb1B, was included in both refinements, which refined to low occupancies and led to considerable decreases in the R factors and weight parameters for both compounds. The bulk occupancies of Rb1A + Rb1B were constrained to give a total occupancy of 1.00. The final residual electron densities in both compounds are < 1 e Å⁻³.

Supporting information

CCDC references: 1860366; 1860365

Crystal structure: contains datablocks RbGa2AsHAsO46, RbGaHAsO42, global. DOI: https://doi.org/10.1107/S2056989018011180/ff2155sup1.cif

Structure factors: contains datablock RbGa2AsHAsO46. DOI: https://doi.org/10.1107/S2056989018011180/ff2155RbGa2AsHAsO46sup2.hkl

Structure factors: contains datablock RbGaHAsO42. DOI: https://doi.org/10.1107/S2056989018011180/ff2155RbGaHAsO42sup3.hkl

checkCIF report

Computing details top

For both 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) for RbGa2AsHAsO46.

Rubidium digallium arsenic(V) hexakis[hydrogen arsenate(V)] (RbGa2AsHAsO46) top

Crystal data top

RbGa₂As(HAsO₄)₆	D_x = 3.586 Mg m⁻³
M_r = 1139.40	Mo Kα radiation, λ = 0.71073 Å
Trigonal, R3c:H	Cell parameters from 2570 reflections
a = 8.491 (1) Å	θ = 2.0–32.6°
c = 50.697 (11) Å	µ = 15.85 mm⁻¹
V = 3165.4 (10) Å³	T = 293 K
Z = 6	Large pseudo-octahedra, colourless
F(000) = 3168	0.13 × 0.12 × 0.12 mm

Data collection top

Nonius KappaCCD single-crystal four-circle diffractometer	1196 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	R_int = 0.016
φ and ω scans	θ_max = 32.5°, θ_min = 2.4°
Absorption correction: multi-scan (SCALEPACK; Otwinowski et al., 2003)	h = −12→12
T_min = 0.232, T_max = 0.252	k = −10→10
4684 measured reflections	l = −75→76
1287 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)] = 0.014	All H-atom parameters refined
wR(F²) = 0.034	w = 1/[σ²(F_o²) + (0.0136P)² + 10.4877P] where P = (F_o² + 2F_c²)/3
S = 1.13	(Δ/σ)_max = 0.008
1287 reflections	Δρ_max = 0.75 e Å⁻³
65 parameters	Δρ_min = −0.83 e Å⁻³
2 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: 0.000271 (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)
Rb1A	0.000000	0.000000	0.750000	0.055 (3)	0.669 (3)
Rb1B	0.000000	−0.048 (2)	0.750000	0.0359 (11)	0.1103 (9)
Ga1	0.333333	0.666667	0.75604 (2)	0.00736 (6)
As1	0.333333	0.666667	0.666667	0.00627 (7)
As2	−0.44400 (2)	−0.40772 (2)	0.71144 (2)	0.00735 (5)
O1	0.40249 (16)	−0.46597 (15)	0.68629 (2)	0.01016 (19)
O2	−0.45254 (15)	−0.27043 (15)	0.73416 (2)	0.01025 (19)
O3	−0.22887 (17)	−0.28592 (18)	0.69874 (3)	0.0194 (3)
O4	0.48817 (15)	−0.12495 (15)	0.77869 (2)	0.0108 (2)
H	−0.176 (4)	−0.337 (4)	0.7027 (6)	0.046 (9)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Rb1A	0.050 (4)	0.050 (4)	0.066 (2)	0.0251 (18)	0.000	0.000
Rb1B	0.024 (4)	0.034 (4)	0.046 (4)	0.012 (2)	0.0044 (14)	0.0022 (7)
Ga1	0.00807 (8)	0.00807 (8)	0.00596 (12)	0.00403 (4)	0.000	0.000
As1	0.00747 (10)	0.00747 (10)	0.00389 (14)	0.00373 (5)	0.000	0.000
As2	0.00844 (7)	0.00803 (7)	0.00670 (7)	0.00495 (5)	0.00010 (5)	0.00053 (5)
O1	0.0138 (5)	0.0110 (5)	0.0078 (4)	0.0077 (4)	−0.0031 (4)	0.0000 (4)
O2	0.0109 (5)	0.0099 (5)	0.0098 (5)	0.0051 (4)	0.0005 (4)	−0.0022 (4)
O3	0.0121 (5)	0.0203 (6)	0.0264 (7)	0.0084 (5)	0.0076 (5)	0.0075 (5)
O4	0.0124 (5)	0.0095 (5)	0.0125 (5)	0.0070 (4)	−0.0030 (4)	−0.0042 (4)

Geometric parameters (Å, º) top

Rb1A—Rb1Bⁱ	0.41 (2)	Rb1B—O2	3.4234 (12)
Rb1A—Rb1Bⁱⁱ	0.41 (2)	Rb1B—O2^iv	3.4234 (12)
Rb1A—O3ⁱⁱⁱ	3.4212 (16)	Rb1B—O3ⁱⁱⁱ	3.694 (14)
Rb1A—O3^iv	3.4212 (16)	Rb1B—O3ⁱⁱ	3.694 (14)
Rb1A—O3ⁱⁱ	3.4212 (15)	Rb1B—O2ⁱⁱ	3.810 (18)
Rb1A—O3^v	3.4212 (16)	Rb1B—O2ⁱⁱⁱ	3.810 (18)
Rb1A—O3ⁱ	3.4212 (15)	Rb1B—O4^vi	3.819 (18)
Rb1A—O3	3.4213 (16)	Rb1B—O4^vii	3.819 (18)
Rb1A—O2^iv	3.4438 (12)	Rb1B—As2^v	3.934 (8)
Rb1A—O2ⁱⁱ	3.4438 (12)	Rb1B—As2ⁱ	3.934 (8)
Rb1A—O2	3.4438 (12)	Ga1—O4^viii	1.9623 (12)
Rb1A—O2^v	3.4438 (12)	Ga1—O4ⁱ	1.9623 (11)
Rb1A—O2ⁱⁱⁱ	3.4438 (12)	Ga1—O4^ix	1.9623 (11)
Rb1A—O2ⁱ	3.4438 (12)	Ga1—O2^x	1.9625 (11)
Rb1A—As2^iv	4.1192 (5)	Ga1—O2ⁱⁱ	1.9625 (11)
Rb1A—As2ⁱⁱⁱ	4.1192 (5)	Ga1—O2^xi	1.9625 (11)
Rb1A—As2^v	4.1192 (5)	As1—O1^xii	1.8067 (11)
Rb1A—As2ⁱⁱ	4.1192 (4)	As1—O1^xiii	1.8068 (11)
Rb1B—Rb1Bⁱ	0.70 (3)	As1—O1^xiv	1.8068 (11)
Rb1B—Rb1Bⁱⁱ	0.70 (3)	As1—O1ⁱ	1.8068 (11)
Rb1B—O2^v	3.136 (14)	As1—O1^ix	1.8068 (11)
Rb1B—O2ⁱ	3.136 (14)	As1—O1^viii	1.8068 (11)
Rb1B—O3^iv	3.269 (6)	As2—O2	1.6658 (11)
Rb1B—O3	3.269 (6)	As2—O4^iv	1.6670 (11)
Rb1B—O3^v	3.358 (2)	As2—O1^xv	1.7100 (11)
Rb1B—O3ⁱ	3.358 (2)	As2—O3	1.7122 (13)

Rb1Bⁱ—Rb1A—Rb1Bⁱⁱ	120.00 (7)	Rb1Bⁱⁱ—Rb1B—O4^vii	153.31 (7)
Rb1Bⁱ—Rb1A—O3ⁱⁱⁱ	64.81 (2)	O2^v—Rb1B—O4^vii	53.4 (3)
Rb1Bⁱⁱ—Rb1A—O3ⁱⁱⁱ	77.69 (5)	O2ⁱ—Rb1B—O4^vii	45.1 (2)
Rb1Bⁱ—Rb1A—O3^iv	77.69 (2)	O3^iv—Rb1B—O4^vii	44.49 (19)
Rb1Bⁱⁱ—Rb1A—O3^iv	129.70 (3)	O3—Rb1B—O4^vii	98.0 (5)
O3ⁱⁱⁱ—Rb1A—O3^iv	68.57 (4)	O3^v—Rb1B—O4^vii	76.7 (3)
Rb1Bⁱ—Rb1A—O3ⁱⁱ	77.69 (2)	O3ⁱ—Rb1B—O4^vii	93.3 (3)
Rb1Bⁱⁱ—Rb1A—O3ⁱⁱ	64.81 (5)	O2—Rb1B—O4^vii	109.4 (4)
O3ⁱⁱⁱ—Rb1A—O3ⁱⁱ	100.59 (5)	O2^iv—Rb1B—O4^vii	71.6 (2)
O3^iv—Rb1A—O3ⁱⁱ	155.38 (5)	O3ⁱⁱⁱ—Rb1B—O4^vii	109.34 (9)
Rb1Bⁱ—Rb1A—O3^v	129.70 (2)	O3ⁱⁱ—Rb1B—O4^vii	157.2 (3)
Rb1Bⁱⁱ—Rb1A—O3^v	64.81 (5)	O2ⁱⁱ—Rb1B—O4^vii	144.11 (3)
O3ⁱⁱⁱ—Rb1A—O3^v	68.57 (4)	O2ⁱⁱⁱ—Rb1B—O4^vii	144.95 (3)
O3^iv—Rb1A—O3^v	68.57 (4)	O4^vi—Rb1B—O4^vii	53.5 (3)
O3ⁱⁱ—Rb1A—O3^v	129.62 (5)	Rb1Bⁱ—Rb1B—As2^v	137.8 (2)
Rb1Bⁱ—Rb1A—O3ⁱ	64.81 (2)	Rb1Bⁱⁱ—Rb1B—As2^v	88.8 (3)
Rb1Bⁱⁱ—Rb1A—O3ⁱ	129.70 (3)	O2^v—Rb1B—As2^v	24.03 (3)
O3ⁱⁱⁱ—Rb1A—O3ⁱ	129.62 (5)	O2ⁱ—Rb1B—As2^v	107.9 (5)
O3^iv—Rb1A—O3ⁱ	100.59 (5)	O3^iv—Rb1B—As2^v	82.2 (2)
O3ⁱⁱ—Rb1A—O3ⁱ	68.57 (4)	O3—Rb1B—As2^v	82.5 (2)
O3^v—Rb1A—O3ⁱ	155.38 (4)	O3^v—Rb1B—As2^v	25.63 (7)
Rb1Bⁱ—Rb1A—O3	129.70 (2)	O3ⁱ—Rb1B—As2^v	145.3 (5)
Rb1Bⁱⁱ—Rb1A—O3	77.69 (5)	O2—Rb1B—As2^v	51.65 (8)
O3ⁱⁱⁱ—Rb1A—O3	155.38 (4)	O2^iv—Rb1B—As2^v	128.9 (3)
O3^iv—Rb1A—O3	129.62 (5)	O3ⁱⁱⁱ—Rb1B—As2^v	91.62 (8)
O3ⁱⁱ—Rb1A—O3	68.57 (4)	O3ⁱⁱ—Rb1B—As2^v	123.66 (15)
O3^v—Rb1A—O3	100.59 (5)	O2ⁱⁱ—Rb1B—As2^v	138.7 (4)
O3ⁱ—Rb1A—O3	68.57 (4)	O2ⁱⁱⁱ—Rb1B—As2^v	90.34 (14)
Rb1Bⁱ—Rb1A—O2^iv	38.519 (18)	O4^vi—Rb1B—As2^v	68.6 (3)
Rb1Bⁱⁱ—Rb1A—O2^iv	153.03 (7)	O4^vii—Rb1B—As2^v	67.9 (3)
O3ⁱⁱⁱ—Rb1A—O2^iv	76.93 (3)	Rb1Bⁱ—Rb1B—As2ⁱ	88.8 (2)
O3^iv—Rb1A—O2^iv	45.66 (3)	Rb1Bⁱⁱ—Rb1B—As2ⁱ	137.8 (2)
O3ⁱⁱ—Rb1A—O2^iv	111.42 (3)	O2^v—Rb1B—As2ⁱ	107.9 (5)
O3^v—Rb1A—O2^iv	113.17 (3)	O2ⁱ—Rb1B—As2ⁱ	24.03 (3)
O3ⁱ—Rb1A—O2^iv	63.90 (3)	O3^iv—Rb1B—As2ⁱ	82.5 (2)
O3—Rb1A—O2^iv	127.31 (3)	O3—Rb1B—As2ⁱ	82.2 (2)
Rb1Bⁱ—Rb1A—O2ⁱⁱ	38.519 (18)	O3^v—Rb1B—As2ⁱ	145.3 (5)
Rb1Bⁱⁱ—Rb1A—O2ⁱⁱ	83.75 (7)	O3ⁱ—Rb1B—As2ⁱ	25.63 (7)
O3ⁱⁱⁱ—Rb1A—O2ⁱⁱ	63.90 (3)	O2—Rb1B—As2ⁱ	128.9 (3)
O3^iv—Rb1A—O2ⁱⁱ	111.42 (3)	O2^iv—Rb1B—As2ⁱ	51.65 (8)
O3ⁱⁱ—Rb1A—O2ⁱⁱ	45.66 (3)	O3ⁱⁱⁱ—Rb1B—As2ⁱ	123.66 (15)
O3^v—Rb1A—O2ⁱⁱ	127.31 (3)	O3ⁱⁱ—Rb1B—As2ⁱ	91.62 (8)
O3ⁱ—Rb1A—O2ⁱⁱ	76.93 (3)	O2ⁱⁱ—Rb1B—As2ⁱ	90.34 (14)
O3—Rb1A—O2ⁱⁱ	113.17 (3)	O2ⁱⁱⁱ—Rb1B—As2ⁱ	138.7 (4)
O2^iv—Rb1A—O2ⁱⁱ	77.04 (4)	O4^vi—Rb1B—As2ⁱ	67.9 (3)
Rb1Bⁱ—Rb1A—O2	153.035 (19)	O4^vii—Rb1B—As2ⁱ	68.6 (3)
Rb1Bⁱⁱ—Rb1A—O2	38.52 (7)	As2^v—Rb1B—As2ⁱ	131.0 (5)
O3ⁱⁱⁱ—Rb1A—O2	111.42 (3)	O4^viii—Ga1—O4ⁱ	89.24 (5)
O3^iv—Rb1A—O2	127.31 (3)	O4^viii—Ga1—O4^ix	89.24 (5)
O3ⁱⁱ—Rb1A—O2	76.93 (3)	O4ⁱ—Ga1—O4^ix	89.24 (5)
O3^v—Rb1A—O2	63.90 (3)	O4^viii—Ga1—O2^x	91.13 (5)
O3ⁱ—Rb1A—O2	113.17 (3)	O4ⁱ—Ga1—O2^x	88.49 (5)
O3—Rb1A—O2	45.67 (3)	O4^ix—Ga1—O2^x	177.69 (5)
O2^iv—Rb1A—O2	167.50 (4)	O4^viii—Ga1—O2ⁱⁱ	177.69 (5)
O2ⁱⁱ—Rb1A—O2	114.733 (13)	O4ⁱ—Ga1—O2ⁱⁱ	91.13 (5)
Rb1Bⁱ—Rb1A—O2^v	153.03 (2)	O4^ix—Ga1—O2ⁱⁱ	88.48 (5)
Rb1Bⁱⁱ—Rb1A—O2^v	83.75 (8)	O2^x—Ga1—O2ⁱⁱ	91.17 (5)
O3ⁱⁱⁱ—Rb1A—O2^v	113.17 (3)	O4^viii—Ga1—O2^xi	88.48 (5)
O3^iv—Rb1A—O2^v	76.93 (3)	O4ⁱ—Ga1—O2^xi	177.69 (5)
O3ⁱⁱ—Rb1A—O2^v	127.31 (3)	O4^ix—Ga1—O2^xi	91.12 (5)
O3^v—Rb1A—O2^v	45.66 (3)	O2^x—Ga1—O2^xi	91.16 (5)
O3ⁱ—Rb1A—O2^v	111.42 (3)	O2ⁱⁱ—Ga1—O2^xi	91.16 (5)
O3—Rb1A—O2^v	63.91 (3)	O4^viii—Ga1—Rb1B^viii	82.77 (12)
O2^iv—Rb1A—O2^v	114.733 (13)	O4ⁱ—Ga1—Rb1B^viii	55.65 (8)
O2ⁱⁱ—Rb1A—O2^v	167.50 (4)	O4^ix—Ga1—Rb1B^viii	143.89 (7)
O2—Rb1A—O2^v	53.93 (4)	O2^x—Ga1—Rb1B^viii	33.99 (5)
Rb1Bⁱ—Rb1A—O2ⁱⁱⁱ	83.749 (19)	O2ⁱⁱ—Ga1—Rb1B^viii	99.31 (13)
Rb1Bⁱⁱ—Rb1A—O2ⁱⁱⁱ	38.52 (7)	O2^xi—Ga1—Rb1B^viii	123.61 (10)
O3ⁱⁱⁱ—Rb1A—O2ⁱⁱⁱ	45.66 (3)	O4^viii—Ga1—Rb1Bⁱ	143.89 (6)
O3^iv—Rb1A—O2ⁱⁱⁱ	113.17 (3)	O4ⁱ—Ga1—Rb1Bⁱ	82.77 (12)
O3ⁱⁱ—Rb1A—O2ⁱⁱⁱ	63.90 (3)	O4^ix—Ga1—Rb1Bⁱ	55.65 (8)
O3^v—Rb1A—O2ⁱⁱⁱ	76.93 (3)	O2^x—Ga1—Rb1Bⁱ	123.61 (9)
O3ⁱ—Rb1A—O2ⁱⁱⁱ	127.31 (3)	O2ⁱⁱ—Ga1—Rb1Bⁱ	33.99 (5)
O3—Rb1A—O2ⁱⁱⁱ	111.42 (3)	O2^xi—Ga1—Rb1Bⁱ	99.31 (12)
O2^iv—Rb1A—O2ⁱⁱⁱ	114.732 (14)	Rb1B^viii—Ga1—Rb1Bⁱ	119.554 (12)
O2ⁱⁱ—Rb1A—O2ⁱⁱⁱ	53.93 (4)	O4^viii—Ga1—Rb1B^ix	55.65 (10)
O2—Rb1A—O2ⁱⁱⁱ	77.04 (4)	O4ⁱ—Ga1—Rb1B^ix	143.89 (7)
O2^v—Rb1A—O2ⁱⁱⁱ	114.731 (14)	O4^ix—Ga1—Rb1B^ix	82.77 (13)
Rb1Bⁱ—Rb1A—O2ⁱ	83.749 (19)	O2^x—Ga1—Rb1B^ix	99.31 (14)
Rb1Bⁱⁱ—Rb1A—O2ⁱ	153.03 (7)	O2ⁱⁱ—Ga1—Rb1B^ix	123.61 (9)
O3ⁱⁱⁱ—Rb1A—O2ⁱ	127.31 (3)	O2^xi—Ga1—Rb1B^ix	33.99 (6)
O3^iv—Rb1A—O2ⁱ	63.90 (3)	Rb1B^viii—Ga1—Rb1B^ix	119.554 (7)
O3ⁱⁱ—Rb1A—O2ⁱ	113.17 (3)	Rb1Bⁱ—Ga1—Rb1B^ix	119.554 (2)
O3^v—Rb1A—O2ⁱ	111.42 (3)	O4^viii—Ga1—Rb1A^viii	80.57 (3)
O3ⁱ—Rb1A—O2ⁱ	45.66 (3)	O4ⁱ—Ga1—Rb1A^viii	57.14 (3)
O3—Rb1A—O2ⁱ	76.93 (3)	O4^ix—Ga1—Rb1A^viii	144.67 (3)
O2^iv—Rb1A—O2ⁱ	53.93 (4)	O2^x—Ga1—Rb1A^viii	33.28 (3)
O2ⁱⁱ—Rb1A—O2ⁱ	114.732 (13)	O2ⁱⁱ—Ga1—Rb1A^viii	101.54 (3)
O2—Rb1A—O2ⁱ	114.732 (13)	O2^xi—Ga1—Rb1A^viii	122.02 (3)
O2^v—Rb1A—O2ⁱ	77.04 (4)	Rb1B^viii—Ga1—Rb1A^viii	2.56 (14)
O2ⁱⁱⁱ—Rb1A—O2ⁱ	167.50 (4)	Rb1Bⁱ—Ga1—Rb1A^viii	122.12 (13)
Rb1Bⁱ—Rb1A—As2^iv	60.329 (4)	Rb1B^ix—Ga1—Rb1A^viii	117.05 (14)
Rb1Bⁱⁱ—Rb1A—As2^iv	151.382 (12)	O4^viii—Ga1—Rb1A	144.67 (3)
O3ⁱⁱⁱ—Rb1A—As2^iv	77.70 (2)	O4ⁱ—Ga1—Rb1A	80.57 (3)
O3^iv—Rb1A—As2^iv	24.04 (2)	O4^ix—Ga1—Rb1A	57.14 (3)
O3ⁱⁱ—Rb1A—As2^iv	134.60 (2)	O2^x—Ga1—Rb1A	122.02 (3)
O3^v—Rb1A—As2^iv	92.58 (3)	O2ⁱⁱ—Ga1—Rb1A	33.28 (3)
O3ⁱ—Rb1A—As2^iv	77.98 (3)	O2^xi—Ga1—Rb1A	101.53 (3)
O3—Rb1A—As2^iv	125.97 (2)	Rb1B^viii—Ga1—Rb1A	117.05 (14)
O2^iv—Rb1A—As2^iv	23.324 (18)	Rb1Bⁱ—Ga1—Rb1A	2.56 (13)
O2ⁱⁱ—Rb1A—As2^iv	98.261 (18)	Rb1B^ix—Ga1—Rb1A	122.12 (13)
O2—Rb1A—As2^iv	146.607 (19)	Rb1A^viii—Ga1—Rb1A	119.614 (1)
O2^v—Rb1A—As2^iv	92.721 (19)	O4^viii—Ga1—Rb1A^xi	57.14 (3)
O2ⁱⁱⁱ—Rb1A—As2^iv	122.596 (19)	O4ⁱ—Ga1—Rb1A^xi	144.67 (4)
O2ⁱ—Rb1A—As2^iv	49.72 (2)	O4^ix—Ga1—Rb1A^xi	80.57 (3)
Rb1Bⁱ—Rb1A—As2ⁱⁱⁱ	67.492 (4)	O2^x—Ga1—Rb1A^xi	101.53 (3)
Rb1Bⁱⁱ—Rb1A—As2ⁱⁱⁱ	60.33 (6)	O2ⁱⁱ—Ga1—Rb1A^xi	122.02 (3)
O3ⁱⁱⁱ—Rb1A—As2ⁱⁱⁱ	24.04 (2)	O2^xi—Ga1—Rb1A^xi	33.28 (3)
O3^iv—Rb1A—As2ⁱⁱⁱ	92.58 (3)	Rb1B^viii—Ga1—Rb1A^xi	122.12 (14)
O3ⁱⁱ—Rb1A—As2ⁱⁱⁱ	77.98 (3)	Rb1Bⁱ—Ga1—Rb1A^xi	117.05 (13)
O3^v—Rb1A—As2ⁱⁱⁱ	77.70 (2)	Rb1B^ix—Ga1—Rb1A^xi	2.56 (14)
O3ⁱ—Rb1A—As2ⁱⁱⁱ	125.97 (2)	Rb1A^viii—Ga1—Rb1A^xi	119.614 (1)
O3—Rb1A—As2ⁱⁱⁱ	134.60 (2)	Rb1A—Ga1—Rb1A^xi	119.614 (1)
O2^iv—Rb1A—As2ⁱⁱⁱ	92.720 (19)	O1^xii—As1—O1^xiii	92.59 (5)
O2ⁱⁱ—Rb1A—As2ⁱⁱⁱ	49.72 (2)	O1^xii—As1—O1^xiv	92.59 (5)
O2—Rb1A—As2ⁱⁱⁱ	98.261 (18)	O1^xiii—As1—O1^xiv	92.59 (5)
O2^v—Rb1A—As2ⁱⁱⁱ	122.595 (19)	O1^xii—As1—O1ⁱ	87.41 (5)
O2ⁱⁱⁱ—Rb1A—As2ⁱⁱⁱ	23.323 (18)	O1^xiii—As1—O1ⁱ	180.00 (9)
O2ⁱ—Rb1A—As2ⁱⁱⁱ	146.608 (19)	O1^xiv—As1—O1ⁱ	87.41 (5)
As2^iv—Rb1A—As2ⁱⁱⁱ	99.334 (9)	O1^xii—As1—O1^ix	180.0
Rb1Bⁱ—Rb1A—As2^v	151.382 (7)	O1^xiii—As1—O1^ix	87.41 (5)
Rb1Bⁱⁱ—Rb1A—As2^v	67.49 (6)	O1^xiv—As1—O1^ix	87.41 (5)
O3ⁱⁱⁱ—Rb1A—As2^v	92.58 (3)	O1ⁱ—As1—O1^ix	92.58 (5)
O3^iv—Rb1A—As2^v	77.70 (2)	O1^xii—As1—O1^viii	87.42 (5)
O3ⁱⁱ—Rb1A—As2^v	125.97 (2)	O1^xiii—As1—O1^viii	87.42 (5)
O3^v—Rb1A—As2^v	24.04 (2)	O1^xiv—As1—O1^viii	180.00 (6)
O3ⁱ—Rb1A—As2^v	134.60 (2)	O1ⁱ—As1—O1^viii	92.58 (5)
O3—Rb1A—As2^v	77.98 (3)	O1^ix—As1—O1^viii	92.58 (5)
O2^iv—Rb1A—As2^v	122.596 (19)	O2—As2—O4^iv	117.31 (6)
O2ⁱⁱ—Rb1A—As2^v	146.608 (19)	O2—As2—O1^xv	115.10 (6)
O2—Rb1A—As2^v	49.72 (2)	O4^iv—As2—O1^xv	100.43 (5)
O2^v—Rb1A—As2^v	23.323 (17)	O2—As2—O3	104.11 (6)
O2ⁱⁱⁱ—Rb1A—As2^v	92.72 (2)	O4^iv—As2—O3	111.03 (6)
O2ⁱ—Rb1A—As2^v	98.261 (19)	O1^xv—As2—O3	108.86 (6)
As2^iv—Rb1A—As2^v	99.334 (9)	O2—As2—Rb1Bⁱⁱ	50.1 (3)
As2ⁱⁱⁱ—Rb1A—As2^v	99.334 (9)	O4^iv—As2—Rb1Bⁱⁱ	114.68 (16)
Rb1Bⁱ—Rb1A—As2ⁱⁱ	60.329 (3)	O1^xv—As2—Rb1Bⁱⁱ	144.86 (16)
Rb1Bⁱⁱ—Rb1A—As2ⁱⁱ	67.49 (6)	O3—As2—Rb1Bⁱⁱ	58.0 (2)
O3ⁱⁱⁱ—Rb1A—As2ⁱⁱ	77.98 (3)	O2—As2—Rb1B	58.6 (2)
O3^iv—Rb1A—As2ⁱⁱ	134.60 (2)	O4^iv—As2—Rb1B	106.7 (3)
O3ⁱⁱ—Rb1A—As2ⁱⁱ	24.04 (2)	O1^xv—As2—Rb1B	151.7 (2)
O3^v—Rb1A—As2ⁱⁱ	125.97 (2)	O3—As2—Rb1B	53.57 (7)
O3ⁱ—Rb1A—As2ⁱⁱ	77.70 (2)	Rb1Bⁱⁱ—As2—Rb1B	10.2 (5)
O3—Rb1A—As2ⁱⁱ	92.58 (2)	O2—As2—Rb1A	54.94 (4)
O2^iv—Rb1A—As2ⁱⁱ	98.261 (18)	O4^iv—As2—Rb1A	111.68 (4)
O2ⁱⁱ—Rb1A—As2ⁱⁱ	23.324 (18)	O1^xv—As2—Rb1A	147.34 (4)
O2—Rb1A—As2ⁱⁱ	92.721 (19)	O3—As2—Rb1A	54.48 (5)
O2^v—Rb1A—As2ⁱⁱ	146.607 (19)	Rb1Bⁱⁱ—As2—Rb1A	5.1 (3)
O2ⁱⁱⁱ—Rb1A—As2ⁱⁱ	49.72 (2)	Rb1B—As2—Rb1A	5.4 (3)
O2ⁱ—Rb1A—As2ⁱⁱ	122.596 (19)	O2—As2—Rb1Bⁱ	56.09 (6)
As2^iv—Rb1A—As2ⁱⁱ	120.658 (6)	O4^iv—As2—Rb1Bⁱ	113.41 (9)
As2ⁱⁱⁱ—Rb1A—As2ⁱⁱ	57.236 (12)	O1^xv—As2—Rb1Bⁱ	145.26 (10)
As2^v—Rb1A—As2ⁱⁱ	134.983 (5)	O3—As2—Rb1Bⁱ	52.42 (10)
Rb1Bⁱ—Rb1B—Rb1Bⁱⁱ	60.00 (2)	Rb1Bⁱⁱ—As2—Rb1Bⁱ	6.1 (3)
Rb1Bⁱ—Rb1B—O2^v	161.6 (2)	Rb1B—As2—Rb1Bⁱ	6.7 (3)
Rb1Bⁱⁱ—Rb1B—O2^v	108.4 (3)	Rb1A—As2—Rb1Bⁱ	2.49 (11)
Rb1Bⁱ—Rb1B—O2ⁱ	108.4 (2)	O2—As2—Rb1B^xvi	93.36 (7)
Rb1Bⁱⁱ—Rb1B—O2ⁱ	161.60 (17)	O4^iv—As2—Rb1B^xvi	42.23 (4)
O2^v—Rb1B—O2ⁱ	86.3 (5)	O1^xv—As2—Rb1B^xvi	80.78 (10)
Rb1Bⁱ—Rb1B—O3^iv	91.2 (3)	O3—As2—Rb1B^xvi	153.23 (5)
Rb1Bⁱⁱ—Rb1B—O3^iv	122.4 (3)	Rb1Bⁱⁱ—As2—Rb1B^xvi	126.58 (16)
O2^v—Rb1B—O3^iv	83.6 (3)	Rb1B—As2—Rb1B^xvi	125.4 (2)
O2ⁱ—Rb1B—O3^iv	69.1 (3)	Rb1A—As2—Rb1B^xvi	127.56 (9)
Rb1Bⁱ—Rb1B—O3	122.4 (3)	Rb1Bⁱ—As2—Rb1B^xvi	130.05 (2)
Rb1Bⁱⁱ—Rb1B—O3	91.2 (3)	O2—As2—Rb1A^xvii	94.58 (4)
O2^v—Rb1B—O3	69.1 (3)	O4^iv—As2—Rb1A^xvii	42.53 (4)
O2ⁱ—Rb1B—O3	83.6 (3)	O1^xv—As2—Rb1A^xvii	79.08 (4)
O3^iv—Rb1B—O3	142.5 (7)	O3—As2—Rb1A^xvii	153.36 (5)
Rb1Bⁱ—Rb1B—O3^v	113.4 (3)	Rb1Bⁱⁱ—As2—Rb1A^xvii	128.36 (6)
Rb1Bⁱⁱ—Rb1B—O3^v	76.7 (3)	Rb1B—As2—Rb1A^xvii	127.17 (12)
O2^v—Rb1B—O3^v	48.28 (11)	Rb1A—As2—Rb1A^xvii	129.347 (10)
O2ⁱ—Rb1B—O3^v	121.7 (5)	Rb1Bⁱ—As2—Rb1A^xvii	131.84 (12)
O3^iv—Rb1B—O3^v	71.12 (11)	Rb1B^xvi—As2—Rb1A^xvii	1.79 (10)
O3—Rb1B—O3^v	105.18 (19)	O2—As2—Rb1B^xviii	92.74 (11)
Rb1Bⁱ—Rb1B—O3ⁱ	76.7 (3)	O4^iv—As2—Rb1B^xviii	46.4 (2)
Rb1Bⁱⁱ—Rb1B—O3ⁱ	113.4 (3)	O1^xv—As2—Rb1B^xviii	76.75 (13)
O2^v—Rb1B—O3ⁱ	121.7 (5)	O3—As2—Rb1B^xviii	157.05 (19)
O2ⁱ—Rb1B—O3ⁱ	48.28 (11)	Rb1Bⁱⁱ—As2—Rb1B^xviii	129.10 (5)
O3^iv—Rb1B—O3ⁱ	105.18 (19)	Rb1B—As2—Rb1B^xviii	128.75 (3)
O3—Rb1B—O3ⁱ	71.12 (11)	Rb1A—As2—Rb1B^xviii	130.52 (5)
O3^v—Rb1B—O3ⁱ	169.0 (7)	Rb1Bⁱ—As2—Rb1B^xviii	132.99 (17)
Rb1Bⁱ—Rb1B—O2	118.6 (3)	Rb1B^xvi—As2—Rb1B^xviii	4.8 (2)
Rb1Bⁱⁱ—Rb1B—O2	60.4 (4)	Rb1A^xvii—As2—Rb1B^xviii	3.88 (18)
O2^v—Rb1B—O2	56.66 (12)	O2—As2—Rb1B^xvii	97.48 (15)
O2ⁱ—Rb1B—O2	124.3 (5)	O4^iv—As2—Rb1B^xvii	39.02 (18)
O3^iv—Rb1B—O2	133.6 (2)	O1^xv—As2—Rb1B^xvii	79.91 (7)
O3—Rb1B—O2	46.84 (5)	O3—As2—Rb1B^xvii	149.72 (18)
O3^v—Rb1B—O2	64.78 (4)	Rb1Bⁱⁱ—As2—Rb1B^xvii	129.012 (18)
O3ⁱ—Rb1B—O2	115.33 (5)	Rb1B—As2—Rb1B^xvii	127.02 (15)
Rb1Bⁱ—Rb1B—O2^iv	60.4 (3)	Rb1A—As2—Rb1B^xvii	129.587 (13)
Rb1Bⁱⁱ—Rb1B—O2^iv	118.6 (3)	Rb1Bⁱ—As2—Rb1B^xvii	132.07 (12)
O2^v—Rb1B—O2^iv	124.3 (5)	Rb1B^xvi—As2—Rb1B^xvii	4.2 (2)
O2ⁱ—Rb1B—O2^iv	56.66 (12)	Rb1A^xvii—As2—Rb1B^xvii	3.66 (17)
O3^iv—Rb1B—O2^iv	46.84 (5)	Rb1B^xviii—As2—Rb1B^xvii	7.4 (3)
O3—Rb1B—O2^iv	133.6 (2)	As2^xix—O1—As1^xx	131.96 (6)
O3^v—Rb1B—O2^iv	115.33 (5)	As2^xix—O1—Rb1B^vii	79.11 (18)
O3ⁱ—Rb1B—O2^iv	64.78 (4)	As1^xx—O1—Rb1B^vii	129.23 (10)
O2—Rb1B—O2^iv	179.0 (7)	As2—O2—Ga1^xvii	123.99 (6)
Rb1Bⁱ—Rb1B—O3ⁱⁱⁱ	48.36 (16)	As2—O2—Rb1Bⁱⁱ	105.9 (2)
Rb1Bⁱⁱ—Rb1B—O3ⁱⁱⁱ	56.58 (15)	Ga1^xvii—O2—Rb1Bⁱⁱ	125.54 (18)
O2^v—Rb1B—O3ⁱⁱⁱ	113.81 (3)	As2—O2—Rb1B	96.8 (3)
O2ⁱ—Rb1B—O3ⁱⁱⁱ	128.32 (3)	Ga1^xvii—O2—Rb1B	130.47 (10)
O3^iv—Rb1B—O3ⁱⁱⁱ	66.90 (12)	Rb1Bⁱⁱ—O2—Rb1B	11.2 (6)
O3—Rb1B—O3ⁱⁱⁱ	147.5 (4)	As2—O2—Rb1A	101.74 (4)
O3^v—Rb1B—O3ⁱⁱⁱ	66.07 (15)	Ga1^xvii—O2—Rb1A	128.51 (4)
O3ⁱ—Rb1B—O3ⁱⁱⁱ	122.7 (4)	Rb1Bⁱⁱ—O2—Rb1A	4.6 (2)
O2—Rb1B—O3ⁱⁱⁱ	105.6 (3)	Rb1B—O2—Rb1A	6.8 (3)
O2^iv—Rb1B—O3ⁱⁱⁱ	73.63 (18)	As2—O2—Rb1Bⁱ	102.64 (6)
Rb1Bⁱ—Rb1B—O3ⁱⁱ	56.58 (18)	Ga1^xvii—O2—Rb1Bⁱ	128.80 (4)
Rb1Bⁱⁱ—Rb1B—O3ⁱⁱ	48.36 (15)	Rb1Bⁱⁱ—O2—Rb1Bⁱ	3.34 (18)
O2^v—Rb1B—O3ⁱⁱ	128.32 (3)	Rb1B—O2—Rb1Bⁱ	9.3 (4)
O2ⁱ—Rb1B—O3ⁱⁱ	113.81 (3)	Rb1A—O2—Rb1Bⁱ	2.77 (12)
O3^iv—Rb1B—O3ⁱⁱ	147.5 (4)	As2—O3—Rb1B	101.51 (6)
O3—Rb1B—O3ⁱⁱ	66.90 (12)	As2—O3—Rb1Bⁱⁱ	96.3 (3)
O3^v—Rb1B—O3ⁱⁱ	122.7 (4)	Rb1B—O3—Rb1Bⁱⁱ	12.1 (6)
O3ⁱ—Rb1B—O3ⁱⁱ	66.07 (15)	As2—O3—Rb1A	101.48 (6)
O2—Rb1B—O3ⁱⁱ	73.63 (18)	Rb1B—O3—Rb1A	6.5 (3)
O2^iv—Rb1B—O3ⁱⁱ	105.6 (3)	Rb1Bⁱⁱ—O3—Rb1A	6.8 (3)
O3ⁱⁱⁱ—Rb1B—O3ⁱⁱ	90.9 (4)	As2—O3—Rb1Bⁱ	106.0 (2)
Rb1Bⁱ—Rb1B—O2ⁱⁱ	15.05 (2)	Rb1B—O3—Rb1Bⁱ	9.3 (5)
Rb1Bⁱⁱ—Rb1B—O2ⁱⁱ	52.10 (7)	Rb1Bⁱⁱ—O3—Rb1Bⁱ	10.1 (5)
O2^v—Rb1B—O2ⁱⁱ	160.5 (4)	Rb1A—O3—Rb1Bⁱ	4.9 (2)
O2ⁱ—Rb1B—O2ⁱⁱ	112.87 (12)	As2^iv—O4—Ga1^xx	126.28 (6)
O3^iv—Rb1B—O2ⁱⁱ	106.2 (3)	As2^iv—O4—Rb1B^xxi	120.71 (10)
O3—Rb1B—O2ⁱⁱ	107.8 (3)	Ga1^xx—O4—Rb1B^xxi	99.25 (5)
O3^v—Rb1B—O2ⁱⁱ	118.1 (4)	As2^iv—O4—Rb1A^xix	121.85 (5)
O3ⁱ—Rb1B—O2ⁱⁱ	72.8 (2)	Ga1^xx—O4—Rb1A^xix	99.67 (4)
O2—Rb1B—O2ⁱⁱ	106.5 (4)	Rb1B^xxi—O4—Rb1A^xix	2.51 (13)
O2^iv—Rb1B—O2ⁱⁱ	72.5 (2)	As2^iv—O4—Rb1B^xix	126.9 (3)
O3ⁱⁱⁱ—Rb1B—O2ⁱⁱ	57.9 (3)	Ga1^xx—O4—Rb1B^xix	96.29 (16)
O3ⁱⁱ—Rb1B—O2ⁱⁱ	41.55 (19)	Rb1B^xxi—O4—Rb1B^xix	7.1 (3)
Rb1Bⁱ—Rb1B—O2ⁱⁱⁱ	52.10 (12)	Rb1A^xix—O4—Rb1B^xix	5.2 (2)
Rb1Bⁱⁱ—Rb1B—O2ⁱⁱⁱ	15.05 (5)	As2^iv—O4—Rb1B^xxii	117.91 (18)
O2^v—Rb1B—O2ⁱⁱⁱ	112.87 (12)	Ga1^xx—O4—Rb1B^xxii	103.25 (18)
O2ⁱ—Rb1B—O2ⁱⁱⁱ	160.5 (4)	Rb1B^xxi—O4—Rb1B^xxii	4.1 (2)
O3^iv—Rb1B—O2ⁱⁱⁱ	107.8 (3)	Rb1A^xix—O4—Rb1B^xxii	3.99 (18)
O3—Rb1B—O2ⁱⁱⁱ	106.2 (3)	Rb1B^xix—O4—Rb1B^xxii	9.0 (4)
O3^v—Rb1B—O2ⁱⁱⁱ	72.8 (2)	As2^iv—O4—Rb1B	53.63 (19)
O3ⁱ—Rb1B—O2ⁱⁱⁱ	118.1 (4)	Ga1^xx—O4—Rb1B	72.96 (19)
O2—Rb1B—O2ⁱⁱⁱ	72.5 (2)	Rb1B^xxi—O4—Rb1B	134.20 (8)
O2^iv—Rb1B—O2ⁱⁱⁱ	106.5 (4)	Rb1A^xix—O4—Rb1B	136.70 (6)
O3ⁱⁱⁱ—Rb1B—O2ⁱⁱⁱ	41.55 (19)	Rb1B^xix—O4—Rb1B	139.53 (16)
O3ⁱⁱ—Rb1B—O2ⁱⁱⁱ	57.9 (3)	Rb1B^xxii—O4—Rb1B	135.79 (4)
O2ⁱⁱ—Rb1B—O2ⁱⁱⁱ	48.4 (2)	As2^iv—O4—Rb1Bⁱ	47.20 (15)
Rb1Bⁱ—Rb1B—O4^vi	153.31 (5)	Ga1^xx—O4—Rb1Bⁱ	80.09 (19)
Rb1Bⁱⁱ—Rb1B—O4^vi	130.76 (15)	Rb1B^xxi—O4—Rb1Bⁱ	130.0 (3)
O2^v—Rb1B—O4^vi	45.1 (2)	Rb1A^xix—O4—Rb1Bⁱ	132.53 (17)
O2ⁱ—Rb1B—O4^vi	53.4 (3)	Rb1B^xix—O4—Rb1Bⁱ	136.12 (3)
O3^iv—Rb1B—O4^vi	98.0 (5)	Rb1B^xxii—O4—Rb1Bⁱ	131.0 (3)
O3—Rb1B—O4^vi	44.50 (19)	Rb1B—O4—Rb1Bⁱ	8.2 (4)
O3^v—Rb1B—O4^vi	93.3 (3)	As2^iv—O4—Rb1A	50.21 (3)
O3ⁱ—Rb1B—O4^vi	76.7 (3)	Ga1^xx—O4—Rb1A	76.56 (3)
O2—Rb1B—O4^vi	71.6 (2)	Rb1B^xxi—O4—Rb1A	133.03 (14)
O2^iv—Rb1B—O4^vi	109.4 (4)	Rb1A^xix—O4—Rb1A	135.53 (3)
O3ⁱⁱⁱ—Rb1B—O4^vi	157.2 (3)	Rb1B^xix—O4—Rb1A	138.77 (15)
O3ⁱⁱ—Rb1B—O4^vi	109.34 (9)	Rb1B^xxii—O4—Rb1A	134.28 (7)
O2ⁱⁱ—Rb1B—O4^vi	144.95 (3)	Rb1B—O4—Rb1A	3.8 (2)
O2ⁱⁱⁱ—Rb1B—O4^vi	144.11 (3)	Rb1Bⁱ—O4—Rb1A	4.5 (2)
Rb1Bⁱ—Rb1B—O4^vii	130.76 (11)

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O3—H···O4^vi	0.80 (3)	1.98 (3)	2.7314 (17)	158 (3)

Symmetry code: (vi) y, x−1, −z+3/2.

Rubidium gallium bis[hydrogen arsenate(V)] (RbGaHAsO42) top

Crystal data top

RbGa(HAsO₄)₂	D_x = 3.964 Mg m⁻³
M_r = 435.05	Mo Kα radiation, λ = 0.71073 Å
Trigonal, R3c:H	Cell parameters from 2663 reflections
a = 8.385 (1) Å	θ = 2.3–30.0°
c = 53.880 (11) Å	µ = 19.42 mm⁻¹
V = 3280.7 (10) Å³	T = 293 K
Z = 18	Hexagonal plate, colourless
F(000) = 3600	0.07 × 0.07 × 0.02 mm

Data collection top

Nonius KappaCCD single-crystal four-circle diffractometer	1027 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	R_int = 0.016
φ and ω scans	θ_max = 30.0°, θ_min = 2.3°
Absorption correction: multi-scan (SCALEPACK; Otwinowski et al., 2003)	h = −11→11
T_min = 0.343, T_max = 0.697	k = −9→9
3896 measured reflections	l = −75→75
1079 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)] = 0.016	All H-atom parameters refined
wR(F²) = 0.040	w = 1/[σ²(F_o²) + (0.0168P)² + 20.8962P] where P = (F_o² + 2F_c²)/3
S = 1.11	(Δ/σ)_max = 0.014
1079 reflections	Δρ_max = 0.79 e Å⁻³
68 parameters	Δρ_min = −0.52 e Å⁻³
2 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: 0.000092 (13)

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	0.0297 (12)	0.909 (3)
Rb1B	0.000000	−0.050 (5)	0.750000	0.011 (3)	0.0304 (9)
Rb2	0.000000	0.000000	0.66714 (2)	0.02912 (12)
Ga1	0.333333	0.666667	0.75374 (2)	0.00733 (9)
Ga2	0.333333	0.666667	0.666667	0.00817 (11)
As	−0.43059 (3)	−0.39514 (3)	0.71280 (2)	0.00799 (7)
O1	0.4536 (2)	−0.4402 (2)	0.68636 (3)	0.0159 (3)
O2	−0.4459 (2)	−0.2541 (2)	0.73338 (3)	0.0106 (3)
O3	−0.1974 (2)	−0.2813 (2)	0.70523 (3)	0.0178 (3)
O4	0.4789 (2)	−0.1223 (2)	0.77582 (3)	0.0103 (3)
H	−0.161 (5)	−0.354 (5)	0.7099 (6)	0.035 (10)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Rb1A	0.0333 (16)	0.0333 (16)	0.0225 (9)	0.0166 (8)	0.000	0.000
Rb1B	0.023 (11)	0.012 (7)	0.004 (7)	0.011 (5)	−0.002 (4)	−0.001 (2)
Rb2	0.03481 (17)	0.03481 (17)	0.0177 (2)	0.01740 (9)	0.000	0.000
Ga1	0.00785 (12)	0.00785 (12)	0.00629 (16)	0.00393 (6)	0.000	0.000
Ga2	0.00943 (15)	0.00943 (15)	0.0057 (2)	0.00472 (8)	0.000	0.000
As	0.00991 (11)	0.00839 (10)	0.00729 (10)	0.00580 (8)	0.00068 (7)	0.00083 (7)
O1	0.0246 (8)	0.0212 (8)	0.0087 (6)	0.0164 (7)	−0.0050 (6)	−0.0011 (6)
O2	0.0105 (7)	0.0106 (6)	0.0104 (6)	0.0049 (5)	0.0026 (5)	−0.0016 (5)
O3	0.0129 (7)	0.0173 (8)	0.0257 (9)	0.0093 (7)	0.0085 (6)	0.0093 (6)
O4	0.0116 (6)	0.0092 (6)	0.0120 (6)	0.0066 (6)	−0.0019 (5)	−0.0038 (5)

Geometric parameters (Å, º) top

Rb1A—Rb1Bⁱ	0.42 (4)	Rb2—O3ⁱⁱ	2.9347 (17)
Rb1A—Rb1Bⁱⁱ	0.42 (4)	Rb2—O1^vi	3.3714 (16)
Rb1A—O3ⁱⁱⁱ	3.197 (2)	Rb2—O1^vii	3.3715 (16)
Rb1A—O3^iv	3.197 (2)	Rb2—O1^viii	3.3715 (17)
Rb1A—O3ⁱⁱ	3.197 (2)	Rb2—O4^ix	3.4960 (16)
Rb1A—O3ⁱ	3.197 (2)	Rb2—O4^x	3.4960 (17)
Rb1A—O3^v	3.197 (2)	Rb2—O4^xi	3.4960 (16)
Rb1A—O3	3.197 (2)	Rb2—O3^xii	3.5327 (19)
Rb1A—O2^iv	3.3698 (16)	Rb2—O3^xiii	3.533 (2)
Rb1A—O2ⁱⁱ	3.3698 (16)	Rb2—O3^xiv	3.5328 (19)
Rb1A—O2^v	3.3699 (16)	Rb2—As^xiv	3.7432 (5)
Rb1A—O2	3.3699 (16)	Rb2—As^xii	3.7432 (5)
Rb1A—O2ⁱⁱⁱ	3.3699 (15)	Rb2—As^xiii	3.7432 (5)
Rb1A—O2ⁱ	3.3699 (15)	Ga1—O2^xv	1.9596 (14)
Rb1A—As^iv	4.0083 (5)	Ga1—O2ⁱⁱ	1.9597 (15)
Rb1B—Rb1Bⁱ	0.72 (7)	Ga1—O2^xvi	1.9597 (15)
Rb1B—Rb1Bⁱⁱ	0.72 (7)	Ga1—O4^xvii	1.9690 (15)
Rb1B—O3^iv	3.019 (15)	Ga1—O4ⁱ	1.9690 (15)
Rb1B—O3	3.019 (15)	Ga1—O4^xviii	1.9690 (15)
Rb1B—O2^v	3.05 (3)	Ga2—O1^viii	1.9625 (15)
Rb1B—O2ⁱ	3.05 (3)	Ga2—O1^xiv	1.9625 (16)
Rb1B—O3ⁱ	3.161 (2)	Ga2—O1^xix	1.9625 (15)
Rb1B—O3^v	3.161 (2)	Ga2—O1ⁱ	1.9626 (15)
Rb1B—O2^iv	3.363 (2)	Ga2—O1^xviii	1.9626 (16)
Rb1B—O2	3.363 (2)	Ga2—O1^xvii	1.9626 (15)
Rb1B—O3ⁱⁱⁱ	3.47 (3)	As—O1^xx	1.6576 (15)
Rb1B—O3ⁱⁱ	3.47 (3)	As—O2	1.6724 (15)
Rb2—O3	2.9346 (17)	As—O4^iv	1.6805 (15)
Rb2—O3ⁱ	2.9347 (17)	As—O3	1.7417 (17)

Rb1Bⁱ—Rb1A—Rb1Bⁱⁱ	120.00 (15)	O1^vi—Rb2—As^xii	26.29 (3)
Rb1Bⁱ—Rb1A—O3ⁱⁱⁱ	61.38 (3)	O1^vii—Rb2—As^xii	88.53 (3)
Rb1Bⁱⁱ—Rb1A—O3ⁱⁱⁱ	81.43 (11)	O1^viii—Rb2—As^xii	105.88 (3)
Rb1Bⁱ—Rb1A—O3^iv	81.43 (3)	O4^ix—Rb2—As^xii	26.56 (2)
Rb1Bⁱⁱ—Rb1A—O3^iv	128.90 (5)	O4^x—Rb2—As^xii	54.15 (3)
O3ⁱⁱⁱ—Rb1A—O3^iv	69.26 (5)	O4^xi—Rb2—As^xii	71.43 (3)
Rb1Bⁱ—Rb1A—O3ⁱⁱ	81.43 (3)	O3^xii—Rb2—As^xii	27.50 (3)
Rb1Bⁱⁱ—Rb1A—O3ⁱⁱ	61.38 (9)	O3^xiii—Rb2—As^xii	63.12 (3)
O3ⁱⁱⁱ—Rb1A—O3ⁱⁱ	102.21 (6)	O3^xiv—Rb2—As^xii	98.11 (3)
O3^iv—Rb1A—O3ⁱⁱ	162.87 (7)	As^xiv—Rb2—As^xii	79.914 (13)
Rb1Bⁱ—Rb1A—O3ⁱ	61.38 (3)	O3—Rb2—As^xiii	177.27 (4)
Rb1Bⁱⁱ—Rb1A—O3ⁱ	128.90 (5)	O3ⁱ—Rb2—As^xiii	100.79 (4)
O3ⁱⁱⁱ—Rb1A—O3ⁱ	122.76 (7)	O3ⁱⁱ—Rb2—As^xiii	102.80 (4)
O3^iv—Rb1A—O3ⁱ	102.21 (6)	O1^vi—Rb2—As^xiii	88.53 (3)
O3ⁱⁱ—Rb1A—O3ⁱ	69.26 (5)	O1^vii—Rb2—As^xiii	105.88 (3)
Rb1Bⁱ—Rb1A—O3^v	128.90 (3)	O1^viii—Rb2—As^xiii	26.29 (3)
Rb1Bⁱⁱ—Rb1A—O3^v	61.38 (9)	O4^ix—Rb2—As^xiii	54.15 (3)
O3ⁱⁱⁱ—Rb1A—O3^v	69.26 (5)	O4^x—Rb2—As^xiii	71.43 (3)
O3^iv—Rb1A—O3^v	69.26 (5)	O4^xi—Rb2—As^xiii	26.56 (3)
O3ⁱⁱ—Rb1A—O3^v	122.76 (6)	O3^xii—Rb2—As^xiii	98.11 (3)
O3ⁱ—Rb1A—O3^v	162.87 (6)	O3^xiii—Rb2—As^xiii	27.50 (3)
Rb1Bⁱ—Rb1A—O3	128.90 (3)	O3^xiv—Rb2—As^xiii	63.12 (3)
Rb1Bⁱⁱ—Rb1A—O3	81.43 (11)	As^xiv—Rb2—As^xiii	79.914 (13)
O3ⁱⁱⁱ—Rb1A—O3	162.87 (6)	As^xii—Rb2—As^xiii	79.914 (13)
O3^iv—Rb1A—O3	122.76 (6)	O2^xv—Ga1—O2ⁱⁱ	91.72 (6)
O3ⁱⁱ—Rb1A—O3	69.26 (5)	O2^xv—Ga1—O2^xvi	91.72 (6)
O3ⁱ—Rb1A—O3	69.26 (5)	O2ⁱⁱ—Ga1—O2^xvi	91.72 (6)
O3^v—Rb1A—O3	102.21 (6)	O2^xv—Ga1—O4^xvii	92.25 (6)
Rb1Bⁱ—Rb1A—O2^iv	37.49 (3)	O2ⁱⁱ—Ga1—O4^xvii	175.98 (6)
Rb1Bⁱⁱ—Rb1A—O2^iv	150.57 (13)	O2^xvi—Ga1—O4^xvii	88.72 (6)
O3ⁱⁱⁱ—Rb1A—O2^iv	70.43 (4)	O2^xv—Ga1—O4ⁱ	88.72 (6)
O3^iv—Rb1A—O2^iv	48.04 (4)	O2ⁱⁱ—Ga1—O4ⁱ	92.25 (6)
O3ⁱⁱ—Rb1A—O2^iv	115.61 (4)	O2^xvi—Ga1—O4ⁱ	175.98 (7)
O3ⁱ—Rb1A—O2^iv	64.84 (4)	O4^xvii—Ga1—O4ⁱ	87.28 (6)
O3^v—Rb1A—O2^iv	113.71 (4)	O2^xv—Ga1—O4^xviii	175.98 (6)
O3—Rb1A—O2^iv	126.47 (4)	O2ⁱⁱ—Ga1—O4^xviii	88.71 (6)
Rb1Bⁱ—Rb1A—O2ⁱⁱ	37.49 (3)	O2^xvi—Ga1—O4^xviii	92.25 (6)
Rb1Bⁱⁱ—Rb1A—O2ⁱⁱ	85.56 (15)	O4^xvii—Ga1—O4^xviii	87.28 (7)
O3ⁱⁱⁱ—Rb1A—O2ⁱⁱ	64.84 (4)	O4ⁱ—Ga1—O4^xviii	87.28 (7)
O3^iv—Rb1A—O2ⁱⁱ	115.61 (4)	O2^xv—Ga1—Rb2^xxi	124.04 (4)
O3ⁱⁱ—Rb1A—O2ⁱⁱ	48.04 (4)	O2ⁱⁱ—Ga1—Rb2^xxi	124.04 (4)
O3ⁱ—Rb1A—O2ⁱⁱ	70.43 (4)	O2^xvi—Ga1—Rb2^xxi	124.04 (4)
O3^v—Rb1A—O2ⁱⁱ	126.47 (4)	O4^xvii—Ga1—Rb2^xxi	52.83 (5)
O3—Rb1A—O2ⁱⁱ	113.71 (4)	O4ⁱ—Ga1—Rb2^xxi	52.83 (5)
O2^iv—Rb1A—O2ⁱⁱ	74.98 (5)	O4^xviii—Ga1—Rb2^xxi	52.83 (4)
Rb1Bⁱ—Rb1A—O2^v	150.57 (3)	O2^xv—Ga1—Rb1A^xvii	32.81 (4)
Rb1Bⁱⁱ—Rb1A—O2^v	85.56 (15)	O2ⁱⁱ—Ga1—Rb1A^xvii	105.67 (4)
O3ⁱⁱⁱ—Rb1A—O2^v	113.71 (4)	O2^xvi—Ga1—Rb1A^xvii	120.04 (5)
O3^iv—Rb1A—O2^v	70.43 (4)	O4^xvii—Ga1—Rb1A^xvii	77.51 (4)
O3ⁱⁱ—Rb1A—O2^v	126.47 (4)	O4ⁱ—Ga1—Rb1A^xvii	59.26 (4)
O3ⁱ—Rb1A—O2^v	115.61 (4)	O4^xviii—Ga1—Rb1A^xvii	143.41 (5)
O3^v—Rb1A—O2^v	48.04 (4)	Rb2^xxi—Ga1—Rb1A^xvii	92.384 (4)
O3—Rb1A—O2^v	64.84 (4)	O2^xv—Ga1—Rb1A	120.04 (5)
O2^iv—Rb1A—O2^v	113.21 (2)	O2ⁱⁱ—Ga1—Rb1A	32.81 (4)
O2ⁱⁱ—Rb1A—O2^v	171.11 (5)	O2^xvi—Ga1—Rb1A	105.67 (4)
Rb1Bⁱ—Rb1A—O2	150.57 (3)	O4^xvii—Ga1—Rb1A	143.41 (5)
Rb1Bⁱⁱ—Rb1A—O2	37.49 (14)	O4ⁱ—Ga1—Rb1A	77.51 (4)
O3ⁱⁱⁱ—Rb1A—O2	115.61 (4)	O4^xviii—Ga1—Rb1A	59.26 (5)
O3^iv—Rb1A—O2	126.47 (4)	Rb2^xxi—Ga1—Rb1A	92.384 (4)
O3ⁱⁱ—Rb1A—O2	70.43 (4)	Rb1A^xvii—Ga1—Rb1A	119.828 (1)
O3ⁱ—Rb1A—O2	113.71 (4)	O2^xv—Ga1—Rb1A^xvi	105.67 (5)
O3^v—Rb1A—O2	64.84 (4)	O2ⁱⁱ—Ga1—Rb1A^xvi	120.04 (5)
O3—Rb1A—O2	48.04 (4)	O2^xvi—Ga1—Rb1A^xvi	32.81 (4)
O2^iv—Rb1A—O2	171.11 (5)	O4^xvii—Ga1—Rb1A^xvi	59.26 (4)
O2ⁱⁱ—Rb1A—O2	113.21 (2)	O4ⁱ—Ga1—Rb1A^xvi	143.41 (5)
O2^v—Rb1A—O2	58.86 (5)	O4^xviii—Ga1—Rb1A^xvi	77.51 (5)
Rb1Bⁱ—Rb1A—O2ⁱⁱⁱ	85.56 (3)	Rb2^xxi—Ga1—Rb1A^xvi	92.384 (4)
Rb1Bⁱⁱ—Rb1A—O2ⁱⁱⁱ	37.49 (14)	Rb1A^xvii—Ga1—Rb1A^xvi	119.828 (1)
O3ⁱⁱⁱ—Rb1A—O2ⁱⁱⁱ	48.04 (4)	Rb1A—Ga1—Rb1A^xvi	119.828 (1)
O3^iv—Rb1A—O2ⁱⁱⁱ	113.71 (4)	O1^viii—Ga2—O1^xiv	93.53 (6)
O3ⁱⁱ—Rb1A—O2ⁱⁱⁱ	64.84 (4)	O1^viii—Ga2—O1^xix	93.53 (6)
O3ⁱ—Rb1A—O2ⁱⁱⁱ	126.47 (4)	O1^xiv—Ga2—O1^xix	93.53 (6)
O3^v—Rb1A—O2ⁱⁱⁱ	70.43 (4)	O1^viii—Ga2—O1ⁱ	180.0
O3—Rb1A—O2ⁱⁱⁱ	115.61 (4)	O1^xiv—Ga2—O1ⁱ	86.48 (6)
O2^iv—Rb1A—O2ⁱⁱⁱ	113.21 (2)	O1^xix—Ga2—O1ⁱ	86.48 (6)
O2ⁱⁱ—Rb1A—O2ⁱⁱⁱ	58.87 (5)	O1^viii—Ga2—O1^xviii	86.48 (6)
O2^v—Rb1A—O2ⁱⁱⁱ	113.21 (2)	O1^xiv—Ga2—O1^xviii	180.0
O2—Rb1A—O2ⁱⁱⁱ	74.98 (5)	O1^xix—Ga2—O1^xviii	86.48 (6)
Rb1Bⁱ—Rb1A—O2ⁱ	85.56 (3)	O1ⁱ—Ga2—O1^xviii	93.52 (6)
Rb1Bⁱⁱ—Rb1A—O2ⁱ	150.57 (14)	O1^viii—Ga2—O1^xvii	86.48 (6)
O3ⁱⁱⁱ—Rb1A—O2ⁱ	126.47 (4)	O1^xiv—Ga2—O1^xvii	86.48 (6)
O3^iv—Rb1A—O2ⁱ	64.84 (4)	O1^xix—Ga2—O1^xvii	180.0
O3ⁱⁱ—Rb1A—O2ⁱ	113.71 (4)	O1ⁱ—Ga2—O1^xvii	93.52 (6)
O3ⁱ—Rb1A—O2ⁱ	48.04 (4)	O1^xviii—Ga2—O1^xvii	93.52 (6)
O3^v—Rb1A—O2ⁱ	115.61 (4)	O1^viii—Ga2—Rb2^xix	63.39 (5)
O3—Rb1A—O2ⁱ	70.43 (4)	O1^xiv—Ga2—Rb2^xix	66.53 (5)
O2^iv—Rb1A—O2ⁱ	58.87 (5)	O1^xix—Ga2—Rb2^xix	146.92 (4)
O2ⁱⁱ—Rb1A—O2ⁱ	113.21 (2)	O1ⁱ—Ga2—Rb2^xix	116.61 (5)
O2^v—Rb1A—O2ⁱ	74.98 (5)	O1^xviii—Ga2—Rb2^xix	113.47 (5)
O2—Rb1A—O2ⁱ	113.21 (2)	O1^xvii—Ga2—Rb2^xix	33.08 (4)
O2ⁱⁱⁱ—Rb1A—O2ⁱ	171.11 (6)	O1^viii—Ga2—Rb2^xvii	116.62 (5)
Rb1Bⁱ—Rb1A—As^iv	60.827 (6)	O1^xiv—Ga2—Rb2^xvii	113.48 (5)
Rb1Bⁱⁱ—Rb1A—As^iv	149.73 (2)	O1^xix—Ga2—Rb2^xvii	33.08 (4)
O3ⁱⁱⁱ—Rb1A—As^iv	73.16 (3)	O1ⁱ—Ga2—Rb2^xvii	63.38 (5)
O3^iv—Rb1A—As^iv	24.86 (3)	O1^xviii—Ga2—Rb2^xvii	66.52 (5)
O3ⁱⁱ—Rb1A—As^iv	139.65 (3)	O1^xvii—Ga2—Rb2^xvii	146.92 (4)
O3ⁱ—Rb1A—As^iv	79.79 (3)	Rb2^xix—Ga2—Rb2^xvii	180.0
O3^v—Rb1A—As^iv	93.74 (3)	O1^viii—Ga2—Rb2^xvi	113.48 (5)
O3—Rb1A—As^iv	123.16 (3)	O1^xiv—Ga2—Rb2^xvi	33.08 (4)
O2^iv—Rb1A—As^iv	24.28 (2)	O1^xix—Ga2—Rb2^xvi	116.62 (6)
O2ⁱⁱ—Rb1A—As^iv	97.93 (3)	O1ⁱ—Ga2—Rb2^xvi	66.52 (5)
O2^v—Rb1A—As^iv	89.76 (3)	O1^xviii—Ga2—Rb2^xvi	146.92 (4)
O2—Rb1A—As^iv	148.57 (3)	O1^xvii—Ga2—Rb2^xvi	63.38 (6)
O2ⁱⁱⁱ—Rb1A—As^iv	121.15 (3)	Rb2^xix—Ga2—Rb2^xvi	60.0
O2ⁱ—Rb1A—As^iv	53.64 (3)	Rb2^xvii—Ga2—Rb2^xvi	120.0
Rb1Bⁱ—Rb1B—Rb1Bⁱⁱ	60.00 (4)	O1^viii—Ga2—Rb2	33.08 (5)
Rb1Bⁱ—Rb1B—O3^iv	94.7 (6)	O1^xiv—Ga2—Rb2	116.62 (5)
Rb1Bⁱⁱ—Rb1B—O3^iv	123.8 (6)	O1^xix—Ga2—Rb2	113.48 (5)
Rb1Bⁱ—Rb1B—O3	123.8 (6)	O1ⁱ—Ga2—Rb2	146.92 (5)
Rb1Bⁱⁱ—Rb1B—O3	94.7 (7)	O1^xviii—Ga2—Rb2	63.38 (5)
O3^iv—Rb1B—O3	136.7 (14)	O1^xvii—Ga2—Rb2	66.52 (5)
Rb1Bⁱ—Rb1B—O2^v	160.6 (4)	Rb2^xix—Ga2—Rb2	60.0
Rb1Bⁱⁱ—Rb1B—O2^v	109.8 (6)	Rb2^xvii—Ga2—Rb2	120.0
O3^iv—Rb1B—O2^v	77.3 (7)	Rb2^xvi—Ga2—Rb2	120.0
O3—Rb1B—O2^v	71.0 (6)	O1^viii—Ga2—Rb2^xxii	66.52 (5)
Rb1Bⁱ—Rb1B—O2ⁱ	109.8 (5)	O1^xiv—Ga2—Rb2^xxii	146.92 (4)
Rb1Bⁱⁱ—Rb1B—O2ⁱ	160.6 (3)	O1^xix—Ga2—Rb2^xxii	63.38 (6)
O3^iv—Rb1B—O2ⁱ	71.0 (6)	O1ⁱ—Ga2—Rb2^xxii	113.47 (5)
O3—Rb1B—O2ⁱ	77.3 (7)	O1^xviii—Ga2—Rb2^xxii	33.08 (4)
O2^v—Rb1B—O2ⁱ	84.6 (10)	O1^xvii—Ga2—Rb2^xxii	116.62 (6)
Rb1Bⁱ—Rb1B—O3ⁱ	72.1 (6)	Rb2^xix—Ga2—Rb2^xxii	120.0
Rb1Bⁱⁱ—Rb1B—O3ⁱ	109.8 (6)	Rb2^xvii—Ga2—Rb2^xxii	60.0
O3^iv—Rb1B—O3ⁱ	107.2 (4)	Rb2^xvi—Ga2—Rb2^xxii	180.0
O3—Rb1B—O3ⁱ	72.0 (2)	Rb2—Ga2—Rb2^xxii	60.0
O2^v—Rb1B—O3ⁱ	127.0 (11)	O1^viii—Ga2—Rb2^xxiii	146.92 (5)
O2ⁱ—Rb1B—O3ⁱ	51.0 (2)	O1^xiv—Ga2—Rb2^xxiii	63.38 (5)
Rb1Bⁱ—Rb1B—O3^v	109.8 (7)	O1^xix—Ga2—Rb2^xxiii	66.52 (5)
Rb1Bⁱⁱ—Rb1B—O3^v	72.1 (7)	O1ⁱ—Ga2—Rb2^xxiii	33.08 (5)
O3^iv—Rb1B—O3^v	72.0 (2)	O1^xviii—Ga2—Rb2^xxiii	116.61 (5)
O3—Rb1B—O3^v	107.2 (4)	O1^xvii—Ga2—Rb2^xxiii	113.47 (5)
O2^v—Rb1B—O3^v	51.0 (2)	Rb2^xix—Ga2—Rb2^xxiii	120.0
O2ⁱ—Rb1B—O3^v	127.0 (11)	Rb2^xvii—Ga2—Rb2^xxiii	60.0
O3ⁱ—Rb1B—O3^v	177.9 (14)	Rb2^xvi—Ga2—Rb2^xxiii	60.0
Rb1Bⁱ—Rb1B—O2^iv	58.5 (7)	Rb2—Ga2—Rb2^xxiii	180.0
Rb1Bⁱⁱ—Rb1B—O2^iv	116.2 (6)	Rb2^xxii—Ga2—Rb2^xxiii	119.997 (1)
O3^iv—Rb1B—O2^iv	49.25 (8)	O1^xx—As—O2	119.20 (8)
O3—Rb1B—O2^iv	133.4 (5)	O1^xx—As—O4^iv	105.45 (8)
O2^v—Rb1B—O2^iv	122.6 (9)	O2—As—O4^iv	114.88 (7)
O2ⁱ—Rb1B—O2^iv	62.0 (3)	O1^xx—As—O3	107.00 (9)
O3ⁱ—Rb1B—O2^iv	65.28 (4)	O2—As—O3	103.30 (8)
O3^v—Rb1B—O2^iv	114.83 (5)	O4^iv—As—O3	106.04 (8)
Rb1Bⁱ—Rb1B—O2	116.2 (7)	O1^xx—As—Rb2^xii	64.25 (6)
Rb1Bⁱⁱ—Rb1B—O2	58.5 (8)	O2—As—Rb2^xii	172.80 (5)
O3^iv—Rb1B—O2	133.4 (5)	O4^iv—As—Rb2^xii	68.49 (5)
O3—Rb1B—O2	49.25 (8)	O3—As—Rb2^xii	69.51 (6)
O2^v—Rb1B—O2	62.0 (3)	O1^xx—As—Rb1Bⁱⁱ	142.0 (2)
O2ⁱ—Rb1B—O2	122.6 (9)	O2—As—Rb1Bⁱⁱ	50.6 (6)
O3ⁱ—Rb1B—O2	114.83 (5)	O4^iv—As—Rb1Bⁱⁱ	111.5 (3)
O3^v—Rb1B—O2	65.28 (4)	O3—As—Rb1Bⁱⁱ	54.9 (5)
O2^iv—Rb1B—O2	174.7 (13)	Rb2^xii—As—Rb1Bⁱⁱ	122.5 (5)
Rb1Bⁱ—Rb1B—O3ⁱⁱⁱ	46.2 (3)	O1^xx—As—Rb1B	146.8 (4)
Rb1Bⁱⁱ—Rb1B—O3ⁱⁱⁱ	58.9 (3)	O2—As—Rb1B	60.0 (4)
O3^iv—Rb1B—O3ⁱⁱⁱ	67.6 (2)	O4^iv—As—Rb1B	103.6 (5)
O3—Rb1B—O3ⁱⁱⁱ	153.6 (10)	O3—As—Rb1B	48.68 (19)
O2^v—Rb1B—O3ⁱⁱⁱ	114.75 (4)	Rb2^xii—As—Rb1B	113.4 (4)
O2ⁱ—Rb1B—O3ⁱⁱⁱ	127.90 (5)	Rb1Bⁱⁱ—As—Rb1B	10.8 (11)
O3ⁱ—Rb1B—O3ⁱⁱⁱ	115.4 (7)	O1^xx—As—Rb1A	143.22 (6)
O3^v—Rb1B—O3ⁱⁱⁱ	66.2 (3)	O2—As—Rb1A	55.94 (5)
O2^iv—Rb1B—O3ⁱⁱⁱ	67.3 (3)	O4^iv—As—Rb1A	108.77 (5)
O2—Rb1B—O3ⁱⁱⁱ	108.7 (7)	O3—As—Rb1A	50.50 (6)
Rb1Bⁱ—Rb1B—O3ⁱⁱ	58.9 (4)	Rb2^xii—As—Rb1A	117.262 (8)
Rb1Bⁱⁱ—Rb1B—O3ⁱⁱ	46.2 (3)	Rb1Bⁱⁱ—As—Rb1A	5.5 (5)
O3^iv—Rb1B—O3ⁱⁱ	153.6 (10)	Rb1B—As—Rb1A	5.7 (6)
O3—Rb1B—O3ⁱⁱ	67.6 (2)	O1^xx—As—Rb2	81.53 (7)
O2^v—Rb1B—O3ⁱⁱ	127.90 (5)	O2—As—Rb2	99.68 (5)
O2ⁱ—Rb1B—O3ⁱⁱ	114.75 (4)	O4^iv—As—Rb2	133.31 (5)
O3ⁱ—Rb1B—O3ⁱⁱ	66.2 (3)	O3—As—Rb2	32.31 (6)
O3^v—Rb1B—O3ⁱⁱ	115.4 (7)	Rb2^xii—As—Rb2	74.193 (8)
O2^iv—Rb1B—O3ⁱⁱ	108.7 (7)	Rb1Bⁱⁱ—As—Rb2	67.2 (2)
O2—Rb1B—O3ⁱⁱ	67.3 (3)	Rb1B—As—Rb2	66.79 (16)
O3ⁱⁱⁱ—Rb1B—O3ⁱⁱ	91.5 (9)	Rb1A—As—Rb2	65.327 (14)
O3—Rb2—O3ⁱ	76.48 (6)	O1^xx—As—Rb1A^xxiv	87.84 (7)
O3—Rb2—O3ⁱⁱ	76.48 (6)	O2—As—Rb1A^xxiv	94.28 (5)
O3ⁱ—Rb2—O3ⁱⁱ	76.48 (6)	O4^iv—As—Rb1A^xxiv	40.78 (5)
O3—Rb2—O1^vi	91.00 (4)	O3—As—Rb1A^xxiv	146.81 (6)
O3ⁱ—Rb2—O1^vi	76.80 (4)	Rb2^xii—As—Rb1A^xxiv	92.146 (8)
O3ⁱⁱ—Rb2—O1^vi	152.49 (5)	Rb1Bⁱⁱ—As—Rb1A^xxiv	126.24 (14)
O3—Rb2—O1^vii	76.80 (5)	Rb1B—As—Rb1A^xxiv	125.1 (3)
O3ⁱ—Rb2—O1^vii	152.49 (5)	Rb1A—As—Rb1A^xxiv	127.415 (12)
O3ⁱⁱ—Rb2—O1^vii	91.00 (4)	Rb2—As—Rb1A^xxiv	165.357 (7)
O1^vi—Rb2—O1^vii	110.14 (3)	O1^xx—As—Rb2^xxiv	42.87 (6)
O3—Rb2—O1^viii	152.49 (5)	O2—As—Rb2^xxiv	127.54 (5)
O3ⁱ—Rb2—O1^viii	91.00 (5)	O4^iv—As—Rb2^xxiv	64.16 (5)
O3ⁱⁱ—Rb2—O1^viii	76.80 (5)	O3—As—Rb2^xxiv	128.20 (6)
O1^vi—Rb2—O1^viii	110.14 (3)	Rb2^xii—As—Rb2^xxiv	59.507 (5)
O1^vii—Rb2—O1^viii	110.13 (2)	Rb1Bⁱⁱ—As—Rb2^xxiv	174.80 (5)
O3—Rb2—O4^ix	126.84 (4)	Rb1B—As—Rb2^xxiv	167.1 (6)
O3ⁱ—Rb2—O4^ix	111.15 (5)	Rb1A—As—Rb2^xxiv	172.736 (5)
O3ⁱⁱ—Rb2—O4^ix	156.15 (4)	Rb2—As—Rb2^xxiv	117.769 (15)
O1^vi—Rb2—O4^ix	45.47 (4)	Rb1A^xxiv—As—Rb2^xxiv	48.647 (11)
O1^vii—Rb2—O4^ix	90.21 (4)	As^xxv—O1—Ga2^xxvi	137.45 (10)
O1^viii—Rb2—O4^ix	80.43 (4)	As^xxv—O1—Rb2^vi	89.47 (6)
O3—Rb2—O4^x	111.15 (5)	Ga2^xxvi—O1—Rb2^vi	128.38 (6)
O3ⁱ—Rb2—O4^x	156.15 (4)	As^xxv—O1—Rb2^xxv	76.24 (6)
O3ⁱⁱ—Rb2—O4^x	126.84 (4)	Ga2^xxvi—O1—Rb2^xxv	92.73 (6)
O1^vi—Rb2—O4^x	80.43 (4)	Rb2^vi—O1—Rb2^xxv	76.74 (3)
O1^vii—Rb2—O4^x	45.46 (4)	As^xxv—O1—Rb2^xxvi	122.41 (7)
O1^viii—Rb2—O4^x	90.21 (4)	Ga2^xxvi—O1—Rb2^xxvi	89.56 (6)
O4^ix—Rb2—O4^x	45.74 (4)	Rb2^vi—O1—Rb2^xxvi	75.20 (3)
O3—Rb2—O4^xi	156.15 (5)	Rb2^xxv—O1—Rb2^xxvi	145.76 (4)
O3ⁱ—Rb2—O4^xi	126.84 (5)	As—O2—Ga1^xxiv	121.66 (8)
O3ⁱⁱ—Rb2—O4^xi	111.15 (5)	As—O2—Rb1Bⁱⁱ	104.3 (5)
O1^vi—Rb2—O4^xi	90.21 (4)	Ga1^xxiv—O2—Rb1Bⁱⁱ	125.9 (3)
O1^vii—Rb2—O4^xi	80.43 (4)	As—O2—Rb1B	94.4 (5)
O1^viii—Rb2—O4^xi	45.46 (4)	Ga1^xxiv—O2—Rb1B	130.14 (12)
O4^ix—Rb2—O4^xi	45.74 (4)	Rb1Bⁱⁱ—O2—Rb1B	11.7 (11)
O4^x—Rb2—O4^xi	45.74 (4)	As—O2—Rb1A	99.78 (6)
O3—Rb2—O3^xii	83.50 (5)	Ga1^xxiv—O2—Rb1A	128.83 (6)
O3ⁱ—Rb2—O3^xii	119.25 (6)	Rb1Bⁱⁱ—O2—Rb1A	4.8 (5)
O3ⁱⁱ—Rb2—O3^xii	150.88 (6)	Rb1B—O2—Rb1A	7.1 (7)
O1^vi—Rb2—O3^xii	46.57 (4)	As—O2—Rb2	60.35 (4)
O1^vii—Rb2—O3^xii	63.66 (4)	Ga1^xxiv—O2—Rb2	162.84 (6)
O1^viii—Rb2—O3^xii	123.76 (4)	Rb1Bⁱⁱ—O2—Rb2	64.9 (2)
O4^ix—Rb2—O3^xii	45.78 (4)	Rb1B—O2—Rb2	63.47 (7)
O4^x—Rb2—O3^xii	43.39 (4)	Rb1A—O2—Rb2	63.10 (2)
O4^xi—Rb2—O3^xii	80.11 (4)	As—O3—Rb2	129.19 (8)
O3—Rb2—O3^xiii	150.89 (6)	As—O3—Rb1B	105.64 (12)
O3ⁱ—Rb2—O3^xiii	83.50 (5)	Rb2—O3—Rb1B	97.7 (5)
O3ⁱⁱ—Rb2—O3^xiii	119.25 (6)	As—O3—Rb1Bⁱⁱ	98.2 (6)
O1^vi—Rb2—O3^xiii	63.66 (4)	Rb2—O3—Rb1Bⁱⁱ	94.64 (16)
O1^vii—Rb2—O3^xiii	123.75 (4)	Rb1B—O3—Rb1Bⁱⁱ	13.2 (13)
O1^viii—Rb2—O3^xiii	46.57 (4)	As—O3—Rb1A	104.65 (8)
O4^ix—Rb2—O3^xiii	43.39 (4)	Rb2—O3—Rb1A	93.37 (5)
O4^x—Rb2—O3^xiii	80.11 (4)	Rb1B—O3—Rb1A	7.0 (7)
O4^xi—Rb2—O3^xiii	45.78 (4)	Rb1Bⁱⁱ—O3—Rb1A	7.5 (7)
O3^xii—Rb2—O3^xiii	88.19 (4)	As—O3—Rb1Bⁱ	109.5 (4)
O3—Rb2—O3^xiv	119.25 (6)	Rb2—O3—Rb1Bⁱ	88.4 (5)
O3ⁱ—Rb2—O3^xiv	150.88 (6)	Rb1B—O3—Rb1Bⁱ	10.0 (9)
O3ⁱⁱ—Rb2—O3^xiv	83.50 (5)	Rb1Bⁱⁱ—O3—Rb1Bⁱ	11.3 (10)
O1^vi—Rb2—O3^xiv	123.76 (4)	Rb1A—O3—Rb1Bⁱ	5.4 (5)
O1^vii—Rb2—O3^xiv	46.57 (4)	As—O3—Rb2^xii	82.99 (7)
O1^viii—Rb2—O3^xiv	63.66 (4)	Rb2—O3—Rb2^xii	96.50 (5)
O4^ix—Rb2—O3^xiv	80.11 (4)	Rb1B—O3—Rb2^xii	152.4 (7)
O4^x—Rb2—O3^xiv	45.78 (4)	Rb1Bⁱⁱ—O3—Rb2^xii	164.5 (4)
O4^xi—Rb2—O3^xiv	43.38 (4)	Rb1A—O3—Rb2^xii	159.28 (6)
O3^xii—Rb2—O3^xiv	88.19 (4)	Rb1Bⁱ—O3—Rb2^xii	159.23 (8)
O3^xiii—Rb2—O3^xiv	88.19 (4)	As^iv—O4—Ga1^xxvi	130.00 (8)
O3—Rb2—As^xiv	102.80 (4)	As^iv—O4—Rb2^xxvii	84.95 (5)
O3ⁱ—Rb2—As^xiv	177.27 (4)	Ga1^xxvi—O4—Rb2^xxvii	100.50 (6)
O3ⁱⁱ—Rb2—As^xiv	100.79 (4)	As^iv—O4—Rb1A^xxv	124.06 (6)
O1^vi—Rb2—As^xiv	105.88 (3)	Ga1^xxvi—O4—Rb1A^xxv	96.95 (5)
O1^vii—Rb2—As^xiv	26.29 (3)	Rb2^xxvii—O4—Rb1A^xxv	118.51 (4)
O1^viii—Rb2—As^xiv	88.53 (3)	As^iv—O4—Rb1A	51.95 (4)
O4^ix—Rb2—As^xiv	71.43 (3)	Ga1^xxvi—O4—Rb1A	78.99 (4)
O4^x—Rb2—As^xiv	26.56 (2)	Rb2^xxvii—O4—Rb1A	104.39 (3)
O4^xi—Rb2—As^xiv	54.15 (3)	Rb1A^xxv—O4—Rb1A	136.81 (4)
O3^xii—Rb2—As^xiv	63.12 (3)	As^iv—O4—Rb2^xxviii	98.27 (5)
O3^xiii—Rb2—As^xiv	98.10 (3)	Ga1^xxvi—O4—Rb2^xxviii	129.76 (6)
O3^xiv—Rb2—As^xiv	27.50 (3)	Rb2^xxvii—O4—Rb2^xxviii	66.64 (2)
O3—Rb2—As^xii	100.79 (4)	Rb1A^xxv—O4—Rb2^xxviii	57.20 (2)
O3ⁱ—Rb2—As^xii	102.80 (4)	Rb1A—O4—Rb2^xxviii	150.18 (3)
O3ⁱⁱ—Rb2—As^xii	177.27 (4)

Symmetry codes: (i) −y, x−y, z; (ii) −x+y, −x, z; (iii) x−y, −y, −z+3/2; (iv) −x, −x+y, −z+3/2; (v) y, x, −z+3/2; (vi) −x+2/3, −y−2/3, −z+4/3; (vii) x−y−4/3, x−2/3, −z+4/3; (viii) y+2/3, −x+y+4/3, −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−1/3, −y−2/3, −z+4/3; (xiii) y+2/3, −x+y+1/3, −z+4/3; (xiv) x−y−1/3, x+1/3, −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+2/3, −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−1, z; (xxv) x+1, y, z; (xxvi) x, y−1, z; (xxvii) −y+1/3, −x−1/3, z+1/6; (xxviii) y+1, x, −z+3/2.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O3—H···O4^xxix	0.85 (3)	1.76 (3)	2.598 (2)	168 (4)

Symmetry code: (xxix) 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: Doc fForte Fellowship of the Austrian Academy of Sciences to K. Schwendtner.

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