Dear Armel UPPW-10 ITO, FJZN and TREOR within Crysfire all give the same orthorhombic cell for UPPW-10 which indexes all but one of the lines with figures of merit M19 = 20.0 and M18 = 25.2, depending on small details of refinement, etc. KOHL finds approximately the same cell, but with b doubled. I am reasonably confident about this solution, despite the quite large discrepancies. Chekcell proposes the spacegroup to be P212121 (as for fluorocinonidide), which I agree is the most likely one. My solution after Celref refinement on a, b, c and 2Theta zero error: a = 13.8916 (0.0096) b = 15.2531 (0.0095) c = 11.7505 (0.0069) V = 2489.80 2Theta zero error = +0.018 (0.0065), Hence Z2Theta correction (to be added) = -0.018 deg. This cell indexes 35 out of the 36 observed lines within a fairly broad tolerance. The four largest 2Theta (obs-calc) errors are: +0.063 deg (line 1) -0.033 deg (line 21) +0.029 deg (line 18) +0.027 deg (line 20) Obs line 7 (14.602 deg, intensity 19) is unindexed (2Theta obs - nearest 2Theta calc = -7.9 deg) and is proposed to be an impurity. After Celref refinement and excluding line 7, M1(19) = 14.5, M1(29) = 10.6 and M1(35) = 8.8. Despite the respectable provenance of this pattern and the use of an internal mica standard, the data appear to be only moderately accurately measured. A specimen displacement correction might be a little more effective than the constant 2Theta correction used here, but I would expect any improved agreement from this to be relatively minor. Robin Shirley 27Jan04 ----------------------------------------------------------------- Summary files, etc: ** Without self-calibration for 2Theta zero correction ** UPP10-36 = Diflorasone acetate C26H32F2O7, ICDD 44-1791, Bernstein & Levin(1993) I20 Merit Volume V/V1 BL IndexProg Date Time Pedig a b c alpha beta gamma Q(A) Q(B) Q(C) Q(D) Q(E) Q(F) 18 25.1 2465.75 1.00 P ITO12/log 26Jan04 00:07:09 117 13.8460 15.2024 11.7142 90.000 90.000 90.000 52.162 43.269 72.874 .000 .000 .000 18 18.5 2468.38 1.00 P ITO12/log 26Jan04 00:07:09 162 13.8525 15.2075 11.7173 90.000 90.000 90.000 52.113 43.240 72.836 .000 .000 .000 and two further almost identical solutions. ** Including self-calibration for 2Theta zero correction = "+0.02" (opposite to Celref!) ** UPP10SCZ = Diflorasone acetate C26H32F2O7, ICDD 44-1791, Bernstein&Z, SCZ=0.020 I20 Merit Volume V/V1 BL IndexProg Date Time Pedig a b c alpha beta gamma Q(A) Q(B) Q(C) Q(D) Q(E) Q(F) 19 19.95 2471.817 1.00 P FJZNv6.22a 26Jan04 00:13:35 442 13.8551 15.2204 11.7214 90.000 90.000 90.000 52.0931 43.1665 72.7848 .0000 .0000 .0000 19 15 2476.923 1.00 P TREOR90/log 26Jan04 00:14:15 Mon__1 15.2360 13.8655 11.7248 90.000 90.000 90.000 43.0781 52.0152 72.7425 .0000 .0000 .0000 18 25.2 2465.75 1.00 P ITO12/log 26Jan04 00:13:00 117 13.8460 15.2024 11.7142 90.000 90.000 90.000 52.162 43.269 72.874 .000 .000 .000 18 9.68 4912.890 1.99 P KOHLv7.01b 26Jan04 00:15:40 1 30.2795 13.8710 11.6977 90.000 90.537 90.000 10.9079 51.9737 73.0867 .0000 .5297 .0000 17 4.6 3369.22 1.36 P ITO12/log 26Jan04 00:13:00 242 15.3032 24.3296 9.2226 95.295 93.230 98.900 43.975 17.492 119.193 9.351 10.396 8.922 16 8.14 1545.671 .63 P FJZNv6.22a 26Jan04 00:13:35 261 12.7179 14.0114 9.9626 84.928 111.891 110.070 80.9226 57.8551 117.2605 7.4719 71.3211 45.9281 16 6.6 3502.32 1.42 P ITO12/log 26Jan04 00:13:00 241 15.8325 24.6125 9.5294 99.505 104.394 78.874 43.624 17.411 119.184 11.231 32.295 -8.766 14 9.4 2193.85 .89 P ITO12/log 26Jan04 00:13:00 123 12.1258 15.6579 11.6871 92.172 91.677 98.112 69.478 41.692 73.408 4.700 4.998 15.325 ** After Celref refinement of a,b,c and 2Theta zero error ** CELREF Version 3. Final values : (Standard errors on 2nd line) Zero Lambda a b c alpha beta gamma volume 0.0180 1.54180 13.8916 15.2531 11.7505 90.00 90.00 90.00 2489.804 0.0065 0.00000 0.0096 0.0095 0.0069 0.000 0.000 0.000 0.000 H K L 2Th(obs) 2Th_obs-shift 2Th(Calc) diff. 0 1 1 9.5640 9.5643 9.5009 0.0634 1 0 1 9.8390 9.8393 9.8588 -0.0196 1 1 1 11.4140 11.4143 11.4426 -0.0283 0 2 0 11.6110 11.6113 11.6029 0.0084 2 0 0 12.7340 12.7343 12.7446 -0.0103 1 2 0 13.2350 13.2353 13.2433 -0.0080 2 0 1 14.8020 14.8023 14.8153 -0.0130 0 0 2 15.0660 15.0663 15.0792 -0.0129 1 2 1 15.2450 15.2453 15.2477 -0.0024 2 1 1 15.8970 15.8973 15.9198 -0.0226 0 1 2 16.1650 16.1653 16.1661 -0.0009 1 0 2 16.3850 16.3853 16.3809 0.0043 2 2 0 17.2610 17.2613 17.2677 -0.0064 2 2 1 18.8660 18.8663 18.8584 0.0079 1 3 1 20.0680 20.0683 20.0733 -0.0050 2 1 2 20.6390 20.6393 20.6387 0.0006 3 1 1 21.4610 21.4613 21.4322 0.0291 2 3 1 22.9780 22.9783 22.9601 0.0182 0 1 3 23.4750 23.4753 23.4486 0.0266 1 4 0 24.1690 24.1693 24.2026 -0.0333 1 1 3 24.3220 24.3223 24.3202 0.0021 0 4 1 24.5460 24.5463 24.5426 0.0036 3 1 2 25.1620 25.1623 25.1732 -0.0110 3 3 1 27.1320 27.1323 27.1292 0.0031 2 4 1 27.8190 27.8193 27.7465 0.0727 2 2 3 28.6570 28.6573 28.6632 -0.0059 4 2 1 29.2490 29.2493 29.2601 -0.0108 1 3 3 29.4950 29.4953 29.4962 -0.0009 3 3 2 30.2110 30.2113 30.2135 -0.0022 0 0 4 30.4270 30.4273 30.4278 -0.0005 1 5 1 30.9140 30.9143 30.9613 -0.0470 1 1 4 31.6650 31.6653 31.6793 -0.0141 5 1 0 32.7690 32.7693 32.7635 0.0058 1 2 4 33.3110 33.3113 33.3139 -0.0026 1 5 2 33.7390 33.7393 33.7272 0.0120 Sqrt(Sum(2Th O-C)**2)/(Nref-Npar)) : 0.0238 Sqrt(Sum(2Th O-C)**2)/Nref ) : 0.0224