++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 06skc0029 started at 11:14:04 on 28-JUL-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 8.147 6.497 9.011 90.00 97.40 90.00 6276 Reflections read from file 06skc0029.hkl; mean (I/sigma) = 7.07 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 3143 3142 3137 3135 4711 4183 4167 6276 N (int>3sigma) = 0 2002 1971 2039 2060 3006 2700 2692 4061 Mean intensity = 0.0 227.3 170.6 180.5 180.4 192.8 205.4 195.2 198.7 Mean int/sigma = 0.0 7.2 6.9 7.1 7.1 7.1 7.2 7.2 7.1 Lattice type: P chosen Volume: 472.95 ------------------------------------------------------------------------------- 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: 6.497 8.147 9.011 97.40 90.00 90.00 Niggli form: a.a = 42.20 b.b = 66.38 c.c = 81.19 b.c = -9.46 a.c = 0.00 a.b = 0.00 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.055 [ 5084] Cell: 8.147 6.497 9.011 90.00 97.40 90.00 Volume: 472.95 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 3143 3142 3137 3135 4711 4183 4167 6276 N (int>3sigma) = 0 2002 1971 2039 2060 3006 2700 2692 4061 Mean intensity = 0.0 227.3 170.6 180.5 180.4 192.8 205.4 195.2 198.7 Mean int/sigma = 0.0 7.2 6.9 7.1 7.1 7.1 7.2 7.2 7.1 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.995 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 16 320 324 322 N I>3s 2 235 242 241 16.4 315.4 361.5 225.9 1.6 9.5 9.3 9.1 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2 # 3 chiral 1 29 0.055 5084 0.0 / 1.6 16.49 [B] P2/m # 10 centro 1 21 0.055 5084 0.0 / 1.6 11.06 [C] Pm # 6 non-cen 1 1 0.055 5084 0.0 / 1.6 63.16 [D] P2(1) # 4 chiral 1 3543 0.055 5084 1.6 / 7.1 8.37 [E] P2(1)/m # 11 centro 1 402 0.055 5084 1.6 / 7.1 1.95 Option [E] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C8H12O4N2 Formula weight = 200.20 Tentative Z (number of formula units/cell) = 2.0 giving rho = 1.406, non-H atomic volume = 16.9 and following cell contents and analysis: C 16.00 47.99 % H 24.00 6.04 % N 4.00 14.00 % O 8.00 31.97 % F(000) = 212.0 Mo-K(alpha) radiation Mu (mm-1) = 0.11 ------------------------------------------------------------------------------- File 06skc0029p21m.ins set up as follows: TITL 06skc0029p21m in P2(1)/m CELL 0.71073 8.1472 6.4965 9.0107 90.000 97.401 90.000 ZERR 2.00 0.0007 0.0005 0.0005 0.000 0.004 0.000 LATT 1 SYMM -X, 0.5+Y, -Z SFAC C H N O UNIT 16 24 4 8 TEMP 0.01 TREF HKLF 4 END 6276 Reflections written to new reflection file 06skc0029p21m.hkl -------------------------------------------------------------------------------