++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 2007src1287 started at 11:06:26 on 28-SEP-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 14.702 14.729 26.771 90.00 90.00 90.00 27831 Reflections read from file 2007src1287.hkl; mean (I/sigma) = 6.64 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 13904 13820 13938 13928 20831 18533 18576 27831 N (int>3sigma) = 0 8646 8443 8483 8711 12786 11599 11688 17443 Mean intensity = 0.0 12.0 10.5 10.7 12.3 11.1 11.4 11.4 11.3 Mean int/sigma = 0.0 6.7 6.5 6.5 6.7 6.6 6.7 6.8 6.7 Lattice type: P chosen Volume: 5797.48 ------------------------------------------------------------------------------- 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: 14.702 14.729 26.771 90.00 90.00 90.00 Niggli form: a.a = 216.16 b.b = 216.96 c.c = 716.69 b.c = 0.00 a.c = 0.00 a.b = 0.00 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.053 deg. TETRAGONAL P-lattice R(int) = 0.536 [ 21105] Cell: 14.702 14.729 26.771 90.00 90.00 90.00 Volume: 5797.48 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.000 deg. ORTHORHOMBIC P-lattice R(int) = 0.051 [ 20639] Cell: 14.702 14.729 26.771 90.00 90.00 90.00 Volume: 5797.48 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 Option B selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 13904 13820 13938 13928 20831 18533 18576 27831 N (int>3sigma) = 0 8646 8443 8483 8711 12786 11599 11688 17443 Mean intensity = 0.0 12.0 10.5 10.7 12.3 11.1 11.4 11.4 11.3 Mean int/sigma = 0.0 6.7 6.5 6.5 6.7 6.6 6.7 6.8 6.7 Crystal system O and Lattice type P selected Mean |E*E-1| = 0.948 [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 705 658 675 14 731 693 718 9 325 301 326 27 N I>3s 292 8 294 1 276 4 280 1 123 3 122 3 18.8 0.2 19.6 0.2 18.2 0.2 18.5 0.4 23.8 0.2 23.8 0.5 5.5 0.7 5.8 1.1 4.9 0.7 5.0 1.1 4.7 0.8 4.7 1.2 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] Pbca # 61 centro 2 2293 0.051 20639 1.2 / 4.7 2.58 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C18H14N4O1 Formula weight = 302.33 Tentative Z (number of formula units/cell) = 16.0 giving rho = 1.386, non-H atomic volume = 15.8 and following cell contents and analysis: C 288.00 71.50 % H 224.00 4.67 % N 64.00 18.54 % O 16.00 5.29 % F(000) = 2528.0 Mo-K(alpha) radiation Mu (mm-1) = 0.09 ------------------------------------------------------------------------------- File pbca.ins set up as follows: TITL pbca in Pbca CELL 0.71073 14.7295 14.7023 26.7711 90.000 90.000 90.000 ZERR 16.00 0.0004 0.0004 0.0008 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 288 224 64 16 TEMP 0.05 TREF HKLF 4 END 27831 Reflections written to new reflection file pbca.hkl -------------------------------------------------------------------------------