++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + 2008lsh170 started at 11:36:05 on 15-Jan-2009 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 7.305 9.455 12.284 90.00 99.93 90.00 10092 Reflections read from file 2008lsh170.hkl; mean (I/sigma) = 6.99 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 5027 5069 5018 5048 7557 6698 6756 10092 N (int>3sigma) = 0 3499 3683 3380 3570 5281 4800 4820 7204 Mean intensity = 0.0 177.1 200.4 171.7 180.5 183.1 184.5 176.7 183.2 Mean int/sigma = 0.0 6.9 7.2 6.7 7.1 6.9 7.1 7.1 7.1 Lattice type: P chosen Volume: 835.64 ------------------------------------------------------------------------------- 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: 7.305 9.455 12.284 90.00 99.93 90.00 Niggli form: a.a = 53.36 b.b = 89.39 c.c = 150.89 b.c = 0.00 a.c = -15.48 a.b = 0.00 ------------------------------------------------------------------------------- Search for higher metric symmetry Identical indices and Friedel opposites combined before calculating R(sym) ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC P-lattice R(sym) = 0.035 [ 1688] Cell: 7.305 9.455 12.284 90.00 99.93 90.00 Volume: 835.64 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 5027 5069 5018 5048 7557 6698 6756 10092 N (int>3sigma) = 0 3499 3683 3380 3570 5281 4800 4820 7204 Mean intensity = 0.0 177.1 200.4 171.7 180.5 183.1 184.5 176.7 183.2 Mean int/sigma = 0.0 6.9 7.2 6.7 7.1 6.9 7.1 7.1 7.1 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.940 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 13 355 363 374 N I>3s 1 0 154 154 4.9 2.0 301.0 292.2 1.5 0.6 4.8 4.6 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)/c # 14 centro 4 19410 0.035 1688 1.5 / 4.6 2.70 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2008lsh170.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) Inf - 2.10 110 116 94.8 6.66 846.8 27.61 0.0622 0.0307 2.10 - 1.65 105 105 100.0 7.67 378.2 28.28 0.0626 0.0270 1.65 - 1.40 136 136 100.0 7.39 181.5 22.35 0.0626 0.0299 1.40 - 1.25 139 139 100.0 7.68 127.6 22.14 0.0737 0.0323 1.25 - 1.15 139 139 100.0 6.88 168.1 21.30 0.0661 0.0334 1.15 - 1.05 187 187 100.0 5.78 128.9 18.03 0.0752 0.0406 1.05 - 1.00 128 128 100.0 5.22 73.4 15.42 0.0798 0.0479 1.00 - 0.95 154 154 100.0 4.81 53.9 11.90 0.1008 0.0566 0.95 - 0.90 187 187 100.0 4.13 62.6 11.56 0.0869 0.0620 0.90 - 0.85 237 237 100.0 3.24 39.4 7.41 0.1154 0.0948 0.85 - 0.80 287 290 99.0 2.99 26.9 5.65 0.1520 0.1273 0.80 - 0.77 228 234 97.4 2.53 25.4 5.02 0.1475 0.1538 ------------------------------------------------------------------------------ 0.90 - 0.77 752 761 98.8 2.93 30.4 6.02 0.1352 0.1207 Inf - 0.77 2037 2052 99.3 4.92 135.0 14.21 0.0695 0.0415 Merged [A], lowest resolution = 6.71 Angstroms, 179 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2008lsh170.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C9 H11 N1 O1 Formula weight = 149.19 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.186, non-H atomic volume = 19.0 and following cell contents and analysis: C 36.00 72.45 % H 44.00 7.43 % N 4.00 9.39 % O 4.00 10.72 % F(000) = 320.0 Mo-K(alpha) radiation Mu (mm-1) = 0.08 ------------------------------------------------------------------------------- File p21c.ins set up as follows: TITL p21c in P2(1)/c CELL 0.71073 12.2837 9.4548 7.3046 90.000 99.932 90.000 ZERR 4.00 0.0004 0.0004 0.0003 0.000 0.002 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O UNIT 36 44 4 4 TEMP 0.04 TREF HKLF 4 END 10092 Reflections written to new reflection file p21c.hkl -------------------------------------------------------------------------------