ARTICLE pubs.acs.org/crystal
A New Lithium Rubidium Borate Li6Rb5B11O22 with Isolated B11O22 Building Blocks Yun Yang,†,‡ Shilie Pan,*,† Jian Han,† Xueling Hou,† Zhongxiang Zhou,† Wenwu Zhao,†,‡ Zhaohui Chen,†,‡ and Min Zhang†,‡ †
Xinjiang Key Laboratory of Electronic Information Materials and Devices, Xinjiang Technical Institute of Physics & Chemistry, Chinese Academy of Sciences, 40-1 South Beijing Road, Urumqi 830011, China ‡ Graduate School of the Chinese Academy of Sciences and College of Chemistry and Chemical Engineering, Beijing 100039, PR China
bS Supporting Information ABSTRACT: A new noncentrosymmetric polyborate, Li6Rb5B11O22, has been designed and synthesized in the Li2O Rb2O B2O3 ternary system. The structure of the title compound was solved by single crystal X-ray diffraction analysis. It crystallizes in the monoclinic space group C2. The new structure contains an infinite three-dimensional matrix that is built from B11O22 building blocks and LiOn (n = 4, 5), RbOn (n = 9, 10) polyhedra. The B11O22 building block has not been reported previously in any anhydrous and hydrated borates. The optical characterization of the compound indicates that its UV cutoff edge is below 190 nm. IR spectroscopy, thermal analysis, and second-harmonic generation were also performed on the reported material.
’ INTRODUCTION Borates are of considerable interest because of their rich structural chemistry and potential applications, such as nonlinear optics.1 15 The success of the borates can be attributed to the ability to bind to either three or four oxygen atoms to form a BO3 triangle or a BO4 tetrahedron. And these BO3 triangles and BO4 tetrahedra can further link together via common oxygen atoms to form isolated rings and cages or polymerize into infinite chains, sheets, and networks. On the basis of the linkage of BO3 and BO4 groups, Burns et al.10 developed a comprehensive description based on fundamental building blocks (FBBs) to have a clearer nomenclature for more complicated polyanions.10,12a According to a recent survey of borate structure types, for further classification of borates, FBBs with certain numbers of borate units are determined, which then allow a simple grouping into mono-, di-, tri-, tetra-, penta-, and hexaborates and higher.12a It was found that even though there exists a considerable number of FBBs, isolated borate FBBs containing eleven borons have not been reported previously in any hydrous and anhydrous borates. Because of the large covalent bond energy of B O bonds in borate, there is no absorption in the UV region.9,16 In addition, the alkali metal oxygen bond is ideal for the transmission of UV light because there are no d d electron transitions in this range.9,17 Herein, we designed and synthesized a new UV NLO alkali mixed-metal borate, Li6Rb5B11O22, containing the new borate building block B11O22, which has not been reported previously in any borates. r 2011 American Chemical Society
’ EXPERIMENTAL PROCEDURES Synthesis and Crystal Growth. Single crystals of Li6Rb5B11O22 were prepared by a high temperature solution method in the Li2O Rb2O B2O3 ternary system. All commercially available chemicals (Li2CO3, Rb2CO3, and H3BO3) are of reagent grade and were used as received. This solution was prepared in a platinum crucible by melting of Li2CO3, Rb2CO3, and H3BO3 at the molar ratio Li2CO3/Rb2CO3/ H3BO3 = 1.5:1:5. It was heated at 750 °C and held at that temperature for 24 h. The furnace was slowly cooled to 570 °C at the rate 0.05 °C/min and then cooled to room temperature at the rate 10 °C/min. Colorless block crystals were separated from the crucible for structure determination. Crystals suitable for X-ray diffraction were selected under an optical microscope. A photograph of Li6Rb5B11O22 small crystals is shown in Figure 1. Polycrystalline samples of Li6Rb5B11O22 were synthesized via a conventional solid state reaction method from powder mixtures of Li2CO3, Rb2CO3, and H3BO3 as starting components at the molar ratio 3:2.5:11. The mixture of Li2CO3, Rb2CO3, and H3BO3 was ground thoroughly. It was heated up to 520 °C slowly and held at this temperature for 48 h with several intermediate grindings and mixings. Li6Rb5B11O22 compounds were studied at room temperature on a Bruker D8 ADVANCE X-ray diffractometer with graphite monochromatized Cu KR (λ = 1.5418 Å) radiation. The diffraction patterns were taken from 10° to 70° (2θ). The purity of the sample was checked by XRD diffraction, as shown in Figure 2. The experimental powder XRD pattern is in agreement with the Received: April 14, 2011 Revised: July 8, 2011 Published: July 15, 2011 3912
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Table 1. Crystal Data and Structure Refinement for Li6Rb5B11O22 empirical formula
Li6Rb5B11O22
formula weight
939.90
temperature
296(2) K
wavelength
0.71073 Å
crystal system
monoclinic
space group, Z
C2, 2
unit cell dimensions
a = 11.6252(5) Å, R = 90.00° b = 7.1010(3) Å, β = 106.871(3)° c = 13.7442(5) Å, γ = 90.00° 1085.76(8) Å3
volume
Figure 1. Photograph of as-grown Li6Rb5B11O22 crystals. (The minimum scale of the ruler is 1 mm.)
density (calcd)
2.875 g/cm
absorption coefficient
11.292/mm
F(000)
868
crystal size
0.15 mm 0.12 mm 0.03 mm
θ range for data collection
3.10 to 27.54° 15 e h e 15, 7 e k e 9, 17 e l e 17
limiting indices reflections collected/unique
5000/2163 [R(int) = 0.0823]
completeness to θ = 27.54
99.0%
refinement method
full-matrix least-squares on F2
data/restraints/parameters
2163/1/179
goodness-of-fit on F2
0.951
final R indices [Fo2 > 2σ(Fo2)]a
R1 = 0.0326, wR2 = 0.0624
R indices (all data)a absolute structure parameter
R1 = 0.0371, wR2 = 0.0641 0.022(11)
extinction coefficient
0.0024(2)
largest diff peak and hole
0.705 and
R1 = ∑||Fo| |Fc||/∑|Fo| and wR2 = [∑w(Fo Fo2 > 2σ(Fo2). a
2
0.589 e 3 Å
3
2 2
Fc ) /∑wFo4]1/2 for
Figure 2. Powder XRD pattern of Li6Rb5B11O22. calculated data on the basis of the single-crystal XRD studies (see Figure S1 in the Supporting Information). X-ray Crystallography. The crystal structure of Li6Rb5B11O22 was investigated by single-crystal X-ray diffraction on a Bruker SMART APEX II CCD diffractometer using monochromatic Mo KR radiation (λ = 0.71073 Å) at 296(2) K and integrated with the SAINT program.18 All calculations were performed with programs from the SHELXTL crystallographic software package.19 The structure was solved by direct methods using SHELXS-97.20 Final least-squares refinement is on Fo2 with data having Fo2 g 2σ(Fo2). The structure was checked for missing symmetry elements with PLATON.21 Crystal data and structure refinement information are summarized in Table 1. The final refined atomic positions and isotropic thermal parameters are given in Table 2. Selected bond distances (Å) and angles (deg) for Li6Rb5B11O22 are listed in Table S1 in the Supporting Information. Differential Thermal Analysis. Thermal analyses were carried out on a NETZSCH STA 449C instrument in the temperature range 30 900 °C with a heating rate of 10 °C/min in an atmosphere of flowing N2. Elemental Analysis. Elemental analysis of a Li6Rb5B11O22 single crystal was measured by using a VISTA-PRO CCD Simultaneous ICPOES. The crystal samples were dissolved in nitric acid at the boiling point for 1 h. Anal. Calcd for the Li6Rb5B11O22: Li, 4.43; Rb, 45.47; B, 12.65. Found: Li, 4.26; Rb, 45.86; B, 12.51. IR Spectroscopy. IR spectroscopy was carried out with the objective of specifying and comparing the coordination of boron in Li6Rb5B11O22 compound. The mid-infrared spectrum was obtained at room temperature
via a BRUKER EQUINOX 55 Fourier transform infrared spectrometer. The sample was mixed thoroughly with dried KBr. The spectrum was collected in a range from 400 to 4000 cm 1. UV Vis NIR Diffuse-Reflectance Spectroscopy. UV Vis NIR diffuse-reflectance data for Li6Rb5B11O22 crystalline sample were collected with a SolidSpec-3700DUV spectrophotometer with fluororesin as the standard in the wavelength range from 190 to 2600 nm. NLO Measurements. Powder second-harmonic generation (SHG) tests were carried out on Li6Rb5B11O22 by the Kurtz Perry method using 1064 nm radiation.22 A detailed description of the equipment and the methodology used has been published.15
’ RESULTS AND DISCUSSION Crystal Growth and Thermal Behavior. The DTA curve of Li6Rb5B11O22 exhibits only one endothermic peak beginning at 636 °C upon heating to 900 °C (see Supporting Information Figure S2). In order to further verify that Li6Rb5B11O22 melts congruently or incongruently, 0.5 g of Li6Rb5B11O22 powder was packed into a platinum crucible, heated to 900 °C, and then rapidly cooled to room temperature. Analysis of the powder XRD pattern of the solidified melt revealed that the entire solid product exhibited a diffraction pattern different from that of the initial Li6Rb5B11O22 powder (see Supporting Information Figure S3). This unambiguously demonstrates that Li6Rb5B11O22 is an incongruently melting compound. Therefore, the flux method is necessary for the purpose of its crystal growth. 3913
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Table 2. Atomic Coordinates (104) and Equivalent Isotropic Displacement Parameters (Å2 103) for Li6Rb5B11O22a
a
atom
x
Rb(1)
6759(1)
Rb(2)
2965(1)
Rb(3)
y
z
Ueq
6266(1)
7871(1)
12(1)
8301(1)
5886(1)
14(1)
10000
9799(1)
10000
14(1)
O(1)
3597(3)
7972(5)
8407(2)
9(1)
O(2) O(3)
6185(3) 2361(3)
1954(4) 4607(5)
8591(2) 6835(2)
7(1) 10(1)
O(4)
5630(3)
8957(4)
9141(2)
9(1)
O(5)
4502(3)
10149(5)
7547(2)
14(1)
O(6)
5000
8193(7)
5000
9(1)
O(7)
3692(3)
3565(5)
5938(2)
11(1)
O(8)
5452(3)
5273(4)
5891(2)
10(1)
O(9)
9299(3)
8456(5)
7749(2)
12(1)
O(10) O(11)
10643(3) 5000
7335(4) 2295(6)
6813(2) 5000
8(1) 6(1)
O(12)
7501(3)
395(4)
9988(2)
9(1)
B(1)
4527(5)
9011(8)
8359(4)
8(1)
B(2)
4939(4)
3375(8)
5904(3)
6(1)
B(3)
10137(5)
6986(7)
7654(3)
7(1)
B(4)
3429(5)
3895(8)
6837(4)
10(1)
B(5)
5000
6319(13)
5000
8(1)
B(6) Li(1)
6473(5) 808(7)
443(7) 5032(13)
9267(3) 5967(6)
5(1) 13(2)
Li(2)
2268(7)
6574(11)
Li(3)
7072(7)
2050(12)
7671(5)
8(2)
10455(5)
14(2)
Ueq is defined as one-third of the trace of the orthogonalized Uij tensor.
Crystal Structure. Li6Rb5B11O22 crystallizes in a monoclinic crystal system with an acentric space group of C2. The structure of Li6Rb5B11O22 features a complicated three-dimensional (3D) network composed of isolated (B11O22) units interconnected by LiOn (n = 4, 5) and RbOn (n = 9, 10) distorted polyhedra that are interconnected via corner or edge sharing as shown in Figure 3. A notable feature in the structure is the B11O22 building block (Figure 4), which is composed of a combination of two B3O7 rings and three B3O8 rings. The dihedral angles between two neighboring six-membered rings in the B11O22 cluster are 77.55°, 66.04°, 66.04°, and 77.55°, respectively. According to the scheme proposed by Burns, Christ, and Clark (1977),10 the B11O22 building block can be classified as 11:[2(5:3Δ+2T)+(1:Δ)]. The triangularly coordinated boron atoms have B O distances in the range 1.313(6) 1.417(6) Å [avg = 1.373 Å] and the tetrahedral B atoms have longer B O distances in the range 1.460(6) 1.494(6) Å [avg = 1.475 Å] (see Table S1 in the Supporting Information). These values are comparable to those in other borate compounds reported previously.15 Though the B O bond lengths display large variations [1.313(6) 1.494(6) Å], a bond valence sum (BVS) calculation for B atoms gives values ranging from 2.974 to 3.022 (average 3.003), in good agreement with the ideal B atom valence. According to a recent survey of borate structure types,12a such hendecaborate building block have not been reported previously in any anhydrous and hydrated borates. Rb(1)O9, Rb(2)O9, and Rb(3)O10 polyhedra (Figure 5) are interconnected via sharing oxygen atoms into a 3D framework (see Figure S4 in the Supporting Information) with Rb O bond distances
Figure 3. View of the structure of Li6Rb5B11O22 down the b axis (orange, Rb; green, Li; blue, B; red, O; purple, BO4 group; light blue, BO3 group).
ranging from 2.689(3) to 3.438(3) Å. Li(1)+ and Li(2)+ cations are located between B11O22 and RbOn (n = 9, 10) groups to hold the groups through coordination with oxygen atoms (Figure 3). Similarly, the coordination polyhedra of Li atoms have two types. Each Li(1)+ and Li(2)+ coordinated to four O atoms forming a distorted tetrahedron (Figure 5). And Li(3)+ is surrounded by five O atoms forming trigonal bipyramids. Li(1)O4, Li(2)O4, and Li(3)O5 polyhedra are interconnected via sharing edges into a 2D sheet network (see Figure S5 in the Supporting Information). The connectivity between the B11O22 building blocks, the LiOn, and RbOn units through their vertex O atoms gives rise to the 3D open framework. The bond valence sums of each atom in Li6Rb5B11O22 were calculated23,24 and are listed in Table S2 in the Supporting Information. These valence sums agree with the expected oxidation states. IR Spectroscopy. The IR spectrum exhibited the following absorptions, which were assigned by referring to the literature (see Figure S6 in the Supporting Information).25 27 The main infrared absorption region between about 1460 and 1300 cm 1 reveals several absorption bands, owing to asymmetric stretching of trigonal BO3 (1416 and 1320 cm 1) groups. The bands at 1102 and 1172 cm 1 are the in-plane bending of B O in BO3. The band at 931 cm 1 is the symmetric stretching of B O in BO3. The bands at 722, 693, and 648 cm 1 are the out-of-plane bending of B O in BO3. The IR absorptions in the region around 1000 cm 1 can originate from the BO4 group's asymmetric stretching (1050 cm 1) and symmetric stretching (989 cm 1). The wavenumbers of the fundamental vibrations of the BO4 group are grouped into bending modes (590 cm 1). The present study is in agreement with the results obtained for other borates. Li6Rb5B11O22 is moisture sensitive, which can be seen from the band at 3432 cm 1. UV Vis NIR Diffuse Reflectance Spectroscopy. The UV Vis NIR diffuse reflectance spectrum of the Li6Rb5B11O22 crystalline sample is shown in Figure S7 in the Supporting Information. It has a cutoff edge below 190 nm, indicating that the crystal may have potential use in UV NLO applications. NLO Measurements. On the basis of the noncentrosymmetric crystal structure of Li6Rb5B11O22, it is expected to possess 3914
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Figure 4. Polyborate building block B11O22.
Figure 5. Coordination of oxygen atoms around Rb and Li cations.
NLO properties. According to the anionic group theory of NLO activity in borates,28 the BO3 trigonal planes are responsible for the large SHG effects, and the BO4 groups contribute less. And also, the different orientations of the structure limit their total NLO contribution. The arrangement of the neighboring sixmembered rings in B11O22 is in an unfavorable manner so that the SHG coefficients are almost canceled. And then the resulting SHG effects are very limited.29 Consequently, the overall SHG efficiency of Li6Rb5B11O22 is merely about 2/3 KDP.
’ CONCLUSIONS In summary, a new lithium rubidium borate containing B11O22 building blocks was synthesized by the conventional solid state reaction method. The three-dimensional network consists of isolated B11O22 linked by LiOn (n = 4, 5) and RbOn (n = 9, 10) distorted polyhedra. The UV Vis NIR diffuse reflectance spectroscopy on powder samples indicates that it has a wide transparent
region with the short-wavelength cutoff edge below 190 nm. The feature of a short UV cut off edge is favorable in practical applications. Further investigation for the growth of large crystals and related physical property studies is underway.
’ ASSOCIATED CONTENT
bS Supporting Information. CIF file, bond distances and angles, bond valences, figures of XRD, DTA curve, infrared spectroscopy, and UV Vis NIR diffuse-reflectance spectrum details. This material is available free of charge via the Internet at http://pubs.acs.org. ’ AUTHOR INFORMATION Corresponding Author
*Phone: (86)991-3674558. Fax: (86)991-3838957. E-mail: slpan@ ms.xjb.ac.cn. 3915
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’ ACKNOWLEDGMENT This work is supported by the Main Direction Program of Knowledge Innovation of the Chinese Academy of Sciences (Grant No. KJCX2-EW-H03-03), the “National Natural Science Foundation of China” (Grant Nos. 50802110 and 21001114), the “One Hundred Talents Project Foundation Program” of the Chinese Academy of Sciences, the “Western Light Joint Scholar Foundation” Program of the Chinese Academy of Sciences, the “High Technology Research and Development Program” of the Xinjiang Uygur Autonomous Region of China (Grant No. 200816120), and the Scientific Research Program of Urumqi of China (Grant No. G09212001). ’ REFERENCES (1) (a) Chen, C. T.; Wu, B. C.; Jiang, A. D.; You, G. M. Sci. Sin. B 1985, 28, 235. (b) Chen, C. T.; Liu, G. Annu. Rev. Mater. Sci. 1986, 16, 203. (c) Chen, C. T.; Wu, Y. C.; Li, R. K. Int. Rev. Phys. Chem. 1989, 8, 65. (d) Chen, C. T.; Wang, Y. B.; Xia, Y. N.; Wu, B. C.; Tang, O. Y.; Wu, K.; Zeng, W.; Yu, L. H. J. Appl. Phys. 1995, 77, 2268. (e) Chen, C. T.; Wang, Y. B.; Wu, B. C.; Wu, K. W.; Yu, L. H. Nature 1995, 373, 322. (f) Chen, C. T.; Lin, Z. S.; Wang, Z. Appl. Phys. B: Laser Opt. 2005, 80, 1. (g) David, C. Nature 2009, 457, 953. (2) (a) Chen, C. T.; Wu, Y. C.; Jiang, A. D.; You, G. M.; Li, R. K.; Lin, S. J. J. Opt. Soc. Am. B 1989, 6, 616. (b) Betourne, E.; Touboul, M. J. Alloys Compd. 1997, 255, 91. (c) Chen, C. T.; Wu, Y. C.; Li, R. C. J. Cryst. Growth 1990, 99, 790. (d) Paul, A. K.; Sachidananda, K.; Natarajan, S. Cryst. Growth Des. 2010, 10, 456. (3) (a) Wu, Y. C.; Sasaki, T.; Nakai, S.; Yokotani, A.; Tang, H.; Chen, C. T. Appl. Phys. Lett. 1993, 62, 2614. (b) Touboul, M.; Penin, N.; Nowogrocki, G. J. Solid State Chem. 1999, 143, 260. (c) Zhang, J. X.; Wu, Y.; Zhang, G. C.; Zu, Y. L.; Fu, P. Z.; Wu, Y. C. Cryst. Growth Des. 2010, 10, 1574. (d) Zhang, J. X.; Zhang, G. C.; Li, Y. G.; Wu, Y.; Fu, P. Z.; Wu, Y. C. Cryst. Growth Des. 2010, 10, 4965. (4) (a) Muller, E. A.; Cannon, R. J.; Sarjeant, A. N.; Ok, K. M.; Halasyamani, P. S.; Norquist, A. J. Cryst. Growth Des. 2005, 5, 1913. (b) Halasyamani, P. S.; O’Hare, D. Chem. Mater. 1998, 10, 646. (c) Halasyamani, P. S.; Francis, R. J.; Walker, S. M.; O’Hare, D. Inorg. Chem. 1999, 38, 271. (d) Halasyamani, P. S.; Poeppelmeier, K. R. Chem. Mater. 1998, 10, 2753. (5) (a) Halasyamani, P. S.; Poeppelmeier, K. R. Inorg. Chem. 2008, 47, 8427. (b) Pan, S. L.; Smit, J. P.; Marvel, M. R.; Stampler, E. S.; Haag, J. M.; Baek, J.; Halasyamani, P. S.; Poeppelmeier, K. R. J. Solid State Chem. 2008, 181, 2087. (c) Hagerman, M. E.; Poeppelmeier, K. R. Chem. Mater. 1995, 7, 602. (d) Maggard, P. A.; Stern, C. L.; Poepplemeier, K. R. J. Am. Chem. Soc. 2001, 123, 7742. (e) Pan, S. L.; Smit, J. P.; Watkins, B.; Marvel, M. R.; Stern, C. L.; Poeppelmeier, K. R. J. Am. Chem. Soc. 2006, 128, 11631. (6) (a) Mori, Y.; Kuroda, I.; Nakajima, S.; Sasaki, T.; Nakai, S. Appl. Phys. Lett. 1995, 67, 1818. (b) Tu, J. M.; Keszler, D. A. Mater. Res. Bull. 1995, 30, 209.(c) Sasaki, T.; Kuroda, I.; Nakajima, S.; Yamaguchi, K.; Watanabe, S.; Mori, Y.; Nakai, S. Proceedings of the Adv. Solid-State Laser Conference, Memphis, Tennessee, USA, 1995. (d) Sasaki, T.; Mori, Y.; Yoshiura, M.; Yap, Y. K.; Kamimura, T. Mater. Sci. Eng. R: Rep. 2000, 30, 1. (7) (a) Becker, P. Adv. Mater. 1998, 10, 979. (b) Becker, P.; Bohaty, L.; Froehlich, R. Acta Crystallogr., C 1995, 51, 1721. (8) (a) Yang, T.; Li, G. B.; You, L. P.; Ju, J.; Liao, F. H.; Lin, J. H. Chem. Commun. 2005, 4225. (b) Wang, C.; Alekseev, E. V.; Depmeier, W.; Albrecht-Schmitt, T. E. Chem. Commun. 2010, 3955. (c) Leonyuk, N. I.; Leonyuk, L. I. Prog. Cryst. Growth Charact. 1995, 31, 179. (d) Paul, A. K.; Sachidananda, K.; Natarajan, S. Cryst. Growth Des. 2010, 10, 456. (9) (a) Zhang, W. L.; Chen, W. D.; Zhang, H.; Geng, L.; Lin, C. S.; He, Z. Z. J. Am. Chem. Soc. 2010, 132, 1508. (b) Mao, J. G.; Jiang, H. L.; Fang, K. Inorg. Chem. 2008, 47, 8498. (c) Kong, F.; Huang, S. P.; Sun, Z. M.; Mao, J. G.; Cheng, W. D. J. Am. Chem. Soc. 2006, 128, 7750. (d) Wang, S. C.; Ye, N.; Li, W.; Zhao, D. J. Am. Chem. Soc. 2010, 132, 8779.
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