Synthesis and Structure Description of a New Tetradecaborate [H_3N(CH_2)_2NH_3]_2[B_(14)O_(20)(OH)_6

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A new tetradecaborate, [H3N(CH2)2NH3]2[B14O20(OH)6](1), was synthesized by a boric acid ‘flux’ method, and characterized by X-ray powder diffraction, ICP, IR, TGA and DTA analyses. Single-crystal X-ray diffraction analysis showed that it crystallized in the monoclinic space group P1(No.2) with a=0.85092(10) nm, b=0.88678(11) nm, c=1.00724(13) nm, α=95.099(2)o, β=96.950(2)o, γ=116.845(2)o, V=0.66425(14) nm3, Z=2, R1=0.0625[I>2σ(I)], and wR2=0.1172(all data). The molecule structure of compound 1 comprises the isolated polyanion clusters [B14O20(OH)6]4– and diprotonated ethylenediamine molecules. Each polyanion cluster contains an 8-ring enclosed by six B3O3 3-ring units. Adjacent clusters are further connected with each other through strong hydrogen-bonding interactions of N(O)―H···O to form a three dimensional(3D) supramolecular structure with 2D pseudo channels along the [010] and [001] directions. The diprotonated ethylenediamine molecules located in the channels interact with the host through extensive hydrogen-bonds. Compound 1 presents few example containing isolated polyborate anions synthesized by a boric acid ‘flux’ method. A new tetradecaborate, [H3N (CH2) 2NH3] 2 [B14O20 (OH) 6] (1), was synthesized by a boric acid ’flux’ method, and characterized by X-ray powder diffraction, ICP, IR, TGA and DTA analyzes of single-crystal X-ray diffraction analysis showed that it crystallized in the monoclinic space group P1 (No.2) with a = 0.85092 (10) nm, b = 0.88678 (11) nm, α = 95.099 (2) o, β = 96.950 (2) o, γ = 116.845 (2) o, V = 0.66425 (14) nm3, Z = 2 and R1 = 0.0625 [I> 2σ = 0.1172 (all data). The molecule structure of compound 1 comprises the isolated polyanion clusters [B14O20 (OH) 6] 4- and diprotonated ethylenediamine molecules. Each polyanion cluster contains an 8-ring enclosed by six B3O3 3-ring units. Adjacent clusters are further connected with each other through strong hydrogen-bonding interactions of N (O) -H ··· O to form a three dimensional (3D) supramolecular structure with 2D pseudo channels along the [010] and [001] directions. The diprotonated ethylenediamine molecules located in the channels intera Compound 1 presents few example containing isolated polyborate anions synthesized by a boric acid ’flux’ method.
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