++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + 2007may0018 started at 16:58:40 on 04-Oct-2007 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 7.163 9.882 10.925 90.00 90.00 90.00 7817 Reflections read from file 2007may0018.hkl; mean (I/sigma) = 8.86 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 3893 3886 3907 3901 5843 5220 5226 7817 N (int>3sigma) = 0 2945 2918 2987 2856 4425 4012 4026 6039 Mean intensity = 0.0 23.6 25.2 22.5 20.9 23.7 25.6 25.6 24.6 Mean int/sigma = 0.0 8.6 8.5 8.7 8.2 8.6 8.9 8.9 8.9 Lattice type: P chosen Volume: 773.31 ------------------------------------------------------------------------------- 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: 7.163 9.882 10.925 90.00 90.00 90.00 Niggli form: a.a = 51.30 b.b = 97.66 c.c = 119.36 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) = 0.035 [ 2311] Cell: 7.163 9.882 10.925 90.00 90.00 90.00 Volume: 773.31 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 3893 3886 3907 3901 5843 5220 5226 7817 N (int>3sigma) = 0 2945 2918 2987 2856 4425 4012 4026 6039 Mean intensity = 0.0 23.6 25.2 22.5 20.9 23.7 25.6 25.6 24.6 Mean int/sigma = 0.0 8.6 8.5 8.7 8.2 8.6 8.9 8.9 8.9 Crystal system O and Lattice type P selected Mean |E*E-1| = 0.796 [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 388 398 396 5 232 234 232 14 194 191 189 21 N I>3s 272 277 257 0 116 116 0 0 90 0 90 0 33.3 49.7 34.4 0.0 26.2 26.0 0.2 0.1 23.6 0.2 24.3 0.2 8.7 9.3 7.5 0.3 7.0 6.9 0.6 0.3 6.4 0.5 6.5 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 3 903 0.035 2311 0.6 / 6.4 2.17 [B] Pnma # 62 centro 2 894 0.035 2311 0.6 / 6.4 4.79 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2007may0018.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) Inf - 2.25 56 60 93.3 6.92 130.7 38.36 0.0356 0.0251 2.25 - 1.70 62 62 100.0 8.94 59.5 46.64 0.0276 0.0178 1.70 - 1.45 60 60 100.0 9.68 35.8 42.93 0.0321 0.0179 1.45 - 1.30 70 70 100.0 9.06 17.7 30.78 0.0464 0.0227 1.30 - 1.20 55 55 100.0 10.25 27.6 35.38 0.0452 0.0231 1.20 - 1.10 84 84 100.0 9.80 23.6 30.38 0.0475 0.0264 1.10 - 1.05 58 58 100.0 9.74 17.1 26.77 0.0638 0.0313 1.05 - 1.00 59 60 98.3 9.33 12.6 23.08 0.0629 0.0317 1.00 - 0.95 84 84 100.0 8.20 11.7 19.10 0.0738 0.0407 0.95 - 0.90 90 90 100.0 7.57 7.4 15.60 0.1011 0.0499 0.90 - 0.85 128 128 100.0 5.48 5.5 10.31 0.1203 0.0725 0.85 - 0.80 151 151 100.0 4.42 4.5 7.93 0.1380 0.1013 0.80 - 0.77 106 106 100.0 3.61 3.6 6.43 0.1981 0.1368 ------------------------------------------------------------------------------ 0.90 - 0.77 385 385 100.0 4.55 4.6 8.31 0.1389 0.0976 Inf - 0.77 1063 1068 99.5 7.32 21.7 22.00 0.0464 0.0305 Merged [A], lowest resolution = 5.99 Angstroms, 317 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2007may0018.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C9H10N2 Formula weight = 146.19 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.256, non-H atomic volume = 17.6 and following cell contents and analysis: C 36.00 73.94 % H 40.00 6.90 % N 8.00 19.17 % F(000) = 312.0 Mo-K(alpha) radiation Mu (mm-1) = 0.08 ------------------------------------------------------------------------------- File ortho.ins set up as follows: TITL ortho in Pna2(1) CELL 0.71073 9.8821 10.9251 7.1627 90.000 90.000 90.000 ZERR 4.00 0.0004 0.0005 0.0003 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 UNIT 36 40 8 TEMP 0.1 TREF HKLF 4 END -------------------------------------------------------------------------------