++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + 2007may0013 started at 17:18:18 on 01-Oct-2007 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 10.582 7.872 11.251 90.00 115.10 90.00 9033 Reflections read from file 2007may0013.hkl; mean (I/sigma) = 5.49 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 4543 4486 4453 4518 6741 6031 6007 9033 N (int>3sigma) = 0 2296 2227 2147 2327 3335 3066 3105 4635 Mean intensity = 0.0 85.2 74.1 77.9 83.0 79.1 84.9 80.3 83.2 Mean int/sigma = 0.0 5.5 5.3 5.4 5.7 5.4 5.6 5.7 5.6 Lattice type: P chosen Volume: 848.73 ------------------------------------------------------------------------------- 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: 7.872 10.582 11.251 115.10 90.00 90.00 Niggli form: a.a = 61.98 b.b = 111.97 c.c = 126.58 b.c = -50.50 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 = 0.000 deg. MONOCLINIC P-lattice R(sym) = 0.051 [ 1658] Cell: 10.582 7.872 11.251 90.00 115.10 90.00 Volume: 848.73 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 4543 4486 4453 4518 6741 6031 6007 9033 N (int>3sigma) = 0 2296 2227 2147 2327 3335 3066 3105 4635 Mean intensity = 0.0 85.2 74.1 77.9 83.0 79.1 84.9 80.3 83.2 Mean int/sigma = 0.0 5.5 5.3 5.4 5.7 5.4 5.6 5.7 5.6 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.952 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 8 410 429 441 N I>3s 0 1 191 190 1.9 3.1 144.1 140.1 0.3 0.6 6.0 5.8 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 0.051 1658 0.6 / 5.6 2.02 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2007may0013.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) Inf - 2.15 106 110 96.4 5.90 398.5 28.48 0.0267 0.0217 2.15 - 1.65 121 121 100.0 6.58 170.6 26.05 0.0389 0.0256 1.65 - 1.45 106 106 100.0 6.42 105.5 19.81 0.0604 0.0316 1.45 - 1.30 116 116 100.0 6.53 63.3 15.34 0.0859 0.0431 1.30 - 1.20 121 121 100.0 6.31 52.2 14.76 0.0949 0.0503 1.20 - 1.10 168 168 100.0 5.66 59.8 13.05 0.0968 0.0519 1.10 - 1.05 110 110 100.0 5.10 62.5 13.51 0.0927 0.0541 1.05 - 1.00 126 126 100.0 4.44 33.6 9.13 0.1356 0.0873 1.00 - 0.95 157 157 100.0 4.13 29.3 7.31 0.1527 0.1046 0.95 - 0.90 193 194 99.5 3.62 24.7 5.83 0.1785 0.1384 0.90 - 0.85 246 246 100.0 2.98 16.5 3.69 0.2543 0.2346 0.85 - 0.80 290 294 98.6 2.52 11.2 2.37 0.3336 0.3829 0.80 - 0.77 227 261 87.0 1.89 10.2 2.02 0.3804 0.4712 ------------------------------------------------------------------------------ 0.90 - 0.77 763 801 95.3 2.45 12.6 2.69 0.3038 0.3416 Inf - 0.77 2087 2130 98.0 4.24 61.3 10.06 0.0698 0.0635 Merged [A], lowest resolution = 6.23 Angstroms, 134 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2007may0013.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C8H5N1O4 Formula weight = 179.13 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.402, non-H atomic volume = 16.3 and following cell contents and analysis: C 32.00 53.64 % H 20.00 2.81 % N 4.00 7.82 % O 16.00 35.73 % F(000) = 368.0 Mo-K(alpha) radiation Mu (mm-1) = 0.12 ------------------------------------------------------------------------------- File q.ins set up as follows: TITL q in P2(1)/c CELL 0.71073 11.2506 7.8725 10.5817 90.000 115.098 90.000 ZERR 4.00 0.0004 0.0004 0.0004 0.000 0.002 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O UNIT 32 20 4 16 TEMP 0.02 TREF HKLF 4 END -------------------------------------------------------------------------------