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1 Supporting Information Pb 3 B 6 O 11 F 2 : A First Noncentrocentric Lead Fluoroborate with Large Second Harmonic Generation Response Hongyi Li, a Hongping Wu, a * Xin Su, a Hongwei Yu, a,b Shilie Pan, a * Zhihua Yang, a * Yi Lu, c Jian Han, a Kenneth R. Poeppelmeier d a Key Laboratory of Functional Materials and Devices for Special Environments of CAS; Xinjiang Key Laboratory of Electronic Information Materials and Devices, Xinjiang Technical Institute of Physics & Chemistry of CAS, 40-1 South Beijing Road, Urumqi , China b University of Chinese Academy of Sciences, Beijing , China c Xinjiang Products Quality Supervision & Inspection Institute of Technology, Urumqi , China d Deparment of Chemistry, Northwestern University, 2145 Sheridan Road, Evanston IL , USA *Corresponding author. E mail: slpan@ms.xjb.ac.cn. Tel: (86) Fax: (86) S1
2 Table S1. Atomic coordinates ( 10 4 ) and equivalent isotropic displacement parameters (Å ) for Pb 3 B 6 O 11 F 2. U eq is defined as one-third of the trace of the orthogonalized U ij tensor. Atoms x y z U(eq) BVS Pb1 4628(1) 8130(1) 9531(1) 14(1) Pb2 5479(1) 8344(1) 5274(1) 13(1) Pb3 214(1) 9879(1) 2269(1) 12(1) B1-720(50) 8370(30) 8590(30) 16(6) B2 1020(40) 1080(30) 9300(30) 4(5) B3 3250(40) 1180(30) 7330(30) 7(5) B4 7280(40) 860(30) 7950(30) 7(5) B5 0(50) 6530(40) 4450(30) 20(6) B6 1010(40) 8710(30) 6300(30) 11(5) F1 6670(20) 247(18) 931(18) 27(4) F2 3790(20) 575(18) 3789(18) 26(4) O1-470(20) 9940(20) 5638(16) 10(3) O2 7290(20) 9287(19) 8088(17) 9(3) O3 5490(30) 1730(20) 7298(17) 12(4) O4 660(20) 9373(18) 9584(18) 13(3) O5 3000(20) 9434(19) 6890(16) 7(3) O6 1510(30) 7518(19) 5229(19) 14(4) O7 1340(20) 1892(17) 764(17) 7(3) O8 130(20) 7810(20) 7375(17) 12(4) O9 2860(20) 1472(18) 8759(16) 9(3) O (20) 1740(17) 8387(17) 7(3) O(11) 8150(20) 7132(18) 3779(17) 9(3) S2
3 Table S2(a). Selected bond lengths (Å) for Pb 3 B 6 O 11 F 2 Atoms Distance Atoms Distance Pb1-O(9)# (15) B1-O(7)#2 1.46(3) Pb1-O (16) B1-O2#7 1.48(3) Pb1-O(5) 2.738(15) B2-O(9) 1.42(3) Pb1-O(4) 2.758(16) B2-O(4)#6 1.47(3) Pb1-F(1) 2.426(16) B2-O(10) 1.47(3) Pb1-F(1)# (15) B2-O(7) 1.52(3) Pb2-O(5) 2.575(15) B3-O(9)#7 1.44(3) Pb2-O(6) 2.628(16) B3-O(11)#8 1.47(3) Pb2-O(11) 2.628(15) B3-O(5) 1.51(3) Pb2-O(3)# (16) B3-O(3) 1.51(3) Pb2-F (15) B4-O2 1.31(3) Pb2-F2# (15) B4-O(10) 1.37(3) Pb3-O(7) 2.399(15) B4-O(3) 1.40(3) Pb3-O(8)# (19) B5-O(1)#3 1.36(4) Pb3-O(4)# (16) B5-O(11) 1.33(3) Pb3-O(10)# (15) B5-O(6)#6 1.37(4) Pb3-F(1) 2.397(16) B6-O(5) 1.42(3) Pb3-F2# (17) B6-O(1) 1.45(3) B(1)-O(4) 1.43(3) B6-O(8) 1.46(3) B(1)-O(8) 1.45(3) B6-O(6) 1.50(3) S3
4 Table S2(b). Selected bond angles (deg) for Pb 3 B 6 O 11 F 2 Atoms Angles Atoms Angles F1-Pb1-O9#1 80.4(5) O8#4-Pb3-O4# (5) F1-Pb1-F1# (3) F2#5-Pb3-O4# (5) O9#1-Pb1-F1#2 74.7(5) F1-Pb3-O10# (5) F1-Pb1-O2 71.1(5) O7-Pb3-O10# (4) O9#1-Pb1-O2 98.1(5) O8#4-Pb3-O10# (5) F1#2-Pb1-O (5) F2#5-Pb3-O10# (5) F1-Pb1-O (5) O4#6-Pb3-O10#1 65.0(5) O9#1-Pb1-O (5) O4-B1-O F1#2-Pb1-O5 99.4(5) O4-B1-O7# O2-Pb1-O5 62.7(5) O8-B1-O7# F1-Pb1-O4 96.9(5) O4-B1-O2# O9#1-Pb1-O (5) O8-B1-O2# F1#2-Pb1-O4 94.8(5) O7#2-B1-O2# (19) O2-Pb1-O (5) O9-B2-O4# (18) O5-Pb1-O4 71.4(5) O9-B2-O (17) F2-Pb2-F2# (4) O4#6-B2-O (17) F2-Pb2-O5 79.7(5) O9-B2-O (17) F2#3-Pb2-O (5) O4#6-B2-O (17) F2-Pb2-O6 82.6(5) O10-B2-O (16) F2#3-Pb2-O6 83.0(5) O9#7-B3-O11# (18) O5-Pb2-O6 52.7(5) O9#7-B3-O (18) F2-Pb2-O (5) O11#8-B3-O (18) F2#3-Pb2-O (5) O9#7-B3-O (18) O5-Pb2-O (5) O11#8-B3-O (17) O6-Pb2-O (5) O5-B3-O (17) F2-Pb2-O3#3 82.0(5) O2-B4-O F2#3-Pb2-O3#3 81.9(5) O2-B4-O S4
5 O5-Pb2-O3# (5) O10-B4-O O6-Pb2-O3#3 79.0(5) O11-B5-F2#3 122(3) O11-Pb2-O3#3 52.5(5) O11-B5-O6#6 120(3) F1-Pb3-O7 87.9(5) F2#3-B5-O6#6 118(2) F1-Pb3-O8#4 81.2(5) O5-B6-F (19) O7-Pb3-O8#4 56.0(5) O5-B6-O (19) F1-Pb3-F2# (5) F2-B6-O (19) O7-Pb3-F2#5 80.4(5) O5-B6-O (19) O8#4-Pb3-F2#5 78.0(5) F2-B6-O6 112(2) F1-Pb3-O4#6 77.4(5) O8-B6-O (19) O7-Pb3-O4#6 55.9(5) Note. Symmetry transformations used to generate equivalent atoms: #1 -x+2,y-1/2,-z+2 #2 -x+1,y-1/2,-z+2 #3 -x+1,y-1/2,-z+1 #4 -x+1,y+1/2,-z+2 #5 x+1,y,z+1 #6 x+1,y,z #7 x-1,y,z #8 -x+1,y+1/2,-z+1 #9 x-1,y,z-1 #10 -x+2,y+1/2,-z+2 S5
6 Table S3. The direction and magnitude of the dipole moments in the PbO x F 2 (x=4, 5, 6) polyhedra, BO 4 tetrahedra and BO 3 triangle groups, and their contributions to the polarization in the unit cell. Species x(a) y(b) z(c) Debye 10-4 esu cma -3 Pb2O 4 F Pb1O 4 F Pb3O 4 F B1O B2O B3O B4O B5O B6O B-O in unit cell Pb-O in unit cell S6
7 Table S4. The refractive indices and birefringence of Pb 3 B 6 O 11 F 2. λ(nm) n x n y n z n=n y -n z S7
8 Figure S1 The 3D framework of Pb 3 B 6 O 11 F 2 with 18-member tunnels viewing along the a-axis where the Pb and F atoms were located (Pb-O bonds are omitted for the clarity). S8
9 Figure S2 The coordinated environments of lead atoms in the structure. S9
10 Figure S3 TG-DSC curves of Pb 3 B 6 O 11 F 2. S10
11 Figure S4 Absorption spectrum of Pb 3 B 6 O 11 F 2. S11
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