++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 04src0995 started at 13:31:09 on 10-NOV-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 10.871 10.915 13.574 90.02 111.90 90.02 15874 Reflections read from file 04src0995.hkl; mean (I/sigma) = 11.68 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 7962 7956 7946 7959 11932 10612 10581 15874 N (int>3sigma) = 0 6307 6047 6310 5977 9332 8405 8328 12524 Mean intensity = 0.0 344.9 310.3 325.8 279.9 327.0 341.5 330.9 335.6 Mean int/sigma = 0.0 11.9 11.3 11.7 11.0 11.6 11.8 11.7 11.7 Lattice type: P chosen Volume: 1494.51 ------------------------------------------------------------------------------- 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: 10.871 10.915 13.574 90.02 111.90 90.02 Niggli form: a.a = 118.19 b.b = 119.14 c.c = 184.25 b.c = -0.04 a.c = -55.03 a.b = -0.04 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.031 deg. MONOCLINIC P-lattice R(int) = 0.033 [ 12245] Cell: 10.871 10.915 13.574 90.02 111.90 90.02 Volume: 1494.51 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 7962 7956 7946 7959 11932 10612 10581 15874 N (int>3sigma) = 0 6307 6047 6310 5977 9332 8405 8328 12524 Mean intensity = 0.0 344.9 310.3 325.8 279.9 327.0 341.5 330.9 335.6 Mean int/sigma = 0.0 11.9 11.3 11.7 11.0 11.6 11.8 11.7 11.7 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.994 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 15 482 479 481 N I>3s 5 224 221 13 21.0 348.8 350.7 3.1 2.3 7.7 7.7 0.7 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/n # 14 centro 1 19410 0.033 12245 2.3 / 7.7 1.76 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C17H22O2 Formula weight = 258.35 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.148, non-H atomic volume = 19.7 and following cell contents and analysis: C 68.00 79.03 % H 88.00 8.58 % O 8.00 12.39 % F(000) = 560.0 Mo-K(alpha) radiation Mu (mm-1) = 0.07 ------------------------------------------------------------------------------- File 04src0995.ins set up as follows: TITL 04src0995 in P2(1)/n CELL 0.71073 10.8714 10.9150 13.5740 90.000 111.897 90.000 ZERR 4.00 0.0017 0.0008 0.0026 0.000 0.015 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H O UNIT 68 88 8 TEMP 0.18 TREF HKLF 4 END -------------------------------------------------------------------------------