++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + 2008lsh082 started at 21:40:38 on 14-Nov-2010 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 8.972 6.863 15.327 90.00 90.09 90.00 14056 Reflections read from file 2008lsh082.hkl; mean (I/sigma) = 3.21 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 7048 7019 7025 7019 10546 9372 9352 14056 N (int>3sigma) = 0 2137 2453 2444 2394 3517 3269 3269 4933 Mean intensity = 0.0 5.7 5.8 7.0 7.0 6.2 7.3 6.7 6.9 Mean int/sigma = 0.0 2.9 3.3 3.3 3.3 3.2 3.4 3.4 3.4 Lattice type: P chosen Volume: 943.80 ------------------------------------------------------------------------------- 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: 6.863 8.972 15.327 90.09 90.00 90.00 Niggli form: a.a = 47.10 b.b = 80.50 c.c = 234.93 b.c = -0.22 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 = 0.092 deg. ORTHORHOMBIC P-lattice R(sym) = 0.575 [ 2952] Cell: 6.863 8.972 15.327 90.09 90.00 90.00 Volume: 943.80 Matrix: 0.0000 -1.0000 0.0000 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.000 deg. MONOCLINIC P-lattice R(sym) = 0.064 [ 1896] Cell: 8.972 6.863 15.327 90.00 90.09 90.00 Volume: 943.80 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option C: FOM = 0.092 deg. MONOCLINIC P-lattice R(sym) = 0.598 [ 1992] Cell: 6.863 15.327 8.972 89.91 90.00 90.00 Volume: 943.80 Matrix: 0.0000 -1.0000 0.0000 0.0000 0.0000 1.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option D: FOM = 0.092 deg. MONOCLINIC P-lattice R(sym) = 0.611 [ 1945] Cell: 6.863 8.972 15.327 90.09 90.00 90.00 Volume: 943.80 Matrix: 0.0000 -1.0000 0.0000 -1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 Option B selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 7048 7019 7025 7019 10546 9372 9352 14056 N (int>3sigma) = 0 2137 2453 2444 2394 3517 3269 3269 4933 Mean intensity = 0.0 5.7 5.8 7.0 7.0 6.2 7.3 6.7 6.9 Mean int/sigma = 0.0 2.9 3.3 3.3 3.3 3.2 3.4 3.4 3.4 Crystal system A and Lattice type P selected Mean |E*E-1| = 1.062 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absences not required for triclinic 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] P-1 # 2 centro 1 8646 0.000 0 0.0 / 3.4 3.86 [B] P1 # 1 chiral 1 700 0.000 0 0.0 / 3.4 13.72 Option [B] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2008lsh082.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) Inf - 2.05 219 230 95.2 4.08 37.7 14.76 0.0353 0.0362 2.05 - 1.60 248 248 100.0 4.38 13.2 12.59 0.0532 0.0410 1.60 - 1.40 238 238 100.0 4.37 6.8 9.35 0.0831 0.0599 1.40 - 1.25 286 286 100.0 4.27 5.3 7.78 0.1057 0.0735 1.25 - 1.15 303 303 100.0 4.28 7.2 8.77 0.0945 0.0701 1.15 - 1.05 411 411 100.0 4.31 5.7 6.74 0.1195 0.0814 1.05 - 1.00 253 253 100.0 4.12 2.3 4.70 0.2392 0.1582 1.00 - 0.95 331 331 100.0 3.61 3.7 5.26 0.1750 0.1323 0.95 - 0.90 402 405 99.3 3.11 2.6 3.64 0.2245 0.2479 0.90 - 0.85 504 509 99.0 2.49 1.6 2.16 0.3779 0.3656 0.85 - 0.80 618 642 96.3 1.86 1.4 1.75 0.4047 0.5249 0.80 - 0.77 435 507 85.8 1.46 1.5 1.48 0.3716 0.5320 ------------------------------------------------------------------------------ 0.90 - 0.77 1557 1658 93.9 1.93 1.5 1.81 0.3859 0.4726 Inf - 0.77 4248 4363 97.4 3.22 5.7 5.52 0.0954 0.1065 Merged [A], lowest resolution = 6.86 Angstroms, 273 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2008lsh082.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C8H10N2O1 Formula weight = 150.18 Tentative Z (number of formula units/cell) = 5.0 giving rho = 1.321, non-H atomic volume = 17.2 and following cell contents and analysis: C 40.00 63.98 % H 50.00 6.71 % N 10.00 18.66 % O 5.00 10.65 % F(000) = 400.0 Mo-K(alpha) radiation Mu (mm-1) = 0.09 ------------------------------------------------------------------------------- File p-1.ins set up as follows: TITL p-1 in P1 CELL 0.71073 8.9722 6.8630 15.3273 90.000 90.092 90.000 ZERR 5.00 0.0006 0.0005 0.0008 0.000 0.004 0.000 LATT -1 SFAC C H N O UNIT 40 50 10 5 TEMP 0.02 TREF HKLF 4 END 14056 Reflections written to new reflection file p-1.hkl -------------------------------------------------------------------------------