++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 16:57:14 on 21-JAN-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 6.808 9.318 17.548 90.00 90.00 90.00 13519 Reflections read from file s92.hkl; mean (I/sigma) = 13.73 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 6761 6733 6758 6736 10126 8984 9005 13519 N (int>3sigma) = 0 6019 5962 6081 6009 9031 8033 8052 12048 Mean intensity = 0.0 167.5 170.4 169.3 161.5 169.1 171.6 169.6 166.7 Mean int/sigma = 0.0 13.8 13.5 13.8 13.8 13.7 13.8 13.8 13.7 Lattice type: P chosen Volume: 1113.21 ------------------------------------------------------------------------------- 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: 6.808 9.318 17.548 90.00 90.00 90.00 Niggli form: a.a = 46.35 b.b = 86.83 c.c = 307.94 b.c = 0.00 a.c = 0.00 a.b = 0.00 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. ORTHORHOMBIC P-lattice R(int) = 0.046 [ 12019] Cell: 6.808 9.318 17.548 90.00 90.00 90.00 Volume: 1113.21 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 6761 6733 6758 6736 10126 8984 9005 13519 N (int>3sigma) = 0 6019 5962 6081 6009 9031 8033 8052 12048 Mean intensity = 0.0 167.5 170.4 169.3 161.5 169.1 171.6 169.6 166.7 Mean int/sigma = 0.0 13.8 13.5 13.8 13.8 13.7 13.8 13.8 13.7 Crystal system O and Lattice type P selected Mean |E*E-1| = 0.851 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: b-- c-- n-- 21-- -c- -a- -n- -21- --a --b --n --21 N 697 681 686 2 375 392 365 16 213 220 205 19 N I>3s 540 522 514 0 300 324 290 2 170 188 158 0 264.5 254.1 257.5 0.3 193.9 248.7 211.5 1.2 103.5 123.0 125.9 0.7 13.3 12.9 13.1 0.3 13.4 14.1 13.0 1.0 11.4 13.3 11.3 0.4 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)2(1)2 # 18 chiral 3 359 0.046 12019 1.0 / 11.3 2.51 [B] P2(1)2(1)2(1) # 19 chiral 1 5917 0.046 12019 1.0 / 11.3 2.25 Option [B] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C13H13NO3 Formula weight = 231.24 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.380, non-H atomic volume = 16.4 and following cell contents and analysis: C 52.00 67.52 % H 52.00 5.67 % N 4.00 6.06 % O 12.00 20.76 % F(000) = 488.0 Mo-K(alpha) radiation Mu (mm-1) = 0.10 ------------------------------------------------------------------------------- File s92.ins set up as follows: TITL s92 in P2(1)2(1)2(1) CELL 0.71073 6.8078 9.3184 17.5481 90.000 90.000 90.000 ZERR 4.00 0.0001 0.0002 0.0003 0.000 0.000 0.000 LATT -1 SYMM 0.5-X, -Y, 0.5+Z SYMM -X, 0.5+Y, 0.5-Z SYMM 0.5+X, 0.5-Y, -Z SFAC C H N O UNIT 52 52 4 12 TREF HKLF 4 END -------------------------------------------------------------------------------