+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 2007/1 for Windows + + Copyright(C) 2007 Bruker-AXS All Rights Reserved + + 2007src1354 started at 11:56:16 on 15-Oct-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 9.768 13.065 16.812 90.00 90.00 90.00 20568 Reflections read from file 2007src1354.hkl; mean (I/sigma) = 9.65 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 10283 10279 10288 10289 15425 13752 13737 20568 N (int>3sigma) = 0 8360 8308 8402 8348 12535 11226 11223 16840 Mean intensity = 0.0 26.0 24.8 25.8 26.6 25.5 26.4 26.3 26.4 Mean int/sigma = 0.0 9.6 9.5 9.6 9.6 9.6 9.6 9.6 9.7 Lattice type: P chosen Volume: 2145.65 ------------------------------------------------------------------------------- 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: 9.768 13.065 16.812 90.00 90.00 90.00 Niggli form: a.a = 95.42 b.b = 170.70 c.c = 282.64 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) = 0.034 [ 6175] Cell: 9.768 13.065 16.812 90.00 90.00 90.00 Volume: 2145.65 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 10283 10279 10288 10289 15425 13752 13737 20568 N (int>3sigma) = 0 8360 8308 8402 8348 12535 11226 11223 16840 Mean intensity = 0.0 26.0 24.8 25.8 26.6 25.5 26.4 26.3 26.4 Mean int/sigma = 0.0 9.6 9.5 9.6 9.6 9.6 9.6 9.6 9.7 Crystal system O and Lattice type P selected Mean |E*E-1| = 0.730 [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 703 706 711 9 502 502 504 23 367 365 374 33 N I>3s 539 544 535 0 316 375 321 0 268 244 262 0 28.2 24.4 33.0 0.3 25.3 27.0 22.3 0.2 46.2 31.1 36.0 0.2 9.2 9.4 9.5 0.6 7.7 9.1 7.8 0.8 10.4 9.1 9.7 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] P2(1)2(1)2(1) # 19 chiral 1 5917 0.034 6175 0.8 / 7.7 1.38 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2007src1354.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) Rsigma Inf - 2.21 142 153 92.8 7.10 123.7 45.88 0.0367 0.0248 2.21 - 1.73 141 141 100.0 9.26 60.7 48.53 0.0403 0.0185 1.73 - 1.50 144 144 100.0 9.49 38.0 42.64 0.0460 0.0199 1.50 - 1.35 151 151 100.0 9.54 28.5 39.70 0.0473 0.0214 1.35 - 1.24 152 152 100.0 9.85 30.2 37.39 0.0472 0.0223 1.24 - 1.16 161 161 100.0 9.55 24.3 34.14 0.0535 0.0249 1.16 - 1.09 167 167 100.0 9.79 24.7 31.07 0.0511 0.0257 1.09 - 1.04 158 158 100.0 9.66 20.6 29.96 0.0585 0.0281 1.04 - 1.00 143 143 100.0 9.33 13.5 26.93 0.0723 0.0325 1.00 - 0.96 175 175 100.0 7.80 11.4 21.18 0.0765 0.0396 0.96 - 0.93 153 153 100.0 7.41 8.4 17.42 0.0908 0.0483 0.93 - 0.90 155 155 100.0 6.97 7.3 15.56 0.1067 0.0530 0.90 - 0.87 197 197 100.0 5.57 5.7 11.81 0.1285 0.0751 0.87 - 0.85 143 143 100.0 4.88 5.9 11.00 0.1171 0.0788 0.85 - 0.83 144 144 100.0 4.42 4.8 8.73 0.1286 0.0993 0.83 - 0.81 187 187 100.0 3.86 4.7 7.72 0.1296 0.1136 0.81 - 0.79 176 176 100.0 3.90 4.6 7.57 0.1426 0.1157 0.79 - 0.77 115 116 99.1 3.62 3.7 6.33 0.1688 0.1510 ------------------------------------------------------------------------------ 0.87 - 0.77 834 835 99.9 4.24 4.8 8.55 0.1320 0.1045 Inf - 0.77 2804 2816 99.6 7.30 22.4 24.21 0.0515 0.0307 Merged [A], lowest resolution = 6.53 Angstroms, 766 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2007src1354.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C22H25N2O5Cl Formula weight = 432.90 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.340, non-H atomic volume = 17.9 and following cell contents and analysis: C 88.00 61.04 % H 100.00 5.82 % N 8.00 6.47 % O 20.00 18.48 % Cl 4.00 8.19 % F(000) = 912.0 Mo-K(alpha) radiation Mu (mm-1) = 0.21 ------------------------------------------------------------------------------- File 2007src1354.ins set up as follows: TITL 2007src1354 in P2(1)2(1)2(1) CELL 0.71073 9.7683 13.0654 16.8119 90.000 90.000 90.000 ZERR 4.00 0.0002 0.0002 0.0004 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 CL UNIT 88 100 8 20 4 TEMP 0.2 TREF HKLF 4 END 20568 Reflections written to new reflection file 2007src1354.hkl -------------------------------------------------------------------------------