Date: Fri, 07 Nov 2003 15:00:49 +0000 To: Armel Le Bail From: Jan Skakle Subject: UPPW-4 Latest Zeolite problem. Doesn't look much like the "proposed" cell. Using Crysfire, various programs gave: I20 Merit Volume V/V1 Pedig a b c alpha beta gamma (ITOH) 20 47.3 1880.16 1.00 251 13.9545 18.3637 7.4362 90.000 99.368 90.000 (FJZN6) 20 47.37 1881.289 1.00 231 13.9580 18.3657 7.4379 90.000 99.365 90.000 (DICVOL91) 20 24.3 1880.929 1.00 Mon__3 16.8463 18.3668 7.4367 90.000 125.171 90.000 20 23.4 1880.722 1.00 Mon__1 13.9582 18.3637 7.4365 90.000 99.370 90.000 (TREOR90) 20 20 1880.299 1.00 Mon__1 16.8522 18.3688 7.4318 90.000 125.182 90.000 (TAUP - no solutions with Merit>7!) (KOHL - no solutions). Taking the results with the high figure of merit given in ITOH and FJZN6 and putting them through Celref gave: CELREF Version 3. 11/7/03 02:12:55 PM ---------------------------------------------------------------------- Initial values : (Refinement keys on 2nd line) -------------- : Zero Lambda a b c alpha beta gamma volume 0.000 1.54180 13.9703 18.3817 7.4400 90.00 99.40 90.00 1884.921 0 0 1 1 1 0 1 0 H K L 2Th(obs) 2Th_obs-shift 2Th(Calc) diff. 1 1 0 8.0100 8.0100 8.0175 -0.0075 0 2 0 9.6200 9.6200 9.6229 -0.0029 0 0 1 12.0700 12.0700 12.0573 0.0127 2 0 0 12.8400 12.8400 12.8456 -0.0056 -1 1 1 13.5800 13.5800 13.5899 -0.0099 0 2 1 15.4200 15.4200 15.4489 -0.0289 1 3 0 15.8300 15.8300 15.8281 0.0019 2 2 0 16.1000 16.1000 16.0746 0.0254 -2 2 1 18.8200 18.8200 18.8236 -0.0036 2 0 1 19.0400 19.0400 19.0496 -0.0096 -1 3 1 19.3000 19.3000 19.2896 0.0104 3 1 0 19.9200 19.9200 19.9198 0.0002 1 3 1 20.5700 20.5700 20.5795 -0.0095 -3 1 1 21.6200 21.6200 21.6239 -0.0039 0 4 1 22.8300 22.8300 22.8305 -0.0005 2 4 0 23.2600 23.2600 23.2647 -0.0047 3 3 0 24.2200 24.2200 24.2127 0.0073 -1 1 2 24.5400 24.5400 24.5419 -0.0019 3 1 1 24.9500 24.9500 24.9608 -0.0108 -2 4 1 25.2800 25.2800 25.2702 0.0098 -3 3 1 25.6400 25.6400 25.6465 -0.0065 4 0 0 25.8600 25.8600 25.8564 0.0036 0 2 2 26.1400 26.1400 26.1445 -0.0045 1 1 2 26.6000 26.6000 26.5805 0.0195 -2 2 2 27.3800 27.3800 27.3758 0.0042 Sqrt(Sum(2Th O-C)**2)/(Nref-Npar)) : 0.0118 Sqrt(Sum(2Th O-C)**2)/Nref ) : 0.0108 Final values : (Standard errors on 2nd line) ------------ Zero Lambda a b c alpha beta gamma volume 0.000 1.54180 13.9703 18.3817 7.4400 90.00 99.40 90.00 1884.948 0.0000 0.00000 0.0082 0.0062 0.0043 0.000 0.115 0.000 H K L 2Th(obs) 2Th_obs-shift 2Th(Calc) diff. 1 1 0 8.0100 8.0100 8.0175 -0.0075 0 2 0 9.6200 9.6200 9.6229 -0.0029 0 0 1 12.0700 12.0700 12.0572 0.0128 2 0 0 12.8400 12.8400 12.8455 -0.0055 -1 1 1 13.5800 13.5800 13.5902 -0.0102 0 2 1 15.4200 15.4200 15.4488 -0.0288 1 3 0 15.8300 15.8300 15.8281 0.0019 2 2 0 16.1000 16.1000 16.0745 0.0255 -2 2 1 18.8200 18.8200 18.8241 -0.0041 2 0 1 19.0400 19.0400 19.0487 -0.0087 -1 3 1 19.3000 19.3000 19.2898 0.0102 3 1 0 19.9200 19.9200 19.9195 0.0005 1 3 1 20.5700 20.5700 20.5790 -0.0090 -3 1 1 21.6200 21.6200 21.6245 -0.0045 0 4 1 22.8300 22.8300 22.8304 -0.0004 2 4 0 23.2600 23.2600 23.2646 -0.0046 3 3 0 24.2200 24.2200 24.2125 0.0075 -1 1 2 24.5400 24.5400 24.5421 -0.0021 3 1 1 24.9500 24.9500 24.9598 -0.0098 -2 4 1 25.2800 25.2800 25.2706 0.0094 -3 3 1 25.6400 25.6400 25.6470 -0.0070 4 0 0 25.8600 25.8600 25.8560 0.0040 0 2 2 26.1400 26.1400 26.1442 -0.0042 1 1 2 26.6000 26.6000 26.5797 0.0203 -2 2 2 27.3800 27.3800 27.3764 0.0036 Sqrt(Sum(2Th O-C)**2)/(Nref-Npar)) : 0.0118 Sqrt(Sum(2Th O-C)**2)/Nref ) : 0.0108 Interestingly, putting this cell through a search of the ICSD spat out: 40594 Col= 75475 Silicon oxide Minr=Ferrierite (siliceous) - synthetic, hydrothermal at 443 K fo r for 7 d Minr=Zeolite group Si O2 11611849 1994 JACSA(678) Journal of the American Chemical Society Morris R E, Weigel S J, Henson N J, Bull L M, Janicke M T Chmelka B F, Cheetham A K Space Group : Pmnn (or Pmnm) (58) Remark : TEM 298 Remark : SNP Remark : NDP Remark : RVP Remark : 1 M PDF 39-1382 Test Flags : 23 76 51675 Col= 40532 Sodium potassium magnesium tecto-alumosilicate hydrate Minr=Ferrierite M - from Altoona, Washington, USA Minr=Zeolite group Na3 K Mg.5 Al5 Si31 O72 (H2 O)18 169 201 1984 ZEKRD(1429) Zeitschrift fuer Kristallographie (149,1979-) 21 983 1966 ACCRA(21) Acta Crystallographica (1,1948-23,1967) Gramlich-Meier R, Gramlich V, Meier W M Space Group : P121/n1 (14) Remark : K R(a-reflections only)=0.061, R(b-reflections)=0. 156 Remark : M PDF 39-1382 (in Immm), mean T-O: 1.60-1.62 Test Flags : 52 but these had ortho unit cells (roughly same dimensions but not obviously crystallographically related). The ortho cell didn't index the pattern satisfactorily. Interesting! Regards Jan. _________________________________________ Dr. Jan Skakle Senior Lecturer College of Physical Sciences Meston Walk, Aberdeen AB24 3UE Scotland UK Tel: 01224-273798 Fax: 01224-272921