++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + 2007jmw0004 started at 10:19:07 on 27-Feb-2007 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 8.171 15.061 14.326 90.00 90.05 90.00 13946 Reflections read from file 2007jmw0004.hkl; mean (I/sigma) = 5.97 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 6964 6993 6951 6939 10454 9277 9318 13946 N (int>3sigma) = 0 4438 4463 4369 4439 6635 5930 5975 8914 Mean intensity = 0.0 194.8 187.4 178.5 164.3 186.9 178.7 182.8 177.5 Mean int/sigma = 0.0 6.1 6.0 6.0 5.9 6.0 6.0 6.1 6.0 Lattice type: P chosen Volume: 1763.01 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 Unitcell: 8.171 14.326 15.061 90.00 90.00 90.05 Niggli form: a.a = 66.77 b.b = 205.24 c.c = 226.82 b.c = 0.00 a.c = 0.00 a.b = -0.11 ------------------------------------------------------------------------------- Search for higher metric symmetry Identical indices and Friedel opposites combined before calculating R(sym) ------------------------------------------------------------------------------ Option A: FOM = 0.053 deg. ORTHORHOMBIC P-lattice R(sym) = 0.073 [ 4563] Cell: 8.171 14.326 15.061 90.00 90.00 90.05 Volume: 1763.01 Matrix: 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.000 deg. MONOCLINIC P-lattice R(sym) = 0.051 [ 2735] Cell: 8.171 15.061 14.326 90.00 90.05 90.00 Volume: 1763.01 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option C: FOM = 0.053 deg. MONOCLINIC P-lattice R(sym) = 0.061 [ 2689] Cell: 14.326 8.171 15.061 90.00 90.00 89.95 Volume: 1763.01 Matrix: 0.0000 0.0000 -1.0000 1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option D: FOM = 0.053 deg. MONOCLINIC P-lattice R(sym) = 0.060 [ 2906] Cell: 8.171 14.326 15.061 90.00 90.00 90.05 Volume: 1763.01 Matrix:-1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 Option D selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 6964 6951 6993 6939 10454 9277 9293 13946 N (int>3sigma) = 0 4438 4369 4463 4439 6635 5930 5901 8914 Mean intensity = 0.0 194.8 178.5 187.4 164.3 186.9 178.7 179.5 177.5 Mean int/sigma = 0.0 6.1 6.0 6.0 5.9 6.0 6.0 6.0 6.0 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.842 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 25 285 309 298 N I>3s 5 12 133 131 14.4 7.3 218.0 226.3 1.4 0.9 4.6 4.7 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)/c # 14 centro 4 19410 0.060 2906 1.4 / 4.6 4.41 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2007jmw0004.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) Inf - 2.10 211 222 95.0 4.71 683.6 22.96 0.0408 0.0323 2.10 - 1.65 225 225 100.0 5.12 364.8 21.56 0.0494 0.0348 1.65 - 1.45 214 214 100.0 5.00 234.8 17.85 0.0607 0.0399 1.45 - 1.30 240 240 100.0 4.79 130.3 14.84 0.0823 0.0494 1.30 - 1.20 239 239 100.0 4.92 167.8 16.60 0.0762 0.0458 1.20 - 1.10 334 334 100.0 4.27 135.4 13.33 0.0811 0.0555 1.10 - 1.05 222 223 99.6 3.95 82.7 10.82 0.1121 0.0716 1.05 - 1.00 253 257 98.4 3.44 73.3 9.49 0.1215 0.0844 1.00 - 0.95 307 309 99.4 3.24 62.3 8.58 0.1367 0.0992 0.95 - 0.90 359 377 95.2 2.77 50.0 6.13 0.1645 0.1318 0.90 - 0.85 473 516 91.7 2.30 43.6 5.02 0.1921 0.1701 0.85 - 0.80 523 604 86.6 1.96 34.3 3.67 0.2851 0.2296 0.80 - 0.77 390 513 76.0 1.44 24.3 2.45 0.4171 0.3643 ------------------------------------------------------------------------------ 0.90 - 0.77 1386 1633 84.9 1.91 34.7 3.79 0.2554 0.2306 Inf - 0.77 3990 4273 93.4 3.26 129.1 10.12 0.0723 0.0653 Merged [A], lowest resolution = 6.67 Angstroms, 457 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2007jmw0004.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C9H9Cl1N2 Formula weight = 180.63 Tentative Z (number of formula units/cell) = 8.0 giving rho = 1.361, non-H atomic volume = 18.4 and following cell contents and analysis: C 72.00 59.84 % H 72.00 5.02 % N 16.00 15.51 % Cl 8.00 19.63 % F(000) = 752.0 Mo-K(alpha) radiation Mu (mm-1) = 0.37 ------------------------------------------------------------------------------- File mono.ins set up as follows: TITL mono in P2(1)/c CELL 0.71073 15.0606 14.3262 8.1711 90.000 90.000 90.000 ZERR 8.00 0.0007 0.0007 0.0005 0.000 0.000 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N CL UNIT 72 72 16 8 TEMP 0.02 TREF HKLF 4 END 13946 Reflections written to new reflection file mono.hkl -------------------------------------------------------------------------------