++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 04skc0003 started at 16:11:24 on 22-JUL-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 13.253 13.220 17.624 90.05 106.46 89.83 12222 Reflections read from file 04skc0003.hkl; mean (I/sigma) = 2.44 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 6095 6095 0 6112 6095 8162 8104 12222 N (int>3sigma) = 0 1743 1743 0 1762 1743 2387 2322 3535 Mean intensity = 0.0 4.7 4.7 0.0 5.8 4.7 5.7 5.9 5.7 Mean int/sigma = 0.0 2.5 2.5 0.0 2.6 2.5 2.6 2.5 2.5 Lattice type: C chosen Volume: 2961.07 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): -0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 0.0000 0.0000 1.0000 Unitcell: 9.345 9.374 17.624 78.41 78.45 89.86 Niggli form: a.a = 87.34 b.b = 87.86 c.c = 310.59 b.c = 33.20 a.c = 32.99 a.b = 0.22 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.173 deg. MONOCLINIC C-lattice R(int) = 0.189 [ 8859] Cell: 13.253 13.220 17.624 90.05 106.46 89.83 Volume: 2961.07 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) = 0.127 [ 6817] Cell: 9.345 9.374 17.624 78.41 78.45 89.86 Volume: 1480.54 Matrix:-0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 0.0000 0.0000 1.0000 Option B selected ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): -0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 0.0000 0.0000 1.0000 Unitcell: 9.345 9.374 17.624 78.41 78.45 89.86 Niggli form: a.a = 87.34 b.b = 87.86 c.c = 310.59 b.c = 33.20 a.c = 32.99 a.b = 0.22 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.173 deg. MONOCLINIC C-lattice R(int) = 0.189 [ 8859] Cell: 13.253 13.220 17.624 90.05 106.46 89.83 Volume: 2961.07 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) = 0.127 [ 6817] Cell: 9.345 9.374 17.624 78.41 78.45 89.86 Volume: 1480.54 Matrix:-0.5000 0.5000 0.0000 -0.5000 -0.5000 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 6095 6095 0 6112 6095 8162 8104 12222 N (int>3sigma) = 0 1743 1743 0 1762 1743 2387 2322 3535 Mean intensity = 0.0 4.7 4.7 0.0 5.8 4.7 5.7 5.9 5.7 Mean int/sigma = 0.0 2.5 2.5 0.0 2.6 2.5 2.6 2.5 2.5 Crystal system M and Lattice type C selected Mean |E*E-1| = 0.834 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -c- N 300 N I>3s 113 9.4 3.3 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] C2 # 5 chiral 1 552 0.189 8859 0.0 / 2.5 5.07 [B] C2/m # 12 centro 1 310 0.189 8859 0.0 / 2.5 6.05 [C] Cm # 8 non-cen 1 32 0.189 8859 0.0 / 2.5 7.92 Option [A] chosen ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): -0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 0.0000 0.0000 1.0000 Unitcell: 9.345 9.374 17.624 78.41 78.45 89.86 Niggli form: a.a = 87.34 b.b = 87.86 c.c = 310.59 b.c = 33.20 a.c = 32.99 a.b = 0.22 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.173 deg. MONOCLINIC C-lattice R(int) = 0.189 [ 8859] Cell: 13.253 13.220 17.624 90.05 106.46 89.83 Volume: 2961.07 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) = 0.127 [ 6817] Cell: 9.345 9.374 17.624 78.41 78.45 89.86 Volume: 1480.54 Matrix:-0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 0.0000 0.0000 1.0000 Option B selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 6148 6149 5957 6095 9127 8135 8131 12222 N (int>3sigma) = 0 1716 1769 1683 1743 2584 2371 2318 3535 Mean intensity = 0.0 5.6 5.2 5.6 4.7 5.5 5.9 5.7 5.7 Mean int/sigma = 0.0 2.5 2.5 2.5 2.5 2.5 2.5 2.5 2.5 Crystal system A and Lattice type P selected Mean |E*E-1| = 0.834 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absences not required for triclinic Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P-1 # 2 centro 1 8646 0.127 6817 0.0 / 2.5 5.75 [B] P1 # 1 chiral 1 700 0.127 6817 0.0 / 2.5 5.02 Option [B] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C24H48O12N1 Formula weight = 542.63 Tentative Z (number of formula units/cell) = 2.0 giving rho = 1.217, non-H atomic volume = 20.0 and following cell contents and analysis: C 48.00 53.12 % H 96.00 8.92 % N 2.00 2.58 % O 24.00 35.38 % F(000) = 590.0 Mo-K(alpha) radiation Mu (mm-1) = 0.10 ------------------------------------------------------------------------------- File 04skc0003p1.ins set up as follows: TITL 04skc0003p1 in P1 CELL 0.71073 9.3454 9.3736 17.6236 78.408 78.446 89.855 ZERR 2.00 0.0019 0.0019 0.0035 0.030 0.030 0.030 LATT -1 SFAC C H N O UNIT 48 96 2 24 TEMP 0.03 TREF HKLF 4 END 12222 Reflections written to new reflection file 04skc0003p1.hkl -------------------------------------------------------------------------------