++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 2007src0860 started at 15:55:11 on 11-JUL-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 13.250 6.908 16.981 90.00 102.29 90.00 21132 Reflections read from file 2007src0860.hkl; mean (I/sigma) = 6.72 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 10537 10569 10562 10582 15834 14084 14115 21132 N (int>3sigma) = 0 6799 6415 6822 6492 10018 9158 9089 13664 Mean intensity = 0.0 22.7 21.7 23.1 21.7 22.5 23.1 23.2 22.8 Mean int/sigma = 0.0 6.8 6.4 6.8 6.5 6.7 6.8 6.8 6.8 Lattice type: P chosen Volume: 1518.81 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 -1.0000 0.0000 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 Unitcell: 6.908 13.250 16.981 102.29 90.00 90.00 Niggli form: a.a = 47.72 b.b = 175.57 c.c = 288.36 b.c = -47.88 a.c = 0.00 a.b = 0.00 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.058 [ 17375] Cell: 13.250 6.908 16.981 90.00 102.29 90.00 Volume: 1518.81 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 10537 10569 10562 10582 15834 14084 14115 21132 N (int>3sigma) = 0 6799 6415 6822 6492 10018 9158 9089 13664 Mean intensity = 0.0 22.7 21.7 23.1 21.7 22.5 23.1 23.2 22.8 Mean int/sigma = 0.0 6.8 6.4 6.8 6.5 6.7 6.8 6.8 6.8 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.939 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 9 1046 1050 1044 N I>3s 0 410 409 1 0.1 31.3 31.2 0.4 0.3 5.3 5.3 0.5 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/n # 14 centro 1 19410 0.058 17375 0.5 / 5.3 2.21 Option [A] chosen ------------------------------------------------------------------------------- ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C14H8Br2O2S2 Formula weight = 432.14 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.890, non-H atomic volume = 19.0 and following cell contents and analysis: C 56.00 38.91 % H 32.00 1.87 % O 8.00 7.40 % S 8.00 14.84 % Br 8.00 36.98 % F(000) = 840.0 Mo-K(alpha) radiation Mu (mm-1) = 5.61 ------------------------------------------------------------------------------- File 2007src0860.ins set up as follows: TITL 2007src0860 in P2(1)/n CELL 0.71073 13.2503 6.9083 16.9813 90.000 102.287 90.000 ZERR 4.00 0.0003 0.0002 0.0005 0.000 0.002 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H O S BR UNIT 56 32 8 8 8 TEMP 0.02 TREF HKLF 4 END -------------------------------------------------------------------------------