++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 07skc0008 started at 11:39:25 on 13-FEB-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 24.589 4.585 18.728 90.00 123.02 90.00 10152 Reflections read from file 07skc0008.hkl; mean (I/sigma) = 3.38 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 5074 5074 0 5089 5074 6794 6748 10152 N (int>3sigma) = 0 1670 1670 0 1745 1670 2525 2550 3783 Mean intensity = 0.0 221.3 221.3 0.0 238.2 221.3 280.9 276.5 268.1 Mean int/sigma = 0.0 3.1 3.1 0.0 3.3 3.1 3.6 3.6 3.5 Lattice type: C chosen Volume: 1770.46 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 -1.0000 0.0000 0.5000 -0.5000 0.0000 0.5000 -0.5000 1.0000 Unitcell: 4.585 12.506 16.006 81.11 81.76 79.44 Niggli form: a.a = 21.03 b.b = 156.41 c.c = 256.18 b.c = 30.93 a.c = 10.51 a.b = 10.51 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC C-lattice R(int) = 0.121 [ 7894] Cell: 24.589 4.585 18.728 90.00 123.02 90.00 Volume: 1770.46 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.000 deg. MONOCLINIC I-lattice R(int) = 0.121 [ 7894] Cell: 18.728 4.585 21.294 90.00 104.49 90.00 Volume: 1770.46 Matrix: 0.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option C: FOM = 0.000 deg. TRICLINIC P-lattice R(int) = 0.108 [ 6335] Cell: 4.585 12.506 16.006 81.11 81.76 79.44 Volume: 885.23 Matrix: 0.0000 -1.0000 0.0000 0.5000 -0.5000 0.0000 0.5000 -0.5000 1.0000 Option A selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 5074 5074 0 5089 5074 6794 6748 10152 N (int>3sigma) = 0 1670 1670 0 1745 1670 2525 2550 3783 Mean intensity = 0.0 221.3 221.3 0.0 238.2 221.3 280.9 276.5 268.1 Mean int/sigma = 0.0 3.1 3.1 0.0 3.3 3.1 3.6 3.6 3.5 Crystal system M and Lattice type C selected Mean |E*E-1| = 0.889 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -c- N 843 N I>3s 1 20.8 0.7 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] C2/c # 15 centro 1 3696 0.121 7894 0.7 / 3.5 4.15 [B] Cc # 9 non-cen 1 566 0.121 7894 0.7 / 3.5 6.02 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C13H28O4N2 Formula weight = 276.37 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.037, non-H atomic volume = 23.3 and following cell contents and analysis: C 52.00 56.49 % H 112.00 10.21 % N 8.00 10.14 % O 16.00 23.16 % F(000) = 608.0 Mo-K(alpha) radiation Mu (mm-1) = 0.08 ------------------------------------------------------------------------------- File 07skc0008c2c.ins set up as follows: TITL 07skc0008c2c in C2/c CELL 0.71073 24.5889 4.5855 18.7275 90.000 123.022 90.000 ZERR 4.00 0.0015 0.0003 0.0014 0.000 0.004 0.000 LATT 7 SYMM -X, Y, 0.5-Z SFAC C H N O UNIT 52 112 8 16 TEMP 0.01 TREF HKLF 4 END 10152 Reflections written to new reflection file 07skc0008c2c.hkl -------------------------------------------------------------------------------