++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 04skc0006 started at 14:07:09 on 31-AUG-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 5.214 11.140 7.489 90.00 95.31 90.02 4139 Reflections read from file 04skc0006.hkl; mean (I/sigma) = 5.83 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 2064 2072 2076 2073 3106 2746 2742 4139 N (int>3sigma) = 0 1325 1371 1286 1375 1991 1791 1827 2692 Mean intensity = 0.0 238.0 309.0 313.9 284.7 287.1 295.2 292.9 294.6 Mean int/sigma = 0.0 5.9 5.9 5.7 5.9 5.8 5.9 5.9 5.9 Lattice type: P chosen Volume: 433.10 ------------------------------------------------------------------------------- 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: 5.214 7.489 11.140 90.00 89.98 84.69 Niggli form: a.a = 27.18 b.b = 56.08 c.c = 124.10 b.c = 0.00 a.c = 0.02 a.b = 3.62 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.020 deg. MONOCLINIC P-lattice R(int) = 0.082 [ 3083] Cell: 5.214 11.140 7.489 90.00 95.31 90.02 Volume: 433.10 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 2064 2072 2076 2073 3106 2746 2742 4139 N (int>3sigma) = 0 1325 1371 1286 1375 1991 1791 1827 2692 Mean intensity = 0.0 238.0 309.0 313.9 284.7 287.1 295.2 292.9 294.6 Mean int/sigma = 0.0 5.9 5.9 5.7 5.9 5.8 5.9 5.9 5.9 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.817 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 15 122 117 119 N I>3s 0 95 86 85 5.1 553.4 416.4 610.8 0.5 8.2 7.1 7.0 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1) # 4 chiral 1 3543 0.082 3083 0.5 / 5.9 2.39 [B] P2(1)/m # 11 centro 1 402 0.082 3083 0.5 / 5.9 4.23 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C5H11O6N1 Formula weight = 181.15 Tentative Z (number of formula units/cell) = 2.0 giving rho = 1.389, non-H atomic volume = 18.0 and following cell contents and analysis: C 10.00 33.15 % H 22.00 6.12 % N 2.00 7.73 % O 12.00 53.00 % F(000) = 192.0 Mo-K(alpha) radiation Mu (mm-1) = 0.13 ------------------------------------------------------------------------------- File 04skc0006p21.ins set up as follows: TITL 04skc0006p21 in P2(1) CELL 0.71073 5.2139 11.1399 7.4889 90.000 95.315 90.000 ZERR 2.00 0.0017 0.0065 0.0029 0.000 0.033 0.000 LATT -1 SYMM -X, 0.5+Y, -Z SFAC C H N O UNIT 10 22 2 12 TEMP 0.1 TREF HKLF 4 END 4139 Reflections written to new reflection file 04skc0006p21.hkl -------------------------------------------------------------------------------