++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 15:23:35 on 15-JUL-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 9.313 9.842 15.444 90.00 90.00 90.00 15417 Reflections read from file s92.hkl; mean (I/sigma) = 9.81 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 7658 7691 7715 7653 11532 10282 10272 15417 N (int>3sigma) = 0 5697 5995 5964 5699 8828 7984 7962 11941 Mean intensity = 0.0 70.8 68.7 71.0 69.4 70.2 74.1 73.7 73.5 Mean int/sigma = 0.0 9.5 9.9 9.9 9.4 9.8 9.9 9.9 9.8 Lattice type: P chosen Volume: 1415.69 ------------------------------------------------------------------------------- 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: 9.313 9.842 15.444 90.00 90.00 90.00 Niggli form: a.a = 86.74 b.b = 96.87 c.c = 238.52 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) = 0.061 [ 13537] Cell: 9.313 9.842 15.444 90.00 90.00 90.00 Volume: 1415.69 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 7658 7691 7715 7653 11532 10282 10272 15417 N (int>3sigma) = 0 5697 5995 5964 5699 8828 7984 7962 11941 Mean intensity = 0.0 70.8 68.7 71.0 69.4 70.2 74.1 73.7 73.5 Mean int/sigma = 0.0 9.5 9.9 9.9 9.4 9.8 9.9 9.9 9.8 Crystal system O and Lattice type P selected Mean |E*E-1| = 0.735 [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 468 479 441 8 502 528 508 11 241 256 261 24 N I>3s 244 243 1 1 345 374 353 0 2 112 114 0 99.1 96.9 0.7 1.5 73.4 93.1 71.6 0.5 0.8 107.9 105.9 0.4 7.8 7.6 0.5 0.9 9.7 10.2 9.5 0.4 0.5 6.9 6.7 0.3 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] Pna2(1) # 33 non-cen 6 903 0.061 13537 0.9 / 6.7 1.71 [B] Pnma # 62 centro 1 894 0.061 13537 0.9 / 6.7 7.13 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C14H22O6 Formula weight = 286.32 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.343, non-H atomic volume = 17.7 and following cell contents and analysis: C 56.00 58.73 % H 88.00 7.75 % O 24.00 33.53 % F(000) = 616.0 Mo-K(alpha) radiation Mu (mm-1) = 0.10 ------------------------------------------------------------------------------- File 1.ins set up as follows: TITL 1 in Pna2(1) CELL 0.71073 9.3133 15.4441 9.8424 90.000 90.000 90.000 ZERR 4.00 0.0003 0.0004 0.0003 0.000 0.000 0.000 LATT -1 SYMM -X, -Y, 0.5+Z SYMM 0.5+X, 0.5-Y, Z SYMM 0.5-X, 0.5+Y, 0.5+Z SFAC C H O UNIT 56 88 24 TREF HKLF 4 END -------------------------------------------------------------------------------