Key Laboratory of Functional Materials and Devices for Special Environments, Xinjiang Technical
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1 Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C. This journal is The Royal Society of Chemistry 2016 KPb 2 (PO 3 ) 5 : A Novel Nonlinear Optical Lead Polyphosphate with Short Deep-UV Cutoff Edge Maierhaba Abudoureheman, a,b Shujuan Han, a * Bing-Hua Lei, a,b Zhihua Yang, a Xifa Long a * and Shilie Pan a * a Key Laboratory of Functional Materials and Devices for Special Environments, Xinjiang Technical Institute of Physics & Chemistry, Chinese Academy of Sciences; Xinjiang Key Laboratory of Electronic Information Materials and Devices, South Beijing Road, Urumqi , China. b University of Chinese Academy of Sciences, Beijing , China. Fax:(86) ; Tel: (86) *To whom correspondence should be addressed: slpan@ms.xjb.ac.cn (Shilie Pan); hansj@ms.xjb.ac.cn (Shujuan Han); lxf@fjirsm.ac.cn (Xifa Long). S1
2 Table S1. The final coordinates ( 10 4 ) and equivalent isotropic displacement parameters (Å ) of non-hydrogen atoms for KPb 2 (PO 3 ) 5, RbPb 2 (PO 3 ) 5 and CsPb 2 (PO 3 ) 5. U eq is defined as one-third of the trace of the orthogonalized U ij tensor for each atom in asymmetric unit. Atom x y z U eq KPb 2 (PO 3 ) 5 K(1) 7187(4) 3593(4) 4056(3) 25(1) Pb(1) 4052(1) 1400(1) 6867(1) 19(1) Pb(2) 9004(1) 1713(1) 7688(1) 19(1) P(1) 751(3) 8561(3) 5202(3) 14(1) P(2) 5797(4) 6536(4) 6841(3) 16(1) P(3) 7238(3) -960(4) 5033(3) 14(1) P(4) 8133(3) 6453(3) 8872(3) 13(1) P(5) 10994(3) 4592(4) 5937(3) 13(1) O(1) 9115(9) 4765(11) 8700(8) 26(2) O(2) 7080(9) 621(10) 5953(7) 22(2) O(3) 1070(11) 10193(11) 5988(9) 28(2) O(4) 7413(10) 7133(12) 7581(8) 19(2) O(5) 1222(10) 6801(11) 5995(9) 22(2) O(6) 5685(10) 4488(11) 6755(8) 27(2) O(7) 4470(9) 7678(11) 7316(8) 23(2) O(8) 8911(9) 8103(10) 9507(8) 22(2) O(9) 6537(9) 5884(12) 9578(8) 25(2) O(10) 6869(12) -557(11) 3701(9) 27(2) O(11) 12044(9) 3825(10) 6949(8) 21(2) O(12) 9293(9) 4087(11) 5973(8) 19(2) O(13) 1362(12) 8453(11) 3916(9) 35(3) O(14) -1074(10) 8133(12) 5048(13) 49(3) O(15) 6231(10) -2702(12) 5445(7) 26(2) RbPb 2 (PO 3 ) 5 Rb(1) 5296(1) 1440(1) 7789(1) 23(1) Pb(1) 8461(1) 3586(1) 4950(1) 19(1) Pb(2) 3593(1) 3307(1) 4093(1) 21(1) P(1) 6659(4) -1464(4) 4937(3) 17(1) P(2) 11535(3) 407(3) 5843(2) 13(1) P(3) 6773(3) 3589(3) 1569(2) 14(1) P(4) 5291(3) -3946(3) 6748(2) 16(1) P(5) 4440(3) -1379(3) 2868(2) 15(1) O(1) 5110(9) -2107(11) 4155(7) 21(2) O(2) 7972(8) -2648(10) 4569(7) 28(2) O(3) 10408(8) 1122(10) 4904(6) 22(2) O(4) 11368(11) -1795(11) 5776(9) 32(2) O(5) 6496(12) 5193(11) 759(8) 41(2) O(6) 6043(8) -880(10) 2215(6) 21(2) O(7) 13202(7) 946(10) 5736(7) 23(2) O(8) 6129(13) 3484(11) 2814(9) 50(3) O(9) 6109(9) -2081(10) 6296(7) 28(2) O(10) 3628(8) -2969(9) 2228(7) 23(2) O(11) 6767(9) 594(10) 4944(7) 27(2) O(12) 3494(7) 345(9) 3028(6) 22(2) O(13) 3573(12) -3258(14) 6829(14) 72(3) O(14) 5757(13) -4264(11) 8030(7) 44(3) O(15) 5523(8) -5484(9) 5861(6) 25(2) CsPb 2 (PO 3 ) 5 Cs(1) 9460(3) 8549(3) -260(3) 52(1) S2
3 Pb(1) 6301(1) 6416(1) 2575(1) 20(1) Pb(2) 11172(1) 6692(1) 3432(1) 22(1) P(1) 13215(7) 9599(8) 1709(5) 16(1) P(2) 9473(7) 3938(8) 784(6) 17(1) P(3) 5312(7) 8626(8) -329(6) 15(1) P(4) 3123(9) 8549(9) -2373(7) 21(2) P(5) 7979(7) 6406(7) 5967(6) 16(1) O(1) 4330(20) 8840(20) 2636(15) 17(3) O(2) 9240(20) 5470(20) 1658(15) 23(4) O(3) 8240(30) 4770(30) 6790(20) 47(6) O(4) 11257(18) 9680(20) 4484(16) 23(4) O(5) 6124(18) 7050(20) 309(15) 19(3) O(6) 3790(20) 8970(30) 338(16) 23(4) O(7) 3012(19) 10600(20) -2380(17) 25(4) O(8) 1788(19) 7320(30) -1981(19) 32(4) O(9) 11550(20) 9020(30) 1781(17) 27(4) O(10) 8550(40) 6520(30) 4700(20) 62(9) O(11) 4625(18) 7990(20) -1554(14) 10(3) O(12) 8710(20) 2110(20) 1273(15) 21(4) O(13) 8310(30) 8180(30) 6980(30) 48(6) O(14) 9010(30) 4300(30) -490(20) 43(6) O(15) 11140(30) 3310(30) 770(30) 56(7) S3
4 Table S2a. Selected bond distances (Å) and bond angles (deg) for KPb 2 (PO 3 ) 5. K(1)-O(12) 2.714(9) P(1)-O(3) 1.459(9) K(1)-O(7)# (8) P(1)-O(13) 1.469(9) K(1)-O(1)# (8) P(1)-O(5) 1.564(8) K(1)-O(11)# (8) P(1)-O(14) 1.591(10) K(1)-O(2) 2.932(8) P(2)-O(6) 1.473(8) K(1)-O(10) 3.008(9) P(2)-O(7) 1.490(8) K(1)-O(8)# (8) P(2)-O(15)# (8) Pb(1)-O(11)# (7) P(2)-O(4) 1.631(8) Pb(1)-O(8)# (8) P(3)-O(10) 1.471(10) Pb(1)-O(6) 2.617(8) P(3)-O(2) 1.502(8) Pb(1)-O(7)# (8) P(3)-O(14)# (9) Pb(1)-O(2)# (7) P(3)-O(15) 1.580(8) Pb(1)-O(13)# (9) P(4)-O(1) 1.483(8) Pb(1)-O(10)# (9) P(4)-O(8) 1.509(8) Pb(1)-O(10)# (9) P(4)-O(4) 1.569(9) Pb(2)-O(1) 2.437(8) P(4)-O(9) 1.614(8) Pb(2)-O(12) 2.505(8) P(5)-O(11) 1.491(9) Pb(2)-O(2) 2.567(8) P(5)-O(12) 1.495(8) Pb(2)-O(13)# (9) P(5)-O(5)# (9) Pb(2)-O(3)# (9) P(5)-O(9)# (8) Pb(2)-O(10)# (9) O(11)#1-Pb(1)-O(8)#2 85.0(3) O(3)-P(1)-O(13) 120.4(5) O(11)#1-Pb(1)-O(6) 76.9(3) O(3)-P(1)-O(14) 112.7(6) O(8)#2-Pb(1)-O(6) 81.6(3) O(13)-P(1)-O(14) 104.7(6) O(11)#1-Pb(1)-O(7)# (2) O(5)-P(1)-O(14) 98.2(5) O(8)#2-Pb(1)-O(7)# (2) O(7)-P(2)-O(4) 109.4(4) O(6)-Pb(1)-O(7)# (2) O(12)-K(1)-O(1)# (2) O(1)-Pb(2)-O(12) 73.0(3) O(7)#5-K(1)-O(1)# (3) O(1)-Pb(2)-O(2) 127.5(3) O(12)-K(1)-O(11)# (3) O(12)-Pb(2)-O(2) 75.9(2) O(7)#5-K(1)-O(11)#2 74.1(2) O(1)-Pb(2)-O(13)#4 81.3(3) O(1)#2-K(1)-O(11)#2 67.2(2) O(12)-Pb(2)-O(13)# (3) O(12)-K(1)-O(2) 66.9(2) O(2)-Pb(2)-O(13)#4 78.4(3) O(7)#5-K(1)-O(2) 103.9(2) O(12)-K(1)-O(7)#5 94.4(2) O(1)#2-K(1)-O(2) 110.3(2) O(11)#2-K(1)-O(2) 171.9(3) O(12)-K(1)-O(10) 106.2(3) O(7)#5-K(1)-O(10) 70.4(2) O(10)-K(1)-O(8)#2 63.3(2) O(1)#2-K(1)-O(10) 107.8(2) O(7)#5-K(1)-O(8)# (2) O(11)#2-K(1)-O(10) 122.1(3) O(1)#2-K(1)-O(8)#2 50.3(2) Symmetry transformations used to generate equivalent atoms: #1 x-1,y,z #2 x-1/2,-y+1,z-1/2 #3 x,y-1,z #4 x+1/2,-y+1,z+1/2 #5 x+1/2,-y+1,z-1/2 #6 x,y+1,z #7 x+1,y-1,z #8 x+1,y,z #9 x-1/2,-y+1,z+1/2 #10 x-1,y+1,z S4
5 Table S2b. Selected bond distances (Å) and bond angles (deg) for RbPb 2 (PO 3 ) 5. Rb(1)-O(3)# (7) Pb(2)-O(5)# (9) Rb(1)-O(12)# (7) P(1)-O(2) 1.468(8) Rb(1)-O(15)# (7) P(1)-O(11) 1.478(7) Rb(1)-O(9) 3.080(8) P(1)-O(9) 1.609(8) Rb(1)-O(14)# (8) P(1)-O(1) 1.625(7) Rb(1)-O(10)# (7) P(2)-O(3) 1.477(8) Rb(1)-O(4)# (10) P(2)-O(7) 1.483(7) Rb(1)-O(11) 3.392(7) P(2)-O(6)# (7) Pb(1)-O(3) 2.428(7) P(2)-O(4) 1.586(8) Pb(1)-O(10)# (7) P(3)-O(8) 1.463(8) Pb(1)-O(11) 2.587(7) P(3)-O(5) 1.461(8) Pb(1)-O(2)# (7) P(3)-O(13)# (11) Pb(1)-O(5)# (9) P(3)-O(4)# (8) Pb(1)-O(14)# (9) P(4)-O(14) 1.450(9) Pb(1)-O(15)# (7) P(4)-O(15) 1.475(7) Pb(1)-O(8)# (1) P(4)-O(13) 1.553(10) Pb(2)-O(12) 2.414(7) P(4)-O(9) 1.589(7) Pb(2)-O(7)# (7) P(5)-O(12) 1.489(7) Pb(2)-O(8) 2.594(9) P(5)-O(10) 1.497(7) Pb(2)-O(15)# (7) P(5)-O(1) 1.580(8) Pb(2)-O(14)# (10) P(5)-O(6) 1.593(7) O(3)#2-Rb(1)-O(12)# (19) O(3)-Pb(1)-O(10)#3 82.2(2) O(3)#2-Rb(1)-O(15)# (2) O(3)-Pb(1)-O(11) 77.4(2) O(12)#3-Rb(1)-O(15)# (19) O(10)#3-Pb(1)-O(11) 83.0(2) O(3)#2-Rb(1)-O(9) 83.63(19) O(3)-Pb(1)-O(2)# (2) O(12)#3-Rb(1)-O(9) 59.07(19) O(10)#3-Pb(1)-O(2)# (2) O(15)#4-Rb(1)-O(9) (18) O(11)-Pb(1)-O(2)# (2) O(3)#2-Rb(1)-O(14)# (2) O(12)-Pb(2)-O(7)#1 74.7(2) O(12)#3-Rb(1)-O(14)# (2) O(12)-Pb(2)-O(8) 79.2(2) O(15)#4-Rb(1)-O(14)# (19) O(7)#1-Pb(2)-O(8) 122.6(3) O(9)-Rb(1)-O(14)# (2) O(12)-Pb(2)-O(15)# (2) O(3)#2-Rb(1)-O(10)# (19) O(7)#1-Pb(2)-O(15)#4 78.4(2) O(12)#3-Rb(1)-O(10)# (18) O(8)-Pb(2)-O(15)#4 81.4(3) O(15)#4-Rb(1)-O(10)# (19) O(12)-Pb(2)-O(14)#6 89.9(2) O(9)-Rb(1)-O(10)# (19) O(7)#1-Pb(2)-O(14)# (2) O(14)#4-Rb(1)-O(10)#3 63.6(2) O(8)-Pb(2)-O(14)# (3) O(3)#2-Rb(1)-O(4)#2 45.0(2) O(15)#4-Pb(2)-O(14)# (2) O(12)#3-Rb(1)-O(4)#2 73.6(2) O(10)#3-Rb(1)-O(4)#2 85.7(2) Symmetry transformations used to generate equivalent atoms: #1 x-1,y,z #2 x-1/2,-y,z+1/2 #3 x+1/2,-y,z+1/2 #4 x,y+1,z # 5x+1/2,-y+1,z-1/2 #6 x-1/2,-y,z-1/2 #7 x+1/2,-y,z-1/2 #8 x+1,y,z #9 x,y-1,z S5
6 Table S2c. Selected bond distances (Å) and bond angles (deg) for CsPb 2 (PO 3 ) 5. Cs(1)-O(1)# (16) Pb(2)-O(14)# (2) Cs(1)-O(4)# (17) P(1)-O(1)# (17) Cs(1)-O(2) 3.039(17) P(1)-O(9) 1.488(18) Cs(1)-O(14) 3.08(2) P(1)-O(13)#2 1.62(3) Cs(1)-O(12)# (17) P(1)-O(6)# (19) Cs(1)-O(5) 3.118(17) P(2)-O(14) 1.45(2) Cs(1)-O(13)#5 3.14(3) P(2)-O(2) 1.462(17) Cs(1)-O(7)# (19) P(2)-O(15) 1.50(3) Pb(1)-O(1) 2.421(16) P(2)-O(12) 1.559(16) Pb(1)-O(5) 2.497(16) P(3)-O(4)# (16) Pb(1)-O(7)# (17) P(3)-O(5) 1.491(16) Pb(1)-O(8)# (19) P(3)-O(11) 1.513(17) Pb(1)-O(3)# (2) P(3)-O(6) 1.516(18) Pb(1)-O(14)# (2) P(4)-O(7) 1.472(18) Pb(1)-O(10)# (2) P(4)-O(8) 1.51(2) Pb(1)-O(2)# (2) P(4)-O(11) 1.600(16) Pb(2)-O(4) 2.428(16) P(4)-O(12)# (18) Pb(2)-O(9) 2.468(19) P(5)-O(10) 1.46(2) Pb(2)-O(10) 2.65(3) P(5)-O(3) 1.49(2) Pb(2)-O(2) 2.661(16) P(5)-O(15)#8 1.59(3) Pb(2)-O(3)# (2) P(5)-O(13) 1.70(3) O(1)#2-Cs(1)-O(4)#3 69.0(5) O(1)-Pb(1)-O(7)#6 78.3(5) O(1)#2-Cs(1)-O(2) 170.7(4) O(5)-Pb(1)-O(7)#6 83.9(6) O(4)#3-Cs(1)-O(2) 107.6(5) O(1)-Pb(1)-O(8)# (5) O(1)#2-Cs(1)-O(14) 124.2(5) O(5)-Pb(1)-O(8)# (6) O(4)#3-Cs(1)-O(14) 107.1(5) O(7)#6-Pb(1)-O(8)# (5) O(2)-Cs(1)-O(14) 47.7(5) O(4)-Pb(2)-O(9) 75.0(6) O(1)#2-Cs(1)-O(12)#4 83.5(4) O(4)-Pb(2)-O(10) 79.4(6) O(4)#3-Cs(1)-O(12)#4 60.8(4) O(9)-Pb(2)-O(10) 121.8(8) O(2)-Cs(1)-O(12)# (4) O(4)-Pb(2)-O(2) 130.1(5) O(14)-Cs(1)-O(12)# (5) O(9)-Pb(2)-O(2) 77.6(6) O(1)#2-Cs(1)-O(5) 110.4(4) O(10)-Pb(2)-O(2) 80.8(8) O(4)#3-Cs(1)-O(5) 48.2(4) O(4)-Pb(2)-O(3)# (6) O(2)-Cs(1)-O(5) 63.1(4) O(9)-Pb(2)-O(3)# (7) O(14)-Cs(1)-O(5) 63.9(5) O(10)-Pb(2)-O(3)# (7) O(12)#4-Cs(1)-O(5) 88.9(4) O(2)-Pb(2)-O(3)# (6) O(1)#2-Cs(1)-O(13)#5 46.5(6) O(12)#4-Cs(1)-O(13)# (6) Symmetry transformations used to generate equivalent atoms: #1 x+1,y,z #2 x+1/2,-y+2,z-1/2 #3 x+1/2,-y+2,z+1/2 #4 x,y+1,z #5 x,y,z-1 #6 x+1/2,-y+2,z+1/2 #7 x+1/2,-y+1,z+1/2 #8 x-1/2,-y+1,z+1/2 #9 x-1/2,-y+2,z+1/2 #10 x+1/2,-y+1,z-1/2 #11 x,y-1,z #12 x-1/2,-y+1,z-1/2 #13 x-1,y,z #14 x,y,z+1 S6
7 Table S3. Detailed contributions from the RbO 10, PbO n polyhedra and PO 4 tetrahedra as well as the total polarization of the whole unit cell in the RbBa 2 (PO 3 ) 5 compound. Dipole moment Species x y z Magnitude Rb(1)O Ba(1)O Ba(2)O P(1)O P(2)O P(3)O P(4)O P(5)O ΣRbO Unit cell ΣBaO Z=2 ΣPO Total polarization S7
8 Figure S1 The coordination environment of the A (K, Rb, Cs) atoms S8
9 Figure S2 The bond lengths and angles of the repeat unit in the structure of RbBa 2 (PO 3 ) 5 S9
10 Figure S3 The IR spectra of KPb 2 (PO 3 ) 5 and RbPb 2 (PO 3 ) 5 S10
11 Calculations Detail The exchange-correlation functional and pseudo potential chosen were generalized gradient approximation (GGA) with Perdew-Burke-Ernzerhof (PBE) functional and norm-conserving pseudo potential (NCP). The energy cut-off of the plane wave basis set was 830 ev for RbBa 2 (PO 3 ) 5 and the Brillouin zone comprised with a separation of Monkhorst-Pack k-point sampling of 0.04 /Å. The optimized valence electronic configurations for NCP are: Rb: 4s 2 4p 6 5s 1, Ba: 5s 2 5p 6 6s 2, P: 3s 2 3p 3, O: 2s 2 2p 4. (a) (b) Figure S4 The band structures of (a) KPb 2 (PO 3 ) 5 and (b) RbBa 2 (PO 3 ) 5 S11
12 (a) (b) Figure S5 PDOS of (a) KPb 2 (PO 3 ) 5 and (b) RbBa 2 (PO 3 ) 5 S12
13 (a) (b) Figure S6 Birefringences of (a) KPb 2 (PO 3 ) 5 and (b) RbBa 2 (PO 3 ) 5 S13
14 Birefringence Measurement The rough birefringence of KPb 2 (PO 3 ) 5 at nm was tested using a GR-5 Gem Refractormeter (Wuhan Zhongdixueyuan Gem Instrument Ltd., China). Drip a drop of contact liquid on the prism surface of refractometer, and put the natural growth surface of KPb 2 (PO 3 ) 5 on the prism. The refractive index can be read through eyepiece. The measuring wavelength is nm, the range of refractive index is and the accuracy is ± It birefringence Δn is about at nm(n 1 = 1.590, n 2 = 1.620, recorded using refractometer at nm). S14
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