++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 06skc0081 started at 16:34:42 on 05-FEB-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 11.629 5.190 11.942 90.00 108.97 90.00 8013 Reflections read from file 06skc0081.hkl; mean (I/sigma) = 6.83 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 3999 3989 3960 3974 5974 5326 5361 8013 N (int>3sigma) = 0 2653 2332 2599 2270 3792 3415 3490 5217 Mean intensity = 0.0 131.6 79.1 127.2 85.4 112.6 129.1 126.6 123.5 Mean int/sigma = 0.0 7.1 6.0 7.0 5.9 6.7 6.9 7.0 6.9 Lattice type: P chosen Volume: 681.62 ------------------------------------------------------------------------------- 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: 5.190 11.629 11.942 108.97 90.00 90.00 Niggli form: a.a = 26.94 b.b = 135.23 c.c = 142.60 b.c = -45.14 a.c = 0.00 a.b = 0.00 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.049 [ 6278] Cell: 11.629 5.190 11.942 90.00 108.97 90.00 Volume: 681.62 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 3999 3989 3960 3974 5974 5326 5361 8013 N (int>3sigma) = 0 2653 2332 2599 2270 3792 3415 3490 5217 Mean intensity = 0.0 131.6 79.1 127.2 85.4 112.6 129.1 126.6 123.5 Mean int/sigma = 0.0 7.1 6.0 7.0 5.9 6.7 6.9 7.0 6.9 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.980 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 11 614 620 600 N I>3s 0 258 258 4 0.6 230.8 228.6 1.3 0.5 5.5 5.5 0.6 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/n # 14 centro 1 19410 0.049 6278 0.6 / 5.5 2.08 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C9H9O5N1 Formula weight = 211.17 Tentative Z (number of formula units/cell) = 3.0 giving rho = 1.543, non-H atomic volume = 15.1 and following cell contents and analysis: C 27.00 51.19 % H 27.00 4.30 % N 3.00 6.63 % O 15.00 37.88 % F(000) = 330.0 Mo-K(alpha) radiation Mu (mm-1) = 0.13 ------------------------------------------------------------------------------- File 06skc0081p21n.ins set up as follows: TITL 06skc0081p21n in P2(1)/n CELL 0.71073 11.6287 5.1904 11.9417 90.000 108.971 90.000 ZERR 3.00 0.0003 0.0002 0.0003 0.000 0.002 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N O UNIT 27 27 3 15 TEMP 0.08 TREF HKLF 4 END 8013 Reflections written to new reflection file 06skc0081p21n.hkl -------------------------------------------------------------------------------