++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + 2009src0683 started at 19:19:13 on 08-Jul-2009 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 12.462 4.755 24.784 90.00 90.03 90.00 17754 Reflections read from file 2009src0683.hkl; mean (I/sigma) = 7.81 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 8864 8884 8832 8841 13290 11859 11838 17754 N (int>3sigma) = 0 6406 6489 6411 6432 9653 8749 8741 13096 Mean intensity = 0.0 346.2 316.0 314.4 301.6 325.5 321.5 321.3 324.7 Mean int/sigma = 0.0 7.7 7.8 7.6 7.6 7.7 7.8 7.8 7.8 Lattice type: P chosen Volume: 1468.67 ------------------------------------------------------------------------------- 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: 4.755 12.462 24.784 90.03 90.00 90.00 Niggli form: a.a = 22.61 b.b = 155.31 c.c = 614.25 b.c = -0.16 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 = 0.029 deg. ORTHORHOMBIC P-lattice R(sym) = 0.055 [ 4347] Cell: 4.755 12.462 24.784 90.03 90.00 90.00 Volume: 1468.67 Matrix: 0.0000 -1.0000 0.0000 1.0000 0.0000 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 8884 8864 8832 8841 13290 11841 11853 17754 N (int>3sigma) = 0 6489 6406 6411 6432 9653 8708 8747 13096 Mean intensity = 0.0 316.0 346.2 314.4 301.6 325.5 321.1 322.4 324.7 Mean int/sigma = 0.0 7.8 7.7 7.6 7.6 7.7 7.8 7.8 7.8 Crystal system O and Lattice type P selected Mean |E*E-1| = 0.727 [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 1489 1481 1480 10 407 420 413 27 233 235 234 64 N I>3s 1049 1011 1010 0 236 304 228 0 142 149 133 1 434.3 422.0 340.5 5.3 300.5 605.8 419.4 6.3 591.8 280.3 485.8 5.6 8.6 8.0 8.2 0.7 6.9 8.6 6.2 0.8 7.5 7.1 6.6 0.8 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)2(1)2(1) # 19 chiral 1 5917 0.055 4347 0.8 / 6.2 1.83 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2009src0683.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) Inf - 2.20 110 116 94.8 14.16 1232.2 52.73 0.0292 0.0158 2.20 - 1.70 114 114 100.0 16.61 598.6 50.91 0.0440 0.0161 1.70 - 1.45 123 123 100.0 13.14 294.3 34.69 0.0612 0.0222 1.45 - 1.30 119 119 100.0 12.53 204.5 31.83 0.0767 0.0252 1.30 - 1.20 105 105 100.0 11.60 225.3 29.41 0.0761 0.0267 1.20 - 1.10 175 175 100.0 10.95 233.5 26.73 0.0787 0.0289 1.10 - 1.00 221 221 100.0 8.89 151.7 20.17 0.1061 0.0434 1.00 - 0.95 135 135 100.0 7.53 100.9 13.95 0.1487 0.0611 0.95 - 0.90 190 190 100.0 6.61 72.3 9.99 0.2004 0.0894 0.90 - 0.85 238 238 100.0 5.61 65.2 8.11 0.2176 0.1057 0.85 - 0.80 268 268 100.0 5.23 54.6 6.83 0.2595 0.1297 0.80 - 0.77 223 230 97.0 4.36 48.7 5.08 0.3028 0.1718 ------------------------------------------------------------------------------ 0.90 - 0.77 729 736 99.0 5.08 56.3 6.72 0.2517 0.1318 Inf - 0.77 2021 2034 99.4 8.73 213.1 20.07 0.0618 0.0357 Merged [A], lowest resolution = 6.88 Angstroms, 914 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2009src0683.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C14H15N1O7 Formula weight = 309.27 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.399, non-H atomic volume = 16.7 and following cell contents and analysis: C 56.00 54.37 % H 60.00 4.89 % N 4.00 4.53 % O 28.00 36.21 % F(000) = 648.0 Mo-K(alpha) radiation Mu (mm-1) = 0.11 ------------------------------------------------------------------------------- File 2009src0683a.ins set up as follows: TITL 2009src0683a in P2(1)2(1)2(1) CELL 0.71073 4.7550 12.4624 24.7840 90.000 90.000 90.000 ZERR 4.00 0.0001 0.0003 0.0007 0.000 0.000 0.000 LATT -1 SYMM 0.5-X, -Y, 0.5+Z SYMM -X, 0.5+Y, 0.5-Z SYMM 0.5+X, 0.5-Y, -Z SFAC C H N O UNIT 56 60 4 28 TEMP 0.01 TREF HKLF 4 END 17754 Reflections written to new reflection file 2009src0683a.hkl -------------------------------------------------------------------------------