++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 04skc0001 started at 13:12:41 on 19-JUL-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 25.066 4.977 19.142 90.15 129.42 89.91 6575 Reflections read from file 04skc0001.hkl; mean (I/sigma) = 2.24 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 3292 3292 0 3293 3292 4400 4392 6575 N (int>3sigma) = 0 712 712 0 721 712 1014 1003 1479 Mean intensity = 0.0 14.2 14.2 0.0 16.0 14.2 16.2 16.3 16.8 Mean int/sigma = 0.0 2.3 2.3 0.0 2.4 2.3 2.4 2.4 2.4 Lattice type: C chosen Volume: 1844.66 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 1.0000 0.0000 -0.5000 0.5000 0.0000 0.5000 0.5000 1.0000 Unitcell: 4.977 12.774 14.995 89.60 80.57 78.86 Niggli form: a.a = 24.77 b.b = 163.16 c.c = 224.86 b.c = 1.33 a.c = 12.23 a.b = 12.29 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.150 deg. MONOCLINIC C-lattice R(int) = 0.199 [ 4312] Cell: 25.065 4.977 19.142 90.15 129.42 89.91 Volume: 1844.66 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.150 deg. MONOCLINIC I-lattice R(int) = 0.199 [ 4312] Cell: 19.142 4.977 19.631 90.03 99.46 89.85 Volume: 1844.66 Matrix: 0.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option C: FOM = 0.000 deg. TRICLINIC P-lattice R(int) = 0.150 [ 2806] Cell: 4.977 12.774 14.995 89.60 80.57 78.86 Volume: 922.33 Matrix: 0.0000 1.0000 0.0000 -0.5000 0.5000 0.0000 0.5000 0.5000 1.0000 Option A selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 3292 3292 0 3293 3292 4400 4392 6575 N (int>3sigma) = 0 712 712 0 721 712 1014 1003 1479 Mean intensity = 0.0 14.2 14.2 0.0 16.0 14.2 16.2 16.3 16.8 Mean int/sigma = 0.0 2.3 2.3 0.0 2.4 2.3 2.4 2.4 2.4 Crystal system M and Lattice type C selected Mean |E*E-1| = 0.864 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -c- N 396 N I>3s 2 2.8 0.6 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] C2/c # 15 centro 1 3696 0.199 4312 0.6 / 2.4 6.50 [B] Cc # 9 non-cen 1 566 0.199 4312 0.6 / 2.4 7.19 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C7H10O6N2 Formula weight = 218.17 Tentative Z (number of formula units/cell) = 6.0 giving rho = 1.178, non-H atomic volume = 20.5 and following cell contents and analysis: C 42.00 38.53 % H 60.00 4.62 % N 12.00 12.84 % O 36.00 44.00 % F(000) = 684.0 Mo-K(alpha) radiation Mu (mm-1) = 0.10 ------------------------------------------------------------------------------- File 04skc0001a.ins set up as follows: TITL 04skc0001a in C2/c CELL 0.71073 25.0655 4.9767 19.1418 90.000 129.418 90.000 ZERR 6.00 0.0050 0.0010 0.0038 0.000 0.030 0.000 LATT 7 SYMM -X, Y, 0.5-Z SFAC C H N O UNIT 42 60 12 36 TEMP 0.06 TREF HKLF 4 END 6575 Reflections written to new reflection file 04skc0001a.hkl -------------------------------------------------------------------------------