++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 06skc0064 started at 09:43:09 on 03-NOV-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 9.265 10.529 10.597 105.47 99.12 93.96 19777 Reflections read from file 06skc0064.hkl; mean (I/sigma) = 4.58 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 9873 9881 9886 9874 14820 13195 13186 19777 N (int>3sigma) = 0 4385 4441 4458 4362 6642 5965 5897 8838 Mean intensity = 0.0 128.5 122.8 117.4 122.7 122.9 123.8 127.8 124.6 Mean int/sigma = 0.0 4.7 4.7 4.7 4.6 4.7 4.7 4.7 4.7 Lattice type: P chosen Volume: 977.01 ------------------------------------------------------------------------------- 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: 9.265 10.529 10.597 105.47 99.12 93.96 Niggli form: a.a = 85.84 b.b = 110.86 c.c = 112.30 b.c = -29.77 a.c = -15.56 a.b = -6.73 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. TRICLINIC P-lattice R(int) = 0.085 [ 15277] Cell: 9.265 10.529 10.597 105.47 99.12 93.96 Volume: 977.01 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 9873 9881 9886 9874 14820 13195 13186 19777 N (int>3sigma) = 0 4385 4441 4458 4362 6642 5965 5897 8838 Mean intensity = 0.0 128.5 122.8 117.4 122.7 122.9 123.8 127.8 124.6 Mean int/sigma = 0.0 4.7 4.7 4.7 4.6 4.7 4.7 4.7 4.7 Crystal system A and Lattice type P selected Mean |E*E-1| = 0.991 [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 0.085 15277 0.0 / 4.7 2.19 [B] P1 # 1 chiral 1 700 0.085 15277 0.0 / 4.7 8.77 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C8H15O4N1 Formula weight = 189.21 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.286, non-H atomic volume = 18.8 and following cell contents and analysis: C 32.00 50.78 % H 60.00 7.99 % N 4.00 7.40 % O 16.00 33.82 % F(000) = 408.0 Mo-K(alpha) radiation Mu (mm-1) = 0.10 ------------------------------------------------------------------------------- File 06skc0064p-1.ins set up as follows: TITL 06skc0064p-1 in P-1 CELL 0.71073 9.2652 10.5292 10.5973 105.472 99.121 93.957 ZERR 4.00 0.0006 0.0010 0.0010 0.004 0.005 0.005 LATT 1 SFAC C H N O UNIT 32 60 4 16 TEMP 0.13 TREF HKLF 4 END 19777 Reflections written to new reflection file 06skc0064p-1.hkl -------------------------------------------------------------------------------