++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 04skc0014 started at 15:49:51 on 08-FEB-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 8.396 13.100 8.819 90.00 97.52 89.93 15796 Reflections read from file 04skc0014.hkl; mean (I/sigma) = 8.39 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 7906 7895 7897 7869 11849 10553 10517 15796 N (int>3sigma) = 0 5433 5537 5210 5432 8090 7376 7354 11064 Mean intensity = 0.0 246.0 248.4 230.6 233.2 241.7 252.6 241.9 242.2 Mean int/sigma = 0.0 8.3 8.5 7.9 8.3 8.2 8.5 8.5 8.4 Lattice type: P chosen Volume: 961.60 ------------------------------------------------------------------------------- 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: 8.396 8.819 13.100 90.00 90.07 97.52 Niggli form: a.a = 70.49 b.b = 77.77 c.c = 171.60 b.c = 0.00 a.c = -0.14 a.b = -9.69 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.074 deg. MONOCLINIC P-lattice R(int) = 0.049 [ 13475] Cell: 8.396 13.100 8.819 90.00 97.52 89.93 Volume: 961.60 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. TRICLINIC P-lattice R(int) = 0.046 [ 11378] Cell: 8.396 8.819 13.100 90.00 90.07 97.52 Volume: 961.60 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 7906 7895 7897 7869 11849 10553 10517 15796 N (int>3sigma) = 0 5433 5537 5210 5432 8090 7376 7354 11064 Mean intensity = 0.0 246.0 248.4 230.6 233.2 241.7 252.6 241.9 242.2 Mean int/sigma = 0.0 8.3 8.5 7.9 8.3 8.2 8.5 8.5 8.4 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.946 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 35 347 356 347 N I>3s 3 2 147 145 5.5 3.5 481.0 493.2 1.1 0.6 6.0 6.1 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/c # 14 centro 4 19410 0.049 13475 1.1 / 6.0 1.97 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C7H16O6N2 Formula weight = 224.22 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.549, non-H atomic volume = 16.0 and following cell contents and analysis: C 28.00 37.49 % H 64.00 7.19 % N 8.00 12.50 % O 24.00 42.82 % F(000) = 480.0 Mo-K(alpha) radiation Mu (mm-1) = 0.14 ------------------------------------------------------------------------------- File 04skc0014p21c.ins set up as follows: TITL 04skc0014p21c in P2(1)/c CELL 0.71073 8.8190 13.0997 8.3959 90.000 97.523 90.000 ZERR 4.00 0.0019 0.0051 0.0019 0.000 0.026 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O UNIT 28 64 8 24 TEMP 0.02 TREF HKLF 4 END 15796 Reflections written to new reflection file 04skc0014p21c.hkl -------------------------------------------------------------------------------