++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 06skc0053 started at 08:49:06 on 12-SEP-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 8.196 8.198 10.505 95.17 95.18 111.78 15274 Reflections read from file 06skc0053.hkl; mean (I/sigma) = 4.11 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 7655 7638 7651 7631 11472 10155 10189 15274 N (int>3sigma) = 0 4316 4311 4407 4233 6517 5619 5662 8518 Mean intensity = 0.0 132.9 133.4 125.1 130.4 130.5 123.9 121.0 124.9 Mean int/sigma = 0.0 4.2 4.2 4.3 4.2 4.3 4.2 4.2 4.2 Lattice type: P chosen Volume: 646.91 ------------------------------------------------------------------------------- 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: 8.196 8.198 10.505 95.17 95.18 111.78 Niggli form: a.a = 67.18 b.b = 67.20 c.c = 110.35 b.c = -7.76 a.c = -7.77 a.b = -24.93 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.010 deg. MONOCLINIC C-lattice R(int) = 0.114 [ 13702] Cell: 9.194 13.573 10.505 90.00 99.25 89.99 Volume: 1293.82 Matrix: 1.0000 1.0000 0.0000 -1.0000 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 7631 7631 0 7646 7631 10143 10176 15274 N (int>3sigma) = 0 4233 4233 0 4232 4233 5701 5661 8518 Mean intensity = 0.0 130.4 130.4 0.0 134.2 130.4 120.7 133.3 124.9 Mean int/sigma = 0.0 4.2 4.2 0.0 4.2 4.2 4.2 4.2 4.2 Crystal system M and Lattice type C selected Mean |E*E-1| = 0.957 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -c- N 345 N I>3s 1 3.2 0.6 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] C2/c # 15 centro 1 3696 0.114 13702 0.6 / 4.2 2.81 [B] Cc # 9 non-cen 1 566 0.114 13702 0.6 / 4.2 7.84 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C6H8O4N2 Formula weight = 172.14 Tentative Z (number of formula units/cell) = 4.0 giving rho = 0.884, non-H atomic volume = 27.0 and following cell contents and analysis: C 24.00 41.86 % H 32.00 4.68 % N 8.00 16.28 % O 16.00 37.18 % F(000) = 360.0 Mo-K(alpha) radiation Mu (mm-1) = 0.08 ------------------------------------------------------------------------------- File 06skc0053c2c.ins set up as follows: TITL 06skc0053c2c in C2/c CELL 0.71073 9.1937 13.5734 10.5047 90.000 99.252 90.000 ZERR 4.00 0.0006 0.0006 0.0005 0.000 0.004 0.000 LATT 7 SYMM -X, Y, 0.5-Z SFAC C H N O UNIT 24 32 8 16 TEMP 0.02 TREF HKLF 4 END 15274 Reflections written to new reflection file 06skc0053c2c.hkl -------------------------------------------------------------------------------