+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 2009/1 for Windows + + Copyright(C) 2009 Bruker-AXS All Rights Reserved + + 2009src0583 started at 13:44:44 on 19-May-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 8.317 12.921 39.923 90.00 90.00 90.00 24263 Reflections read from file 2009src0583.hkl; mean (I/sigma) = 5.88 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 12135 12142 12135 12098 18206 16179 16175 24263 N (int>3sigma) = 0 7359 6971 6812 6948 10571 9775 9744 14650 Mean intensity = 0.0 52.7 48.4 41.7 47.8 47.6 51.7 52.3 52.0 Mean int/sigma = 0.0 6.0 5.8 5.5 5.7 5.7 6.0 5.9 6.0 Lattice type: P chosen Volume: 4290.35 ------------------------------------------------------------------------------- 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: 8.317 12.921 39.923 90.00 90.00 90.00 Niggli form: a.a = 69.17 b.b = 166.96 c.c = 1593.82 b.c = 0.00 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. ORTHORHOMBIC P-lattice R(sym) = 0.051 [ 8333] Cell: 8.317 12.921 39.923 90.00 90.00 90.00 Volume: 4290.35 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 12135 12142 12135 12098 18206 16179 16175 24263 N (int>3sigma) = 0 7359 6971 6812 6948 10571 9775 9744 14650 Mean intensity = 0.0 52.7 48.4 41.7 47.8 47.6 51.7 52.3 52.0 Mean int/sigma = 0.0 6.0 5.8 5.5 5.7 5.7 6.0 5.9 6.0 Crystal system O and Lattice type P selected Mean |E*E-1| = 0.929 [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 1112 1161 1153 8 647 624 629 11 174 183 189 53 N I>3s 3 441 440 0 237 237 6 0 0 73 73 3 0.9 92.2 92.7 0.5 119.3 123.6 1.2 0.6 0.6 49.4 47.8 2.6 0.6 4.4 4.4 0.6 4.4 4.5 0.8 0.7 0.6 4.7 4.5 1.4 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] Pbcn # 60 centro 5 571 0.051 8333 1.4 / 4.4 3.08 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2009src0583.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) Rsigma Inf - 2.21 280 294 95.2 6.91 260.0 25.72 0.0430 0.0282 2.21 - 1.73 282 282 100.0 8.05 92.4 24.50 0.0516 0.0274 1.73 - 1.50 285 285 100.0 7.35 67.6 22.30 0.0591 0.0307 1.50 - 1.35 296 297 99.7 6.32 27.2 15.90 0.0774 0.0416 1.35 - 1.25 280 281 99.6 6.09 33.1 16.45 0.0735 0.0413 1.25 - 1.17 289 290 99.7 5.33 35.9 15.29 0.0786 0.0454 1.17 - 1.11 284 284 100.0 5.29 35.5 14.78 0.0764 0.0473 1.11 - 1.05 338 339 99.7 5.02 28.3 11.90 0.0861 0.0548 1.05 - 1.00 363 369 98.4 4.50 19.6 10.02 0.1058 0.0677 1.00 - 0.96 331 335 98.8 3.70 13.8 7.69 0.1321 0.0997 0.96 - 0.92 377 385 97.9 3.19 11.5 5.81 0.1451 0.1291 0.92 - 0.89 355 362 98.1 2.79 8.8 4.47 0.1861 0.1700 0.89 - 0.86 372 384 96.9 2.62 8.8 4.48 0.1905 0.1845 0.86 - 0.84 298 305 97.7 2.56 6.7 3.53 0.2346 0.2402 0.84 - 0.82 306 315 97.1 2.56 7.3 3.44 0.2060 0.2160 0.82 - 0.80 377 387 97.4 2.35 7.5 3.40 0.2133 0.2448 0.80 - 0.78 363 379 95.8 2.34 7.7 3.46 0.2326 0.2385 0.78 - 0.77 3 4 75.0 1.00 5.2 1.93 1.0197 0.5022 ------------------------------------------------------------------------------ 0.87 - 0.77 1600 1650 97.0 2.46 7.5 3.60 0.2187 0.2289 Inf - 0.77 5479 5577 98.2 4.35 36.1 10.71 0.0637 0.0532 Merged [A], lowest resolution = 6.99 Angstroms, 379 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2009src0583.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C12H13N1O2 Formula weight = 203.24 Tentative Z (number of formula units/cell) = 16.0 giving rho = 1.259, non-H atomic volume = 17.9 and following cell contents and analysis: C 192.00 70.92 % H 208.00 6.45 % N 16.00 6.89 % O 32.00 15.74 % F(000) = 1728.0 Mo-K(alpha) radiation Mu (mm-1) = 0.09 ------------------------------------------------------------------------------- File pbcn.ins set up as follows: TITL pbcn in Pbcn CELL 0.71073 39.9227 8.3170 12.9213 90.000 90.000 90.000 ZERR 16.00 0.0015 0.0003 0.0005 0.000 0.000 0.000 LATT 1 SYMM 0.5-X, 0.5-Y, 0.5+Z SYMM -X, Y, 0.5-Z SYMM 0.5+X, 0.5-Y, -Z SFAC C H N O UNIT 192 208 16 32 TEMP 0.04 TREF HKLF 4 END 24263 Reflections written to new reflection file pbcn.hkl -------------------------------------------------------------------------------