Home Physical Sciences Crystal structure of cesium beryllophosphate, Be3Cs2P4O14
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Crystal structure of cesium beryllophosphate, Be3Cs2P4O14

  • Wang Fang EMAIL logo and Chen Yigang
Published/Copyright: February 14, 2018

Abstract

Be3Cs2P4O14, orthorhombic, Pnma (no. 62), a = 15.0612(3) Å, b = 11.0386(2) Å, c = 15.5316(3) Å, V = 2582.19(8) Å3, Z = 8, Rgt(F) = 0.0229, wRref(F2) = 0.0594, T = 293(2) K.

CCDC no.: 1820644

The asymmetric unit of the title crystal structure is shown in the figure. Tables 1 and 2 contain details of the measurement method and a list of the atoms including atomic coordinates and displacement parameters.

Table 1:

Data collection and handling.

Crystal:Colourless block
Size:0.28 × 0.15 × 0.10 mm
Wavelength:Mo Kα radiation (0.71073 Å)
μ:62.2 cm−1
Diffractometer, scan mode:Xcalibur Eos Gemini, ω scans
2θmax, completeness:56.6°, >99%
N(hkl)measured, N(hkl)unique, Rint:44175, 3365, 0.051
Criterion for Iobs, N(hkl)gt:Iobs > 2 σ(Iobs), 2998
N(param)refined:221
Programs:SHELX [1, 2] , OLEX2 [3], CryAlisPRO [4]
Table 2:

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2).

AtomxyzUiso*/Ueq
Cs10.64319(2)0.25001.01594(2)0.01977(8)
Cs20.84235(2)0.25000.73987(2)0.02377(9)
Cs30.63719(2)0.25000.51783(2)0.02293(8)
Cs40.62556(2)0.75000.74636(2)0.02529(9)
P10.58748(4)0.38411(6)0.78149(4)0.00710(13)
P20.89228(4)0.38285(6)0.97422(4)0.00708(13)
P30.61584(4)0.61397(6)0.97915(4)0.00700(13)
P40.88237(4)0.61673(6)0.78097(4)0.00714(13)
O10.62116(18)0.75001.01745(16)0.0095(5)
O20.58445(19)0.25000.74146(16)0.0105(5)
O30.83999(17)0.75000.79052(16)0.0098(5)
O40.89389(18)0.25001.01692(16)0.0104(5)
O50.58799(13)0.46634(17)0.70407(11)0.0133(4)
O60.50494(13)0.39707(18)0.83622(12)0.0151(4)
O70.46248(13)0.38324(17)0.59597(11)0.0121(4)
O80.45512(13)0.60956(17)0.65109(12)0.0137(4)
O90.53086(13)0.60503(17)0.92828(12)0.0154(4)
O100.91640(13)0.60730(17)0.69073(12)0.0141(4)
O110.61784(12)0.53286(17)1.05737(11)0.0117(4)
O120.69795(13)0.59961(17)0.92378(12)0.0132(4)
O130.80469(13)0.53309(17)0.79677(11)0.0122(4)
O140.79980(12)0.40005(18)0.93982(12)0.0134(4)
O150.67130(13)0.39248(17)0.83389(12)0.0131(4)
Be10.7437(2)0.4848(3)0.8744(2)0.0087(6)
Be20.5222(2)0.4992(3)0.6251(2)0.0095(6)
O160.91163(13)0.46618(17)1.04817(11)0.0123(4)
Be30.9604(2)0.5157(3)0.6208(2)0.0099(6)

Source of materials

All reagents and solvents employed were commercially available and used as received without further purification. The raw materials BeO (1.5 mmol, 0.037 g), LiF (2 mmol, 0.052 g), NH4H2PO4 (7 mmol, 0.805 g), Cs2CO3 (1.5 mmol, 0.489 g), and Y2O3 (0.3 mmol, 0.068 g) were ground in an agate mortar, pressed into a pellet, placed in a Pt crucible and preheated in a muffle furnace at 773 K for 10 h to eliminate the water and gas. And then, it was reground thoroughly, placed in a Pt crucible and heated at 1223 K for 20 h to homogenize the solution, and slowly cooled to 873 K at a rate of 3 K ⋅ h−1 before the furnace was turned off. Colorless block crystals were then obtained.

Comment

Beryllium phosphate crystals have attracted intensive attention ascribed to many important applications such as laser hosts, phosphors, electrode materials, birefringent optics and nonlinear optical materials [5], [6], [7], [8]. Different from structural diversity of borates [9], [10], [11], [12], beryllium phosphates only possess the PO4 or BeO4 tetrahedra having more opportunities to form ordered arrangements such as infinite chains, rings, and isolated clusters [13]. However, there has been little research in the combination of the PO4 and BeO4 tetrahedra. Hence, preparation and study of new beryllophosphate compounds are interesting to crystal chemistry and materials science.

The title compound crystallizes in an orthorhombic space group and its asymmetric unit contains two Cs atoms, four P atoms, three Be atoms, and fourteen O atoms. It features a novel [Be3P4O14]2− three-dimensional network composed of the PO4 and BeO4 tetrahedra with the P—O and Be—O bond lengths of 1.496(18)−1.617(11) Å and 1.602(4)−1.637(4) Å, respectively. The structure along the b axis can be viewed as a layered stacking, and each layer consists of a [Be3P4O20]14− fundamental unit further interconnected by O-sharing. The adjacent layers are bridged via O atoms from the PO4 tetrahedra, and the Cs cations reside between the layers and maintain the charge balance.

Acknowledgements

This work was supported by the National Natural Science Foundation of China (Grant No. 21302003).

References

Sheldrick, G. M.: SHELXL-97: Program for the Refinement of Crystal Structures. University of Goettingen, Germany (1997).Search in Google Scholar

Sheldrick, G. M.: Crystal structure refinement with SHELXL. Acta Crystallogr. C71 (2015) 3–8.10.1107/S2053229614024218Search in Google Scholar PubMed PubMed Central

Dolomanov, O. V.; Bourhis, L. J.; Gildea, R. J.; Howard, J. A. K.; Puschmann, H.: OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. 42 (2009) 339–341.10.1107/S0021889808042726Search in Google Scholar

Agilent Technologies: CrysAlis Pro. Software system, version 1.171.39.27b, Agilent Technologies UK Ltd., Oxford, UK (2015).Search in Google Scholar

Huang, H. W.; Liu, L. J.; Jin, S. F.; Yao, W. J.; Zhang, Y. H.; Chen, C. T.: Deep-ultraviolet nonlinear optical materials: Na2Be4B4O11 and LiNa5Be12B12O33. J. Am. Chem. Soc. 135 (2013) 18319–18322.10.1021/ja410543wSearch in Google Scholar PubMed

Xu, Y. M.; Richard, P.; Nakayama, K.; Kawahara, T.; Sekiba, Y.; Qian, T.; Neupane, M.; Souma, S.; Sato, T.; Takahashi, T.; Luo, H.-Q.; Wen, H.-H.; Chen, G.-F.; Wang, N.-L.; Wang, Z.; Fang, Z.; Dai, X.; Ding, H.: Fermi surface dichotomy of the superconducting gap and pseudogap in underdoped pnictides. Nat. Commun. 2 (2011) 394.10.1038/ncomms1394Search in Google Scholar PubMed

Chen, Y. G.; Xing, M. L.; Liu, P. F.; Guo, Y.; Yang, N.; Zhang, X. M.: Two phosphates: noncentrosymmetric Cs6Mg6(PO3)18 and centrosymmetric Cs2MgZn2(P2O7)2. Inorg. Chem. 56 (2017) 845–851.10.1021/acs.inorgchem.6b02303Search in Google Scholar PubMed

Wang, Y.; Pan, S. L.: Recent development of metal borate halides: crystal chemistry and application in second-order NLO materials. Coord. Chem. Rev. 323 (2016) 15–35.10.1016/j.ccr.2015.12.008Search in Google Scholar

Yao, W. J.; Jiang, X. X.; Huang, H. W.; Xu, T.; Wang, X. S.; Lin, Z. S.; Chen, C. T.: Sr8MgBr18O36: A new Alkaline-Earth borate with a novel zero-dimensional (B18O36)18− anion ring. Inorg. Chem. 52 (2013) 8291–8293.10.1021/ic401167zSearch in Google Scholar PubMed

Ju, J.; Lin, J. H.; Li, G. B.; Yang, T.; Li, H. M.; Liao, F. H.; Loong, C. K.; You, L. P.: Aluminoborate-based molecular sieves with 18-octahedral-atom tunnels. Angew. Chem. Int. Ed. 42 (2003) 5607–5610.10.1002/anie.200352263Search in Google Scholar PubMed

Attfield, J. P.; Bell, A. M. T.; Rodriguez-Martinez, L. M.; Greneche, J. M.; Cernik, R. J.; Clarke, J. F.; Perkins, D. A.: Electrostatically driven charge-ordering in Fe2OBO3. Nature 396 (1998) 655–658.10.1038/25309Search in Google Scholar

Chen, C. T.; Wu, B. C.; Jiang, A. D.; You, G. M.: A new type ultraviolet SHG crystal: β-BaB2O4. Sci. Sin. Ser. B28 (1985) 235–243.Search in Google Scholar

Kim, S. C.; Lee, M. S.; Kang, J.; Kim, Y. I.; Kim, S. J.: Crystal structure and ion conductivity of a new mixed-anion phosphate LiMg3(PO4)P2O7. J. Solid State Chem. 225 (2015) 335–339.10.1016/j.jssc.2015.01.011Search in Google Scholar

Received: 2017-11-1
Accepted: 2018-1-30
Published Online: 2018-2-14
Published in Print: 2018-3-28

©2018 Wang Fang et al., published by De Gruyter, Berlin/Boston

This work is licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 4.0 License.

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