++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + 2007src0238 started at 18:36:30 on 11-Mar-2007 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 7.232 11.072 18.165 90.00 90.00 90.00 17431 Reflections read from file 2007src0238.hkl; mean (I/sigma) = 13.98 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 8721 8718 8727 8695 13083 11601 11617 17431 N (int>3sigma) = 0 7438 7705 7639 7662 11391 10253 10289 15409 Mean intensity = 0.0 22.4 31.3 30.4 30.9 28.0 30.4 30.3 30.0 Mean int/sigma = 0.0 12.9 14.2 13.9 13.9 13.7 14.1 14.0 14.0 Lattice type: P chosen Volume: 1454.51 ------------------------------------------------------------------------------- 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: 7.232 11.072 18.165 90.00 90.00 90.00 Niggli form: a.a = 52.31 b.b = 122.58 c.c = 329.95 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) = 0.028 [ 4279] Cell: 7.232 11.072 18.165 90.00 90.00 90.00 Volume: 1454.51 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 Current cell not changed ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 8721 8718 8727 8695 13083 11601 11617 17431 N (int>3sigma) = 0 7438 7705 7639 7662 11391 10253 10289 15409 Mean intensity = 0.0 22.4 31.3 30.4 30.9 28.0 30.4 30.3 30.0 Mean int/sigma = 0.0 12.9 14.2 13.9 13.9 13.7 14.1 14.0 14.0 Crystal system O and Lattice type P selected Mean |E*E-1| = 0.743 [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 729 727 728 11 415 399 400 22 342 343 345 27 N I>3s 531 565 466 0 288 308 310 0 294 299 279 1 30.6 34.5 26.8 0.1 33.4 43.8 42.3 0.2 33.8 37.8 36.9 0.2 12.7 13.2 10.2 1.0 13.0 14.2 14.3 0.5 16.3 16.2 15.2 0.6 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 0.028 4279 1.0 / 10.2 1.03 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2007src0238.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) Inf - 2.20 99 108 91.7 8.43 110.3 74.45 0.0331 0.0170 2.20 - 1.70 110 110 100.0 11.29 84.2 87.37 0.0240 0.0106 1.70 - 1.45 111 111 100.0 11.66 44.9 74.27 0.0283 0.0111 1.45 - 1.30 121 121 100.0 11.81 41.2 62.96 0.0321 0.0122 1.30 - 1.20 109 109 100.0 11.64 33.3 57.02 0.0330 0.0142 1.20 - 1.10 153 153 100.0 12.03 28.9 48.56 0.0390 0.0167 1.10 - 1.05 104 104 100.0 12.13 19.6 41.01 0.0451 0.0203 1.05 - 1.00 120 120 100.0 11.10 17.1 36.10 0.0526 0.0227 1.00 - 0.95 139 139 100.0 10.09 15.2 31.83 0.0572 0.0263 0.95 - 0.90 174 175 99.4 8.91 12.3 25.43 0.0673 0.0333 0.90 - 0.85 228 228 100.0 6.89 9.3 19.07 0.0816 0.0427 0.85 - 0.80 266 270 98.5 5.15 8.3 14.88 0.0897 0.0585 0.80 - 0.77 206 217 94.9 4.29 7.6 11.74 0.0971 0.0718 ------------------------------------------------------------------------------ 0.90 - 0.77 700 715 97.9 5.44 8.4 15.32 0.0875 0.0563 Inf - 0.77 1940 1965 98.7 8.87 27.0 38.48 0.0384 0.0204 Merged [A], lowest resolution = 6.72 Angstroms, 747 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2007src0238.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C13H21N1O2Si1 Formula weight = 251.40 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.148, non-H atomic volume = 21.4 and following cell contents and analysis: C 52.00 62.10 % H 84.00 8.42 % N 4.00 5.57 % O 8.00 12.73 % Si 4.00 11.17 % F(000) = 544.0 Mo-K(alpha) radiation Mu (mm-1) = 0.15 ------------------------------------------------------------------------------- File 2007src0238.ins set up as follows: TITL 2007src0238 in P2(1)2(1)2(1) CELL 0.71073 7.2323 11.0717 18.1646 90.000 90.000 90.000 ZERR 4.00 0.0001 0.0003 0.0005 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 SI UNIT 52 84 4 8 4 TEMP 0.34 TREF HKLF 4 END -------------------------------------------------------------------------------