++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 06skc0059 started at 08:10:24 on 06-OCT-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 7.053 8.217 10.068 75.73 89.99 89.97 7124 Reflections read from file 06skc0059.hkl; mean (I/sigma) = 6.21 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 3677 3583 3532 3563 5396 4753 4722 7124 N (int>3sigma) = 0 2431 2415 2226 2300 3536 3059 3066 4641 Mean intensity = 0.0 471.7 461.4 415.5 390.4 449.9 442.3 448.9 444.3 Mean int/sigma = 0.0 6.2 6.4 6.1 6.1 6.2 6.2 6.2 6.2 Lattice type: P chosen Volume: 565.47 ------------------------------------------------------------------------------- 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: 7.053 8.217 10.068 75.73 89.99 89.97 Niggli form: a.a = 49.75 b.b = 67.51 c.c = 101.36 b.c = 20.38 a.c = 0.01 a.b = 0.03 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.034 deg. MONOCLINIC P-lattice R(int) = 0.066 [ 6379] Cell: 8.217 7.053 10.068 90.01 104.27 89.97 Volume: 565.47 Matrix: 0.0000 1.0000 0.0000 1.0000 0.0000 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 3583 3677 3532 3563 5396 4753 4722 7124 N (int>3sigma) = 0 2415 2431 2226 2300 3536 3059 3066 4641 Mean intensity = 0.0 461.4 471.7 415.5 390.4 449.9 442.3 448.9 444.3 Mean int/sigma = 0.0 6.4 6.2 6.1 6.1 6.2 6.2 6.2 6.2 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.676 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 21 323 348 369 N I>3s 0 171 233 240 7.6 337.0 491.3 547.0 0.4 5.1 5.9 5.7 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1) # 4 chiral 1 3543 0.066 6379 0.4 / 5.1 2.36 [B] P2(1)/m # 11 centro 1 402 0.066 6379 0.4 / 5.1 10.76 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C8H10O4N2 Formula weight = 198.18 Tentative Z (number of formula units/cell) = 2.0 giving rho = 1.164, non-H atomic volume = 20.2 and following cell contents and analysis: C 16.00 48.48 % H 20.00 5.09 % N 4.00 14.14 % O 8.00 32.29 % F(000) = 208.0 Mo-K(alpha) radiation Mu (mm-1) = 0.09 ------------------------------------------------------------------------------- File 06skc0059p21.ins set up as follows: TITL 06skc0059p21 in P2(1) CELL 0.71073 8.2165 7.0534 10.0677 90.000 104.266 90.000 ZERR 2.00 0.0004 0.0005 0.0007 0.000 0.004 0.000 LATT -1 SYMM -X, 0.5+Y, -Z SFAC C H N O UNIT 16 20 4 8 TEMP 0.03 TREF HKLF 4 END 7124 Reflections written to new reflection file 06skc0059p21.hkl -------------------------------------------------------------------------------