Multifunctinality and Crystal Dynamics of Highly Stable Porous Metal-Organic Framework [Zn 4 O(NTB) 2 ]

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Supporting Information Multifunctinality and Crystal Dynamics of Highly Stable Porous Metal-Organic Framework [Zn 4 O(NTB) 2 ] Eun Young Lee, Seung Yeon Jang, and Myunghyun Paik Suh* School of Chemistry, Seoul National University, Seoul 151-747, Republic of Korea. S1

Figure S1. TGA/DSC trace for 1. S2

(a) (b) Figure S2. Photos for the crystal (a) [Zn 4 O(NTB) 2 ] 3DEF EtOH (1), and (b) [Zn 4 O(NTB) 2 ] (1 ) obtained by heating 1 at 400 C and 10-5 torr for 0.5 h. S3

Figure S3. An ORTEP drawing of resolvated crystal, [Zn 4 O(NTB) 2 ] xdef yetoh (1 ), with the atomic numbering scheme. Statistically disordered structure is separated into two independent structures. Thermal ellipsoids are drawn with 30% probability. Zn, yellow; O, red; N, blue; C, gray. S4

Table S1. Crystallographic data for [Zn 4 O(NTB) 2 ] 3DEF EtOH (1) [squeezed data] formula C 59 H 63 N 5 O 17 Zn 4 crystal system cubic space group Ia-3 fw 1375.73 a, Å 22.541(5) V Å 3 11453(4) Z 8 ρ calc, g/cm 3 1.596 temperature 293(2) K λ, Å 0.71073 µ, mm -1 1.733 GOF 1.070 F(000) 5664 no. of data collcd 4234 no. of unique data 2201 no. of obsd data [I>2σ(I)] 1180 no. of variables 118 Crystal size 0.3 x 0.15 x 0.15 mm θ range for data collection 3.13 to 27.47 º Limiting indices -29 h 29, -20 k 20, -20 l 20 Completeness to theta = 27.47 99.8 % Refinement method Full-matrix least-squares on F 2 Final R indices [I>2σ(I)] [a] R 1 = 0.0898, [b] wr2 = 0.2815 R indices (all data) R [a] 1 = 0.1358, wr [b] 2 = 0.3019 Largest diff. peak and hole 0.783 and -0.610 e Å -3 [a] R = Σ Fo - F c /Σ F o [b] wr(f 2 ) = [Σw(F o 2 - Fc 2 ) 2 /Σw(F o 2 ) 2 ] ½ where w = 1/[σ 2 (F o 2 ) + (0.1890P) 2 + (0.0000)P], P = (Fo 2 + 2F c 2 )/3 S5

Table S2. Fractional atomic coordinates and equivalent displacement parameters (Å 2 ) for [Zn 4 O(NTB) 2 ] 3DEF EtOH (1) [squeezed data] atom x y z U eq * O1 0.2500 0.7500 0.2500 0.0296(15) Zn1 0.23669(5) 0.71183(5) 0.32732(5) 0.0398(5) Zn2 0.29885(5) 0.70115(5) 0.20115(5) 0.0453(7) N1 0.4000(2) 0.4000(2) 0.4000(2) 0.080(3) O2 0.1540(3) 0.7066(4) 0.3460(4) 0.060(2) O3 0.2739(3) 0.7565(5) 0.3921(4) 0.071(3) O4 0.3319(3) 0.6367(4) 0.2499(4) 0.066(2) O5 0.2600(5) 0.6279(4) 0.3129(7) 0.104(4) C1 0.3091(3) 0.6104(3) 0.2920(3) 0.0688(19) C2 0.3330(2) 0.5556(2) 0.3193(2) 0.0626(17) C3 0.3925(4) 0.5436(4) 0.3252(5) 0.161(5) C4 0.4159(3) 0.4966(3) 0.3515(4) 0.127(4) C5 0.3782(3) 0.4520(2) 0.3721(3) 0.0730(18) C6 0.3183(3) 0.4601(3) 0.3654(3) 0.091(2) C7 0.2963(3) 0.5099(3) 0.3395(3) 0.092(3) * U eq = (1/3) ΣiΣj U ij a* i a* jai aj S6

Table S3. Selected bond distances (Å) and angles ( ) for [Zn 4 O(NTB) 2 ] 3DEF EtOH (1) [squeezed data] Zn1---Zn2 3.179(2) Zn1---Zn1A 3.195(2) N1-C5 1.418(5) Zn2-O1 1.907(2) Zn2-O4 1.967(7) Zn1-O2 1.914(8) Zn1-O3 1.962(9) Zn1-O1 1.9667(11) Zn1-O5 1.990(10) C1-O2B 1.288(11) Zn2-Zn1-Zn1A 59.8(9) Zn1-Zn2-Zn1A 60.3(1) C5-N1-C5D 119.94(4) O1-Zn2-O4 108.8(3) O4D-Zn2-O4 110.1(3) O2-Zn1-O1 111.7(3) O3-Zn1-O1 111.7(3) O5-Zn1-O1 103.4(4) O2-Zn1-O3 106.5(3) O2-Zn1-O5 103.5(4) O3-Zn1-O5 119.8(6) Zn1-O1-Zn2 110.31(3) Zn1E-O1-Zn1 108.62(3) C1C-O2-Zn1 126.8(6) C1B-O3-Zn1 126.2(7) C1-O4-Zn2 128.8(6) C1-O5-Zn1 125.9(7) C1-O3C 1.254(12) O4-C1 1.232(10) O5-C1 1.266(11) C1-C2 1.482(8) C2-C3 1.374(9) C2-C7 1.398(8) C3-C4 1.324(10) C4-C5 1.395(9) C5-C6 1.371(8) C6-C7 1.360(8) O2B-C1-O3C 130.8(8) O4-C1-O5 120.3(8) O2B-C1-C2 113.0(8) O3C-C1-C2 116.2(8) O4-C1-C2 124.7(6) O5-C1-C2 108.6(8) C3-C2-C7 113.6(5) C3-C2-C1 124.0(6) C7-C2-C1 122.3(5) C4-C3-C2 126.1(7) C3-C4-C5 118.9(7) C6-C5-C4 117.9(5) C6-C5-N1 119.9(5) C4-C5-N1 122.2(5) C7-C6-C5 121.1(6) C6-C7-C2 122.2(6) Symmetry code: A: 0.5-z, 1-x, y-0.5, B: z, 0.5+x, 1-y, C: y-0.5, 1-z, x, D: y, z, x, E: z, x, y. S7

Table S4. Crystallographic data for [Zn 4 O(NTB) 2 ] (1 ) formula C 42 H 24 N 2 O 13 Zn 4 crystal system cubic space group Pa-3 fw 1026.22 a, Å 22.393(5) V Å 3 11229(4) Z 8 ρ calc, g/cm 3 1.214 temperature 293(2) K λ, Å 0.71073 µ, mm -1 1.738 GOF 1.154 F(000) 4112 no. of data collcd 6952 no. of unique data 4287 no. of obsd data [I>2σ(I)] 2367 no. of variables 184 Crystal size 0.3 x 0.15 x 0.15 mm θ range for data collection 1.57 to 27.47 º Limiting indices -29 h 29, -20 k 20, -20 l 20 Completeness to theta = 27.47 99.8 % Refinement method Full-matrix least-squares on F 2 Final R indices [I>2σ(I)] R [a] [b] 1 = 0.0720, wr 2 = 0.1888 R indices (all data) R [a] [b] 1 = 0.1584, wr 2 = 0.2537 Largest diff. peak and hole 0.971 and 1.691 e Å -3 [a] R = Σ Fo - F c /Σ F o [b] wr(f 2 ) = [Σw(F o 2 - Fc 2 ) 2 /Σw(F o 2 ) 2 ] ½ where w = 1/[σ 2 (F o 2 ) + (0.1152P) 2 + (13.74)P], P = (Fo 2 + 2F c 2 )/3 S8

Table S5. Fractional atomic coordinates and equivalent displacement parameters (Å 2 ) for [Zn 4 O(NTB) 2 ] (1 ) atom x y z U eq * O1 0.24977(19) 0.75023(19) 0.25023(19) 0.0525(17) Zn1 0.22345(3) 0.66780(3) 0.25134(3) 0.0544(3) Zn2 0.19954(3) 0.80046(3) 0.30046(3) 0.0510(4) N1 0.44253(13) 0.44253(12) 0.44253(12) 0.074(3) O2 0.27857(13) 0.61845(12) 0.29474(12) 0.0798(15) O3 0.36108(13) 0.67219(12) 0.29728(12) 0.0856(17) C1 0.33146(13) 0.62692(12) 0.30982(12) 0.0629(18) C2 0.35971(13) 0.58016(12) 0.34510(12) 0.0614(18) C3 0.42226(13) 0.58021(12) 0.35643(12) 0.073(2) C4 0.4480(4) 0.5349(3) 0.3880(3) 0.073(2) C5 0.4147(3) 0.4898(3) 0.4102(3) 0.0660(19) C6 0.3531(4) 0.4881(4) 0.3996(4) 0.083(2) C7 0.3271(4) 0.5334(4) 0.3683(4) 0.080(2) N2-0.1012(3) 0.6012(3) 0.3988(3) 0.070(3) O4 0.1272(2) 0.7572(2) 0.3238(2) 0.0682(13) O5 0.1519(3) 0.6646(3) 0.2980(4) 0.114(2) C8 0.1166(3) 0.7026(3) 0.3190(3) 0.0643(18) C9 0.0594(3) 0.6782(3) 0.3404(3) 0.067(2) C10 0.0140(4) 0.7131(3) 0.3609(4) 0.080(2) C11-0.0387(3) 0.6891(3) 0.3782(4) 0.082(2) C12-0.0472(3) 0.6272(3) 0.3782(3) 0.067(2) C13-0.0011(4) 0.5915(4) 0.3588(5) 0.097(3) C14 0.05124(13) 0.61577(12) 0.33962(12) 0.097(3) * U eq = (1/3) Σ i Σ j U ij a * i a* j a i a j S9

Table S6. Selected bond distances (Å) and angles ( ) for [Zn 4 O(NTB) 2 ] (1 ) Zn1---Zn2 3.213(2) Zn1---Zn1A 3.123(1) O1-Zn1 1.938(3) O1-Zn2 1.948(8) Zn1-O5 1.914(6) Zn1-O2 1.921(5) Zn1-O3B 1.943(5) Zn2-O4 1.960(4) O2-C1 1.246(9) O3-C1 1.244(9) N1-C5 1.426(7) C1-C2 1.456(10) C2-C7 1.378(10) C2-C3 1.423(10) Zn2-Zn1-Zn1A 58.2(0) Zn1-Zn2-Zn1A 60.9(0) Zn1-O1-Zn1B 107.3(2) Zn1-O1-Zn2 111.5(2) O5-Zn1-O2 103.9(3) O5-Zn1-O1 107.3(3) O2-Zn1-O1 111.04(18) O5-Zn1-O3B 106.6(3) O2-Zn1-O3B 115.1(2) O1-Zn1-O3B 112.2(2) O1-Zn2-O4 110.26(15) O4-Zn2-O4B 108.67(16) C1-O2-Zn1 131.3(5) C1-O3-Zn1C 128.3(5) C5-N1-C5D 118.7(2) O3-C1-O2 124.7(7) O3-C1-C2 118.5(7) O2-C1-C2 116.8(7) C7-C2-C3 117.1(7) C7-C2-C1 121.4(7) C3-C2-C1 121.6(7) C4-C3-C2 120.5(7) C3-C4 1.365(10) C4-C5 1.349(10) C5-C6 1.401(11) C6-C7 1.364(10) O4-C8 1.250(8) O5-C8 1.253(9) N2-C12 1.419(7) C8-C9 1.472(10) C9-C10 1.363(11) C9-C14 1.411(11) C10-C11 1.354(10) C11-C12 1.399(10) C12-C13 1.375(11) C13-C14 1.362(11) C5-C4-C3 120.9(7) C4-C5-C6 120.2(7) C4-C5-N1 120.1(7) C6-C5-N1 119.7(7) C7-C6-C5 119.1(8) C6-C7-C2 122.2(8) C8-O4-Zn2 128.1(5) C8-O5-Zn1 135.0(5) C12-N2-C12E 119.56(14) O4-C8-O5 125.3(7) O4-C8-C9 119.9(6) O5-C8-C9 114.8(7) C10-C9-C14 118.4(7) C10-C9-C8 123.2(7) C14-C9-C8 118.4(7) C11-C10-C9 121.3(7) C10-C11-C12 120.8(7) C13-C12-C11 118.3(7) C13-C12-N2 120.2(7) C11-C12-N2 121.5(7) C14-C13-C12 121.0(8) C13-C14-C9 120.2(8) Symmetry code: A: 1-y, 0.5+z, 0.5-x, B: 0.5-z, 1-x, -0.5+y, C: 1-y, 0.5+z, 0.5-z, D: y, z, x, E: 0.5-y, 1-z, 0.5+x. S10

Table S7. Crystallographic data for [Zn 4 O(NTB) 2 ] xdef yetoh (1 ) crystal system cubic space group Ia-3 a, Å 22.4509(4) V Å 3 11316.2(3) temperature 293(2) K λ, Å 0.71073 GOF 1.170 no. of data collcd 4164 no. of unique data 2165 no. of obsd data [I>2σ(I)] 1505 no. of variables 118 Crystal size 0.5 x 0.25 x 0.25 mm θ range for data collection 3.40 to 27.45 º Limiting indices -29 h 29, -20 k 20, -20 l 20 Completeness to theta = 27.45 99.8 % Refinement method Full-matrix least-squares on F 2 Final R indices [I>2σ(I)] R [a] 1 = 0.0823, wr [b] 2 = 0.2442 R indices (all data) R [a] 1 = 0.1185, wr [b] 2 = 0.2854 Largest diff. peak and hole 0.961 and 0.366 e Å -3 [a] R = Σ Fo - F c /Σ F o [b] wr(f 2 ) = [Σw(F o 2 - F c 2 ) 2 /Σw(F o 2 ) 2 ]½ where w = 1/[σ 2 (F o 2 ) + (0.1616P) 2 + (21.90)P], P =(Fo 2 + 2Fc 2 )/3. S11

Table S8. Fractional atomic coordinates and equivalent displacement parameters (Å 2 ) for [Zn 4 O(NTB) 2 ] xdef yetoh (1 ) * atom x y z U eq O1 0.2500 0.7500 0.2500 0.0442(15) Zn1 0.23503(4) 0.71399(4) 0.32880(4) 0.0457(4) Zn2 0.29728(4) 0.70272(4) 0.20272(4) 0.0409(5) N1 0.3987(3) 0.3987(3) 0.3987(3) 0.087(3) O2 0.1493(4) 0.7131(5) 0.3449(4) 0.073(2) O3 0.2789(4) 0.7542(4) 0.3907(4) 0.065(2) O4 0.3326(4) 0.6376(4) 0.2492(4) 0.064(2) O5 0.2588(5) 0.6315(4) 0.3171(5) 0.088(3) C1 0.3079(3) 0.6098(2) 0.2928(2) 0.0577(13) C2 0.3320(2) 0.5548(2) 0.3182(2) 0.0582(13) C3 0.3912(3) 0.5448(3) 0.3234(4) 0.100(3) C4 0.4137(3) 0.4934(3) 0.3487(4) 0.105(3) C5 0.3764(3) 0.4515(3) 0.3707(3) 0.0749(18) C6 0.3167(3) 0.4579(3) 0.3639(3) 0.086(2) C7 0.2941(3) 0.5102(3) 0.3388(3) 0.0797(19) * U eq = (1/3) Σ i Σ j U ij a * i a* j a i a j S12

Table S9. Selected bond distances (Å) and angles ( ) for [Zn 4 O(NTB) 2 ] xdef yetoh (1 ) Zn1---Zn2 3.167(2) Zn1---Zn1A 3.164(2) N1-C5 1.432(5) Zn2-O1 1.838(2) Zn2-O4 1.965(8) Zn1-O2 1.958(8) Zn1-O3 1.929(7) Zn1-O1 1.974(1) Zn1-O5 1.945(9) C1-O2B 1.224(10) Zn2-Zn1-Zn1A 60.04(2) Zn1-Zn2-Zn1A 59.93(4) C5-N1-C5D 119.94(5) O1-Zn2-O4 110.9(3) O4D-Zn2-O4 108.0(3) O2-Zn1-O1 109.7(3) O3-Zn1-O1 111.6(3) O5-Zn1-O1 102.8(3) O2-Zn1-O3 111.9(4) O2-Zn1-O5 106.6(5) O3-Zn1-O5 113.7(5) Zn1-O1-Zn2 112.29(3) Zn1E-O1-Zn1 106.51(3) C1C-O2-Zn1 126.1(6) C1B-O3-Zn1 125.0(6) C1-O4-Zn2 126.2(6) C1-O5-Zn1 129.5(6) C1-O3C 1.245(10) O4-C1 1.285(10) O5-C1 1.323(10) C1-C2 1.463(7) C2-C3 1.355(8) C2-C7 1.393(8) C3-C4 1.382(9) C4-C5 1.352(8) C5-C6 1.356(9) C6-C7 1.398(8) O2B-C1-O3C 129.6(7) O4-C1-O5 119.6(6) O2B-C1-C2 113.8(7) O3C-C1-C2 116.5(6) O4-C1-C2 123.1(6) O5-C1-C2 117.2(5) C3-C2-C7 116.9(5) C3-C2-C1 122.4(5) C7-C2-C1 120.7(5) C4-C3-C2 122.2(6) C3-C4-C5 120.3(6) C6-C5-C4 119.8(5) C6-C5-N1 118.8(6) C4-C5-N1 121.4(6) C7-C6-C5 119.6(6) C6-C7-C2 121.0(5) Symmetry code: A: 0.5-z, 1-x, y-0.5, B: z, 0.5+x, 1-y, C: y-0.5, 1-z, x, D: y, z, x, E: z, x, y. S13

Table S10. Crystallographic data for [Zn 4 O(NTB) 2 ] 3DEF EtOH (1) [raw data] formula C 59 H 63 N 5 O 17 Zn 4 crystal system cubic space group Ia-3 fw 1375.73 a, Å 22.541(5) V Å 3 11453(4) Z 8 ρ calc, g/cm 3 1.596 temperature 293(2) K λ, Å 0.71073 µ, mm -1 1.733 GOF 1.102 F(000) 5664 no. of data collcd 4234 no. of unique data 2201 no. of obsd data [I>2σ(I)] 1185 no. of variables 134 Crystal size 0.3 x 0.15 x 0.15 mm θ range for data collection 3.13 to 27.47 º Limiting indices -29 h 29, -20 k 20, -20 l 20 Completeness to theta = 27.47 99.8 % Refinement method Full-matrix least-squares on F 2 Final R indices [I>2σ(I)] [a] R 1 = 0.0978, [b] wr2 = 0.2775 R indices (all data) R [a] 1 = 0.1605, wr [b] 2 = 0.3103 Largest diff. peak and hole 0.764 and -0.649 e Å -3 [a] R = Σ Fo - F c /Σ F o [b] wr(f 2 ) = [Σw(F o 2 - Fc 2 ) 2 /Σw(F o 2 ) 2 ] ½ where w = 1/[σ 2 (F o 2 ) + (0.1890P) 2 + (0.0000)P], P = (Fo 2 + 2F c 2 )/3 S14

Table S11. Fractional atomic coordinates and equivalent displacement parameters (Å 2 ) for [Zn 4 O(NTB) 2 ] 3DEF EtOH (1) [raw data] atom x y z U eq * O1 0.2500 0.7500 0.2500 0.0283(16) Zn1 0.23683(5) 0.71200(5) 0.32714(5) 0.0394(5) Zn2 0.29878(5) 0.70122(5) 0.20122(5) 0.0453(7) N1 0.4001(3) 0.4001(3) 0.4001(3) 0.075(3) O2 0.1528(4) 0.7084(5) 0.3455(4) 0.066(3) O3 0.2751(4) 0.7550(5) 0.3921(4) 0.067(3) O4 0.3313(4) 0.6354(5) 0.2477(5) 0.065(3) O5 0.2613(6) 0.6305(5) 0.3190(7) 0.107(4) C1 0.3098(4) 0.6104(3) 0.2913(3) 0.067(2) C2 0.3332(3) 0.5551(3) 0.3190(3) 0.0600(17) C3 0.3921(4) 0.5445(4) 0.3248(5) 0.128(4) C4 0.4156(4) 0.4959(4) 0.3514(5) 0.122(4) C5 0.3784(3) 0.4524(3) 0.3724(3) 0.0647(18) C6 0.3190(3) 0.4601(3) 0.3657(4) 0.101(3) C7 0.2958(3) 0.5104(3) 0.3383(4) 0.094(3) C1S 0.2696(3) 0.6430(3) 0.5587(4) 0.186(13) N1S 0.2500(3) 0.6154(3) 0.5001(4) 0.74(7) C2S 0.1884(3) 0.5803(3) 0.4722(4) 0.28(2) t * U eq =(1/3)Σ i Σ j U ij a * i a* j a i a j S15

Table S12. Selected bond distances (Å) and angles ( ) for [Zn 4 O(NTB) 2 ] 3DEF EtOH (1) [raw data] Zn1---Zn2 3.173(2) Zn1---Zn1A 3.185(2) N1-C5 1.421(5) Zn2-O1 1.905(2) Zn2-O4 1.959(8) Zn1-O5 1.927(11) Zn1-O2 1.940(8) Zn1-O3 1.957(8) Zn1-O1 1.9610(12) O4-C1 1.232(10) O5-C1 1.337(14) C1-O2B 1.249(12) C1-O3C 1.289(12) C1-C2 1.492(8) C2-C3 1.355(10) C2-C7 1.385(9) C3-C4 1.356(11) C4-C5 1.374(10) C5-C6 1.358(10) C6-C7 1.393(9) Zn2-Zn1-Zn1A 59.87(3) Zn1-Zn2-Zn1A 60.26(5) C5-N1-C5D 119.93(5) O1-Zn2-O4 110.2(3) O4D-Zn2-O4 108.8(3) O5-Zn1-O2 105.1(5) O5-Zn1-O3 114.7(6) O2-Zn1-O3 106.9(4) O5-Zn1-O1 106.8(4) O2-Zn1-O1 110.8(3) O3-Zn1-O1 112.4(3) Zn2-O1-Zn1 110.31(3) Zn1-O1-Zn1E 108.62(3) C1C-O2-Zn1 127.5(7) C1B-O3-Zn1 124.5(7) C1-O4-Zn2 128.7(7) C1-O5-Zn1 126.9(8) O2B-C1-O3C 130.8(8) O4-C1-O5 122.7(8) O4-C1-C2 125.2(7) O2B-C1-C2 114.2(8) O3C-C1-C2 114.9(8) O5-C1-C2 112.1(7) C3-C2-C7 116.0(6) C3-C2-C1 122.3(6) C7-C2-C1 121.6(6) C2-C3-C4 124.6(7) C3-C4-C5 119.4(7) C6-C5-C4 118.1(6) C6-C5-N1 119.6(6) C4-C5-N1 122.3(6) C5-C6-C7 121.6(7) C2-C7-C6 120.1(6) Symmetry code: A: 0.5-z, 1-x, y-0.5, B: z, 0.5+x, 1-y, C: y-0.5, 1-z, x, D: y, z, x, E: z, x, y. S16

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