M³⁺(H₂AsO₄)(H₂As₂O₇) (M³⁺ = Al, Ga) and In₂(H₂AsO₄)₂(H₂As₂O₇)₂: a new layer structure type and a new framework structure type containing the rare H₂As₂O₇²⁻ group

The crystal structures of hydro­thermally synthesized aluminium di­hydrogen arsenate(V) di­hydrogen diarsenate(V), Al(H₂AsO₄)(H₂As₂O₇), gallium di­hydrogen arsenate(V) di­hydrogen diarsenate(V), Ga(H₂AsO₄)(H₂As₂O₇), and diindium bis­[di­hydrogen arsenate(V)] bis­[di­hydrogen diarsenate(V)], In₂(H₂AsO₄)₂(H₂As₂O₇)₂, were determined from single-crystal X-ray diffraction data collected at room temperature. The first two compounds are representatives of a novel sheet structure type, whereas the third compound crystallizes in a novel framework structure. In all three structures, the basic building units are M³⁺O₆ octa­hedra (M = Al, Ga, In) that are connected via one H₂AsO₄⁻ and two H₂As₂O₇²⁻ groups into chains, and further via H₂As₂O₇²⁻ groups into layers. In Al/Ga(H₂AsO₄)(H₂As₂O₇), these layers are inter­connected by weak-to-medium–strong hydrogen bonds. In In₂(H₂AsO₄)₂(H₂As₂O₇)₂, the H₂As₂O₇²⁻ groups link the chains in three dimensions, thus creating a framework topology, which is reinforced by weak-to-medium–strong hydrogen bonds. The three title arsenates represent the first compounds containing both H₂AsO₄⁻ and H₂As₂O₇²⁻ groups.

Computing details

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

Aluminium [dihydrogen arsenate(V)] dihydrogen diarsenate(V) (AlH2AsO4H2As2O7)

Crystal data

Al(H2AsO4)(H2As2O7)	Dx = 3.366 Mg m^−3
Mr = 431.77	Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, Pnma	Cell parameters from 1830 reflections
a = 4.869 (1) Å	θ = 2.0–32.6°
b = 11.071 (2) Å	µ = 11.85 mm^−1
c = 15.807 (3) Å	T = 293 K
V = 852.1 (3) Å^3	Acicular, colourless
Z = 4	0.70 × 0.02 × 0.02 mm
F(000) = 816

Data collection

Nonius KappaCCD single-crystal four-circle diffractometer	1319 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.022
φ and ω scans	θmax = 32.5°, θmin = 2.6°
Absorption correction: multi-scan (SCALEPACK; Otwinowski et al., 2003)	h = −7→7
Tmin = 0.044, Tmax = 0.798	k = −16→16
2892 measured reflections	l = −23→23
1611 independent reflections

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: mixed
R[F^2 > 2σ(F^2)] = 0.028	H atoms treated by a mixture of independent and constrained refinement
wR(F^2) = 0.062	w = 1/[σ^2(Fo^2) + (0.029P)^2 + 0.9297P] where P = (Fo^2 + 2Fc^2)/3
S = 1.10	(Δ/σ)max = 0.001
1611 reflections	Δρmax = 2.01 e Å^−3
85 parameters	Δρmin = −1.04 e Å^−3
2 restraints	Extinction correction: SHELXL2016 (Sheldrick, 2015), Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0013 (2)

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
As1	0.06052 (8)	0.250000	0.60042 (2)	0.01204 (10)
As2	0.49189 (5)	0.10541 (2)	0.38736 (2)	0.01111 (9)
Al1	0.000000	0.000000	0.500000	0.0111 (2)
O1	0.1841 (4)	0.12665 (17)	0.55450 (12)	0.0155 (4)
O2	−0.2878 (6)	0.250000	0.61117 (17)	0.0197 (6)
H2	−0.356100	0.206796	0.574663	0.030*	0.5
O3	0.1406 (6)	0.250000	0.70586 (18)	0.0242 (7)
H3	0.324 (4)	0.250000	0.712 (4)	0.050 (18)*
O4	0.7385 (4)	0.11224 (16)	0.45768 (12)	0.0158 (4)
O5	0.2171 (4)	0.02170 (17)	0.40087 (12)	0.0156 (4)
O6	0.6338 (4)	0.0664 (2)	0.29152 (12)	0.0221 (4)
H6	0.503 (6)	0.063 (3)	0.253 (2)	0.036 (11)*
O7	0.3652 (6)	0.250000	0.37052 (19)	0.0222 (6)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
As1	0.00932 (16)	0.01492 (18)	0.01188 (17)	0.000	0.00002 (13)	0.000
As2	0.00772 (12)	0.01349 (14)	0.01212 (13)	−0.00032 (8)	−0.00065 (8)	0.00040 (9)
Al1	0.0073 (4)	0.0131 (5)	0.0128 (5)	−0.0009 (4)	−0.0006 (4)	0.0006 (4)
O1	0.0104 (8)	0.0152 (9)	0.0210 (9)	0.0001 (7)	−0.0012 (7)	−0.0038 (8)
O2	0.0094 (12)	0.0338 (17)	0.0159 (14)	0.000	0.0000 (10)	0.000
O3	0.0191 (15)	0.0401 (18)	0.0133 (14)	0.000	−0.0039 (11)	0.000
O4	0.0122 (8)	0.0173 (10)	0.0177 (9)	0.0019 (7)	−0.0052 (7)	−0.0006 (7)
O5	0.0106 (8)	0.0197 (10)	0.0166 (8)	−0.0044 (7)	0.0017 (7)	−0.0016 (8)
O6	0.0138 (9)	0.0379 (13)	0.0145 (9)	−0.0010 (9)	0.0023 (7)	−0.0037 (9)
O7	0.0184 (14)	0.0138 (13)	0.0343 (17)	0.000	−0.0145 (13)	0.000

Geometric parameters (Å, º)

As1—O1^i	1.6594 (19)	Al1—O1^ii	1.8740 (18)
As1—O1	1.6594 (19)	Al1—O4^iii	1.9008 (18)
As1—O2	1.704 (3)	Al1—O4^iv	1.9008 (18)
As1—O3	1.712 (3)	Al1—O5	1.9053 (19)
As2—O4	1.6379 (18)	Al1—O5^ii	1.9053 (19)
As2—O5	1.6416 (19)	O2—H2	0.8200
As2—O6	1.720 (2)	O2—H2^i	0.82 (6)
As2—O7	1.7361 (11)	O3—H3	0.90 (2)
Al1—O1	1.8739 (18)	O6—H6	0.879 (18)
O1^i—As1—O1	110.76 (13)	O1—Al1—O5	91.05 (8)
O1^i—As1—O2	113.85 (8)	O1^ii—Al1—O5	88.95 (8)
O1—As1—O2	113.85 (8)	O4^iii—Al1—O5	89.99 (8)
O1^i—As1—O3	110.07 (9)	O4^iv—Al1—O5	90.01 (8)
O1—As1—O3	110.08 (8)	O1—Al1—O5^ii	88.95 (8)
O2—As1—O3	97.44 (14)	O1^ii—Al1—O5^ii	91.06 (8)
O4—As2—O5	122.36 (9)	O4^iii—Al1—O5^ii	90.01 (8)
O4—As2—O6	108.35 (9)	O4^iv—Al1—O5^ii	89.99 (8)
O5—As2—O6	107.48 (10)	O5—Al1—O5^ii	180.0
O4—As2—O7	108.79 (10)	As1—O1—Al1	130.04 (11)
O5—As2—O7	104.52 (12)	As1—O2—H2	109.5
O6—As2—O7	103.83 (13)	As1—O2—H2^i	109.5 (14)
O1—Al1—O1^ii	180.0	H2—O2—H2^i	71.4
O1—Al1—O4^iii	89.60 (8)	As1—O3—H3	109 (4)
O1^ii—Al1—O4^iii	90.40 (8)	As2—O4—Al1^v	134.40 (11)
O1—Al1—O4^iv	90.40 (8)	As2—O5—Al1	129.08 (11)
O1^ii—Al1—O4^iv	89.60 (8)	As2—O6—H6	109 (3)
O4^iii—Al1—O4^iv	180.00 (10)	As2—O7—As2^i	134.45 (17)

Symmetry codes: (i) x, −y+1/2, z; (ii) −x, −y, −z+1; (iii) x−1, y, z; (iv) −x+1, −y, −z+1; (v) x+1, y, z.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O2—H2···O4^iii	0.82	2.17	2.869 (3)	143
O2—H2···O1^iii	0.82	2.43	3.046 (3)	133
O3—H3···O3^vi	0.90 (2)	2.02 (3)	2.806 (3)	146 (5)
O6—H6···O6^vii	0.88 (2)	1.93 (2)	2.7659 (19)	158 (4)

Symmetry codes: (iii) x−1, y, z; (vi) x+1/2, y, −z+3/2; (vii) x−1/2, y, −z+1/2.

Gallium dihydrogen arsenate(V) dihydrogen diarsenate(V) (GaH2AsO4H2As2O7)

Crystal data

Ga(H2AsO4)(H2As2O7)	Dx = 3.607 Mg m^−3
Mr = 474.51	Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, Pnma	Cell parameters from 1874 reflections
a = 4.916 (1) Å	θ = 2.0–32.6°
b = 11.213 (2) Å	µ = 14.47 mm^−1
c = 15.853 (3) Å	T = 293 K
V = 873.9 (3) Å^3	Acicular, colourless
Z = 4	0.15 × 0.07 × 0.03 mm
F(000) = 888

Data collection

Nonius KappaCCD single-crystal four-circle diffractometer	1470 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.015
φ and ω scans	θmax = 32.5°, θmin = 3.6°
Absorption correction: multi-scan (SCALEPACK; Otwinowski et al., 2003)	h = −7→7
Tmin = 0.220, Tmax = 0.671	k = −16→16
2970 measured reflections	l = −23→23
1652 independent reflections

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.031	All H-atom parameters refined
wR(F^2) = 0.082	w = 1/[σ^2(Fo^2) + (0.0405P)^2 + 3.2043P] where P = (Fo^2 + 2Fc^2)/3
S = 1.14	(Δ/σ)max = 0.001
1652 reflections	Δρmax = 1.89 e Å^−3
84 parameters	Δρmin = −1.52 e Å^−3
0 restraints	Extinction correction: SHELXL2016 (Sheldrick, 2015), Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0010 (3)

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
As1	0.06428 (10)	0.250000	0.60150 (3)	0.01201 (12)
As2	0.49079 (6)	0.10749 (3)	0.38577 (2)	0.01114 (10)
Ga1	0.000000	0.000000	0.500000	0.01141 (12)
O1	0.1911 (5)	0.1282 (2)	0.55641 (16)	0.0167 (4)
O2	−0.2805 (7)	0.250000	0.6100 (2)	0.0204 (7)
O3	0.1365 (8)	0.250000	0.7066 (2)	0.0240 (8)
H3	0.29 (2)	0.250000	0.722 (6)	0.06 (3)*
O4	0.7303 (5)	0.1157 (2)	0.45776 (15)	0.0161 (5)
O5	0.2196 (5)	0.0229 (2)	0.39671 (14)	0.0163 (4)
O6	0.6400 (5)	0.0699 (3)	0.29132 (16)	0.0229 (6)
H6	0.519 (13)	0.057 (6)	0.253 (5)	0.06 (2)*
O7	0.3627 (8)	0.250000	0.3692 (3)	0.0231 (8)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
As1	0.0093 (2)	0.0144 (2)	0.0123 (2)	0.000	0.00000 (15)	0.000
As2	0.00747 (16)	0.01327 (17)	0.01268 (16)	−0.00040 (9)	−0.00065 (9)	0.00038 (10)
Ga1	0.0076 (2)	0.0128 (2)	0.0137 (2)	−0.00118 (15)	−0.00056 (15)	0.00067 (16)
O1	0.0089 (9)	0.0146 (10)	0.0265 (12)	0.0003 (8)	−0.0014 (9)	−0.0049 (9)
O2	0.0092 (14)	0.035 (2)	0.0175 (16)	0.000	0.0014 (11)	0.000
O3	0.0181 (17)	0.042 (2)	0.0122 (15)	0.000	−0.0011 (13)	0.000
O4	0.0132 (10)	0.0172 (11)	0.0179 (11)	0.0026 (9)	−0.0054 (8)	−0.0025 (8)
O5	0.0123 (10)	0.0206 (11)	0.0160 (10)	−0.0054 (9)	0.0023 (8)	−0.0006 (9)
O6	0.0141 (11)	0.0387 (16)	0.0159 (11)	−0.0026 (11)	0.0020 (9)	−0.0052 (10)
O7	0.0199 (17)	0.0120 (15)	0.037 (2)	0.000	−0.0172 (16)	0.000

Geometric parameters (Å, º)

As1—O1^i	1.663 (2)	Ga1—O1	1.936 (2)
As1—O1	1.663 (2)	Ga1—O1^ii	1.936 (2)
As1—O2	1.700 (4)	Ga1—O4^iii	1.972 (2)
As1—O3	1.704 (4)	Ga1—O4^iv	1.972 (2)
As2—O4	1.642 (2)	Ga1—O5^ii	1.978 (2)
As2—O5	1.645 (2)	Ga1—O5	1.978 (2)
As2—O6	1.720 (3)	O3—H3	0.78 (10)
As2—O7	1.7377 (15)	O6—H6	0.87 (7)
O1—As1—O1^i	110.44 (18)	O4^iii—Ga1—O4^iv	180.00 (13)
O1—As1—O2	114.08 (10)	O1—Ga1—O5^ii	88.79 (10)
O1^i—As1—O2	114.08 (10)	O1^ii—Ga1—O5^ii	91.21 (10)
O1—As1—O3	110.02 (11)	O4^iii—Ga1—O5^ii	90.02 (10)
O1^i—As1—O3	110.02 (11)	O4^iv—Ga1—O5^ii	89.98 (10)
O2—As1—O3	97.46 (18)	O1—Ga1—O5	91.21 (10)
O4—As2—O5	122.69 (12)	O1^ii—Ga1—O5	88.79 (10)
O4—As2—O6	108.24 (12)	O4^iii—Ga1—O5	89.98 (10)
O5—As2—O6	107.23 (13)	O4^iv—Ga1—O5	90.02 (10)
O4—As2—O7	108.26 (14)	O5^ii—Ga1—O5	180.0
O5—As2—O7	104.62 (15)	As1—O1—Ga1	128.78 (13)
O6—As2—O7	104.37 (18)	As1—O3—H3	120 (7)
O1—Ga1—O1^ii	180.0	As2—O4—Ga1^v	132.90 (13)
O1—Ga1—O4^iii	90.31 (10)	As2—O5—Ga1	127.18 (13)
O1^ii—Ga1—O4^iii	89.69 (10)	As2—O6—H6	111 (5)
O1—Ga1—O4^iv	89.69 (10)	As2—O7—As2^i	133.7 (2)
O1^ii—Ga1—O4^iv	90.31 (10)

Symmetry codes: (i) x, −y+1/2, z; (ii) −x, −y, −z+1; (iii) −x+1, −y, −z+1; (iv) x−1, y, z; (v) x+1, y, z.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O3—H3···O3^vi	0.78 (10)	2.06 (10)	2.817 (4)	164 (10)
O6—H6···O5^vii	0.87 (7)	2.59 (7)	3.052 (3)	114 (5)
O6—H6···O6^viii	0.87 (7)	1.99 (7)	2.785 (2)	151 (6)

Symmetry codes: (vi) x+1/2, y, −z+3/2; (vii) x+1/2, y, −z+1/2; (viii) x−1/2, y, −z+1/2.

Diindium bis[dihydrogen arsenate(V)] bis[dihydrogen diarsenate(V)] (In2H2AsO42H2As2O72)

Crystal data

In2(H2AsO4)2(H2As2O7)2	F(000) = 1920
Mr = 1039.22	Dx = 3.897 Mg m^−3
Monoclinic, P21/n	Mo Kα radiation, λ = 0.71073 Å
a = 12.487 (2) Å	Cell parameters from 6682 reflections
b = 11.529 (2) Å	θ = 2.0–32.6°
c = 12.553 (3) Å	µ = 13.84 mm^−1
β = 101.40 (3)°	T = 293 K
V = 1771.5 (6) Å^3	Blocky, colourless
Z = 4	0.08 × 0.07 × 0.03 mm

Data collection

Nonius KappaCCD single-crystal four-circle diffractometer	5562 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.021
φ and ω scans	θmax = 32.6°, θmin = 2.1°
Absorption correction: multi-scan (SCALEPACK; Otwinowski et al., 2003)	h = −18→18
Tmin = 0.403, Tmax = 0.682	k = −17→17
12567 measured reflections	l = −19→18
6428 independent reflections

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.034	Only H-atom coordinates refined
wR(F^2) = 0.072	w = 1/[σ^2(Fo^2) + 19.0117P] where P = (Fo^2 + 2Fc^2)/3
S = 1.22	(Δ/σ)max = 0.001
6428 reflections	Δρmax = 2.14 e Å^−3
299 parameters	Δρmin = −1.68 e Å^−3
6 restraints	Extinction correction: SHELXL2016 (Sheldrick, 2015), Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.00083 (3)

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
In1	0.74844 (3)	1.00138 (3)	0.73467 (3)	0.00950 (7)
In2	0.73920 (3)	0.98874 (3)	0.23819 (3)	0.00933 (7)
As1	0.77893 (4)	0.60833 (4)	0.51413 (4)	0.01103 (9)
As2	0.77259 (4)	0.88225 (4)	0.49339 (4)	0.01012 (9)
As3	0.99559 (4)	0.60869 (4)	0.21703 (4)	0.01123 (9)
As4	0.99662 (4)	0.88304 (4)	0.22744 (4)	0.00994 (9)
As5	0.89658 (4)	0.75944 (4)	0.83829 (4)	0.01077 (9)
As6	0.66222 (4)	0.72935 (4)	0.10470 (4)	0.01034 (9)
O1	0.7315 (3)	0.6058 (3)	0.3820 (3)	0.0155 (7)
O2	0.7086 (3)	0.5319 (3)	0.5889 (3)	0.0165 (7)
O3	0.9141 (3)	0.5786 (4)	0.5351 (3)	0.0240 (9)
O4	0.7653 (4)	0.7507 (3)	0.5572 (3)	0.0211 (8)
O5	0.7187 (3)	0.8680 (3)	0.3629 (3)	0.0141 (7)
O6	0.7124 (3)	0.9760 (3)	0.5620 (3)	0.0150 (7)
O7	0.9101 (3)	0.9130 (4)	0.5153 (3)	0.0235 (8)
O8	1.1287 (3)	0.6170 (3)	0.2610 (3)	0.0170 (7)
O9	0.9331 (3)	0.5205 (3)	0.2893 (3)	0.0166 (7)
O10	0.9713 (3)	0.5814 (4)	0.0812 (3)	0.0223 (8)
O11	0.9421 (3)	0.7458 (3)	0.2327 (4)	0.0205 (8)
O12	0.9160 (3)	0.9635 (3)	0.2866 (3)	0.0168 (7)
O13	1.1270 (3)	0.8780 (3)	0.2866 (3)	0.0136 (6)
O14	0.9824 (3)	0.9163 (4)	0.0927 (3)	0.0232 (8)
O15	0.8697 (3)	0.6343 (3)	0.7753 (3)	0.0160 (7)
O16	0.8751 (3)	0.8757 (3)	0.7583 (3)	0.0154 (7)
O17	1.0297 (3)	0.7632 (4)	0.9070 (3)	0.0205 (8)
O18	0.8227 (3)	0.7661 (4)	0.9400 (3)	0.0197 (8)
O19	0.7244 (3)	0.8566 (3)	0.1211 (3)	0.0156 (7)
O20	0.7432 (3)	0.6155 (3)	0.1360 (3)	0.0159 (7)
O21	0.5922 (3)	0.7177 (4)	−0.0267 (3)	0.0212 (8)
O22	0.5595 (3)	0.7290 (3)	0.1772 (3)	0.0192 (7)
H3A	0.936 (11)	0.560 (12)	0.604 (4)	0.02 (4)*	0.5
H3B	0.943 (10)	0.512 (6)	0.520 (11)	0.02 (3)*	0.5
H7	0.941 (6)	0.936 (7)	0.464 (6)	0.03 (2)*
H10A	1.000 (11)	0.522 (9)	0.051 (10)	0.025*	0.5
H10B	0.906 (6)	0.612 (12)	0.083 (12)	0.03 (4)*	0.5
H21	0.628 (6)	0.702 (7)	−0.077 (5)	0.03 (2)*
H22	0.529 (5)	0.661 (4)	0.172 (6)	0.024 (18)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
In1	0.00939 (13)	0.00917 (13)	0.01059 (13)	−0.00086 (10)	0.00358 (10)	−0.00067 (10)
In2	0.01051 (14)	0.00885 (13)	0.00893 (13)	0.00052 (11)	0.00267 (10)	0.00043 (10)
As1	0.0149 (2)	0.0097 (2)	0.0086 (2)	−0.00043 (17)	0.00253 (17)	0.00048 (15)
As2	0.0126 (2)	0.00937 (19)	0.00821 (19)	0.00074 (16)	0.00163 (16)	−0.00008 (15)
As3	0.0088 (2)	0.0096 (2)	0.0156 (2)	0.00034 (16)	0.00322 (17)	0.00050 (16)
As4	0.0083 (2)	0.00968 (19)	0.0118 (2)	0.00057 (16)	0.00176 (16)	−0.00085 (15)
As5	0.0101 (2)	0.0105 (2)	0.0120 (2)	−0.00028 (16)	0.00279 (16)	0.00020 (16)
As6	0.0114 (2)	0.0098 (2)	0.0100 (2)	0.00007 (16)	0.00235 (16)	−0.00102 (15)
O1	0.0265 (19)	0.0121 (15)	0.0079 (14)	0.0042 (14)	0.0036 (13)	−0.0029 (12)
O2	0.0187 (18)	0.0185 (17)	0.0128 (16)	−0.0053 (14)	0.0045 (13)	0.0020 (13)
O3	0.0156 (19)	0.035 (2)	0.0211 (19)	0.0050 (17)	0.0037 (15)	0.0078 (17)
O4	0.042 (2)	0.0101 (16)	0.0112 (16)	−0.0009 (16)	0.0055 (16)	−0.0006 (12)
O5	0.0219 (18)	0.0108 (15)	0.0086 (14)	−0.0037 (13)	0.0000 (13)	0.0008 (11)
O6	0.0189 (17)	0.0146 (16)	0.0116 (15)	0.0057 (13)	0.0031 (13)	−0.0018 (12)
O7	0.0128 (18)	0.037 (2)	0.021 (2)	0.0001 (16)	0.0037 (15)	0.0000 (17)
O8	0.0077 (15)	0.0158 (16)	0.0276 (19)	0.0029 (13)	0.0036 (14)	−0.0059 (14)
O9	0.0108 (16)	0.0171 (17)	0.0217 (18)	−0.0037 (13)	0.0029 (13)	0.0075 (14)
O10	0.020 (2)	0.033 (2)	0.0142 (17)	−0.0040 (17)	0.0045 (15)	−0.0016 (15)
O11	0.0105 (16)	0.0086 (15)	0.043 (2)	−0.0003 (13)	0.0066 (16)	0.0007 (15)
O12	0.0100 (16)	0.0213 (18)	0.0185 (17)	0.0031 (13)	0.0013 (13)	−0.0054 (14)
O13	0.0092 (15)	0.0131 (15)	0.0176 (16)	−0.0030 (12)	0.0009 (12)	0.0029 (13)
O14	0.024 (2)	0.033 (2)	0.0117 (17)	−0.0002 (17)	0.0021 (15)	0.0028 (15)
O15	0.0165 (17)	0.0118 (16)	0.0217 (18)	−0.0021 (13)	0.0088 (14)	−0.0025 (13)
O16	0.0164 (17)	0.0119 (15)	0.0191 (17)	0.0048 (13)	0.0063 (14)	0.0041 (13)
O17	0.0121 (16)	0.030 (2)	0.0181 (18)	−0.0018 (15)	0.0005 (14)	0.0015 (15)
O18	0.0192 (18)	0.029 (2)	0.0141 (16)	−0.0033 (15)	0.0103 (14)	0.0009 (15)
O19	0.0197 (18)	0.0128 (16)	0.0149 (16)	−0.0031 (13)	0.0050 (14)	−0.0032 (12)
O20	0.0186 (18)	0.0122 (15)	0.0177 (17)	0.0021 (13)	0.0058 (14)	0.0044 (13)
O21	0.0181 (18)	0.034 (2)	0.0096 (16)	0.0027 (16)	−0.0015 (14)	−0.0051 (15)
O22	0.0187 (18)	0.0192 (18)	0.0213 (18)	−0.0041 (15)	0.0077 (15)	−0.0053 (15)

Geometric parameters (Å, º)

In1—O8^i	2.098 (4)	As3—O10	1.701 (4)
In1—O15^ii	2.114 (4)	As3—O11	1.743 (4)
In1—O16	2.122 (4)	As4—O12	1.650 (4)
In1—O13^iii	2.142 (3)	As4—O13	1.651 (3)
In1—O6	2.145 (4)	As4—O14	1.709 (4)
In1—O2^ii	2.201 (4)	As4—O11	1.728 (4)
In2—O19	2.099 (4)	As5—O15	1.647 (4)
In2—O1^iv	2.110 (3)	As5—O16	1.664 (4)
In2—O20^iv	2.130 (4)	As5—O17	1.715 (4)
In2—O9^iv	2.143 (4)	As5—O18	1.718 (4)
In2—O5	2.148 (3)	As6—O19	1.654 (4)
In2—O12	2.190 (4)	As6—O20	1.657 (4)
As1—O1	1.648 (3)	As6—O21	1.712 (4)
As1—O2	1.660 (4)	As6—O22	1.714 (4)
As1—O3	1.691 (4)	O3—H3A	0.88 (4)
As1—O4	1.747 (4)	O3—H3B	0.88 (4)
As2—O5	1.651 (3)	O7—H7	0.86 (8)
As2—O6	1.653 (3)	O10—H10A	0.89 (4)
As2—O7	1.721 (4)	O10—H10B	0.89 (4)
As2—O4	1.726 (4)	O21—H21	0.86 (4)
As3—O8	1.648 (4)	O22—H22	0.87 (4)
As3—O9	1.657 (4)
O8^i—In1—O15^ii	88.30 (14)	O10—As3—O11	106.6 (2)
O8^i—In1—O16	93.93 (14)	O8—As3—H10B	134 (3)
O15^ii—In1—O16	174.56 (15)	O9—As3—H10B	104 (4)
O8^i—In1—O13^iii	178.09 (14)	O10—As3—H10B	29 (2)
O15^ii—In1—O13^iii	92.16 (14)	O11—As3—H10B	85 (3)
O16—In1—O13^iii	85.46 (14)	O12—As4—O13	116.89 (18)
O8^i—In1—O6	93.25 (15)	O12—As4—O14	111.5 (2)
O15^ii—In1—O6	91.97 (14)	O13—As4—O14	110.69 (19)
O16—In1—O6	92.87 (14)	O12—As4—O11	102.54 (19)
O13^iii—In1—O6	88.58 (14)	O13—As4—O11	108.15 (18)
O8^i—In1—O2^ii	89.12 (15)	O14—As4—O11	106.2 (2)
O15^ii—In1—O2^ii	88.41 (14)	O15—As5—O16	115.00 (19)
O16—In1—O2^ii	86.66 (14)	O15—As5—O17	110.4 (2)
O13^iii—In1—O2^ii	89.04 (14)	O16—As5—O17	107.88 (19)
O6—In1—O2^ii	177.61 (15)	O15—As5—O18	107.91 (19)
O19—In2—O1^iv	88.12 (14)	O16—As5—O18	111.48 (19)
O19—In2—O20^iv	176.74 (15)	O17—As5—O18	103.57 (19)
O1^iv—In2—O20^iv	94.84 (14)	O19—As6—O20	115.11 (19)
O19—In2—O9^iv	93.69 (14)	O19—As6—O21	109.1 (2)
O1^iv—In2—O9^iv	94.94 (15)	O20—As6—O21	109.8 (2)
O20^iv—In2—O9^iv	87.44 (14)	O19—As6—O22	108.55 (18)
O19—In2—O5	91.91 (14)	O20—As6—O22	110.97 (19)
O1^iv—In2—O5	176.90 (15)	O21—As6—O22	102.6 (2)
O20^iv—In2—O5	85.07 (14)	As1—O1—In2^v	130.7 (2)
O9^iv—In2—O5	88.15 (15)	As1—O2—In1^vi	127.1 (2)
O19—In2—O12	92.45 (14)	As1—O3—H3A	108 (9)
O1^iv—In2—O12	88.59 (15)	As1—O3—H3B	125 (9)
O20^iv—In2—O12	86.25 (14)	H3A—O3—H3B	86 (10)
O9^iv—In2—O12	173.01 (14)	As2—O4—As1	131.6 (2)
O5—In2—O12	88.31 (15)	As2—O5—In2	125.06 (19)
O1—As1—O2	115.77 (19)	As2—O6—In1	126.13 (19)
O1—As1—O3	107.6 (2)	As2—O7—H7	122 (5)
O2—As1—O3	115.3 (2)	As3—O8—In1^vii	127.7 (2)
O1—As1—O4	106.90 (18)	As3—O9—In2^v	125.7 (2)
O2—As1—O4	103.23 (19)	As3—O10—H10A	124 (9)
O3—As1—O4	107.3 (2)	As3—O10—H10B	83 (9)
O5—As2—O6	116.35 (18)	H10A—O10—H10B	140 (10)
O5—As2—O7	112.1 (2)	As4—O11—As3	131.6 (2)
O6—As2—O7	108.9 (2)	As4—O12—In2	128.4 (2)
O5—As2—O4	108.92 (17)	As4—O13—In1^iii	126.65 (19)
O6—As2—O4	105.14 (19)	As5—O15—In1^vi	137.5 (2)
O7—As2—O4	104.4 (2)	As5—O16—In1	131.3 (2)
O8—As3—O9	113.89 (19)	As6—O19—In2	134.9 (2)
O8—As3—O10	108.4 (2)	As6—O20—In2^v	133.5 (2)
O9—As3—O10	115.2 (2)	As6—O21—H21	119 (5)
O8—As3—O11	107.04 (18)	As6—O22—H22	109 (5)
O9—As3—O11	105.20 (19)

Symmetry codes: (i) x−1/2, −y+3/2, z+1/2; (ii) −x+3/2, y+1/2, −z+3/2; (iii) −x+2, −y+2, −z+1; (iv) −x+3/2, y+1/2, −z+1/2; (v) −x+3/2, y−1/2, −z+1/2; (vi) −x+3/2, y−1/2, −z+3/2; (vii) x+1/2, −y+3/2, z−1/2.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O3—H3A···O9^viii	0.88 (4)	2.11 (9)	2.853 (6)	142 (12)
O3—H3A···O15	0.88 (4)	2.60 (11)	3.235 (6)	130 (11)
O3—H3B···O3^viii	0.88 (4)	2.29 (8)	3.069 (9)	146 (11)
O7—H7···O7^iii	0.86 (8)	2.52 (8)	3.091 (9)	125 (6)
O7—H7···O12	0.86 (8)	2.21 (8)	2.944 (6)	143 (7)
O10—H10A···O6^vii	0.89 (4)	2.62 (13)	3.137 (6)	118 (11)
O10—H10A···O10^ix	0.89 (4)	2.13 (7)	2.961 (8)	155 (12)
O10—H10B···O18^x	0.89 (4)	2.59 (13)	3.134 (6)	120 (11)
O10—H10B···O20	0.89 (4)	2.26 (8)	3.085 (6)	153 (13)
O21—H21···O13^xi	0.86 (4)	1.95 (5)	2.702 (5)	147 (7)
O21—H21···O18^x	0.86 (4)	2.52 (7)	3.041 (6)	120 (6)
O22—H22···O7^xi	0.87 (4)	2.38 (6)	2.965 (6)	125 (6)
O22—H22···O12^v	0.87 (4)	2.41 (6)	3.100 (6)	137 (6)
O22—H22···O16^xi	0.87 (4)	2.42 (6)	2.952 (5)	120 (6)

Symmetry codes: (iii) −x+2, −y+2, −z+1; (v) −x+3/2, y−1/2, −z+1/2; (vii) x+1/2, −y+3/2, z−1/2; (viii) −x+2, −y+1, −z+1; (ix) −x+2, −y+1, −z; (x) x, y, z−1; (xi) x−1/2, −y+3/2, z−1/2.