++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + 07skc0032 started at 17:42:46 on 22-Jul-2007 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 13.558 9.191 25.277 90.00 105.23 90.00 31753 Reflections read from file 07skc0032.hkl; mean (I/sigma) = 3.82 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 15848 15835 15867 15812 23775 21146 21184 31753 N (int>3sigma) = 0 5917 5085 5892 6016 8447 8045 8029 12017 Mean intensity = 0.0 98.8 51.4 97.0 101.2 82.4 99.3 95.8 96.5 Mean int/sigma = 0.0 4.0 3.3 3.9 4.0 3.7 4.0 4.0 4.0 Lattice type: P chosen Volume: 3039.18 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 -1.0000 0.0000 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 Unitcell: 9.191 13.558 25.277 105.23 90.00 90.00 Niggli form: a.a = 84.48 b.b = 183.81 c.c = 638.92 b.c = -90.04 a.c = 0.00 a.b = 0.00 ------------------------------------------------------------------------------- Search for higher metric symmetry Identical indices and Friedel opposites combined before calculating R(sym) ------------------------------------------------------------------------------ Option A: FOM = 0.324 deg. ORTHORHOMBIC C-lattice R(sym) = 0.633 [ 9229] Cell: 13.558 48.778 9.191 90.00 90.00 89.68 Volume: 6078.36 Matrix: 1.0000 0.0000 0.0000 1.0000 0.0000 2.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.000 deg. MONOCLINIC P-lattice R(sym) = 0.090 [ 5757] Cell: 13.558 9.191 25.277 90.00 105.23 90.00 Volume: 3039.18 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option C: FOM = 0.324 deg. MONOCLINIC C-lattice R(sym) = 0.631 [ 6117] Cell: 13.558 48.778 9.191 90.00 90.00 89.68 Volume: 6078.36 Matrix:-1.0000 0.0000 0.0000 -1.0000 0.0000 -2.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option D: FOM = 0.324 deg. MONOCLINIC C-lattice R(sym) = 0.680 [ 5945] Cell: 48.778 13.558 9.191 90.00 90.00 90.32 Volume: 6078.36 Matrix:-1.0000 0.0000 -2.0000 1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 Option B selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 15848 15835 15867 15812 23775 21146 21184 31753 N (int>3sigma) = 0 5917 5085 5892 6016 8447 8045 8029 12017 Mean intensity = 0.0 98.8 51.4 97.0 101.2 82.4 99.3 95.8 96.5 Mean int/sigma = 0.0 4.0 3.3 3.9 4.0 3.7 4.0 4.0 4.0 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.915 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 11 1145 1115 1146 N I>3s 1 265 6 267 10.0 72.7 8.1 72.8 1.3 2.8 0.7 2.8 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] P2(1)/c # 14 centro 1 19410 0.090 5757 1.3 / 2.8 5.02 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C12H23O4N1 Formula weight = 245.31 Tentative Z (number of formula units/cell) = 8.0 giving rho = 1.072, non-H atomic volume = 22.3 and following cell contents and analysis: C 96.00 58.75 % H 184.00 9.45 % N 8.00 5.71 % O 32.00 26.09 % F(000) = 1072.0 Mo-K(alpha) radiation Mu (mm-1) = 0.08 ------------------------------------------------------------------------------- File 07skc0032p21c.ins set up as follows: TITL 07skc0032p21c in P2(1)/c CELL 0.71073 13.5578 9.1913 25.2768 90.000 105.232 90.000 ZERR 8.00 0.0005 0.0003 0.0009 0.000 0.002 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O UNIT 96 184 8 32 TEMP 0.01 TREF HKLF 4 END 31753 Reflections written to new reflection file 07skc0032p21c.hkl ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 07skc0032.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) Inf - 2.10 391 406 96.3 7.52 422.3 26.71 0.0377 0.0245 2.10 - 1.65 405 405 100.0 8.02 158.1 19.63 0.0679 0.0345 1.65 - 1.40 494 494 100.0 6.62 84.6 12.98 0.1107 0.0594 1.40 - 1.25 495 495 100.0 5.55 69.9 10.65 0.1274 0.0789 1.25 - 1.15 487 487 100.0 5.13 52.5 8.03 0.1732 0.1067 1.15 - 1.05 702 703 99.9 4.64 49.3 7.07 0.1808 0.1177 1.05 - 1.00 459 462 99.4 3.77 32.0 4.55 0.2787 0.2065 1.00 - 0.95 557 557 100.0 3.55 25.2 3.27 0.3496 0.2742 0.95 - 0.90 672 676 99.4 3.28 20.9 2.68 0.4301 0.3716 0.90 - 0.85 848 855 99.2 3.09 14.8 1.82 0.6414 0.5363 0.85 - 0.80 1086 1098 98.9 2.80 15.1 1.68 0.6364 0.5669 0.80 - 0.77 785 874 89.8 2.33 14.5 1.41 0.7458 0.6524 ------------------------------------------------------------------------------ 0.90 - 0.77 2719 2827 96.2 2.74 14.8 1.64 0.6637 0.5816 Inf - 0.77 7381 7512 98.3 4.23 60.8 6.66 0.1094 0.1200 Merged [A], lowest resolution = 6.90 Angstroms, 390 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 07skc0032.hkl -------------------------------------------------------------------------------