++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + 2008lsh161 started at 20:12:02 on 22-Nov-2010 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 4.585 9.431 10.940 90.00 102.09 90.00 9660 Reflections read from file 2008lsh161.hkl; mean (I/sigma) = 10.78 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 4815 4832 4847 4846 7247 6448 6447 9660 N (int>3sigma) = 0 3895 3968 3893 3931 5878 5334 5348 7957 Mean intensity = 0.0 32.7 32.1 24.7 33.3 29.8 33.1 32.8 32.2 Mean int/sigma = 0.0 10.9 10.8 10.4 10.9 10.7 10.8 10.9 10.8 Lattice type: P chosen Volume: 462.60 ------------------------------------------------------------------------------- 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: 4.585 9.431 10.940 90.00 102.09 90.00 Niggli form: a.a = 21.02 b.b = 88.94 c.c = 119.69 b.c = 0.00 a.c = -10.51 a.b = 0.00 ------------------------------------------------------------------------------- Search for higher metric symmetry Identical indices and Friedel opposites combined before calculating R(sym) ------------------------------------------------------------------------------ Option A: FOM = 0.007 deg. ORTHORHOMBIC C-lattice R(sym) = 0.023 [ 1461] Cell: 4.585 21.395 9.431 90.00 90.00 90.01 Volume: 925.20 Matrix:-1.0000 0.0000 0.0000 1.0000 0.0000 2.0000 0.0000 1.0000 0.0000 Option A selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 4847 4847 0 4812 4847 6447 6402 9660 N (int>3sigma) = 0 3893 3893 0 3797 3893 5348 5300 7957 Mean intensity = 0.0 24.7 24.7 0.0 33.0 24.7 32.8 31.8 32.2 Mean int/sigma = 0.0 10.4 10.4 0.0 10.3 10.4 10.9 10.9 10.8 Crystal system O and Lattice type C selected Mean |E*E-1| = 0.771 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: c-- n-- -c- -n- --a --b --21 N 634 634 129 129 353 353 27 N I>3s 437 437 0 0 267 267 0 27.2 27.2 0.3 0.3 70.1 70.1 0.2 9.3 9.3 0.6 0.6 12.0 12.0 0.6 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] Cmc2(1) # 36 non-cen 1 102 0.023 1461 0.6 / 9.3 2.24 [B] Cmcm # 63 centro 1 100 0.023 1461 0.6 / 9.3 6.02 [C] Ama2 # 40 non-cen 4 21 0.023 1461 0.6 / 9.3 5.82 Option [A] chosen ------------------------------------------------------------------------------- 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: 4.585 9.431 10.940 90.00 102.09 90.00 Niggli form: a.a = 21.02 b.b = 88.94 c.c = 119.69 b.c = 0.00 a.c = -10.51 a.b = 0.00 ------------------------------------------------------------------------------- Search for higher metric symmetry Identical indices and Friedel opposites combined before calculating R(sym) ------------------------------------------------------------------------------ Option A: FOM = 0.007 deg. ORTHORHOMBIC C-lattice R(sym) = 0.023 [ 1461] Cell: 4.585 21.395 9.431 90.00 90.00 90.01 Volume: 925.20 Matrix:-1.0000 0.0000 0.0000 1.0000 0.0000 2.0000 0.0000 1.0000 0.0000 Option A selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 4847 4847 0 4812 4847 6447 6402 9660 N (int>3sigma) = 0 3893 3893 0 3797 3893 5348 5300 7957 Mean intensity = 0.0 24.7 24.7 0.0 33.0 24.7 32.8 31.8 32.2 Mean int/sigma = 0.0 10.4 10.4 0.0 10.3 10.4 10.9 10.9 10.8 Crystal system M and Lattice type C selected Mean |E*E-1| = 0.771 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -c- N 129 N I>3s 0 0.3 0.6 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] C2/c # 15 centro 1 3696 0.020 1016 0.6 / 10.8 4.88 [B] Cc # 9 non-cen 1 566 0.020 1016 0.6 / 10.8 1.27 Option [B] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2008lsh161.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) Inf - 2.05 62 65 95.4 10.11 164.7 55.50 0.0363 0.0200 2.05 - 1.60 61 61 100.0 11.39 70.1 61.45 0.0311 0.0137 1.60 - 1.40 68 68 100.0 12.22 34.0 55.31 0.0370 0.0151 1.40 - 1.25 74 74 100.0 11.88 21.6 43.21 0.0447 0.0177 1.25 - 1.15 62 62 100.0 11.89 40.6 45.85 0.0358 0.0171 1.15 - 1.05 108 108 100.0 11.50 24.5 38.42 0.0454 0.0193 1.05 - 1.00 74 74 100.0 11.39 18.0 35.65 0.0590 0.0235 1.00 - 0.95 76 76 100.0 9.45 9.8 22.64 0.0789 0.0330 0.95 - 0.90 98 98 100.0 8.62 9.1 20.62 0.0866 0.0374 0.90 - 0.85 131 131 100.0 6.60 9.1 17.27 0.0910 0.0447 0.85 - 0.80 162 162 100.0 5.12 5.9 10.84 0.1270 0.0769 0.80 - 0.77 119 120 99.2 4.33 3.6 7.37 0.1772 0.1233 ------------------------------------------------------------------------------ 0.90 - 0.77 412 413 99.8 5.36 6.3 11.88 0.1138 0.0697 Inf - 0.77 1095 1099 99.6 8.79 26.6 29.60 0.0440 0.0237 Merged [A], lowest resolution = 5.35 Angstroms, 364 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2008lsh161.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C10H13N1O1 Formula weight = 163.21 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.172, non-H atomic volume = 19.3 and following cell contents and analysis: C 40.00 73.58 % H 52.00 8.03 % N 4.00 8.58 % O 4.00 9.80 % F(000) = 352.0 Mo-K(alpha) radiation Mu (mm-1) = 0.08 ------------------------------------------------------------------------------- File q.ins set up as follows: TITL q in Cc CELL 0.71073 4.5852 21.3953 9.4310 90.000 90.000 90.000 ZERR 4.00 0.0002 0.0010 0.0004 0.000 0.000 0.000 LATT -7 SYMM X, -Y, 0.5+Z SFAC C H N O UNIT 40 52 4 4 TEMP 0.02 TREF HKLF 4 END -------------------------------------------------------------------------------