++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 2008src0076 started at 13:42:29 on 22-FEB-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 9.775 12.860 16.824 90.00 90.00 90.00 18843 Reflections read from file 2008src0076.hkl; mean (I/sigma) = 8.20 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 9418 9426 9412 9409 14128 12552 12591 18843 N (int>3sigma) = 0 6499 6475 6602 6644 9788 8857 8895 13297 Mean intensity = 0.0 27.3 28.0 26.5 30.5 27.3 29.0 28.9 29.0 Mean int/sigma = 0.0 8.1 8.0 8.2 8.2 8.1 8.2 8.2 8.2 Lattice type: P chosen Volume: 2114.88 ------------------------------------------------------------------------------- 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: 9.775 12.860 16.824 90.00 90.00 90.00 Niggli form: a.a = 95.55 b.b = 165.37 c.c = 283.06 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) = 0.055 [ 16076] Cell: 9.775 12.860 16.824 90.00 90.00 90.00 Volume: 2114.88 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 9418 9426 9412 9409 14128 12552 12591 18843 N (int>3sigma) = 0 6499 6475 6602 6644 9788 8857 8895 13297 Mean intensity = 0.0 27.3 28.0 26.5 30.5 27.3 29.0 28.9 29.0 Mean int/sigma = 0.0 8.1 8.0 8.2 8.2 8.1 8.2 8.2 8.2 Crystal system O and Lattice type P selected Mean |E*E-1| = 0.741 [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 652 659 655 8 461 455 460 25 362 357 363 26 N I>3s 415 430 413 0 282 296 276 0 227 200 219 0 30.7 34.1 31.1 0.4 40.7 30.3 32.8 0.5 69.7 48.4 40.4 0.2 8.8 8.9 8.7 0.4 8.1 8.5 7.4 0.5 9.1 7.7 7.7 0.5 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)2(1)2(1) # 19 chiral 1 5917 0.055 16076 0.5 / 7.4 1.40 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C22H25B1N2O1F4 Formula weight = 420.25 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.320, non-H atomic volume = 17.6 and following cell contents and analysis: C 88.00 62.87 % H 100.00 6.00 % B 4.00 2.57 % N 8.00 6.67 % O 4.00 3.81 % F 16.00 18.08 % F(000) = 880.0 Mo-K(alpha) radiation Mu (mm-1) = 0.10 ------------------------------------------------------------------------------- File 2008src0076.ins set up as follows: TITL 2008src0076 in P2(1)2(1)2(1) CELL 0.71073 9.7751 12.8596 16.8243 90.000 90.000 90.000 ZERR 4.00 0.0003 0.0004 0.0004 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 B N O F UNIT 88 100 4 8 4 16 TEMP 0.17 TREF HKLF 4 END -------------------------------------------------------------------------------