+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 2008/2 for Windows + + Copyright(C) 2008 Bruker-AXS All Rights Reserved + + 2008src0844 started at 12:22:02 on 15-Aug-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 12.791 11.804 26.873 90.00 100.37 90.00 40518 Reflections read from file 2008src0844.hkl; mean (I/sigma) = 8.51 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 20293 20296 20241 20266 30415 26953 27054 40518 N (int>3sigma) = 0 12628 12413 12227 12872 18634 16853 16989 25397 Mean intensity = 0.0 18.8 14.8 18.1 19.9 17.2 19.0 19.6 19.1 Mean int/sigma = 0.0 8.6 8.2 8.2 8.8 8.3 8.5 8.6 8.6 Lattice type: P chosen Volume: 3991.14 ------------------------------------------------------------------------------- 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: 11.804 12.791 26.873 100.37 90.00 90.00 Niggli form: a.a = 139.33 b.b = 163.62 c.c = 722.14 b.c = -61.90 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 = 0.000 deg. MONOCLINIC P-lattice R(sym) = 0.032 [ 7788] Cell: 12.791 11.804 26.873 90.00 100.37 90.00 Volume: 3991.14 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 20293 20296 20241 20266 30415 26953 27054 40518 N (int>3sigma) = 0 12628 12413 12227 12872 18634 16853 16989 25397 Mean intensity = 0.0 18.8 14.8 18.1 19.9 17.2 19.0 19.6 19.1 Mean int/sigma = 0.0 8.6 8.2 8.2 8.8 8.3 8.5 8.6 8.6 Crystal system M and Lattice type P selected Mean |E*E-1| = 1.002 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 28 1111 1116 1127 N I>3s 0 2 401 399 0.1 0.2 12.5 12.4 0.5 0.5 5.8 5.7 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 4 19410 0.032 7788 0.5 / 5.7 2.03 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2008src0844.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) Rsigma Inf - 2.10 488 518 94.2 8.05 64.2 53.73 0.0264 0.0148 2.10 - 1.67 497 497 100.0 6.51 39.3 40.28 0.0292 0.0171 1.67 - 1.45 513 513 100.0 5.97 24.6 31.22 0.0381 0.0224 1.45 - 1.32 492 492 100.0 5.57 17.2 24.24 0.0467 0.0269 1.32 - 1.22 531 531 100.0 4.90 15.1 20.20 0.0473 0.0330 1.22 - 1.15 489 489 100.0 4.50 18.1 18.70 0.0465 0.0344 1.15 - 1.09 497 498 99.8 4.30 17.5 17.61 0.0504 0.0376 1.09 - 1.04 547 547 100.0 4.07 14.4 15.40 0.0570 0.0442 1.04 - 1.00 489 489 100.0 4.00 10.4 12.30 0.0767 0.0550 1.00 - 0.96 613 613 100.0 3.69 7.9 10.18 0.0811 0.0676 0.96 - 0.93 494 494 100.0 3.59 5.4 7.64 0.1077 0.0928 0.93 - 0.90 591 591 100.0 3.48 5.0 7.16 0.1278 0.1064 0.90 - 0.87 657 658 99.8 3.31 4.9 6.29 0.1264 0.1136 0.87 - 0.85 491 492 99.8 3.21 4.1 5.73 0.1434 0.1364 0.85 - 0.83 570 570 100.0 3.04 3.8 5.02 0.1595 0.1579 0.83 - 0.81 595 595 100.0 2.94 3.8 4.70 0.1661 0.1675 0.81 - 0.79 672 675 99.6 2.76 3.3 4.03 0.1882 0.2018 0.79 - 0.77 380 407 93.4 2.44 3.4 3.97 0.1863 0.2098 ------------------------------------------------------------------------------ 0.87 - 0.77 2934 2965 99.0 2.92 3.7 4.77 0.1627 0.1678 Inf - 0.77 9606 9669 99.3 4.19 14.0 15.44 0.0455 0.0432 Merged [A], lowest resolution = 6.84 Angstroms, 1117 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2008src0844.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C24H23N1O5 Formula weight = 405.44 Tentative Z (number of formula units/cell) = 8.0 giving rho = 1.349, non-H atomic volume = 16.6 and following cell contents and analysis: C 192.00 71.10 % H 184.00 5.72 % N 8.00 3.45 % O 40.00 19.73 % F(000) = 1712.0 Mo-K(alpha) radiation Mu (mm-1) = 0.09 ------------------------------------------------------------------------------- File 2008src0844m.ins set up as follows: TITL 2008src0844m in P2(1)/c CELL 0.71073 26.8727 11.8039 12.7914 90.000 100.374 90.000 ZERR 8.00 0.0005 0.0002 0.0003 0.000 0.001 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O UNIT 192 184 8 40 TEMP 0.15 TREF HKLF 4 END -------------------------------------------------------------------------------