Supplementary information Zou-2005-04-4749
Supplementary Information by Zou et al.
Content:
Figure 1 Nitrogen adsorption and desorption isotherm and pore-size distribution plot for SU-M.
Figure 2 In situ X-ray powder diffraction of SU-M.
Figure 3 A curve of thermogravimetrical analysis of SU-M.
Figure 4 SEM image of a SU-MB crystal.
Table 1 Crystal Data and Details of the Structure Determination for SU-M.
Table 2 Atomic coordinates and equivalent isotropic (for all Ge and O1 - O24) and isotropic (for the rest of the atoms) displacement parameters for SU-M.
Table 3 Crystal Data and Details of the Structure Determination for SU-MB.
Table 4 Atomic coordinates and equivalent isotropic (for all Ge) and isotropic (for the rest of the atoms) displacement parameters for SU-MB.
Figure 1 Nitrogen adsorption and desorption isotherm for as-synthesized SU-M. The inset is a pore-width distribution plot calculated by NLDFT28 using a slit model. The isotherm was measured using a Micromeritics ASAP 2020 system. The sample was degassed first at 297 K for 5h and then at 357 K for 5h.
Figure 2 In situ X-ray powder diffraction of as synthesized SU-M, performed on a Huber Guinier camera 670 equipped with an imaging plate, using synchrotron radiation at Beamline I711, Max-lab, Lund University, Sweden. The sample was heated in air to 200 C with 50 C /step and from 200 to 340 C with 20 C /step, with an average heating rate of 7 C /min. X-ray powder diffraction data were collected at each step.
Figure 3 A curve of thermogravimetrical analysis of as synthesized SU-M in N2, with a heating rate of 5 C min-1. The sample was kept under N2 flow for 1h before heating, resulting in 5% weight loss of surface water.
Figure 4 SEM image of a SU-MB crystal. The shape of the crystals of SU-M is similar, but with larger sizes (160x160x160 m3).
Table 1 - Crystal Data and Details of the Structure Determination for SU-M.
Crystal Data
------
Crystal System Cubic
Space group Ia-3d (No.230)
a, b, c [Å] 51.335(3) 51.335(3) 51.335(3)
V [Å3] 135282(14)
Z 8
D(calc) [g/cm3] 1.692
Mu(MoKa) [/mm ] 5.330
F(000) 64800
Crystal Size [mm] 0.16 x 0.16 x 0.16
Data Collection
------
Temperature (K) 170
Radiation [Å] MoK 0.71073
Theta Min-Max [Deg] 2.2, 24.1
Dataset -58: 45 ; -58: 51 ; -50: 58
Tot., Uniq. Data, R(int) 134976, 8922, 0.141
Observed data [I > 2.0 sigma(I)] 6519
Refinement
------
Nref, Npar 8922, 409
R, wR2, S 0.0744, 0.2362, 1.01
w = 1/[\S2(FO2)+(0.1452P)2+3863.4155P] Where P=(FO2+2FC2)/3
Max. and Av. Shift/Error 0.00, 0.00
Min. and Max. Resd. Dens. [e/Å3] -1.43, 1.53
------
Table 2 Atomic coordinates and equivalent isotropic (for all Ge and O1-O24) and isotropic (for the rest of the atoms) displacement parameters for SU-M.
Atom / x / y / z / Ueq/Uiso(Å2) / OccupancyGe1 / 0.20570(2) / 0.35477(2) / 0.15033(2) / 0.0297(4) / 1.00
Ge2 / 0.24867(2) / 0.32670(2) / 0.12261(2) / 0.0295(4) / 1.00
Ge3 / 0.25472(2) / 0.38345(2) / 0.13662(2) / 0.0250(4) / 1.00
Ge4 / 0.25521(3) / 0.34264(3) / 0.17806(2) / 0.0358(4) / 1.00
Ge5 / 0.20155(2) / 0.40713(2) / 0.12204(2) / 0.0238(3) / 1.00
Ge6 / 0.26654(2) / 0.36543(2) / 0.08078(2) / 0.0243(4) / 1.00
Ge7 / 0.20495(2) / 0.37344(2) / 0.06974(2) / 0.0255(4) / 1.00
Ge8 / 0.20300(3) / 0.34340(3) / 0.21087(3) / 0.0389(4) / 1.00
Ge9 / 0.19267(3) / 0.32118(3) / 0.10204(3) / 0.0398(5) / 1.00
Ge10 / 0.28449(4) / 0.39537(4) / 0.18792(3) / 0.0622(7) / 1.00
O1 / 0.18764(16) / 0.38555(17) / 0.14439(16) / 0.032(3) / 1.00
O2 / 0.18844(17) / 0.34957(19) / 0.18082(18) / 0.041(3) / 1.00
O3 / 0.23445(16) / 0.37361(17) / 0.16733(16) / 0.034(3) / 1.00
O4 / 0.22871(15) / 0.36031(16) / 0.11931(15) / 0.027(2) / 1.00
O5 / 0.22960(17) / 0.32587(17) / 0.15508(16) / 0.034(3) / 1.00
O6 / 0.18264(17) / 0.33476(18) / 0.13170(18) / 0.038(3) / 1.00
O7 / 0.27079(15) / 0.34995(17) / 0.14394(15) / 0.029(2) / 1.00
O8 / 0.26747(16) / 0.33390(16) / 0.09274(16) / 0.031(3) / 1.00
O9 / 0.26866(18) / 0.29812(18) / 0.12952(18) / 0.040(3) / 1.00
O10 / 0.22381(18) / 0.30788(17) / 0.1051(2) / 0.043(3) / 1.00
O11 / 0.23439(15) / 0.41183(15) / 0.12887(16) / 0.028(2) / 1.00
O12 / 0.27815(18) / 0.40244(18) / 0.15521(18) / 0.041(3) / 1.00
O13 / 0.27383(15) / 0.38728(16) / 0.10594(15) / 0.028(2) / 1.00
O14 / 0.23615(18) / 0.3359(2) / 0.20722(18) / 0.050(3) / 1.00
O15 / 0.27879(19) / 0.3635(2) / 0.19564(18) / 0.048(3) / 1.00
O16 / 0.27434(18) / 0.3128(2) / 0.18296(18) / 0.045(3) / 1.00
O17 / 0.18827(17) / 0.43827(17) / 1/8 / 0.029(3) / 1.00
O18 / 0.19439(16) / 0.39880(17) / 0.08945(15) / 0.031(3) / 1.00
O19 / 0.28840(16) / 0.36736(19) / 0.05524(16) / 0.036(2) / 1.00
O20 / 0.23831(14) / 0.37356(17) / 0.06344(16) / 0.029(3) / 1.00
O21 / 0.19024(17) / 0.34360(18) / 0.07610(19) / 0.040(3) / 1.00
O22 / 0.1708(2) / 0.2970(2) / 0.0915(3) / 0.066(3) / 1.00
O23 / 0.2662(5) / 0.4156(4) / 0.2083(3) / 0.121(9) / 1.00
O24 / 0.3170(4) / 0.4019(6) / 0.1939(4) / 0.153(12) / 1.00
N1 / 0.3928(3) / 1.0724(4) / 0.1300(4) / 0.084(5) / 1.00
C1 / 0.3804(6) / 1.0876(6) / 0.1099(5) / 0.140(12) / 1.00
C2 / 0.3564(5) / 1.1025(5) / 0.1200(5) / 0.125(10) / 1.00
C3 / 0.3513(5) / 1.125 / 0.1013(5) / 0.146(18) / 1.00
N2 / 0.3038(4) / 0.2920(4) / 0.0847(3) / 0.084(5) / 1.00
C4 / 0.3097(4) / 0.2904(5) / 0.0570(4) / 0.082(6) / 1.00
C5 / 0.2866(8) / 0.2948(9) / 0.0401(5) / 0.165(15) / 1.00
N3 / 0.2781(3) / 1.1104(3) / 0.1398(3) / 0.061(4) / 1.00
C6 / 0.2597(3) / 1.1171(3) / 0.1136(3) / 0.048(3) / 1.00
N4 / 0.7884(4) / 0.5599(4) / 0.0953(4) / 0.097(6) / 1.00
C7 / 0.9052(3) / 1.2145(3) / 0.0716(3) / 0.058(4) / 1.00
C8 / 0.9308(3) / 1.2244(3) / 0.0775(3) / 0.053(4) / 1.00
OW1 / 0.2896(2) / 1.1250(2) / 0.0557(2) / 0.011(3) / 0.50
OW2 / 0.2200(3) / 1.1176(3) / 0.1402(3) / 0.097(5) / 1.00
OW3 / 0.2772(5) / 1.1720(5) / 0.2158(5) / 0.160(9) / 1.00
OW4 / 0.2965(4) / 1.1715(4) / 0.1630(4) / 0.104(5) / 1.00
OW5 / 0.9415(5) / 1.2663(5) / 0.1784(5) / 0.136(7) / 1.00
OW6 / 0.2058(4) / 1.1340(4) / 0.0876(4) / 0.119(6) / 1.00
OW7 / 0.2277(5) / 1.1643(5) / 0.1043(5) / 0.136(7) / 1.00
OW8 / 0.2866(3) / 1.1547(3) / 0.1072(3) / 0.020(4) / 0.53(2)
OW9 / 0.2851(2) / 1.1589(2) / 0.0831(3) / 0.009(4) / 0.47(2)
OW10 / 0.8630(7) / 0.7557(7) / 0.0394(7) / 0.203(13) / 1.00
OW11 / 0.2369(4) / 1.1092(4) / 0.0820(4) / 0.112(6) / 1.00
OW12 / 3/4 / 5/8 / 0 / 0.33(6) / 1.00
OW13 / 0.6219(9) / 0.4962(9) / -0.0018(9) / 0.254(18) / 1.00
OW14 / 0.9589(3) / 1.2575(3) / 0.1196(3) / 0.021(7) / 0.42(3)
OW15 / 0.2504(7) / 1.1351(7) / 0.0574(7) / 0.113(13) / 0.58(3)
Table 3 Crystal Data and Details of the Structure Determination for SU-MB.
Crystal Data
------
Crystal System Cubic
Space group I4132 (No.214)
a, b, c [Å] 50.873(3) 50.873(3) 50.873(3)
V [Å3] 131663(13)
Z 1
D(calc) [g/cm3] 1.962
Mu(MoK) [/mm ] 7.325
F(000) 72140
Crystal Size [mm] 0.08 x 0.08 x 0.08
Data Collection
------
Temperature (K) 170
Radiation [Å] MoKa 0.71073
Theta Min-Max [Deg] 4.0, 21.5
Dataset -45: 17 ; -43: 52 ; -44: 52
Tot., Uniq. Data, R(int) 34928, 11888, 0.198
Observed data [I > 2.0 sigma(I)] 6403
Refinement
------
Nref, Npar 11888, 583
R, wR2, S 0.0858, 0.2309, 0.97
w = 1/[\S2(FO2)+(0.1452P)2+3863.4155P] Where P=(FO2+2FC2)/3
Max. and Av. Shift/Error 0.00, 0.00
Flack x 0.50(4)
Min. and Max. Resd. Dens. [e/Å3] -1.47, 1.68
------
Table 4 Atomic coordinates and equivalent isotropic (for all Ge) and isotropic (for the rest of the atoms) displacement parameters for SU-MB.
Atom / x / y / z / Ueq/Uiso(Å2) / OccupancyGe1 / 0.20957(7) / 0.36020(7) / 0.15378(7) / 0.0213(12) / 1.00
Ge2 / 0.25038(7) / 0.32807(7) / 0.12594(7) / 0.0220(12) / 1.00
Ge3 / 0.25889(8) / 0.38558(8) / 0.13562(8) / 0.0237(12) / 1.00
Ge4 / 0.25999(8) / 0.34770(8) / 0.18023(8) / 0.0250(12) / 1.00
Ge5 / 0.20630(8) / 0.41166(8) / 0.12239(7) / 0.0225(12) / 1.00
Ge6 / 0.26727(7) / 0.36318(8) / 0.08009(8) / 0.0226(12) / 1.00
Ge7 / 0.20572(7) / 0.37447(8) / 0.07196(7) / 0.0203(12) / 1.00
Ge8 / 0.20834(7) / 0.34973(8) / 0.21495(8) / 0.0261(12) / 1.00
Ge9 / 0.19298(7) / 0.32425(7) / 0.10825(8) / 0.0231(12) / 1.00
Ge10 / 0.29160(14) / 0.39988(12) / 0.18441(11) / 0.063(3) / 0.88(2)
Ge11 / -0.20482(7) / -0.35576(7) / -0.14892(7) / 0.0200(12) / 1.00
Ge12 / -0.24567(7) / -0.32566(7) / -0.11970(7) / 0.0220(12) / 1.00
Ge13 / -0.25605(8) / -0.38142(8) / -0.13765(7) / 0.0220(12) / 1.00
Ge14 / -0.25333(7) / -0.33726(8) / -0.17611(7) / 0.0220(12) / 1.00
Ge15 / -0.20459(8) / -0.41006(8) / -0.12294(8) / 0.0217(12) / 1.00
Ge16 / -0.26765(7) / -0.36586(8) / -0.08086(7) / 0.0220(12) / 1.00
Ge17 / -0.20662(8) / -0.37737(8) / -0.06919(7) / 0.0227(12) / 1.00
Ge18 / -0.20080(7) / -0.34006(7) / -0.20856(7) / 0.0227(12) / 1.00
Ge19 / -0.18925(8) / -0.32520(8) / -0.09922(8) / 0.0270(12) / 1.00
Ge20 / -0.28551(8) / -0.38710(8) / -0.19126(8) / 0.0270(14) / 1.00
Ge21 / 0.12081(8) / 0.21109(8) / 0.12527(8) / 0.0327(17) / 1.00
Ge22 / 0.11518(8) / 0.27589(8) / 0.15962(8) / 0.0270(12) / 1.00
Ge23 / 0.15244(8) / 0.27458(8) / 0.11525(8) / 0.0260(12) / 1.00
Ge24 / 0.07404(9) / 0.24958(8) / 0.12284(9) / 0.0367(17) / 1.00
Ge25 / 0.11334(9) / 0.24688(9) / 0.07720(8) / 0.0383(17) / 1.00
Ge26 / 0.13762(8) / 0.22407(8) / 0.18231(8) / 0.0317(16) / 1.00
Ge27 / 0.17803(8) / 0.22520(8) / 0.13851(8) / 0.0307(16) / 1.00
O1 / 0.1928(4) / 0.3917(4) / 0.1464(4) / 0.021(6) / 1.00
O2 / 0.1927(5) / 0.3576(5) / 0.1845(5) / 0.031(7) / 1.00
O3 / 0.2394(4) / 0.3782(4) / 0.1681(4) / 0.021(6) / 1.00
O4 / 0.2322(4) / 0.3630(4) / 0.1219(4) / 0.024(6) / 1.00
O5 / 0.2323(4) / 0.3297(4) / 0.1606(4) / 0.021(6) / 1.00
O6 / 0.1856(4) / 0.3410(4) / 0.1370(4) / 0.017(6) / 1.00
O7 / 0.2734(4) / 0.3519(4) / 0.1438(4) / 0.017(5) / 1.00
O8 / 0.2667(4) / 0.3322(4) / 0.0943(4) / 0.023(6) / 1.00
O9 / 0.2702(4) / 0.2988(4) / 0.1343(4) / 0.026(6) / 1.00
O10 / 0.2251(5) / 0.3090(5) / 0.1108(5) / 0.028(6) / 1.00
O11 / 0.2398(5) / 0.4146(5) / 0.1268(5) / 0.027(6) / 1.00
O12 / 0.2835(4) / 0.4052(4) / 0.1523(4) / 0.025(6) / 1.00
O13 / 0.2771(4) / 0.3866(4) / 0.1034(4) / 0.010(5) / 1.00
O14 / 0.2425(4) / 0.3445(4) / 0.2113(4) / 0.017(5) / 1.00
O15 / 0.2856(5) / 0.3685(5) / 0.1961(5) / 0.029(6) / 1.00
O16 / 0.2786(4) / 0.3182(4) / 0.1865(4) / 0.021(6) / 1.00
O17 / 0.1944(4) / 0.4444(4) / 1/8 / 0.021(8) / 1.00
O18 / 0.1973(5) / 0.4022(5) / 0.0901(5) / 0.044(8) / 1.00
O19 / 0.2886(5) / 0.3624(5) / 0.0531(5) / 0.030(6) / 1.00
O20 / 0.2377(4) / 0.3724(5) / 0.0634(5) / 0.024(6) / 1.00
O21 / 0.1917(5) / 0.3458(5) / 0.0806(5) / 0.028(6) / 1.00
O22 / 0.1692(5) / 0.3004(5) / 0.0991(5) / 0.031(6) / 1.00
O23 / 0.2798(9) / 0.4236(9) / 0.2061(9) / 0.103(15) / 0.88(2)
O24 / 0.3287(12) / 0.4058(13) / 0.1857(13) / 0.15(2) / 0.88(2)
O25 / -0.1884(5) / -0.3895(5) / -0.1454(5) / 0.029(6) / 1.00
O26 / -0.1873(5) / -0.3492(5) / -0.1787(5) / 0.031(6) / 1.00
O27 / -0.2345(4) / -0.3702(4) / -0.1679(4) / 0.015(5) / 1.00
O28 / -0.2284(4) / -0.3608(4) / -0.1184(4) / 0.022(6) / 1.00
O29 / -0.2263(4) / -0.3249(4) / -0.1517(4) / 0.020(6) / 1.00
O30 / -0.1801(4) / -0.3376(4) / -0.1293(4) / 0.022(6) / 1.00
O31 / -0.2687(4) / -0.3461(4) / -0.1429(4) / 0.018(6) / 1.00
O32 / -0.2653(5) / -0.3333(5) / -0.0895(5) / 0.028(6) / 1.00
O33 / -0.2627(4) / -0.2945(4) / -0.1241(5) / 0.029(6) / 1.00
O34 / -0.2188(4) / -0.3104(4) / -0.1008(4) / 0.020(6) / 1.00
O35 / -0.2377(5) / -0.4130(5) / -0.1308(5) / 0.030(7) / 1.00
O36 / -0.2815(5) / -0.3963(5) / -0.1573(5) / 0.027(6) / 1.00
O37 / -0.2745(4) / -0.3869(4) / -0.1075(4) / 0.021(6) / 1.00
O38 / -0.2331(4) / -0.3301(4) / -0.2052(4) / 0.021(6) / 1.00
O39 / -0.2787(5) / -0.3550(5) / -0.1951(5) / 0.030(6) / 1.00
O40 / -0.2725(5) / -0.3055(5) / -0.1786(5) / 0.028(6) / 1.00
O41 / -0.1921(4) / -0.4421(4) / -0.125 / 0.015(8) / 1.00
O42 / -0.1977(5) / -0.4034(5) / -0.0897(5) / 0.026(6) / 1.00
O43 / -0.2900(5) / -0.3679(5) / -0.0562(5) / 0.028(6) / 1.00
O44 / -0.2399(5) / -0.3751(5) / -0.0627(5) / 0.030(6) / 1.00
O45 / -0.1882(4) / -0.3476(4) / -0.0740(4) / 0.025(6) / 1.00
O46 / -0.1659(5) / -0.3020(5) / -0.0895(5) / 0.043(7) / 1.00
O47 / -0.2649(5) / -0.4082(5) / -0.2118(5) / 0.032(6) / 1.00
O48 / -0.3184(5) / -0.3937(5) / -0.1965(5) / 0.041(7) / 1.00
F49 / 0.1136(4) / 0.1772(4) / 0.1191(4) / 0.038(5) / 1.00
O50 / 0.1217(4) / 0.2024(4) / 0.1610(4) / 0.028(6) / 1.00
O51 / 0.1559(4) / 0.2036(4) / 0.1234(5) / 0.027(6) / 1.00
O52 / 0.1194(5) / 0.2159(5) / 0.0884(5) / 0.035(7) / 1.00
O53 / 0.1294(4) / 0.2488(4) / 0.1323(4) / 0.026(6) / 1.00
O54 / 0.0846(5) / 0.2176(5) / 0.1285(5) / 0.035(7) / 1.00
O55 / 0.1397(4) / 0.2932(4) / 0.1416(4) / 0.022(6) / 1.00
O56 / 0.0829(5) / 0.2733(5) / 0.1462(5) / 0.032(7) / 1.00
O57 / 0.1377(5) / 0.2690(5) / 0.0849(5) / 0.037(7) / 1.00
O58 / 0.1807(5) / 0.2550(5) / 0.1243(5) / 0.035(7) / 1.00
O59 / 0.0831(5) / 0.2594(5) / 0.0892(5) / 0.042(7) / 1.00
F60 / 0.0405(6) / 0.2518(5) / 0.1218(5) / 0.076(8) / 1.00
F61 / 0.1098(5) / 0.2446(5) / 0.0429(5) / 0.059(7) / 1.00
O62 / 0.1707(5) / 0.2280(5) / 0.1729(5) / 0.029(6) / 1.00
O63 / 0.1374(5) / 0.2113(5) / 0.2133(5) / 0.033(6) / 1.00
O64 / 0.1251(5) / 0.2545(5) / 0.1855(5) / 0.029(6) / 1.00
N1 / 0.0950(6) / 0.2058(6) / 0.9385(6) / 0.031(8) / 1.00
C1 / -0.0328(13) / 0.6733(13) / 0.2053(13) / 0.10(2) / 1.00
C2 / -0.0025(11) / 0.6773(10) / 0.1988(10) / 0.072(16) / 1.00
N2 / 0.1014(6) / 0.3892(6) / 0.0791(6) / 0.046(9) / 1.00
C3 / 0.1262(6) / 0.3792(7) / 0.0907(8) / 0.047(11) / 1.00
C4 / 0.1210(10) / 0.3548(8) / 0.1069(10) / 0.089(18) / 1.00
N3 / 0.0854(5) / 0.6977(6) / 0.2087(6) / 0.030(8) / 1.00
C5 / 0.0574(5) / 0.6917(7) / 0.2123(7) / 0.029(10) / 1.00
N4 / 0 / 0.75 / 0.1278(16) / 0.16(3) / 1.00
C6 / 0 / 0.75 / 0.0987(16) / 0.10(3) / 1.00
OW1 / 0.0558(8) / 0.8302(7) / 0.0469(8) / 0.091(12) / 1.00
OW2 / -0.1355(7) / -0.2895(7) / -0.1001(7) / 0.083(11) / 1.00
OW3 / 0.1176(9) / 0.6710(9) / 0.1416(9) / 0.121(16) / 1.00
OW4 / 0.0767(8) / 0.8289(8) / 0.3270(8) / 0.092(11) / 1.00
OW5 / 0.0435(11) / 0.4420(11) / 0.0687(11) / 0.15(2) / 1.00
OW6 / 0.3541(6) / 0.4041(6) / 0.2078(6) / 0.056(8) / 1.00
OW7 / 0.3403(7) / 0.4370(7) / 0.1730(7) / 0.084(11) / 1.00
OW8 / 0.0046(9) / 0.5099(9) / 0.3570(9) / 0.122(15) / 1.00
OW9 / 0.1005(5) / 0.1005(5) / 0.1005(5) / 0.043(13) / 1.00
OW10 / 0.0818(10) / 0.5444(10) / 0.5873(10) / 0.10(3) / 0.83(12)
OW11 / 0.0860(10) / 0.5170(10) / 0.8596(10) / 0.02(2) / 0.41(8)
OW12 / 0.3310(9) / 0.4362(10) / 0.2137(9) / 0.02(2) / 0.45(8)
1