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K2sbb3o8: a Novel Boroantimonate with Isolated [B3O8] Groups No

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K2sbb3o8: a Novel Boroantimonate with Isolated [B3O8] Groups No 35 卷 8 期 结 构 化 学 （JIEGOU HUAXUE） Vol. 35, No. 8 2016. 8 Chinese J. Struct. Chem. 1269─1276 K2SbB3O8: A Novel Boroantimonate 7- ① with Isolated [B3O8] Groups SHEN Yao-Guoa ZHAO San-Genb LUO Jun-Huab② a (Department of Physics and Electronic Information Engineering, Minjiang University, Fuzhou 350108, China) b (Key Laboratory of Optoelectronic Materials Chemistry and Physics, Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences, Fuzhou 350002, China) ABSTRACT A new boroantimonate K2SbB3O8 has been synthesized by high-temperature solid- state reactions, and its crystals have been obtained by the flux method. The crystal structure has been determined from single-crystal X-ray diffraction analysis. The compound crystallizes in the monoclinic space group P21/c with a = 5.8890(2), b = 11.0512(4), c = 10.8951(4) Å, β = 3 3 103.200(4)°, V = 690.32(4) Å , Z = 4, F(000) = 672, ρc = 3.467 g/cm , Mr = 360.38 and μ = 5.215 -1 mm . Its structure feature is a three-dimensional framework composed of SbO6 octahedra and 7- + isolated [B3O8] groups with K cations residing in the one-dimensional tunnels along the a-axis. 7- 7- Interestingly, the isolated [B3O8] groups are distinct from the known [B3O8] groups, which always connect to each other. The UV-vis-NIR absorption, thermal stability and infrared spectrum are also discussed in this paper. Keywords: borate, crystal structure, isolated group, infrared spectrum; DOI: 10.14102/j.cnki.0254-5861.2011-1143 [5] [6] 1 INTRODUCTION optical materials, such as β-BaB2O4 , LiB3O5 , [7] and CsB3O5 . This structural diversity endows the In the past few decades, metal borates have borates various properties and functions. A newest attracted great interest owing to their rich structural example is KZnB3O6. The borate exhibits an 3- chemistry and important applications in the field of unusual [B3O6] group (composed of two edged- materials science such as phosphors, nonlinear sharing BO4 tetrahedra), which leads to extraor- optics, and optoelectronic applications[1-4]. They dinary unidirectional thermal expansion phenomena 3- 5- [8] often take [BO3] planar triangles or [BO4] in KZnB3O6 . Therefore, the search for new tetrahedra as the basic structural element, which borates with novel structures is not only important could be further connected to each other to con- for the structural chemistry but also favorable for stitute various patterns of connection and arrange- the explorations of new functional materials. ment. Common derivative groups are as follows: A general strategy of designing new borates is to 3- 3- 5- [BO3] , [B3O6] and [B3O7] , which have been introduce metal ions with high coordination ability found in crystal structures of a number of nonlinear into the structural units of borates, which can adjust Received 20 January 2016; accepted 14 April 2016 (CCDC 1438577) ① Supported by NSFC (21171166, 21222102, 21301172, 21373220, 21571178, 21525104, 51277091, 51402296, 51502288 and 51502290), Chunmiao Project of Haixi Institute of Chinese Academy of Sciences (CMZX-2015-003) and NSF of Fujian Province (2015J01219, 2015J05040) ② Corresponding author. E-mail: [email protected] 7- 1270 SHEN Y. G. et al.: K2SbB3O8: A Novel Boroantimonate with Isolated [B3O8] Groups No. 8 the connection modes of B–O groups. These units KNO3 (Aladdin, 99.0%), K2CO3 (Aladdin, 99%), may include distorted octahedra of d0 cation centers CsNO3 (Aladdin, 99.0%), Sb2O3 (Sinopharm, 4+ 5+ 5+ 6+ 3+ (Ti , Nb , V , Mo , etc.), lone pair cations (Bi , 99.0%), and H3BO3 (Aladdin, ≥99.5%) were used 2+ 2+ 2+ Pb , etc.), or d10 cations (Cd , Zn , etc.), which as received. [2, 3, 9-14] are also nonlinear optical active units . 2. 2 Synthesis of K2SbB3O8 Among them, the A–Sb–B–O (A = alkaline metal or Pure polycrystalline samples of K2SbB3O8 were alkaline earth metal) systems are still rarely obtained via the conventional high temperature investigated[15]. Recently, Mao and his co-workers solid-state reactions. A stoichiometric mixture of -3 discovered several boroantimonates, including 0.51 g KNO3 (5.04 × 10 mol), 0.36 g Sb2O3 [16] -3 K3BSb4O13 and KSbB2O6 , which show interes- (1.23 × 10 mol), and 0.48 g H3BO3 (7.74 × -3 ting structures with edge-sharing Sb2O10 dimers and 10 mol) was ground well using an agate mortar 4- [B2O5] groups, respectively. and then put into a platinum crucible. It will be Herein, we report a new boroantimonate heated to 773 K at a rate of 50 K/h to be sintered for K2SbB3O8 who features a three-dimensional frame- 24 h, cooled and ground, sintered again at 1073 K work composed of SbO6 octahedra and isolated for 120 h with several intermediate grindings, and 7- 7- [B3O8] groups. Remarkably, the isolated [B3O8] then cooled slowly to 273 K at a rate of 3 K/h. The 7- groups are distinct from the known [B3O8] groups, product was found to be a single phase of poly- which are always connected to each other. In crystalline K2SbB3O8 powders, which was con- addition, the synthesis, crystal growth, infrared firmed by powder X-ray diffraction (XRD) analysis spectrum, UV-vis-NIR diffuse reflectance spectrum, on a Rigaku MiniFlex II diffractometer equipped and thermal behavior of K2SbB3O8 are also reported with CuKα radiation. The scanning 2θ range is 7～ in this paper. 70° with step size of 0.02° and fixed scanning rate of 0.12°/min. The measured powder XRD pattern is 2 EXPERIMENTAL in good agreement with that of the simulated one from single-crystal data (Fig. 1). 2. 1 Reagents Fig. 1. Experimental and simulated X-ray powder diffraction patterns for K2SbB3O8 2. 3 Crystal growth spontaneous crystallization technique using Cs2O- -3 Single crystals of K2SbB3O8 were grown from K2O-B2O3 as a flux. CsNO3 (8.88 × 10 mol), 2016 Vol. 35 结 构 化 学（JIEGOU HUAXUE）Chinese J. Struct. Chem. 1271 -3 Sb2O3 (1.11 × 10 mol), and H3BO3 (11.10 × were collected by means of graphite-monochro- 10-3 mol) were first ground and subsequently loaded matized MoKα radiation (λ = 0.71073 Å) at 100(2) into a platinum crucible. It was gradually heated to K on an Agilent SuperNova Dual diffractometer 873 K in a temperature-programmable electric fur- with an Atlas detector. The collection of the inten- nace, dwelt for 2 d, and cooled to room temperature sity data, cell refinement, and data reduction were for further grinding, which was named powdered I. carried out with the program CrysAlisPro[17]. A total -3 Powdered I, K2CO3 (14.47 × 10 mol), and of 4348 reflections were collected in the range of -3 H3BO3 (32.26 × 10 mol) were mixed together in 3.55<θ<26.37° (–7≤h≤7, –13≤k≤13, –13≤h≤ the same crucible. The above mixture was heated to 13), of which 1413 were independent (Rint = 0.0299) 1273 K, following a dwelling of 2 h to assure that and 1294 were observed with I > 2σ(I). The struc- the melt is homogeneous and transparent. The ture was solved by direct methods with program cooling temperature process is divided three steps, SHELXS and refined with the least-squares pro- which include initial crystallization temperature gram SHELXL[18]. Final refinement includes aniso- (1173 K), final crystallization temperature (1073 K) tropic displacement parameters. The structure was and room temperature. In these steps, the verified using the ADDSYM algorithm from the corresponding cooling down rate is rapid (15 K/h), program PLATON[19], and no higher symmetries slow (4.5 K/h) and rapid (switching off the power). were found. The final R = 0.0262, wR = 0.0540, 2 K2SbB3O8 was gotten as colorless block crystals. where R = Σ||Fo| – |Fc||/Σ|Fo| and wR = [Σ[w(Fo – 2 2 2 2 1/2 2 2 2. 4 Single-crystal structure determination Fc ) ]/Σ[w(Fo ) ]] for Fo > 2σ(Fc ). The selected A transparent bulk K2SbB3O8 crystal was picked bond distances and bond angles are presented in out with the help of an optical microscope for Table 1. single-crystal XRD analysis. The diffraction data Table 1. Selected Bond Lengths (Å) and Bond Angles (°) Bond Dist. Angle (°) K(1)–O(1)vi 2.630(3) O(7)i–Sb(1)–O(2) 177.00(11) K(1)–O(7) 2.694(3) O(7)i–Sb(1)–O(4)ii 90.84(11) K(1)–O(5)iv 2.709(3) O(2)–Sb(1)–O(4)ii 91.14(11) K(1)–O(3)vii 2.759(3) O(7)i–Sb(1)–O(3)iii 87.14(11) K(1)–O(3)iii 2.826(3) O(2)–Sb(1)–O(3)iii 90.72(11) K(1)–O(8)iii 2.863(3) O(4)ii–Sb(1)–O(3)iii 86.76(11) K(2)–O(2)ix 2.608(3) O(7)i–Sb(1)–O(8)i 90.69(11) K(2)–O(6)i 2.616(3) O(2)–Sb(1)–O(8)i 91.50(11) K(2)–O(6)x 2.732(3) O(4)ii–Sb(1)–O(8)i 91.83(11) K(2)–O(4)i 2.773(3) O(3)iii–Sb(1)–O(8)i 177.39(10) K(2)–O(8)xi 2.935(3) O(7)i–Sb(1)–O(5) 87.78(11) Sb(1)–O(7)i 1.925(3) O(2)–Sb(1)–O(5) 90.03(11) Sb(1)–O(2) 1.926(3) O(4)ii–Sb(1)–O(5) 174.09(11) Sb(1)–O(4)ii 1.985(3) O(3)iii–Sb(1)–O(5) 87.43(11) Sb(1)–O(3)iii 1.989(3) O(8)i–Sb(1)–O(5) 93.94(11) Sb(1)–O(8)i 1.990(3) O(4)–B(1)–O(6) 116.2(4) Sb(1)–O(5) 2.003(3) O(4)–B(1)–O(5) 122.3(4) B(1)–O(4) 1.366(5) O(6)–B(1)–O(5) 121.5(4) B(1)–O(6) 1.368(5) O(1)–B(2)–O(8) 123.6(4) B(1)–O(5) 1.376(5) O(1)–B(2)–O(3) 119.2(4) B(2)–O(1) 1.348(5) O(8)–B(2)–O(3) 116.9(3) B(2)–O(3) 1.395(5) O(7)–B(3)–O(2) 108.1(3) B(2)–O(8) 1.387(5) O(7)–B(3)–O(6) 109.0(3) B(3)–O(1) 1.482(5) O(2)–B(3)–O(6) 111.8(3) To be continued 7- 1272 SHEN Y.
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