++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + 2008src1007 started at 17:30:19 on 17-Oct-2008 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 8.738 9.116 16.479 90.00 91.06 90.00 17448 Reflections read from file 2008src1007.hkl; mean (I/sigma) = 11.37 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 8717 8746 8739 8730 13101 11648 11637 17448 N (int>3sigma) = 0 6156 6450 6720 6530 9663 8716 8660 13072 Mean intensity = 0.0 27.3 36.2 36.3 36.1 33.3 36.8 36.1 36.4 Mean int/sigma = 0.0 10.3 11.4 11.6 11.4 11.1 11.4 11.4 11.4 Lattice type: P chosen Volume: 1312.40 ------------------------------------------------------------------------------- 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: 8.738 9.116 16.479 90.00 91.06 90.00 Niggli form: a.a = 76.36 b.b = 83.09 c.c = 271.54 b.c = 0.00 a.c = -2.67 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) = 0.019 [ 2676] Cell: 8.738 9.116 16.479 90.00 91.06 90.00 Volume: 1312.40 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 8717 8746 8739 8730 13101 11648 11637 17448 N (int>3sigma) = 0 6156 6450 6720 6530 9663 8716 8660 13072 Mean intensity = 0.0 27.3 36.2 36.3 36.1 33.3 36.8 36.1 36.4 Mean int/sigma = 0.0 10.3 11.4 11.6 11.4 11.1 11.4 11.4 11.4 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.985 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 18 584 586 588 N I>3s 0 241 2 243 0.1 34.6 0.2 34.4 0.3 7.7 0.5 7.6 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)/c # 14 centro 1 19410 0.019 2676 0.5 / 7.6 1.44 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2008src1007.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) Inf - 2.10 169 176 96.0 6.25 115.7 52.19 0.0207 0.0170 2.10 - 1.65 174 177 98.3 7.07 73.1 52.46 0.0261 0.0146 1.65 - 1.40 210 210 100.0 7.24 54.2 44.79 0.0284 0.0148 1.40 - 1.25 208 208 100.0 7.25 44.3 41.39 0.0307 0.0171 1.25 - 1.15 219 219 100.0 7.17 46.4 35.86 0.0334 0.0192 1.15 - 1.05 307 307 100.0 7.20 27.5 28.55 0.0440 0.0236 1.05 - 1.00 193 193 100.0 7.04 22.1 23.68 0.0527 0.0269 1.00 - 0.95 242 242 100.0 6.01 17.5 19.96 0.0600 0.0345 0.95 - 0.90 294 294 100.0 5.27 14.8 15.76 0.0699 0.0437 0.90 - 0.85 371 371 100.0 4.12 13.8 12.94 0.0737 0.0510 0.85 - 0.80 468 468 100.0 3.10 11.0 9.79 0.0790 0.0731 0.80 - 0.77 349 352 99.1 2.69 8.2 7.18 0.0922 0.1017 ------------------------------------------------------------------------------ 0.90 - 0.77 1188 1191 99.7 3.30 11.1 10.01 0.0786 0.0707 Inf - 0.77 3204 3217 99.6 5.42 30.4 24.50 0.0364 0.0269 Merged [A], lowest resolution = 6.31 Angstroms, 605 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2008src1007.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C28H32N2S4 Formula weight = 524.80 Tentative Z (number of formula units/cell) = 2.0 giving rho = 1.328, non-H atomic volume = 19.3 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) = 0.38 ------------------------------------------------------------------------------- File 2008src1007.ins set up as follows: TITL 2008src1007 in P2(1)/c CELL 0.71073 8.7385 9.1156 16.4786 90.000 91.064 90.000 ZERR 2.00 0.0002 0.0001 0.0003 0.000 0.001 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N S UNIT 56 64 4 8 TEMP 0.2 TREF HKLF 4 END -------------------------------------------------------------------------------