++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + 2008lsh067 started at 11:15:05 on 06-Mar-2009 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 4.567 9.637 15.387 90.00 90.00 90.00 6708 Reflections read from file 2008lsh067.hkl; mean (I/sigma) = 14.68 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 3317 3341 3346 3366 5002 4459 4455 6708 N (int>3sigma) = 0 3191 3242 3239 3265 4836 4341 4335 6521 Mean intensity = 0.0 655.5 639.8 643.9 644.1 646.4 643.9 642.4 643.8 Mean int/sigma = 0.0 14.5 14.6 14.7 14.7 14.6 14.7 14.7 14.7 Lattice type: P chosen Volume: 677.19 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): -1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 -1.0000 Unitcell: 4.567 9.637 15.387 90.00 90.00 90.00 Niggli form: a.a = 20.86 b.b = 92.86 c.c = 236.77 b.c = 0.00 a.c = 0.00 a.b = 0.00 ------------------------------------------------------------------------------- Search for higher metric symmetry Identical indices and Friedel opposites combined before calculating R(sym) ------------------------------------------------------------------------------ Option A: FOM = 0.002 deg. ORTHORHOMBIC P-lattice R(sym) = 0.023 [ 1895] Cell: 4.567 9.637 15.387 90.00 90.00 90.00 Volume: 677.19 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 Option A selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 3317 3341 3346 3366 5002 4459 4455 6708 N (int>3sigma) = 0 3191 3242 3239 3265 4836 4341 4335 6521 Mean intensity = 0.0 655.5 639.8 643.9 644.1 646.4 643.9 642.4 643.8 Mean int/sigma = 0.0 14.5 14.6 14.7 14.7 14.6 14.7 14.7 14.7 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.634 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 12 229 210 217 N I>3s 1 210 166 186 2.2 763.3 284.8 814.3 0.9 13.6 11.0 13.2 Identical indices and Friedel opposites combined before calculating R(sym) Option Space Group No. Type Axes CSD R(sym) N(eq) Syst. Abs. CFOM [A] P2(1) # 4 chiral 1 3543 0.018 1234 0.9 / 11.0 1.99 [B] P2(1)/m # 11 centro 1 402 0.018 1234 0.9 / 11.0 12.32 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2008lsh067.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) Inf - 2.10 86 91 94.5 5.08 1975.5 39.61 0.0224 0.0274 2.10 - 1.65 89 89 100.0 5.92 1290.9 41.54 0.0289 0.0232 1.65 - 1.45 82 83 98.8 5.82 899.2 42.23 0.0285 0.0238 1.45 - 1.30 97 98 99.0 5.94 863.8 43.23 0.0288 0.0222 1.30 - 1.20 84 84 100.0 5.93 656.9 39.41 0.0364 0.0242 1.20 - 1.10 136 136 100.0 5.88 551.6 38.39 0.0395 0.0240 1.10 - 1.05 88 88 100.0 4.95 396.3 33.94 0.0381 0.0275 1.05 - 1.00 106 106 100.0 4.49 338.7 29.85 0.0394 0.0292 1.00 - 0.95 111 111 100.0 4.11 390.4 28.25 0.0417 0.0325 0.95 - 0.90 155 155 100.0 3.72 286.7 23.56 0.0473 0.0377 0.90 - 0.85 198 200 99.0 2.91 226.3 19.61 0.0526 0.0467 0.85 - 0.80 232 239 97.1 2.32 182.2 15.15 0.0600 0.0623 0.80 - 0.77 146 166 88.0 1.66 134.4 11.28 0.0589 0.0815 ------------------------------------------------------------------------------ 0.90 - 0.77 576 605 95.2 2.33 185.2 15.70 0.0560 0.0593 Inf - 0.77 1610 1646 97.8 4.08 520.3 28.12 0.0330 0.0304 Merged [A], lowest resolution = 6.01 Angstroms, 220 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2008lsh067.hkl ------------------------------------------------------------------------------- ------------------------------------------------------------------------------- ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C8 H8 I1 N1 O2 Formula weight = 277.05 Tentative Z (number of formula units/cell) = 3.0 giving rho = 2.038, non-H atomic volume = 18.8 and following cell contents and analysis: C 24.00 34.68 % H 24.00 2.91 % N 3.00 5.06 % O 6.00 11.55 % I 3.00 45.80 % F(000) = 396.0 Mo-K(alpha) radiation Mu (mm-1) = 3.50 ------------------------------------------------------------------------------- File 2008lsh067.ins set up as follows: TITL 2008lsh067 in P2(1) CELL 0.71073 4.5670 9.6365 15.3873 90.000 90.002 90.000 ZERR 3.00 0.0001 0.0003 0.0005 0.000 0.002 0.000 LATT -1 SYMM -X, 0.5+Y, -Z SFAC C H N O I UNIT 24 24 3 6 3 TEMP file. TREF HKLF 4 END -------------------------------------------------------------------------------