++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 06skc0040 started at 11:15:42 on 01-SEP-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 5.749 6.541 9.903 80.40 78.70 71.71 6445 Reflections read from file 06skc0040.hkl; mean (I/sigma) = 3.16 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 3245 3253 3222 3224 4860 4306 4323 6445 N (int>3sigma) = 0 1097 1035 1034 1015 1583 1362 1334 2040 Mean intensity = 0.0 72.8 53.8 60.5 79.5 62.3 79.2 55.5 70.8 Mean int/sigma = 0.0 3.6 3.3 3.3 3.4 3.4 3.4 3.3 3.4 Lattice type: P chosen Volume: 344.53 ------------------------------------------------------------------------------- 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: 5.749 6.541 9.903 80.40 78.70 71.71 Niggli form: a.a = 33.05 b.b = 42.79 c.c = 98.08 b.c = 10.81 a.c = 11.15 a.b = 11.80 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. TRICLINIC P-lattice R(int) = 0.143 [ 4991] Cell: 5.749 6.541 9.903 80.40 78.70 71.71 Volume: 344.53 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 3245 3253 3222 3224 4860 4306 4323 6445 N (int>3sigma) = 0 1097 1035 1034 1015 1583 1362 1334 2040 Mean intensity = 0.0 72.8 53.8 60.5 79.5 62.3 79.2 55.5 70.8 Mean int/sigma = 0.0 3.6 3.3 3.3 3.4 3.4 3.4 3.3 3.4 Crystal system A and Lattice type P selected Mean |E*E-1| = 0.879 [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 0.143 4991 0.0 / 3.4 3.77 [B] P1 # 1 chiral 1 700 0.143 4991 0.0 / 3.4 5.17 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C7H13O5N1 Formula weight = 191.18 Tentative Z (number of formula units/cell) = 1.0 giving rho = 0.921, non-H atomic volume = 26.5 and following cell contents and analysis: C 7.00 43.97 % H 13.00 6.85 % N 1.00 7.33 % O 5.00 41.84 % F(000) = 102.0 Mo-K(alpha) radiation Mu (mm-1) = 0.08 ------------------------------------------------------------------------------- File 06skc0040p-1.ins set up as follows: TITL 06skc0040p-1 in P-1 CELL 0.71073 5.7489 6.5414 9.9035 80.396 78.704 71.706 ZERR 1.00 0.0025 0.0028 0.0045 0.021 0.020 0.025 LATT 1 SFAC C H N O UNIT 7 13 1 5 TEMP 0.07 TREF HKLF 4 END 6445 Reflections written to new reflection file 06skc0040p-1.hkl -------------------------------------------------------------------------------