++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 07skc0010 started at 08:51:28 on 12-FEB-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 8.856 8.850 9.680 70.38 70.36 77.32 10419 Reflections read from file 07skc0010.hkl; mean (I/sigma) = 7.64 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 5227 5197 5236 5176 7830 6938 6956 10419 N (int>3sigma) = 0 4041 3997 4218 3927 6128 5456 5424 8127 Mean intensity = 0.0 121.6 123.4 129.8 129.9 124.9 143.7 139.4 140.9 Mean int/sigma = 0.0 7.6 7.6 7.9 7.5 7.7 7.8 7.7 7.7 Lattice type: P chosen Volume: 668.16 ------------------------------------------------------------------------------- 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: 8.850 8.856 9.680 70.36 70.38 77.32 Niggli form: a.a = 78.32 b.b = 78.43 c.c = 93.70 b.c = 28.81 a.c = 28.76 a.b = 17.21 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.044 deg. MONOCLINIC C-lattice R(int) = 0.067 [ 8781] Cell: 13.826 11.061 9.680 90.03 115.48 89.96 Volume: 1336.33 Matrix: 1.0000 1.0000 0.0000 1.0000 -1.0000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.044 deg. MONOCLINIC I-lattice R(int) = 0.067 [ 8781] Cell: 9.680 11.061 13.028 89.97 106.65 89.97 Volume: 1336.33 Matrix: 0.0000 0.0000 1.0000 1.0000 -1.0000 0.0000 1.0000 1.0000 -1.0000 Option A selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 5176 5176 0 5220 5176 6939 6934 10419 N (int>3sigma) = 0 3927 3927 0 3953 3927 5410 5400 8127 Mean intensity = 0.0 129.9 129.9 0.0 131.0 129.9 141.4 142.5 140.9 Mean int/sigma = 0.0 7.5 7.5 0.0 7.3 7.5 7.7 7.7 7.7 Crystal system M and Lattice type C selected Mean |E*E-1| = 0.751 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -c- N 255 N I>3s 3 2.2 0.7 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] C2/c # 15 centro 1 3696 0.067 8781 0.7 / 7.7 6.17 [B] Cc # 9 non-cen 1 566 0.067 8781 0.7 / 7.7 1.62 Option [B] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C12H24O4N1 Formula weight = 246.32 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.224, non-H atomic volume = 19.7 and following cell contents and analysis: C 48.00 58.51 % H 96.00 9.82 % N 4.00 5.69 % O 16.00 25.98 % F(000) = 540.0 Mo-K(alpha) radiation Mu (mm-1) = 0.09 ------------------------------------------------------------------------------- File 07skc0010cc.ins set up as follows: TITL 07skc0010cc in Cc CELL 0.71073 13.8261 11.0607 9.6798 90.000 115.478 90.000 ZERR 4.00 0.0010 0.0010 0.0009 0.000 0.007 0.000 LATT -7 SYMM X, -Y, 0.5+Z SFAC C H N O UNIT 48 96 4 16 TEMP 0.02 TREF HKLF 4 END 10419 Reflections written to new reflection file 07skc0010cc.hkl -------------------------------------------------------------------------------