++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + 2009lsh069 started at 15:55:03 on 23-Jul-2009 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 16.298 16.298 17.083 90.00 90.00 90.00 16398 Reflections read from file 2009lsh069.hkl; mean (I/sigma) = 3.20 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 8205 8184 8211 0 12300 10901 10961 16398 N (int>3sigma) = 0 3292 3312 3480 0 5042 4583 4591 6868 Mean intensity = 0.0 16.6 16.8 19.2 0.0 17.5 20.1 20.0 19.5 Mean int/sigma = 0.0 3.2 3.2 3.4 0.0 3.3 3.3 3.3 3.3 Lattice type: I chosen Volume: 4537.86 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.5000 -0.5000 0.5000 -0.5000 -0.5000 -0.5000 0.5000 0.5000 -0.5000 Unitcell: 14.345 14.345 14.345 106.91 110.77 110.77 Niggli form: a.a = 205.78 b.b = 205.78 c.c = 205.78 b.c = -59.86 a.c = -72.96 a.b = -72.96 ------------------------------------------------------------------------------- Search for higher metric symmetry Identical indices and Friedel opposites combined before calculating R(sym) ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. TETRAGONAL I-lattice R(sym) = 0.114 [ 6478] Cell: 16.298 16.298 17.083 90.00 90.00 90.00 Volume: 4537.86 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 8205 8184 8211 0 12300 10901 10961 16398 N (int>3sigma) = 0 3292 3312 3480 0 5042 4583 4591 6868 Mean intensity = 0.0 16.6 16.8 19.2 0.0 17.5 20.1 20.0 19.5 Mean int/sigma = 0.0 3.2 3.2 3.4 0.0 3.3 3.3 3.3 3.3 Crystal system T and Lattice type I selected Mean |E*E-1| = 0.760 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: 41/43 a-- -c- --d N 9 332 644 386 N I>3s 0 103 4 3 0.7 13.4 1.1 1.2 0.7 2.8 0.6 0.6 Identical indices and Friedel opposites combined before calculating R(sym) Option Space Group No. Type Axes CSD R(sym) N(eq) Syst. Abs. CFOM [A] I4(1)cd #110 non-cen 1 24 0.125 7663 0.7 / 2.8 14.64 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2009lsh069.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) Inf - 2.20 82 86 95.3 11.20 114.8 27.95 0.0378 0.0315 2.20 - 1.70 80 80 100.0 13.65 67.0 25.16 0.0596 0.0423 1.70 - 1.45 90 90 100.0 14.21 18.9 17.40 0.1178 0.0443 1.45 - 1.30 86 86 100.0 13.99 19.2 16.99 0.1433 0.0509 1.30 - 1.20 91 91 100.0 14.43 15.0 13.46 0.1568 0.0573 1.20 - 1.10 119 119 100.0 14.43 16.6 13.59 0.1581 0.0587 1.10 - 1.05 76 76 100.0 14.72 12.0 10.55 0.2287 0.0749 1.05 - 1.00 93 93 100.0 13.84 8.7 8.83 0.3099 0.0931 1.00 - 0.95 112 112 100.0 12.14 7.5 7.61 0.3519 0.1136 0.95 - 0.90 134 134 100.0 10.88 4.2 4.82 0.5550 0.1941 0.90 - 0.85 169 170 99.4 8.23 3.9 3.65 0.6113 0.2663 0.85 - 0.80 220 221 99.5 6.11 2.7 2.05 0.8290 0.4778 0.80 - 0.77 150 153 98.0 5.60 2.4 1.65 0.9433 0.5757 ------------------------------------------------------------------------------ 0.90 - 0.77 539 544 99.1 6.63 3.0 2.44 0.7469 0.4142 Inf - 0.77 1502 1511 99.4 10.85 17.4 9.73 0.1402 0.0723 Merged [A], lowest resolution = 6.86 Angstroms, 742 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2009lsh069.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C12 H17 N1 O1 Formula weight = 191.27 Tentative Z (number of formula units/cell) = 16.0 giving rho = 1.120, non-H atomic volume = 20.3 and following cell contents and analysis: C 192.00 75.35 % H 272.00 8.96 % N 16.00 7.32 % O 16.00 8.37 % F(000) = 1664.0 Mo-K(alpha) radiation Mu (mm-1) = 0.07 ------------------------------------------------------------------------------- File 2009lsh069.ins set up as follows: TITL 2009lsh069 in I4(1)cd CELL 0.71073 16.2982 16.2982 17.0833 90.000 90.000 90.000 ZERR 16.00 0.0006 0.0006 0.0006 0.000 0.000 0.000 LATT -2 SYMM 0.5-X, 0.5-Y, 0.5+Z SYMM -Y, 0.5+X, 0.25+Z SYMM 0.5+Y, -X, 0.75+Z SYMM X, -Y, 0.5+Z SYMM 0.5-X, 0.5+Y, Z SYMM -Y, 0.5-X, 0.75+Z SYMM 0.5+Y, X, 0.25+Z SFAC C H N O UNIT 192 272 16 16 TEMP file. TREF HKLF 4 END -------------------------------------------------------------------------------