++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 15:24:55 on 30-MAY-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 8.489 11.535 31.927 90.00 90.00 90.00 11451 Reflections read from file s92.hkl; mean (I/sigma) = 6.58 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 5699 5722 5727 5719 8574 7653 7630 11451 N (int>3sigma) = 0 3461 3461 3494 3458 5208 4680 4628 6955 Mean intensity = 0.0 44.1 47.3 43.8 43.3 45.1 44.6 44.3 44.0 Mean int/sigma = 0.0 6.6 6.6 6.6 6.6 6.6 6.7 6.7 6.6 Lattice type: P chosen Volume: 3126.32 ------------------------------------------------------------------------------- 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: 8.489 11.535 31.927 90.00 90.00 90.00 Niggli form: a.a = 72.06 b.b = 133.06 c.c = 1019.37 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) = 0.096 [ 7442] Cell: 8.489 11.535 31.927 90.00 90.00 90.00 Volume: 3126.32 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 5699 5722 5727 5719 8574 7653 7630 11451 N (int>3sigma) = 0 3461 3461 3494 3458 5208 4680 4628 6955 Mean intensity = 0.0 44.1 47.3 43.8 43.3 45.1 44.6 44.3 44.0 Mean int/sigma = 0.0 6.6 6.6 6.6 6.6 6.6 6.7 6.7 6.6 Crystal system O and Lattice type P selected Mean |E*E-1| = 0.731 [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 497 497 500 5 336 322 330 9 117 110 117 22 N I>3s 312 309 313 0 222 207 201 0 81 70 65 0 67.0 75.0 64.2 0.3 61.8 80.8 68.8 0.5 73.7 55.6 38.1 0.8 7.8 7.8 7.9 0.3 8.3 7.9 7.6 0.5 7.8 7.6 5.7 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 0.096 7442 0.5 / 5.7 1.80 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C25 H30 O8 N4 Cl1 Formula weight = 549.98 Tentative Z (number of formula units/cell) = 5.0 giving rho = 1.461, non-H atomic volume = 16.5 and following cell contents and analysis: C 125.00 54.59 % H 150.00 5.50 % N 20.00 10.19 % O 40.00 23.27 % Cl 5.00 6.45 % F(000) = 1445.0 Mo-K(alpha) radiation Mu (mm-1) = 0.21 ------------------------------------------------------------------------------- File s92.ins set up as follows: TITL s92 in P2(1)2(1)2(1) CELL 0.71073 8.4889 11.5350 31.9275 90.000 90.000 90.000 ZERR 5.00 0.0017 0.0023 0.0064 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 N O CL UNIT 125 150 20 40 5 TREF HKLF 4 END -------------------------------------------------------------------------------