++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 06skc0070 started at 16:33:17 on 16-NOV-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 7.049 16.431 11.399 90.00 89.86 90.00 13321 Reflections read from file 06skc0070.hkl; mean (I/sigma) = 5.36 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 6684 6629 6601 6689 9957 8860 8890 13321 N (int>3sigma) = 0 4280 4306 4104 4266 6345 5663 5672 8517 Mean intensity = 0.0 78.2 71.5 52.8 68.0 67.6 73.8 75.4 72.1 Mean int/sigma = 0.0 5.4 5.4 5.0 5.4 5.3 5.4 5.4 5.4 Lattice type: P chosen Volume: 1320.39 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): -1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 Unitcell: 7.049 11.399 16.431 90.00 90.00 89.86 Niggli form: a.a = 49.69 b.b = 129.95 c.c = 269.99 b.c = 0.00 a.c = 0.00 a.b = 0.20 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.144 deg. ORTHORHOMBIC P-lattice R(int) = 0.101 [ 11534] Cell: 7.049 11.399 16.431 90.00 90.00 89.86 Volume: 1320.39 Matrix:-1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.088 [ 10188] Cell: 7.049 16.431 11.399 90.00 90.14 90.00 Volume: 1320.39 Matrix:-1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option C: FOM = 0.144 deg. MONOCLINIC P-lattice R(int) = 0.095 [ 10137] Cell: 7.049 11.399 16.431 90.00 90.00 89.86 Volume: 1320.39 Matrix: 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option D: FOM = 0.144 deg. MONOCLINIC P-lattice R(int) = 0.095 [ 10060] Cell: 11.399 7.049 16.431 90.00 90.00 90.14 Volume: 1320.39 Matrix: 0.0000 0.0000 1.0000 -1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 Option A selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 6684 6601 6629 6689 9957 8860 8849 13321 N (int>3sigma) = 0 4280 4104 4306 4266 6345 5663 5625 8517 Mean intensity = 0.0 78.2 52.8 71.5 68.0 67.6 73.8 74.5 72.1 Mean int/sigma = 0.0 5.4 5.0 5.4 5.4 5.3 5.4 5.4 5.4 Crystal system O and Lattice type P selected Mean |E*E-1| = 0.733 [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 709 702 731 9 351 343 344 22 245 244 257 30 N I>3s 489 407 490 2 160 194 194 4 124 101 121 0 104.4 49.8 107.6 9.0 48.2 58.0 69.2 4.3 108.2 28.1 92.2 3.9 6.6 5.3 6.4 1.5 3.9 5.0 4.9 1.7 4.8 3.5 4.3 1.0 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 0.101 11534 1.7 / 3.5 4.49 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C12H15O3N2S1 Formula weight = 267.32 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.345, non-H atomic volume = 18.3 and following cell contents and analysis: C 48.00 53.91 % H 60.00 5.66 % N 8.00 10.48 % O 12.00 17.96 % S 4.00 11.99 % F(000) = 564.0 Mo-K(alpha) radiation Mu (mm-1) = 0.25 ------------------------------------------------------------------------------- File .ins set up as follows: TITL in P2(1)2(1)2(1) CELL 0.71073 7.0493 11.3995 16.4313 90.000 90.000 90.000 ZERR 4.00 0.0004 0.0005 0.0009 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 S UNIT 48 60 8 12 4 TEMP 0.01 TREF HKLF 4 END ------------------------------------------------------------------------------- File 06skc0070p212121.ins set up as follows: TITL 06skc0070p212121 in P2(1)2(1)2(1) CELL 0.71073 7.0493 11.3995 16.4313 90.000 90.000 90.000 ZERR 4.00 0.0004 0.0005 0.0009 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 S UNIT 48 60 8 12 4 TEMP 0.01 TREF HKLF 4 END 13321 Reflections written to new reflection file 06skc0070p212121.hkl -------------------------------------------------------------------------------