Ethyl­enediammonium bis­(dihydrogenarsenate): R₄³(14) loops built up from O—H...O hydrogen bonds

The title compound, C₂H₁₀N₂²⁺·2H₂AsO₄⁻, contains a network of centrosymmetric doubly protonated ethyl­ene­diammonium cations and dihydogenarsenate anions. The component species inter­act by way of cation-to-anion N—H...O and anion-to-anion O—H...O hydrogen bonds, the latter leading to infinite (001) sheets of the (H₂AsO₄)⁻ anions containing unusual R₄³(14) loops.

Key indicators

• Single-crystal X-ray study
• T = 293 K
• Mean [sigma](C-C) = 0.002 Å
• R factor = 0.020
• wR factor = 0.051
• Data-to-parameter ratio = 27.0

checkCIF/PLATON results

No syntax errors found



Alert level B
PLAT411_ALERT_2_B Short Inter H...H Contact  H3     ..  H3      ..       2.09 Ang.

Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT062_ALERT_4_C Rescale T(min) & T(max) by .....................       0.98

Alert level G
PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature        293 K
PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature .        293 K

   0 ALERT level A = In general: serious problem
   1 ALERT level B = Potentially serious problem
   2 ALERT level C = Check and explain
   2 ALERT level G = General alerts; check

   3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   1 ALERT type 2 Indicator that the structure model may be wrong or deficient
   0 ALERT type 3 Indicator that the structure quality may be low
   1 ALERT type 4 Improvement, methodology, query or suggestion
   0 ALERT type 5 Informative message, check

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Computing details

Data collection: SMART (Bruker, 1999); cell refinement: SAINT (Bruker, 1999); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: SHELXL97.

Ethylenediammonium bis(dihydrogenarsenate)

Crystal data

C2H10N2^2+·2AsH2O4^−	F(000) = 340
Mr = 343.98	Dx = 2.320 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 4016 reflections
a = 4.8971 (3) Å	θ = 2.3–32.5°
b = 8.8054 (5) Å	µ = 6.81 mm^−1
c = 11.4894 (6) Å	T = 293 K
β = 96.381 (1)°	Blade, colourless
V = 492.36 (5) Å^3	0.41 × 0.16 × 0.05 mm
Z = 2

Data collection

Bruker SMART1000 CCD area-detector diffractometer	1783 independent reflections
Radiation source: fine-focus sealed tube	1525 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.020
ω scans	θmax = 32.7°, θmin = 2.9°
Absorption correction: multi-scan (SADABS; Bruker, 1999)	h = −7→6
Tmin = 0.166, Tmax = 0.726	k = −13→13
5015 measured reflections	l = −17→15

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: difmap and geom
R[F^2 > 2σ(F^2)] = 0.020	H-atom parameters constrained
wR(F^2) = 0.051	w = 1/[σ^2(Fo^2) + (0.028P)^2 + 0.0051P] where P = (Fo^2 + 2Fc^2)/3
S = 1.06	(Δ/σ)max = 0.001
1783 reflections	Δρmax = 0.38 e Å^−3
66 parameters	Δρmin = −0.72 e Å^−3
0 restraints	Extinction correction: SHELXL97 (Sheldrick, 1997), Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0075 (10)

Special details

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
As1	0.40423 (3)	0.114763 (17)	0.171802 (14)	0.01641 (6)
O1	0.2873 (3)	0.22888 (15)	0.27646 (13)	0.0323 (3)
H1	0.3012	0.3290	0.2667	0.039*
O2	0.1638 (3)	−0.02569 (15)	0.16072 (13)	0.0307 (3)
H2	−0.0045	0.0063	0.1779	0.037*
O3	0.6920 (2)	0.03393 (15)	0.23023 (11)	0.0255 (3)
O4	0.4120 (3)	0.20611 (16)	0.04810 (11)	0.0280 (3)
C1	0.8817 (3)	0.0462 (2)	0.51576 (17)	0.0239 (3)
H3	0.7115	−0.0084	0.4944	0.029*
H4	0.9003	0.0633	0.5997	0.029*
N1	0.8731 (3)	0.19290 (17)	0.45429 (13)	0.0231 (3)
H5	0.7330	0.2477	0.4744	0.028*
H6	0.8515	0.1770	0.3773	0.028*
H7	1.0295	0.2428	0.4739	0.028*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
As1	0.01382 (8)	0.01548 (9)	0.02023 (9)	−0.00028 (6)	0.00327 (5)	0.00022 (6)
O1	0.0448 (8)	0.0201 (7)	0.0356 (7)	−0.0029 (6)	0.0201 (6)	−0.0071 (5)
O2	0.0210 (6)	0.0212 (6)	0.0517 (9)	−0.0065 (5)	0.0124 (6)	−0.0114 (6)
O3	0.0171 (5)	0.0299 (7)	0.0289 (6)	0.0037 (5)	0.0005 (5)	0.0048 (5)
O4	0.0252 (6)	0.0331 (7)	0.0259 (6)	0.0029 (5)	0.0042 (5)	0.0107 (5)
C1	0.0210 (7)	0.0206 (8)	0.0312 (9)	0.0041 (6)	0.0081 (6)	0.0065 (7)
N1	0.0247 (7)	0.0209 (7)	0.0238 (7)	0.0029 (5)	0.0028 (5)	0.0030 (5)

Geometric parameters (Å, º)

As1—O4	1.6372 (12)	C1—C1^i	1.493 (3)
As1—O3	1.6532 (12)	C1—H3	0.9700
As1—O2	1.7026 (13)	C1—H4	0.9700
As1—O1	1.7136 (13)	N1—H5	0.8900
O1—H1	0.8920	N1—H6	0.8900
O2—H2	0.9131	N1—H7	0.8900
C1—N1	1.470 (2)
O4—As1—O3	117.58 (6)	C1^i—C1—H3	109.6
O4—As1—O2	111.99 (7)	N1—C1—H4	109.6
O3—As1—O2	105.59 (7)	C1^i—C1—H4	109.6
O4—As1—O1	111.28 (7)	H3—C1—H4	108.1
O3—As1—O1	107.68 (7)	C1—N1—H5	109.5
O2—As1—O1	101.32 (7)	C1—N1—H6	109.5
As1—O1—H1	117.1	H5—N1—H6	109.5
As1—O2—H2	113.1	C1—N1—H7	109.5
N1—C1—C1^i	110.14 (17)	H5—N1—H7	109.5
N1—C1—H3	109.6	H6—N1—H7	109.5

Symmetry code: (i) −x+2, −y, −z+1.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O2—H2···O3^ii	0.91	1.68	2.5810 (18)	168
O1—H1···O3^iii	0.89	1.81	2.689 (2)	171
N1—H5···O4^iv	0.89	1.91	2.7554 (19)	158
N1—H6···O3	0.89	2.18	2.978 (2)	149
N1—H7···O4^v	0.89	2.02	2.8783 (19)	162

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