++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 09:25:40 on 26-MAR-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 7.556 8.045 22.955 90.00 90.00 90.00 4772 Reflections read from file s92.hkl; mean (I/sigma) = 8.69 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 2395 2396 2409 2394 3600 3171 3169 4772 N (int>3sigma) = 0 1819 1798 1811 1755 2714 2354 2363 3577 Mean intensity = 0.0 267.2 219.7 231.8 253.2 239.5 244.5 246.0 247.5 Mean int/sigma = 0.0 9.0 8.6 8.7 8.6 8.8 8.7 8.7 8.7 Lattice type: P chosen Volume: 1395.24 ------------------------------------------------------------------------------- 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: 7.556 8.045 22.955 90.00 90.00 90.00 Niggli form: a.a = 57.09 b.b = 64.72 c.c = 526.93 b.c = 0.00 a.c = 0.00 a.b = 0.00 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. ORTHORHOMBIC P-lattice R(int) = 0.078 [ 3201] Cell: 7.556 8.045 22.955 90.00 90.00 90.00 Volume: 1395.24 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 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 2395 2396 2409 2394 3600 3171 3169 4772 N (int>3sigma) = 0 1819 1798 1811 1755 2714 2354 2363 3577 Mean intensity = 0.0 267.2 219.7 231.8 253.2 239.5 244.5 246.0 247.5 Mean int/sigma = 0.0 9.0 8.6 8.7 8.6 8.8 8.7 8.7 8.7 Crystal system O and Lattice type P selected Mean |E*E-1| = 0.805 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: b-- c-- n-- 21-- -c- -a- -n- -21- --a --b --n --21 N 163 151 150 5 220 228 218 4 68 70 70 7 N I>3s 108 93 99 0 147 162 137 0 47 50 43 0 221.4 186.6 238.1 1.4 486.1 424.2 346.4 1.6 347.0 364.4 170.8 1.6 9.2 8.0 9.0 0.4 9.1 9.6 8.4 0.4 8.8 10.3 7.6 0.6 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)2(1)2 # 18 chiral 5 359 0.078 3201 0.6 / 7.6 2.06 [B] P2(1)2(1)2(1) # 19 chiral 1 5917 0.078 3201 0.6 / 7.6 1.80 Option [B] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C15 H20 O4 Formula weight = 264.31 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.258, non-H atomic volume = 18.4 and following cell contents and analysis: C 60.00 68.16 % H 80.00 7.63 % O 16.00 24.21 % F(000) = 568.0 Mo-K(alpha) radiation Mu (mm-1) = 0.09 ------------------------------------------------------------------------------- File s92.ins set up as follows: TITL s92 in P2(1)2(1)2(1) CELL 0.71073 7.5556 8.0446 22.9549 90.000 90.000 90.000 ZERR 4.00 0.0015 0.0016 0.0046 0.000 0.000 0.000 LATT -1 SYMM 0.5-X, -Y, 0.5+Z SYMM -X, 0.5+Y, 0.5-Z SYMM 0.5+X, 0.5-Y, -Z SFAC C H O UNIT 60 80 16 TREF HKLF 4 END -------------------------------------------------------------------------------