++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 07skc0020 started at 18:45:14 on 18-FEB-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 5.754 14.855 10.183 90.00 100.80 90.00 8850 Reflections read from file 07skc0020.hkl; mean (I/sigma) = 4.55 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 4434 4392 4438 4394 6632 5920 5919 8850 N (int>3sigma) = 0 2040 2075 1979 2015 3047 2751 2738 4065 Mean intensity = 0.0 116.6 117.8 115.2 126.0 116.5 118.8 114.6 118.7 Mean int/sigma = 0.0 4.7 4.8 4.6 4.7 4.7 4.7 4.7 4.7 Lattice type: P chosen Volume: 854.92 ------------------------------------------------------------------------------- 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: 5.754 10.183 14.855 90.00 90.00 100.80 Niggli form: a.a = 33.10 b.b = 103.69 c.c = 220.67 b.c = 0.00 a.c = 0.00 a.b = -10.98 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.090 [ 6803] Cell: 5.754 14.855 10.183 90.00 100.80 90.00 Volume: 854.92 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 4434 4392 4438 4394 6632 5920 5919 8850 N (int>3sigma) = 0 2040 2075 1979 2015 3047 2751 2738 4065 Mean intensity = 0.0 116.6 117.8 115.2 126.0 116.5 118.8 114.6 118.7 Mean int/sigma = 0.0 4.7 4.8 4.6 4.7 4.7 4.7 4.7 4.7 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.877 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 21 238 222 214 N I>3s 0 78 1 79 5.0 302.5 5.9 336.0 0.6 4.3 0.8 4.7 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/c # 14 centro 1 19410 0.090 6803 0.8 / 4.3 3.66 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C10H20O4N2 Formula weight = 232.28 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.805, non-H atomic volume = 13.4 and following cell contents and analysis: C 40.00 51.70 % H 80.00 8.68 % N 8.00 12.06 % O 16.00 27.55 % F(000) = 504.0 Mo-K(alpha) radiation Mu (mm-1) = 0.14 ------------------------------------------------------------------------------- File 07skc0020p21c.ins set up as follows: TITL 07skc0020p21c in P2(1)/c CELL 0.71073 5.7536 14.8551 10.1829 90.000 100.799 90.000 ZERR 4.00 0.0006 0.0024 0.0015 0.000 0.009 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O UNIT 40 80 8 16 TEMP 0.01 TREF HKLF 4 END 8850 Reflections written to new reflection file 07skc0020p21c.hkl -------------------------------------------------------------------------------