Potassium deca­borate monohydrate

Yi-Hong Gao

doi:10.1107/S1600536811039109

. 2011 Sep 30;67(Pt 10):i57. doi: 10.1107/S1600536811039109

Potassium decaborate monohydrate

Yi-Hong Gao ^a,^*

PMCID: PMC3201280 PMID: 22058681

Abstract

In the crystal structure of the title compound, K₂[B₁₀O₁₄(OH)₄]·H₂O, the polyborate [B₁₀O₁₄(OH)₄]²⁻ anions are linked together through their common O atoms, forming a helical chain-like structure. Adjacent chains are further connected into a three-dimensional structure by O—H⋯O hydrogen bonds. The water molecules and potassium cations are located between these chains. Further O—H⋯O hydrogen bonds occur between the anions and the water molecules

Related literature

For phases previously obtained in the K₂O—B₂O₃—H₂O system, see: Marezio (1969 ▶); Marezio et al. (1963 ▶); Dewey et al. (1975 ▶); Salentine (1987 ▶); Touboul et al. (2003 ▶); Zhang et al. (2005 ▶); Wang et al. (2006 ▶); Li et al. (2007 ▶). For a closely related structure, (NH₄)₂[B₁₀O₁₄(OH)₄]·H₂O, see: Li et al. (2003 ▶). For the non-linear optical properties of alkali metal borates, see: Mori et al. (1995 ▶).

Experimental

Crystal data

K₂[B₁₀O₁₄(OH)₄]·H₂O
M _r = 496.35
Triclinic,
a = 7.5612 (7) Å
b = 9.2236 (10) Å
c = 11.7298 (13) Å
α = 99.038 (6)°
β = 106.595 (6)°
γ = 91.314 (6)°
V = 772.26 (14) Å³
Z = 2
Mo Kα radiation
μ = 0.72 mm⁻¹
T = 100 K
0.16 × 0.08 × 0.05 mm

Data collection

Bruker APEXII diffractometer
Absorption correction: numerical (SADABS, Sheldrick, 2008a ▶) T _min = 0.895, T _max = 0.962
11219 measured reflections
3148 independent reflections
2141 reflections with I > 2σ(I)
R _int = 0.055

Refinement

R[F ² > 2σ(F ²)] = 0.045
wR(F ²) = 0.113
S = 1.00
3148 reflections
298 parameters
5 restraints
All H-atom parameters refined
Δρ_max = 0.42 e Å⁻³
Δρ_min = −0.46 e Å⁻³

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

Supplementary Material

Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536811039109/ru2014sup1.cif

e-67-00i57-sup1.cif^{(38.5KB, cif)}

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536811039109/ru2014Isup2.hkl

e-67-00i57-Isup2.hkl^{(154.4KB, hkl)}

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

Table 1. Hydrogen-bond geometry (Å, °).

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1—H1⋯O11ⁱ	0.88 (2)	1.76 (2)	2.599 (3)	159 (3)
O9—H9⋯O18ⁱⁱ	0.87 (2)	1.98 (2)	2.797 (3)	157 (3)
O11—H11⋯O19ⁱⁱⁱ	0.92 (2)	1.65 (2)	2.553 (3)	167 (3)
O18—H18⋯O5^iv	0.89 (2)	2.10 (2)	2.940 (3)	157 (3)
O18—H18⋯O12^iv	0.89 (2)	2.66 (3)	3.193 (3)	119 (3)
O19—H19A⋯O6^v	0.90 (2)	1.79 (3)	2.678 (3)	169 (3)
O19—H19B⋯O16^vi	0.91 (2)	1.79 (3)	2.696 (3)	173 (3)

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

Acknowledgments

This project was supported by the National Natural Science Foundation of China (No. 20871078).

supplementary crystallographic information

Comment

Boron can form many compounds because of the complexity of the structures involved. In the past several decades, much interest has focused on studies of alkali metals borates because some of these compounds show interesting physical properties, such as nonlinear optical behavior for CsLiB₆O₁₀ (Mori et al., 1995). So far, several phases had been obtained in the K₂O—B₂O₃—H₂O system (Marezio et al., 1963; Marezio, 1969; Dewey et al., 1975; Salentine,1987; Touboul et al., 2003; Zhang et al., 2005; Wang et al., 2006; Li et al., 2007). In this paper, we describe the synthesis and the crystal structure of a new potassium borate of K₂[B₁₀O₁₄(OH)₄]^.H₂O.

Single crystal diffraction has revealed that the title compound crystallizes in the triclinic space group P-1. It is composed of two K₊ cation and polyborate anion [B₁₀O₁₄(OH)₄]_2- (Fig.1), which is closely related to the reported compound of (NH₄)₂[B₁₀O₁₄(OH)₄]^.H₂O (Li et al., 2003).

The [B₁₀O₁₄(OH)₄]_2- anion could be considered as two [B₅O₇(OH)₂]_- cluster linked by the common oxygen atom (O3). Each of the [B₅O₇(OH)₂]_- cluster consists of two six-membered rings linked by a common BO₄ tetrahedron. Each six-membered ring consists of one BO₃ triangle, one BO₂(OH) triangle and a common BO₄ tetrahedron. The [B₁₀O₁₄(OH)₄]_2- units are linked together through common oxygen atoms (O17) to neighboring units, forming a 1-D helical chainlike structure (Fig. 2). Adjacent chains are further connected into a three-dimensional structure by O—H···O hydrogen bonds interactions (Fig.3). Water molecules and potassium ions are located among these chains. In addition, there exist O—H···O hydrogen bonds between the oxygen atoms in polyborate anions and Water molecules (Table 1).

Experimental

All reagents used in the synthesis were of analytic grade and were used without further purification. A mixture of K₂TeO₄ (0.216 g) and H₃BO₃ (0.992 g) was sealed in a teflon-lined bomb and heated at 473 K for 5 days and then cooled to room temperature. The resulting colorless and transparent crystals were recovered by washed with deionized water and dried at room temperature.