++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 06skc0058 started at 12:02:34 on 04-OCT-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 7.555 8.117 10.918 90.01 90.00 68.43 6196 Reflections read from file 06skc0058.hkl; mean (I/sigma) = 11.21 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 3064 3056 3222 3060 4671 4147 4164 6196 N (int>3sigma) = 0 2193 2252 2347 2234 3396 3099 3116 4631 Mean intensity = 0.0 393.1 420.5 421.3 439.0 411.8 400.7 396.7 409.7 Mean int/sigma = 0.0 10.9 11.0 11.0 11.2 11.0 11.3 11.2 11.3 Lattice type: P chosen Volume: 622.69 ------------------------------------------------------------------------------- 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: 7.555 8.117 10.918 90.01 90.00 111.57 Niggli form: a.a = 57.08 b.b = 65.89 c.c = 119.20 b.c = -0.02 a.c = 0.00 a.b = -22.54 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.015 deg. MONOCLINIC P-lattice R(int) = 0.034 [ 5498] Cell: 7.555 10.918 8.117 89.99 111.57 90.00 Volume: 622.69 Matrix: 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 Option A selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 3064 3222 3056 3060 4671 4132 4147 6196 N (int>3sigma) = 0 2193 2347 2252 2234 3396 3031 3099 4631 Mean intensity = 0.0 393.1 421.3 420.5 439.0 411.8 402.1 400.7 409.7 Mean int/sigma = 0.0 10.9 11.0 11.0 11.2 11.0 11.1 11.3 11.3 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.892 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 34 202 260 214 N I>3s 0 70 0 70 1.7 504.0 2.4 475.8 0.4 5.8 0.5 5.5 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/c # 14 centro 1 19410 0.034 5498 0.5 / 5.5 2.55 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C8H18O4N2 Formula weight = 206.24 Tentative Z (number of formula units/cell) = 2.0 giving rho = 1.100, non-H atomic volume = 22.2 and following cell contents and analysis: C 16.00 46.59 % H 36.00 8.80 % N 4.00 13.59 % O 8.00 31.03 % F(000) = 224.0 Mo-K(alpha) radiation Mu (mm-1) = 0.09 ------------------------------------------------------------------------------- File test.ins set up as follows: TITL 06skc0058p21c in P2(1)/c CELL 0.71073 7.5550 10.9180 8.1170 90.000 111.565 90.000 ZERR 2.00 0.0003 0.0004 0.0002 0.000 0.002 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O UNIT 16 36 4 8 TEMP 0.18 TREF HKLF 4 END 6196 Reflections written to new reflection file test.hkl -------------------------------------------------------------------------------