++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 17:08:23 on 17-JUN-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 10.938 8.297 17.310 90.00 96.67 90.00 15091 Reflections read from file s92.hkl; mean (I/sigma) = 5.65 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 7565 7500 7551 7523 11308 10069 10079 15091 N (int>3sigma) = 0 4868 4689 4837 4757 7197 6419 6443 9708 Mean intensity = 0.0 71.5 67.7 69.3 67.8 69.5 70.8 68.9 70.3 Mean int/sigma = 0.0 5.8 5.6 5.7 5.6 5.7 5.7 5.7 5.7 Lattice type: P chosen Volume: 1560.33 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 -1.0000 0.0000 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 Unitcell: 8.297 10.938 17.310 96.67 90.00 90.00 Niggli form: a.a = 68.84 b.b = 119.65 c.c = 299.63 b.c = -21.98 a.c = 0.00 a.b = 0.00 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.079 [ 11293] Cell: 10.938 8.297 17.310 90.00 96.67 90.00 Volume: 1560.33 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 7565 7500 7551 7523 11308 10069 10079 15091 N (int>3sigma) = 0 4868 4689 4837 4757 7197 6419 6443 9708 Mean intensity = 0.0 71.5 67.7 69.3 67.8 69.5 70.8 68.9 70.3 Mean int/sigma = 0.0 5.8 5.6 5.7 5.6 5.7 5.7 5.7 5.7 Crystal system M and Lattice type P selected Mean |E*E-1| = 1.056 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 10 464 466 422 N I>3s 0 202 201 7 1.4 73.7 73.5 1.0 1.0 4.2 4.2 0.6 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/n # 14 centro 1 19410 0.079 11293 1.0 / 4.2 3.58 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C18H16O6N2 Formula weight = 356.33 Tentative Z (number of formula units/cell) = 3.0 giving rho = 1.138, non-H atomic volume = 20.0 and following cell contents and analysis: C 54.00 60.67 % H 48.00 4.53 % N 6.00 7.86 % O 18.00 26.94 % F(000) = 558.0 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 10.9384 8.2970 17.3097 90.000 96.667 90.000 ZERR 3.00 0.0003 0.0002 0.0005 0.000 0.002 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N O UNIT 54 48 6 18 TREF HKLF 4 END -------------------------------------------------------------------------------