++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 07skc0011 started at 20:03:39 on 15-FEB-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 7.781 22.358 9.196 90.00 103.33 90.00 14939 Reflections read from file 07skc0011.hkl; mean (I/sigma) = 4.33 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 7478 7493 7493 7462 11232 9993 9971 14939 N (int>3sigma) = 0 3457 3463 3496 3575 5208 4700 4576 7000 Mean intensity = 0.0 30.4 26.9 33.3 26.5 30.2 32.1 30.0 31.6 Mean int/sigma = 0.0 4.4 4.4 4.5 4.4 4.4 4.5 4.4 4.5 Lattice type: P chosen Volume: 1556.76 ------------------------------------------------------------------------------- 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: 7.781 9.196 22.358 90.00 90.00 103.33 Niggli form: a.a = 60.55 b.b = 84.56 c.c = 499.90 b.c = 0.00 a.c = 0.00 a.b = -16.50 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.089 [ 11286] Cell: 7.781 22.358 9.196 90.00 103.33 90.00 Volume: 1556.76 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 7478 7493 7493 7462 11232 9993 9971 14939 N (int>3sigma) = 0 3457 3463 3496 3575 5208 4700 4576 7000 Mean intensity = 0.0 30.4 26.9 33.3 26.5 30.2 32.1 30.0 31.6 Mean int/sigma = 0.0 4.4 4.4 4.5 4.4 4.4 4.5 4.4 4.5 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.974 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 34 203 193 190 N I>3s 0 59 3 56 0.9 9.2 1.7 10.0 0.6 2.7 0.7 2.8 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/c # 14 centro 1 19410 0.089 11286 0.7 / 2.7 5.06 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C9H14O5N2 Formula weight = 230.22 Tentative Z (number of formula units/cell) = 4.0 giving rho = 0.982, non-H atomic volume = 24.3 and following cell contents and analysis: C 36.00 46.95 % H 56.00 6.13 % N 8.00 12.17 % O 20.00 34.75 % F(000) = 488.0 Mo-K(alpha) radiation Mu (mm-1) = 0.08 ------------------------------------------------------------------------------- File 07skc0011p21c.ins set up as follows: TITL 07skc0011p21c in P2(1)/c CELL 0.71073 7.7814 22.3584 9.1957 90.000 103.329 90.000 ZERR 4.00 0.0003 0.0011 0.0005 0.000 0.003 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O UNIT 36 56 8 20 TEMP 0.04 TREF HKLF 4 END 14939 Reflections written to new reflection file 07skc0011p21c.hkl -------------------------------------------------------------------------------