++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 2005src0284 started at 13:53:19 on 15-MAR-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 10.135 15.445 15.877 90.01 90.49 90.02 30827 Reflections read from file 2005src0284.hkl; mean (I/sigma) = 5.47 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 15391 15418 15443 15449 23126 20550 20550 30827 N (int>3sigma) = 0 8523 8372 8257 8348 12576 11467 11472 17181 Mean intensity = 0.0 200.6 188.6 165.2 191.4 184.8 200.7 194.2 198.6 Mean int/sigma = 0.0 5.5 5.4 5.2 5.4 5.4 5.5 5.6 5.5 Lattice type: P chosen Volume: 2485.32 ------------------------------------------------------------------------------- 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: 10.135 15.445 15.877 90.01 90.49 90.02 Niggli form: a.a = 102.72 b.b = 238.54 c.c = 252.09 b.c = -0.02 a.c = -1.38 a.b = -0.06 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.492 deg. ORTHORHOMBIC P-lattice R(int) = 0.534 [ 27589] Cell: 10.135 15.445 15.877 90.01 90.49 90.02 Volume: 2485.32 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.023 deg. MONOCLINIC P-lattice R(int) = 0.082 [ 24930] Cell: 10.135 15.445 15.877 90.01 90.49 90.02 Volume: 2485.32 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option C: FOM = 0.491 deg. MONOCLINIC P-lattice R(int) = 0.526 [ 24922] Cell: 10.135 15.877 15.445 89.99 90.02 89.51 Volume: 2485.32 Matrix: 1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option D: FOM = 0.492 deg. MONOCLINIC P-lattice R(int) = 0.527 [ 24858] Cell: 15.445 10.135 15.877 89.51 90.01 89.98 Volume: 2485.32 Matrix: 0.0000 1.0000 0.0000 -1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 Option B selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 15391 15418 15443 15449 23126 20550 20550 30827 N (int>3sigma) = 0 8523 8372 8257 8348 12576 11467 11472 17181 Mean intensity = 0.0 200.6 188.6 165.2 191.4 184.8 200.7 194.2 198.6 Mean int/sigma = 0.0 5.5 5.4 5.2 5.4 5.4 5.5 5.6 5.5 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.906 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 38 623 627 632 N I>3s 24 249 250 1 34.7 266.8 265.4 5.5 4.1 4.7 4.7 0.5 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2/n # 13 centro 1 292 0.082 24930 0.5 / 4.1 3.47 [B] Pn # 7 non-cen 1 226 0.082 24930 0.5 / 4.1 6.09 Option [A] chosen ------------------------------------------------------------------------------- TOLERANCES CHANGED Maximum deviation (deg.) in higher symmetry cell search = 1.000 Threshold (deg.) for terminating search = 0.050 R(int) maximum for terminating cell search = 0.120 R(int) maximum for space group determination = 0.300 Minimum number of data in group for syst. absence test = 500 Maximum mean I/sigma(I) for systematic absences = 99.000 Minimum I/sigma gap between absences and rest = 1.000 ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C138H120O120S72Al8Na18 Formula weight = 6636.32 Tentative Z (number of formula units/cell) = 1.0 giving rho = 4.434, non-H atomic volume = 7.0 and following cell contents and analysis: C 138.00 24.97 % H 120.00 1.82 % O 120.00 28.93 % Na 18.00 6.24 % Al 8.00 3.25 % S 72.00 34.78 % F(000) = 3362.0 Mo-K(alpha) radiation Mu (mm-1) = 1.92 ------------------------------------------------------------------------------- Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 15391 15418 15443 15449 23126 20550 20550 30827 N (int>3sigma) = 0 8523 8372 8257 8348 12576 11467 11472 17181 Mean intensity = 0.0 200.6 188.6 165.2 191.4 184.8 200.7 194.2 198.6 Mean int/sigma = 0.0 5.5 5.4 5.2 5.4 5.4 5.5 5.6 5.5 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.906 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 38 623 627 632 N I>3s 24 249 250 1 34.7 266.8 265.4 5.5 4.1 4.7 4.7 0.5 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2/n # 13 centro 1 292 0.082 24930 0.5 / 4.7 3.09 [B] Pn # 7 non-cen 1 226 0.082 24930 0.5 / 4.7 5.72 [C] P2(1)/n # 14 centro 1 19410 0.082 24930 0.5 / 4.7 2.76 Option [C] chosen ------------------------------------------------------------------------------- File 2005src0284.ins set up as follows: TITL 2005src0284 in P2(1)/n CELL 0.71073 10.1353 15.4448 15.8774 90.000 90.491 90.000 ZERR 1.00 0.0015 0.0013 0.0023 0.000 0.013 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H O NA AL S UNIT 138 120 120 18 8 72 TEMP 0.05 TREF HKLF 4 END -------------------------------------------------------------------------------