+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 2008/2 for Windows + + Copyright(C) 2008 Bruker-AXS All Rights Reserved + + 2008lsh068 started at 17:51:38 on 03-Nov-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 4.560 10.026 29.066 90.00 90.00 90.00 8707 Reflections read from file 2008lsh068.hkl; mean (I/sigma) = 7.85 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 4367 4385 4350 4384 6551 5828 5803 8707 N (int>3sigma) = 0 2890 2706 2486 2747 4041 3750 3749 5605 Mean intensity = 0.0 19.7 15.5 13.9 16.0 16.3 17.7 18.0 17.4 Mean int/sigma = 0.0 8.1 7.5 6.9 7.6 7.5 7.9 7.9 7.9 Lattice type: P chosen Volume: 1328.83 ------------------------------------------------------------------------------- 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: 4.560 10.026 29.066 90.00 90.00 90.00 Niggli form: a.a = 20.79 b.b = 100.53 c.c = 844.83 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) = 0.039 [ 3224] Cell: 4.560 10.026 29.066 90.00 90.00 90.00 Volume: 1328.83 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 4367 4385 4350 4384 6551 5828 5803 8707 N (int>3sigma) = 0 2890 2706 2486 2747 4041 3750 3749 5605 Mean intensity = 0.0 19.7 15.5 13.9 16.0 16.3 17.7 18.0 17.4 Mean int/sigma = 0.0 8.1 7.5 6.9 7.6 7.5 7.9 7.9 7.9 Crystal system O and Lattice type P selected Mean |E*E-1| = 0.823 [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 682 686 688 8 275 291 282 16 118 115 111 22 N I>3s 0 278 278 0 118 118 0 0 76 80 54 0 0.1 29.2 29.1 0.1 33.8 32.0 0.2 0.2 22.7 34.0 19.1 0.2 0.5 6.2 6.1 0.4 6.2 5.9 0.5 0.8 9.7 11.2 7.4 0.5 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] Pna2(1) # 33 non-cen 2 903 0.039 3224 0.8 / 5.9 2.71 [B] Pnma # 62 centro 3 894 0.039 3224 0.8 / 5.9 4.07 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2008lsh068.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) Rsigma Inf - 2.23 94 101 93.1 7.27 79.3 33.22 0.0346 0.0242 2.23 - 1.77 93 94 98.9 8.32 42.4 36.65 0.0335 0.0225 1.77 - 1.51 96 98 98.0 6.29 19.6 27.87 0.0353 0.0276 1.51 - 1.37 92 94 97.9 6.06 12.8 24.90 0.0514 0.0296 1.37 - 1.26 98 98 100.0 5.77 14.7 22.62 0.0531 0.0366 1.26 - 1.17 102 104 98.1 4.88 15.6 22.46 0.0529 0.0363 1.17 - 1.11 94 94 100.0 4.27 17.4 18.25 0.0475 0.0407 1.11 - 1.06 98 99 99.0 4.62 10.2 15.99 0.0611 0.0459 1.06 - 1.01 108 109 99.1 4.20 8.7 13.39 0.0720 0.0554 1.01 - 0.97 109 109 100.0 4.20 8.4 12.28 0.0790 0.0550 0.97 - 0.93 108 108 100.0 4.07 6.7 10.61 0.0949 0.0668 0.93 - 0.90 125 125 100.0 3.91 4.9 8.53 0.1002 0.0792 0.90 - 0.87 126 126 100.0 3.98 3.6 7.32 0.1385 0.1040 0.87 - 0.84 145 145 100.0 3.68 3.2 5.70 0.1644 0.1279 0.84 - 0.82 108 108 100.0 3.65 2.8 5.33 0.1635 0.1403 0.82 - 0.80 108 108 100.0 3.60 3.6 6.28 0.1687 0.1279 0.80 - 0.77 118 122 96.7 3.37 1.8 4.00 0.2503 0.2238 ------------------------------------------------------------------------------ 0.87 - 0.77 521 525 99.2 3.61 2.9 5.50 0.1763 0.1412 Inf - 0.77 1822 1842 98.9 4.73 13.8 15.23 0.0480 0.0408 Merged [A], lowest resolution = 6.97 Angstroms, 290 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2008lsh068.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C9H11N1O3 Formula weight = 181.19 Tentative Z (number of formula units/cell) = 6.0 giving rho = 1.359, non-H atomic volume = 17.0 and following cell contents and analysis: C 54.00 59.66 % H 66.00 6.12 % N 6.00 7.73 % O 18.00 26.49 % F(000) = 576.0 Mo-K(alpha) radiation Mu (mm-1) = 0.10 ------------------------------------------------------------------------------- File pna21.ins set up as follows: TITL pna21 in Pna2(1) CELL 0.71073 10.0265 4.5597 29.0659 90.000 90.000 90.000 ZERR 6.00 0.0003 0.0002 0.0011 0.000 0.000 0.000 LATT -1 SYMM -X, -Y, 0.5+Z SYMM 0.5+X, 0.5-Y, Z SYMM 0.5-X, 0.5+Y, 0.5+Z SFAC C H N O UNIT 54 66 6 18 TEMP 0.08 TREF HKLF 4 END -------------------------------------------------------------------------------