++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + 2007may0010 started at 14:49:58 on 29-Sep-2007 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 15.161 4.332 15.328 90.00 108.58 90.00 10884 Reflections read from file 2007may0010.hkl; mean (I/sigma) = 7.46 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 5431 5442 5417 5461 8145 7206 7235 10884 N (int>3sigma) = 0 3418 3276 3010 3500 4852 4440 4455 6741 Mean intensity = 0.0 180.3 171.3 166.2 171.8 172.6 192.4 196.8 192.1 Mean int/sigma = 0.0 7.7 7.3 6.8 7.8 7.3 7.5 7.5 7.6 Lattice type: P chosen Volume: 954.38 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 -1.0000 0.0000 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 Unitcell: 4.332 15.161 15.328 108.58 90.00 90.00 Niggli form: a.a = 18.77 b.b = 229.87 c.c = 234.94 b.c = -74.03 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 = 0.660 deg. ORTHORHOMBIC C-lattice R(sym) = 0.582 [ 2594] Cell: 17.797 24.756 4.332 90.00 90.00 89.34 Volume: 1908.76 Matrix: 1.0000 0.0000 1.0000 -1.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.000 deg. MONOCLINIC P-lattice R(sym) = 0.032 [ 1445] Cell: 15.161 4.332 15.328 90.00 108.58 90.00 Volume: 954.38 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option C: FOM = 0.660 deg. MONOCLINIC C-lattice R(sym) = 0.599 [ 1771] Cell: 24.756 17.797 4.332 90.00 90.00 90.66 Volume: 1908.76 Matrix: 1.0000 0.0000 -1.0000 1.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option D: FOM = 0.660 deg. MONOCLINIC C-lattice R(sym) = 0.608 [ 1674] Cell: 17.797 24.756 4.332 90.00 90.00 89.34 Volume: 1908.76 Matrix:-1.0000 0.0000 -1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 Option B selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 5431 5442 5417 5461 8145 7206 7235 10884 N (int>3sigma) = 0 3418 3276 3010 3500 4852 4440 4455 6741 Mean intensity = 0.0 180.3 171.3 166.2 171.8 172.6 192.4 196.8 192.1 Mean int/sigma = 0.0 7.7 7.3 6.8 7.8 7.3 7.5 7.5 7.6 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.967 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 5 958 1010 1032 N I>3s 0 5 459 460 2.2 3.6 165.2 161.6 0.4 0.6 6.4 6.3 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 4 19410 0.032 1445 0.6 / 6.3 1.78 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2007may0010.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) Inf - 2.15 127 135 94.1 5.59 726.4 30.29 0.0249 0.0214 2.15 - 1.70 133 133 100.0 6.19 394.5 28.64 0.0325 0.0223 1.70 - 1.45 132 132 100.0 6.64 256.4 28.30 0.0410 0.0236 1.45 - 1.30 164 164 100.0 6.36 157.1 21.35 0.0560 0.0305 1.30 - 1.20 141 141 100.0 6.66 149.0 20.89 0.0614 0.0320 1.20 - 1.10 176 176 100.0 5.85 186.5 18.91 0.0524 0.0332 1.10 - 1.05 132 132 100.0 5.27 105.2 15.84 0.0768 0.0446 1.05 - 1.00 161 161 100.0 4.73 83.4 12.30 0.0845 0.0543 1.00 - 0.95 192 192 100.0 4.54 57.9 10.74 0.1064 0.0676 0.95 - 0.90 218 218 100.0 3.89 60.8 9.17 0.1132 0.0769 0.90 - 0.85 277 277 100.0 3.14 52.2 6.89 0.1177 0.1070 0.85 - 0.80 352 358 98.3 2.38 46.8 5.22 0.1193 0.1444 0.80 - 0.77 256 273 93.8 1.91 32.9 3.73 0.1773 0.2216 ------------------------------------------------------------------------------ 0.90 - 0.77 885 908 97.5 2.47 44.5 5.31 0.1267 0.1472 Inf - 0.77 2461 2492 98.8 4.37 141.9 13.82 0.0499 0.0441 Merged [A], lowest resolution = 6.19 Angstroms, 206 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2007may0010.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C10H8Cl1N1O1S1 Formula weight = 225.68 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.571, non-H atomic volume = 17.0 and following cell contents and analysis: C 40.00 53.22 % H 32.00 3.57 % N 4.00 6.21 % O 4.00 7.09 % S 4.00 14.21 % Cl 4.00 15.71 % F(000) = 464.0 Mo-K(alpha) radiation Mu (mm-1) = 0.58 ------------------------------------------------------------------------------- File monop.ins set up as follows: TITL monop in P2(1)/c CELL 0.71073 15.3278 4.3325 15.1614 90.000 108.576 90.000 ZERR 4.00 0.0004 0.0002 0.0005 0.000 0.002 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O S CL UNIT 40 32 4 4 4 4 TEMP 0.01 TREF HKLF 4 END 10884 Reflections written to new reflection file monop.hkl -------------------------------------------------------------------------------