++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 06skc0003 started at 20:34:34 on 28-JAN-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 6.008 9.690 8.153 90.00 90.04 90.00 5340 Reflections read from file 06skc0003.hkl; mean (I/sigma) = 5.74 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 2661 2657 2668 2693 3993 3551 3559 5340 N (int>3sigma) = 0 1533 1547 1590 1593 2335 2116 2106 3162 Mean intensity = 0.0 147.9 149.9 166.8 146.5 154.9 156.9 149.1 156.2 Mean int/sigma = 0.0 5.7 5.8 5.8 5.8 5.8 5.8 5.8 5.8 Lattice type: P chosen Volume: 474.67 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 Unitcell: 6.008 8.153 9.690 90.00 90.00 90.04 Niggli form: a.a = 36.10 b.b = 66.46 c.c = 93.90 b.c = 0.00 a.c = 0.00 a.b = -0.03 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.039 deg. ORTHORHOMBIC P-lattice R(int) = 0.080 [ 4661] Cell: 6.008 8.153 9.690 90.00 90.00 90.04 Volume: 474.67 Matrix: 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 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 2661 2668 2657 2693 3993 3579 3551 5340 N (int>3sigma) = 0 1533 1590 1547 1593 2335 2123 2116 3162 Mean intensity = 0.0 147.9 166.8 149.9 146.5 154.9 156.0 156.9 156.2 Mean int/sigma = 0.0 5.7 5.8 5.8 5.8 5.8 5.8 5.8 5.8 Crystal system O and Lattice type P selected Mean |E*E-1| = 0.790 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: b-- c-- n-- 21-- -c- -a- -n- -21- --a --b --n --21 N 257 253 254 16 245 248 243 13 176 172 174 18 N I>3s 155 153 160 0 148 149 127 0 127 121 118 3 261.4 177.6 243.9 4.7 167.6 188.9 148.4 4.4 897.2 529.8 523.4 7.6 6.9 6.6 6.8 0.7 6.9 7.3 6.0 0.7 7.8 7.7 7.0 1.5 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)2(1)2(1) # 19 chiral 1 5917 0.080 4661 1.5 / 5.8 2.38 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C4H6N2 Formula weight = 82.11 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.149, non-H atomic volume = 19.8 and following cell contents and analysis: C 16.00 58.51 % H 24.00 7.37 % N 8.00 34.13 % F(000) = 176.0 Mo-K(alpha) radiation Mu (mm-1) = 0.07 ------------------------------------------------------------------------------- File 06skc0003p212121.ins set up as follows: TITL 06skc0003p212121 in P2(1)2(1)2(1) CELL 0.71073 6.0084 8.1526 9.6903 90.000 90.000 90.000 ZERR 4.00 0.0008 0.0013 0.0013 0.000 0.000 0.000 LATT -1 SYMM 0.5-X, -Y, 0.5+Z SYMM -X, 0.5+Y, 0.5-Z SYMM 0.5+X, 0.5-Y, -Z SFAC C H N UNIT 16 24 8 TEMP 0.02 TREF HKLF 4 END 5340 Reflections written to new reflection file 06skc0003p212121.hkl -------------------------------------------------------------------------------