Redetermination of (NH(4))(2)HAsO(4).

In comparison with the original determination based on Weissenberg film data [Khan et al. (1970 ▶). Acta Cryst. B26, 1889-1892], the current redetermination of diammonium hydrogenarsenate(V) reveals all atoms with anisotropic displacement parameters and all H atoms localized. This allowed an unambiguous assignment of the hydrogen-bonding pattern, which is similar to that of the isotypic phosphate analogue (NH(4))(2)HPO(4). The structure of the title compound consists of slightly distorted AsO(3)(OH) and NH(4) tetra-hedra, linked into a three-dimensional structure by an extensive network of O-H⋯O and N-H⋯O hydrogen bonds.

Related literature

For the previous determination of (NH4)2HAsO4, see: Khan et al. (1970 ▶). The arsenate compound is isotypic with the phosphate analogue (NH4)2HPO4 (Khan et al., 1972 ▶), for which another modification with Z′ = 2 has also recently been described (Kunz et al., 2010 ▶).

Experimental

Crystal data

(NH4)2HAsO4

M = 176.01

Monoclinic,

a = 11.3426 (4) Å

b = 6.8512 (3) Å

c = 8.1130 (3) Å

β = 113.784 (4)°

V = 576.92 (4) Å3

Z = 4

Mo Kα radiation

μ = 5.82 mm−1

T = 293 K

0.14 × 0.12 × 0.02 mm

Data collection

Bruker APEXII CCD diffractometer

Absorption correction: multi-scan (SADABS; Bruker, 2009 ▶) T min = 0.496, T max = 0.873

6318 measured reflections

1674 independent reflections

1413 reflections with I > 2σ(I)

R int = 0.033

Refinement

R[F 2 > 2σ(F 2)] = 0.022

wR(F 2) = 0.055

S = 1.04

1676 reflections

101 parameters

All H-atom parameters refined

Δρmax = 0.59 e Å−3

Δρmin = −0.84 e Å−3

Data collection: APEX2 (Bruker, 2009 ▶); cell refinement: SAINT (Bruker, 2009 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: ATOMS (Dowty, 2006) ▶; software used to prepare material for publication: publCIF (Westrip, 2010 ▶).

Click here for additional data file.

Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536812043565/hb6976sup1.cif

Click here for additional data file.

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536812043565/hb6976Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

(NH4)2HAsO4	F(000) = 352
Mr = 176.01	Dx = 2.026 Mg m−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 2800 reflections
a = 11.3426 (4) Å	θ = 3.6–30.0°
b = 6.8512 (3) Å	µ = 5.82 mm−1
c = 8.1130 (3) Å	T = 293 K
β = 113.784 (4)°	Plate, colourless
V = 576.92 (4) Å3	0.14 × 0.12 × 0.02 mm
Z = 4

Bruker APEXII CCD diffractometer	1674 independent reflections
Radiation source: fine-focus sealed tube	1413 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.033
ω– and φ–scans	θmax = 30.0°, θmin = 2.0°
Absorption correction: multi-scan (SADABS; Bruker, 2009)	h = −15→15
Tmin = 0.496, Tmax = 0.873	k = −6→9
6318 measured reflections	l = −11→10

Refinement on F2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.022	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.055	All H-atom parameters refined
S = 1.04	w = 1/[σ2(Fo2) + (0.0304P)2] where P = (Fo2 + 2Fc2)/3
1676 reflections	(Δ/σ)max = 0.001
101 parameters	Δρmax = 0.59 e Å−3
0 restraints	Δρmin = −0.84 e Å−3

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

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

	x	y	z	Uiso*/Ueq
As1	0.249593 (18)	0.89261 (3)	0.42786 (3)	0.00648 (7)
O1	0.20879 (15)	0.9789 (2)	0.2115 (2)	0.0126 (3)
O2	0.25894 (13)	0.0977 (2)	0.5442 (2)	0.0098 (3)
O3	0.38858 (13)	0.7692 (2)	0.4982 (2)	0.0114 (3)
O4	0.13017 (13)	0.7484 (2)	0.4289 (2)	0.0098 (3)
N1	0.44933 (18)	0.1231 (3)	0.1532 (3)	0.0111 (3)
N2	0.12140 (18)	0.3798 (3)	0.2643 (3)	0.0100 (3)
H1N1	0.494 (3)	0.131 (3)	0.275 (4)	0.017 (7)*
H2N1	0.422 (2)	0.003 (4)	0.114 (4)	0.013 (6)*
H3N1	0.388 (3)	0.209 (4)	0.117 (4)	0.022 (7)*
H4N1	0.509 (3)	0.167 (4)	0.111 (4)	0.016 (7)*
H1N2	0.118 (3)	0.491 (5)	0.302 (4)	0.020 (7)*
H2N2	0.169 (3)	0.392 (3)	0.201 (4)	0.013 (7)*
H3N2	0.046 (3)	0.336 (4)	0.209 (4)	0.022 (7)*
H4N2	0.164 (2)	0.297 (4)	0.358 (4)	0.013 (6)*
H1O	0.186 (3)	0.907 (4)	0.139 (5)	0.032 (10)*

	U11	U22	U33	U12	U13	U23
As1	0.00865 (10)	0.00455 (11)	0.00669 (11)	0.00021 (7)	0.00355 (7)	−0.00027 (8)
O1	0.0228 (7)	0.0084 (8)	0.0071 (7)	−0.0016 (6)	0.0064 (6)	−0.0004 (6)
O2	0.0134 (7)	0.0062 (7)	0.0105 (7)	−0.0002 (5)	0.0056 (6)	−0.0026 (6)
O3	0.0102 (6)	0.0113 (7)	0.0131 (7)	0.0031 (5)	0.0051 (6)	0.0011 (6)
O4	0.0111 (6)	0.0068 (7)	0.0119 (7)	−0.0018 (5)	0.0051 (5)	0.0003 (6)
N1	0.0117 (8)	0.0096 (9)	0.0123 (9)	0.0008 (7)	0.0052 (7)	0.0006 (7)
N2	0.0121 (8)	0.0071 (9)	0.0120 (9)	0.0003 (7)	0.0059 (7)	−0.0005 (7)

As1—O2i	1.6718 (14)	N1—H2N1	0.89 (3)
As1—O3	1.6732 (14)	N1—H3N1	0.87 (3)
As1—O4	1.6793 (14)	N1—H4N1	0.92 (3)
As1—O1	1.7293 (15)	N2—H1N2	0.83 (3)
O1—H1O	0.73 (3)	N2—H2N2	0.89 (3)
O2—As1ii	1.6718 (14)	N2—H3N2	0.85 (3)
N1—H1N1	0.91 (3)	N2—H4N2	0.92 (3)
O2i—As1—O3	113.29 (7)	H1N1—N1—H4N1	103 (2)
O2i—As1—O4	111.04 (7)	H2N1—N1—H4N1	112 (2)
O3—As1—O4	110.62 (7)	H3N1—N1—H4N1	105 (2)
O2i—As1—O1	102.46 (7)	H1N2—N2—H2N2	105 (2)
O3—As1—O1	110.40 (7)	H1N2—N2—H3N2	110 (3)
O4—As1—O1	108.67 (7)	H2N2—N2—H3N2	116 (3)
As1—O1—H1O	117 (3)	H1N2—N2—H4N2	111 (3)
H1N1—N1—H2N1	114 (2)	H2N2—N2—H4N2	107 (2)
H1N1—N1—H3N1	110 (2)	H3N2—N2—H4N2	108 (2)
H2N1—N1—H3N1	113 (3)

D—H···A	D—H	H···A	D···A	D—H···A
N1—H3N1···O2iii	0.87 (3)	1.88 (3)	2.750 (2)	178 (3)
N1—H1N1···O3iv	0.91 (3)	1.91 (3)	2.780 (3)	158 (2)
N1—H2N1···O3iii	0.89 (3)	2.06 (3)	2.930 (3)	167 (2)
N1—H4N1···O3v	0.92 (3)	1.86 (3)	2.777 (2)	173 (3)
N2—H4N2···O2	0.92 (3)	2.00 (3)	2.910 (2)	174 (2)
N2—H2N2···O2iii	0.89 (3)	1.93 (3)	2.809 (2)	174 (2)
N2—H1N2···O4	0.83 (3)	2.02 (3)	2.840 (2)	171 (3)
N2—H3N2···O4vi	0.85 (3)	1.95 (3)	2.793 (2)	176 (3)
O1—H1O···O4vii	0.73 (3)	1.89 (3)	2.613 (2)	171 (4)

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
N1—H3N1⋯O2i	0.87 (3)	1.88 (3)	2.750 (2)	178 (3)
N1—H1N1⋯O3ii	0.91 (3)	1.91 (3)	2.780 (3)	158 (2)
N1—H2N1⋯O3i	0.89 (3)	2.06 (3)	2.930 (3)	167 (2)
N1—H4N1⋯O3iii	0.92 (3)	1.86 (3)	2.777 (2)	173 (3)
N2—H4N2⋯O2	0.92 (3)	2.00 (3)	2.910 (2)	174 (2)
N2—H2N2⋯O2i	0.89 (3)	1.93 (3)	2.809 (2)	174 (2)
N2—H1N2⋯O4	0.83 (3)	2.02 (3)	2.840 (2)	171 (3)
N2—H3N2⋯O4iv	0.85 (3)	1.95 (3)	2.793 (2)	176 (3)
O1—H1O⋯O4v	0.73 (3)	1.89 (3)	2.613 (2)	171 (4)

Symmetry codes: (i) ; (ii) ; (iii) ; (iv) ; (v) .