++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 06skc0077 started at 14:16:17 on 01-DEC-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 5.938 5.000 19.987 90.00 90.02 90.00 6364 Reflections read from file 06skc0077.hkl; mean (I/sigma) = 7.06 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 3191 3220 3193 3197 4802 4242 4262 6364 N (int>3sigma) = 0 2480 2515 2507 2442 3751 3320 3337 4981 Mean intensity = 0.0 325.0 287.5 364.5 343.9 325.6 333.6 339.1 336.4 Mean int/sigma = 0.0 7.0 7.0 7.1 7.0 7.0 7.1 7.1 7.1 Lattice type: P chosen Volume: 593.47 ------------------------------------------------------------------------------- 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: 5.000 5.938 19.987 90.02 90.00 90.00 Niggli form: a.a = 25.00 b.b = 35.26 c.c = 399.46 b.c = -0.04 a.c = 0.00 a.b = 0.00 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.020 deg. ORTHORHOMBIC P-lattice R(int) = 0.077 [ 5513] Cell: 5.000 5.938 19.987 90.02 90.00 90.00 Volume: 593.47 Matrix: 0.0000 -1.0000 0.0000 1.0000 0.0000 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 3220 3191 3193 3197 4802 4253 4221 6364 N (int>3sigma) = 0 2515 2480 2507 2442 3751 3316 3318 4981 Mean intensity = 0.0 287.5 325.0 364.5 343.9 325.6 335.4 337.2 336.4 Mean int/sigma = 0.0 7.0 7.0 7.1 7.0 7.0 7.1 7.1 7.1 Crystal system O and Lattice type P selected Mean |E*E-1| = 0.734 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: b-- c-- n-- 21-- -c- -a- -n- -21- --a --b --n --21 N 404 399 391 9 318 317 313 5 110 107 101 34 N I>3s 337 281 258 0 230 246 214 0 86 77 63 1 629.2 496.9 470.0 3.7 522.1 791.1 605.5 4.5 332.8 204.6 268.9 8.2 8.6 7.0 6.7 0.5 7.1 7.5 6.8 0.7 7.3 6.8 5.6 1.0 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)2(1)2(1) # 19 chiral 1 5917 0.077 5513 1.0 / 5.6 2.07 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C7H12O5N2 Formula weight = 204.19 Tentative Z (number of formula units/cell) = 2.0 giving rho = 1.143, non-H atomic volume = 21.2 and following cell contents and analysis: C 14.00 41.17 % H 24.00 5.92 % N 4.00 13.72 % O 10.00 39.18 % F(000) = 216.0 Mo-K(alpha) radiation Mu (mm-1) = 0.10 ------------------------------------------------------------------------------- File 06skc0077p212121.ins set up as follows: TITL 06skc0077p212121 in P2(1)2(1)2(1) CELL 0.71073 5.0003 5.9383 19.9866 90.000 90.000 90.000 ZERR 2.00 0.0003 0.0002 0.0010 0.000 0.000 0.000 LATT -1 SYMM 0.5-X, -Y, 0.5+Z SYMM -X, 0.5+Y, 0.5-Z SYMM 0.5+X, 0.5-Y, -Z SFAC C H N O UNIT 14 24 4 10 TEMP 0.2 TREF HKLF 4 END 6364 Reflections written to new reflection file 06skc0077p212121.hkl -------------------------------------------------------------------------------