++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 16:23:00 on 08-APR-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 10.034 14.336 19.670 86.34 75.24 69.52 9658 Reflections read from file s92.hkl; mean (I/sigma) = 6.56 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 4815 4814 4825 4819 7227 6457 6477 9658 N (int>3sigma) = 0 2934 2967 2943 2858 4422 3942 3993 5960 Mean intensity = 0.0 56.3 57.6 52.5 53.8 55.4 49.8 56.1 56.4 Mean int/sigma = 0.0 6.5 6.6 6.6 6.4 6.6 6.5 6.6 6.7 Lattice type: P chosen Volume: 2562.14 ------------------------------------------------------------------------------- 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: 10.034 14.336 19.670 86.34 75.24 69.52 Niggli form: a.a = 100.68 b.b = 205.52 c.c = 386.93 b.c = 18.01 a.c = 50.30 a.b = 50.33 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.013 deg. MONOCLINIC C-lattice R(int) = 0.075 [ 6337] Cell: 26.860 10.034 22.976 90.01 124.15 90.00 Volume: 5124.27 Matrix: 1.0000 -2.0000 0.0000 1.0000 0.0000 0.0000 -1.0000 1.0000 1.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.013 deg. MONOCLINIC I-lattice R(int) = 0.075 [ 6337] Cell: 22.976 10.034 23.589 90.01 109.56 89.99 Volume: 5124.27 Matrix: 1.0000 -1.0000 -1.0000 1.0000 0.0000 0.0000 0.0000 -1.0000 1.0000 Option A selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 4815 4815 0 4819 4815 6474 6445 9658 N (int>3sigma) = 0 2934 2934 0 2858 2934 3965 4009 5960 Mean intensity = 0.0 56.3 56.3 0.0 53.8 56.3 56.9 56.6 56.4 Mean int/sigma = 0.0 6.5 6.5 0.0 6.4 6.5 6.6 6.7 6.7 Crystal system M and Lattice type C selected Mean |E*E-1| = 0.971 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -c- N 363 N I>3s 6 1.5 0.6 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] C2/c # 15 centro 1 3696 0.075 6337 0.6 / 6.7 1.68 [B] Cc # 9 non-cen 1 566 0.075 6337 0.6 / 6.7 7.35 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C33H24BrNO2P Formula weight = 577.41 Tentative Z (number of formula units/cell) = 8.0 giving rho = 1.497, non-H atomic volume = 16.9 and following cell contents and analysis: C 264.00 68.64 % H 192.00 4.19 % N 8.00 2.43 % O 16.00 5.54 % P 8.00 5.36 % Br 8.00 13.84 % F(000) = 2360.0 Mo-K(alpha) radiation Mu (mm-1) = 1.70 ------------------------------------------------------------------------------- File 1.ins set up as follows: TITL 1 in C2/c CELL 0.71073 26.8598 10.0338 22.9758 90.000 124.152 90.000 ZERR 8.00 0.0029 0.0009 0.0029 0.000 0.011 0.000 LATT 7 SYMM -X, Y, 0.5-Z SFAC C H N O P BR UNIT 264 192 8 16 8 8 TREF HKLF 4 END -------------------------------------------------------------------------------