++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + 2008src0131 started at 19:08:28 on 26-Feb-2008 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 7.992 9.154 17.789 90.00 98.16 90.00 11993 Reflections read from file 2008src0131.hkl; mean (I/sigma) = 5.21 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 5997 5980 5997 5991 8987 8021 8043 11993 N (int>3sigma) = 0 3410 3338 3428 3320 5088 4605 4645 6858 Mean intensity = 0.0 98.3 91.4 103.6 90.4 97.8 99.5 96.8 95.9 Mean int/sigma = 0.0 5.3 5.2 5.3 5.2 5.3 5.3 5.3 5.3 Lattice type: P chosen Volume: 1288.19 ------------------------------------------------------------------------------- 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: 7.992 9.154 17.789 90.00 98.16 90.00 Niggli form: a.a = 63.87 b.b = 83.79 c.c = 316.44 b.c = 0.00 a.c = -20.18 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. MONOCLINIC P-lattice R(sym) = 0.056 [ 2361] Cell: 7.992 9.154 17.789 90.00 98.16 90.00 Volume: 1288.19 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 5997 5980 5997 5991 8987 8021 8043 11993 N (int>3sigma) = 0 3410 3338 3428 3320 5088 4605 4645 6858 Mean intensity = 0.0 98.3 91.4 103.6 90.4 97.8 99.5 96.8 95.9 Mean int/sigma = 0.0 5.3 5.2 5.3 5.2 5.3 5.3 5.3 5.3 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.924 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 14 489 474 471 N I>3s 0 185 182 7 3.9 154.2 161.5 8.1 0.8 4.5 4.6 0.7 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)/n # 14 centro 1 19410 0.056 2361 0.8 / 4.5 2.81 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2008src0131.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) Inf - 2.15 157 163 96.3 5.34 330.3 19.86 0.0538 0.0410 2.15 - 1.65 183 183 100.0 5.85 185.6 19.23 0.0717 0.0454 1.65 - 1.40 209 209 100.0 5.61 106.9 16.04 0.0855 0.0473 1.40 - 1.25 214 214 100.0 5.71 87.7 14.40 0.0914 0.0489 1.25 - 1.15 200 200 100.0 5.39 84.2 14.51 0.0948 0.0507 1.15 - 1.05 302 302 100.0 4.49 57.6 10.80 0.1124 0.0701 1.05 - 1.00 185 186 99.5 4.12 48.4 9.49 0.1233 0.0872 1.00 - 0.95 238 239 99.6 3.69 32.8 7.09 0.1452 0.1180 0.95 - 0.90 301 302 99.7 3.40 32.0 6.38 0.1584 0.1240 0.90 - 0.85 359 362 99.2 2.70 27.2 4.83 0.1770 0.1712 0.85 - 0.80 430 438 98.2 2.21 26.6 3.90 0.1953 0.2036 0.80 - 0.77 335 348 96.3 1.74 21.0 3.03 0.2213 0.2783 ------------------------------------------------------------------------------ 0.90 - 0.77 1124 1148 97.9 2.22 25.1 3.94 0.1917 0.2110 Inf - 0.77 3113 3146 99.0 3.81 69.3 9.32 0.0878 0.0768 Merged [A], lowest resolution = 6.86 Angstroms, 162 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2008src0131.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C28H32N2S4 Formula weight = 524.80 Tentative Z (number of formula units/cell) = 2.0 giving rho = 1.353, non-H atomic volume = 18.9 and following cell contents and analysis: C 56.00 64.08 % H 64.00 6.15 % N 4.00 5.34 % S 8.00 24.44 % F(000) = 556.0 Mo-K(alpha) radiation Mu (mm-1) = 0.39 ------------------------------------------------------------------------------- File 2008src0131.ins set up as follows: TITL 2008src0131 in P2(1)/n CELL 0.71073 7.9919 9.1538 17.7888 90.000 98.160 90.000 ZERR 2.00 0.0004 0.0005 0.0007 0.000 0.003 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N S UNIT 56 64 4 8 TEMP 0.01 TREF HKLF 4 END -------------------------------------------------------------------------------