++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 11:14:08 on 23-JAN-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 13.238 16.923 15.068 90.00 99.94 90.00 22399 Reflections read from file s92.hkl; mean (I/sigma) = 6.42 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 11206 11197 11227 11193 16815 14921 14904 22399 N (int>3sigma) = 0 6437 6331 6576 6362 9672 8545 8575 12919 Mean intensity = 0.0 26.4 25.3 25.7 26.6 25.8 26.5 27.0 26.8 Mean int/sigma = 0.0 6.5 6.3 6.6 6.4 6.5 6.5 6.5 6.5 Lattice type: P chosen Volume: 3324.96 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 Unitcell: 13.238 15.068 16.923 90.00 90.00 99.94 Niggli form: a.a = 175.26 b.b = 227.04 c.c = 286.38 b.c = 0.00 a.c = 0.00 a.b = -34.45 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.075 [ 14690] Cell: 13.238 16.923 15.068 90.00 99.94 90.00 Volume: 3324.96 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 11206 11197 11227 11193 16815 14921 14904 22399 N (int>3sigma) = 0 6437 6331 6576 6362 9672 8545 8575 12919 Mean intensity = 0.0 26.4 25.3 25.7 26.6 25.8 26.5 27.0 26.8 Mean int/sigma = 0.0 6.5 6.3 6.6 6.4 6.5 6.5 6.5 6.5 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.745 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 30 392 398 380 N I>3s 20 169 169 0 56.1 46.2 45.3 0.8 11.3 6.3 6.2 0.5 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2/n # 13 centro 1 292 0.075 14690 0.5 / 6.2 7.06 [B] Pn # 7 non-cen 1 226 0.075 14690 0.5 / 6.2 2.21 Option [B] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C18 H18 N3 O2 Cl2 Formula weight = 379.25 Tentative Z (number of formula units/cell) = 7.0 giving rho = 1.326, non-H atomic volume = 19.0 and following cell contents and analysis: C 126.00 57.00 % H 126.00 4.78 % N 21.00 11.08 % O 14.00 8.44 % Cl 14.00 18.69 % F(000) = 1379.0 Mo-K(alpha) radiation Mu (mm-1) = 0.36 ------------------------------------------------------------------------------- File s92.ins set up as follows: TITL s92 in Pn CELL 0.71073 13.2385 16.9228 15.0678 90.000 99.944 90.000 ZERR 7.00 0.0004 0.0005 0.0004 0.000 0.002 0.000 LATT -1 SYMM 0.5+X, -Y, 0.5+Z SFAC C H N O CL UNIT 126 126 21 14 14 TREF HKLF 4 END -------------------------------------------------------------------------------