++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + s92 started at 11:02:03 on 16-Sep-2002 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 8.833 15.605 19.097 90.00 102.45 90.00 21289 Reflections read from file s92.hkl; mean (I/sigma) = 5.11 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 10646 10604 10644 10573 15947 14207 14213 21289 N (int>3sigma) = 0 5371 5261 5324 5298 7978 7169 7140 10759 Mean intensity = 0.0 18.2 17.7 17.1 18.6 17.7 18.5 18.8 18.6 Mean int/sigma = 0.0 5.2 5.1 5.2 5.2 5.1 5.2 5.2 5.2 Lattice type: P chosen Volume: 2570.62 ------------------------------------------------------------------------------- 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: 8.833 15.605 19.097 90.00 102.45 90.00 Niggli form: a.a = 78.03 b.b = 243.53 c.c = 364.70 b.c = 0.00 a.c = -36.36 a.b = 0.00 ------------------------------------------------------------------------------- Search for higher metric symmetry Identical indices and Friedel opposites combined before calculating R(sym) ------------------------------------------------------------------------------ Option A: FOM = 0.924 deg. ORTHORHOMBIC C-lattice R(sym) = 0.562 [ 6998] Cell: 8.833 37.301 15.605 90.00 90.00 90.92 Volume: 5141.25 Matrix:-1.0000 0.0000 0.0000 1.0000 0.0000 2.0000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.000 deg. MONOCLINIC P-lattice R(sym) = 0.051 [ 4288] Cell: 8.833 15.605 19.097 90.00 102.45 90.00 Volume: 2570.62 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option C: FOM = 0.924 deg. MONOCLINIC C-lattice R(sym) = 0.639 [ 4044] Cell: 37.301 8.833 15.605 90.00 90.00 89.08 Volume: 5141.25 Matrix: 1.0000 0.0000 2.0000 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option D: FOM = 0.924 deg. MONOCLINIC C-lattice R(sym) = 0.586 [ 4745] Cell: 8.833 37.301 15.605 90.00 90.00 90.92 Volume: 5141.25 Matrix: 1.0000 0.0000 0.0000 -1.0000 0.0000 -2.0000 0.0000 1.0000 0.0000 Option B selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 10646 10604 10644 10573 15947 14207 14213 21289 N (int>3sigma) = 0 5371 5261 5324 5298 7978 7169 7140 10759 Mean intensity = 0.0 18.2 17.7 17.1 18.6 17.7 18.5 18.8 18.6 Mean int/sigma = 0.0 5.2 5.1 5.2 5.2 5.1 5.2 5.2 5.2 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.939 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 22 329 320 275 N I>3s 0 137 138 1 0.7 34.0 34.9 0.6 0.6 4.9 5.0 0.5 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)/n # 14 centro 1 19410 0.051 4288 0.6 / 4.9 2.32 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 s92.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) Inf - 2.15 1131 543 208.3 2.08 119.7 15.98 0.0532 2.15 - 1.75 1074 465 231.0 2.31 49.4 11.83 0.0664 1.75 - 1.50 1399 598 233.9 2.34 24.1 8.63 0.0872 1.50 - 1.35 1472 607 242.5 2.43 16.9 6.67 0.1088 1.35 - 1.25 1323 551 240.1 2.40 13.9 5.80 0.1292 1.25 - 1.15 1954 797 245.2 2.45 15.7 5.71 0.1322 1.15 - 1.10 1221 496 246.2 2.46 18.6 5.66 0.1293 1.10 - 1.05 1509 627 240.7 2.41 12.5 4.74 0.1593 1.05 - 1.00 1646 725 227.0 2.27 9.0 3.69 0.2105 1.00 - 0.95 1734 889 195.1 1.95 7.8 3.32 0.2408 0.95 - 0.90 1879 1098 171.1 1.71 5.1 2.34 0.3585 0.90 - 0.85 1898 1389 136.6 1.37 3.6 1.63 0.5369 0.85 - 0.80 1861 1747 106.5 1.07 3.3 1.39 0.6506 0.80 - 0.77 1188 1271 93.5 0.93 2.7 1.07 0.8562 ------------------------------------------------------------------------------ 0.90 - 0.77 4947 4407 112.3 1.12 3.3 1.41 0.6440 Inf - 0.77 21289 11803 180.4 1.80 18.4 5.11 0.1249 Merged [N], lowest resolution = 6.50 Angstroms, 0 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 s92.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C20H20N3O3 Formula weight = 350.39 Tentative Z (number of formula units/cell) = 6.0 giving rho = 1.358, non-H atomic volume = 16.5 and following cell contents and analysis: C 120.00 68.55 % H 120.00 5.75 % N 18.00 12.00 % O 18.00 13.70 % F(000) = 1110.0 Mo-K(alpha) radiation Mu (mm-1) = 0.09 ------------------------------------------------------------------------------- File s92.ins set up as follows: TITL s92 in P2(1)/n CELL 0.71073 8.8334 15.6053 19.0971 90.000 102.447 90.000 ZERR 6.00 0.0002 0.0004 0.0007 0.000 0.001 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N O UNIT 120 120 18 18 TREF HKLF 4 END -------------------------------------------------------------------------------