Two-dimensional dysprosium(III) triiodate(V) dihydrate, Dy(IO(3))(3)(H(2)O)·H(2)O.

During our research into novel nonlinear optical materials using 1,10-phenanthroline as an appending ligand on lanthanide iodates, crystals of an infinite layered Dy(III) iodate compound, Dy(IO(3))(3)(H(2)O)·H(2)O, were obtained under hydro-thermal conditions. The Dy(III) cation has a dicapped trigonal prismatic coordination environment consisting of one water O atom and seven other O atoms from seven iodate anions. These iodate anions bridge the Dy(III) cations into a two-dimensional structure. Through O-H⋯O hydrogen bonds, all of these layers stack along [111], giving a supra-molecular channel, with the solvent water mol-ecules filling the voids.

Related literature

For related materials with non-linear optical propertie, see: Rosenzweig & Morosin (1966 ▶); Liminga et al. (1977 ▶); Ok & Halasyamani (2005 ▶). The method of preparation was based on HIO3, which is different to the previous method of obtaining periodates (Douglas et al., 2004 ▶; Assefa et al., 2006 ▶). For noncentrosymmetric inorganic–organic framework structures synthesized from organic ligands, see: Sun et al. (2009 ▶). For related structrues, see: Sun et al. (2009 ▶); Assefa et al. (2006 ▶); Douglas et al. (2004 ▶); Ok & Halasyamani (2005 ▶); Chen et al. (2005 ▶).

Experimental

Crystal data

Dy(IO3)3H2O·H2O

M = 723.23

Triclinic,

a = 7.15990 (10) Å

b = 7.4292 (1) Å

c = 10.64430 (10) Å

α = 95.161 (12)°

β = 104.858 (7)°

γ = 110.081 (8)°

V = 504.00 (5) Å3

Z = 2

Mo Kα radiation

μ = 16.65 mm−1

T = 293 K

0.16 × 0.12 × 0.06 mm

Data collection

Rigaku R-AXIS RAPID diffractometer

Absorption correction: multi-scan (ABSCOR; Higashi, 1995 ▶) T min = 0.136, T max = 0.435 (expected range = 0.115–0.368)

3819 measured reflections

2260 independent reflections

2067 reflections with I > 2σ(I)

R int = 0.027

Refinement

R[F 2 > 2σ(F 2)] = 0.038

wR(F 2) = 0.109

S = 1.06

2260 reflections

141 parameters

2 restraints

H atoms treated by a mixture of independent and constrained refinement

Δρmax = 2.79 e Å−3

Δρmin = −3.20 e Å−3

Data collection: PROCESS-AUTO (Rigaku, 1998 ▶); cell refinement: PROCESS-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2004 ▶); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶) and PLATON (Spek, 2009 ▶; van der Sluis & Spek, 1990 ▶); molecular graphics: SHELXTL (Sheldrick, 2008 ▶); software used to prepare material for publication: SHELXTL.

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536809027068/br2111sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809027068/br2111Isup2.hkl

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

Dy(IO3)3H2O·H2O	Z = 2
Mr = 723.23	F(000) = 634
Triclinic, P1	Dx = 4.766 Mg m−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71075 Å
a = 7.1599 (1) Å	Cell parameters from 1561 reflections
b = 7.4292 (1) Å	θ = 2.0–27.5°
c = 10.6443 (1) Å	µ = 16.65 mm−1
α = 95.161 (12)°	T = 293 K
β = 104.858 (7)°	Block, colourless
γ = 110.081 (8)°	0.16 × 0.12 × 0.06 mm
V = 504.00 (5) Å3

Rigaku R-AXIS RAPID diffractometer	2260 independent reflections
Radiation source: fine-focus sealed tube	2067 reflections with I > 2σ(I)
graphite	Rint = 0.027
Detector resolution: 14.6306 pixels mm-1	θmax = 27.5°, θmin = 3.2°
CCD profile fitting scans	h = −9→9
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	k = −7→9
Tmin = 0.136, Tmax = 0.435	l = −13→13
3819 measured reflections

Refinement on F2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.038	H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.109	w = 1/[σ2(Fo2) + (0.0647P)2 + 5.3292P] where P = (Fo2 + 2Fc2)/3
S = 1.06	(Δ/σ)max < 0.001
2260 reflections	Δρmax = 2.79 e Å−3
141 parameters	Δρmin = −3.20 e Å−3
2 restraints	Extinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0126 (8)

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
Dy1	0.11491 (7)	−0.58338 (7)	−0.21096 (4)	0.01105 (18)
I1	0.30890 (8)	−0.14149 (8)	0.07303 (5)	0.00659 (18)
I2	0.28110 (8)	−0.63445 (8)	0.16834 (5)	0.00652 (18)
I3	0.27848 (9)	−0.26870 (9)	−0.45631 (6)	0.00862 (19)
O1	0.1496 (11)	−0.2711 (12)	−0.0929 (7)	0.0178 (15)
O2	0.0966 (11)	−0.1450 (11)	0.1365 (7)	0.0144 (14)
O3	0.3778 (11)	0.1033 (10)	0.0380 (7)	0.0134 (14)
O4	0.2940 (11)	−0.5350 (11)	0.0209 (7)	0.0155 (15)
O5	0.2291 (10)	−0.4405 (11)	0.2502 (7)	0.0131 (14)
O6	0.5556 (10)	−0.5510 (11)	0.2555 (7)	0.0121 (14)
O7	0.0908 (11)	−0.3710 (11)	−0.3699 (7)	0.0130 (14)
O8	0.1065 (11)	−0.1986 (11)	−0.5813 (7)	0.0125 (14)
O9	0.4335 (11)	−0.0352 (12)	−0.3515 (8)	0.0187 (16)
O10	0.2235 (12)	−0.8611 (12)	−0.2319 (8)	0.0185 (16)
H10A	0.198 (15)	−0.928 (9)	−0.179 (7)	0.028*
H10B	0.346 (4)	−0.8277 (13)	−0.221 (10)	0.028*
O11	0.2419 (13)	−0.7837 (13)	0.3943 (9)	0.0257 (18)
H11A	0.225 (3)	−0.897 (15)	0.3811 (19)	0.039*
H11B	0.144 (13)	−0.7725 (18)	0.412 (2)	0.039*

	U11	U22	U33	U12	U13	U23
Dy1	0.0094 (3)	0.0136 (3)	0.0131 (3)	0.00658 (19)	0.00455 (18)	0.00444 (19)
I1	0.0048 (3)	0.0061 (3)	0.0105 (3)	0.0031 (2)	0.0028 (2)	0.0041 (2)
I2	0.0040 (3)	0.0067 (3)	0.0111 (3)	0.0040 (2)	0.0027 (2)	0.0039 (2)
I3	0.0076 (3)	0.0109 (3)	0.0101 (3)	0.0063 (2)	0.0032 (2)	0.0026 (2)
O1	0.014 (3)	0.023 (4)	0.012 (3)	0.010 (3)	−0.004 (3)	−0.002 (3)
O2	0.011 (3)	0.014 (4)	0.022 (4)	0.006 (3)	0.009 (3)	0.007 (3)
O3	0.020 (3)	0.006 (3)	0.020 (4)	0.007 (3)	0.011 (3)	0.006 (3)
O4	0.019 (4)	0.013 (4)	0.014 (3)	0.006 (3)	0.005 (3)	0.006 (3)
O5	0.006 (3)	0.014 (4)	0.021 (4)	0.005 (3)	0.007 (3)	0.002 (3)
O6	0.001 (3)	0.016 (4)	0.018 (3)	0.002 (3)	0.003 (3)	0.007 (3)
O7	0.014 (3)	0.020 (4)	0.013 (3)	0.012 (3)	0.007 (3)	0.013 (3)
O8	0.014 (3)	0.013 (4)	0.013 (3)	0.005 (3)	0.007 (3)	0.006 (3)
O9	0.011 (3)	0.018 (4)	0.022 (4)	0.005 (3)	0.000 (3)	−0.002 (3)
O10	0.022 (4)	0.023 (4)	0.025 (4)	0.019 (3)	0.013 (3)	0.011 (3)
O11	0.022 (4)	0.022 (4)	0.034 (5)	0.007 (4)	0.012 (4)	0.005 (4)

Dy1—O4	2.401 (7)	I2—O6	1.798 (6)
Dy1—O2i	2.408 (7)	I2—O4	1.804 (7)
Dy1—O8ii	2.412 (7)	I2—O5	1.812 (7)
Dy1—O6iii	2.415 (6)	I3—O9	1.783 (8)
Dy1—O7	2.429 (6)	I3—O8	1.812 (7)
Dy1—O1	2.438 (8)	I3—O7	1.813 (7)
Dy1—O10	2.453 (7)	O2—Dy1i	2.408 (7)
Dy1—O5i	2.461 (6)	O5—Dy1i	2.461 (6)
I1—O1	1.804 (7)	O6—Dy1iii	2.415 (6)
I1—O2	1.809 (7)	O8—Dy1ii	2.412 (7)
I1—O3	1.814 (7)
O4—Dy1—O2i	75.1 (2)	O7—Dy1—O10	126.1 (2)
O4—Dy1—O8ii	149.7 (2)	O1—Dy1—O10	151.9 (2)
O2i—Dy1—O8ii	78.5 (2)	O4—Dy1—O5i	112.2 (2)
O4—Dy1—O6iii	90.6 (2)	O2i—Dy1—O5i	73.6 (2)
O2i—Dy1—O6iii	142.8 (2)	O8ii—Dy1—O5i	73.6 (2)
O8ii—Dy1—O6iii	101.7 (2)	O6iii—Dy1—O5i	142.8 (2)
O4—Dy1—O7	135.1 (3)	O7—Dy1—O5i	72.9 (2)
O2i—Dy1—O7	141.9 (2)	O1—Dy1—O5i	69.4 (2)
O8ii—Dy1—O7	75.1 (2)	O10—Dy1—O5i	132.9 (3)
O6iii—Dy1—O7	70.3 (2)	O1—I1—O2	96.8 (3)
O4—Dy1—O1	69.2 (2)	O1—I1—O3	97.2 (3)
O2i—Dy1—O1	111.8 (3)	O2—I1—O3	97.7 (3)
O8ii—Dy1—O1	136.0 (2)	O6—I2—O4	99.6 (3)
O6iii—Dy1—O1	93.9 (3)	O6—I2—O5	97.8 (3)
O7—Dy1—O1	72.0 (2)	O4—I2—O5	95.5 (3)
O4—Dy1—O10	84.5 (3)	O9—I3—O8	99.4 (3)
O2i—Dy1—O10	68.8 (3)	O9—I3—O7	101.4 (3)
O8ii—Dy1—O10	72.1 (2)	O8—I3—O7	96.1 (3)
O6iii—Dy1—O10	75.9 (3)

D—H···A	D—H	H···A	D···A	D—H···A
O10—H10A···O3iv	0.80	2.29	2.873 (10)	131
O10—H10B···O9iv	0.80	2.33	2.753 (11)	114
O11—H11A···O8v	0.80	2.22	2.954 (11)	153
O11—H11B···O7i	0.80	2.26	2.946 (11)	145

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O10—H10A⋯O3i	0.80	2.29	2.873 (10)	131
O10—H10B⋯O9i	0.80	2.33	2.753 (11)	114
O11—H11A⋯O8ii	0.80	2.22	2.954 (11)	153
O11—H11B⋯O7iii	0.80	2.26	2.946 (11)	145

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