++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 06skc0049 started at 10:15:33 on 08-SEP-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 5.380 8.154 12.659 78.35 82.96 84.50 12525 Reflections read from file 06skc0049.hkl; mean (I/sigma) = 2.77 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 6246 6248 6290 6276 9392 8378 8359 12525 N (int>3sigma) = 0 2415 2402 2459 2359 3638 3156 3228 4789 Mean intensity = 0.0 86.0 88.5 94.2 91.6 89.6 92.5 87.7 85.7 Mean int/sigma = 0.0 2.9 2.9 2.9 2.9 2.9 2.8 2.9 2.9 Lattice type: P chosen Volume: 538.37 ------------------------------------------------------------------------------- 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: 5.380 8.154 12.659 78.35 82.96 84.50 Niggli form: a.a = 28.94 b.b = 66.49 c.c = 160.26 b.c = 20.84 a.c = 8.34 a.b = 4.21 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. TRICLINIC P-lattice R(int) = 0.158 [ 10011] Cell: 5.380 8.154 12.659 78.35 82.96 84.50 Volume: 538.37 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 6246 6248 6290 6276 9392 8378 8359 12525 N (int>3sigma) = 0 2415 2402 2459 2359 3638 3156 3228 4789 Mean intensity = 0.0 86.0 88.5 94.2 91.6 89.6 92.5 87.7 85.7 Mean int/sigma = 0.0 2.9 2.9 2.9 2.9 2.9 2.8 2.9 2.9 Crystal system A and Lattice type P selected Mean |E*E-1| = 0.927 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absences not required for triclinic Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P-1 # 2 centro 1 8646 0.158 10011 0.0 / 2.9 3.66 [B] P1 # 1 chiral 1 700 0.158 10011 0.0 / 2.9 7.28 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C9H14O4N2 Formula weight = 214.22 Tentative Z (number of formula units/cell) = 2.0 giving rho = 1.321, non-H atomic volume = 17.9 and following cell contents and analysis: C 18.00 50.46 % H 28.00 6.59 % N 4.00 13.08 % O 8.00 29.88 % F(000) = 228.0 Mo-K(alpha) radiation Mu (mm-1) = 0.10 ------------------------------------------------------------------------------- File 06skc0049p-1.ins set up as follows: TITL 06skc0049p-1 in P-1 CELL 0.71073 5.3800 8.1542 12.6592 78.350 82.962 84.496 ZERR 2.00 0.0003 0.0006 0.0010 0.004 0.004 0.004 LATT 1 SFAC C H N O UNIT 18 28 4 8 TEMP 0.02 TREF HKLF 4 END 12525 Reflections written to new reflection file 06skc0049p-1.hkl -------------------------------------------------------------------------------