++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 04skc0004 started at 10:46:45 on 17-AUG-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 7.615 8.200 10.111 98.68 106.42 105.16 12526 Reflections read from file 04skc0004.hkl; mean (I/sigma) = 12.78 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 6295 6286 6261 6273 9421 8361 8343 12526 N (int>3sigma) = 0 4750 4743 4787 4695 7140 6370 6361 9501 Mean intensity = 0.0 309.4 317.8 302.7 285.6 310.0 299.0 305.0 301.5 Mean int/sigma = 0.0 12.9 12.8 12.8 12.6 12.8 12.8 12.8 12.8 Lattice type: P chosen Volume: 567.11 ------------------------------------------------------------------------------- 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: 7.615 8.200 10.111 98.68 106.42 105.16 Niggli form: a.a = 57.99 b.b = 67.24 c.c = 102.24 b.c = -12.51 a.c = -21.76 a.b = -16.33 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. TRICLINIC P-lattice R(int) = 0.030 [ 9909] Cell: 7.615 8.200 10.111 98.68 106.42 105.16 Volume: 567.11 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 6295 6286 6261 6273 9421 8361 8343 12526 N (int>3sigma) = 0 4750 4743 4787 4695 7140 6370 6361 9501 Mean intensity = 0.0 309.4 317.8 302.7 285.6 310.0 299.0 305.0 301.5 Mean int/sigma = 0.0 12.9 12.8 12.8 12.6 12.8 12.8 12.8 12.8 Crystal system A and Lattice type P selected Mean |E*E-1| = 1.004 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absences not required for triclinic Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P-1 # 2 centro 1 8646 0.030 9909 0.0 / 12.8 0.92 [B] P1 # 1 chiral 1 700 0.030 9909 0.0 / 12.8 8.12 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C8H15O7N1 Formula weight = 237.21 Tentative Z (number of formula units/cell) = 4.0 giving rho = 2.778, non-H atomic volume = 8.9 and following cell contents and analysis: C 32.00 40.50 % H 60.00 6.37 % N 4.00 5.91 % O 28.00 47.22 % F(000) = 504.0 Mo-K(alpha) radiation Mu (mm-1) = 0.25 ------------------------------------------------------------------------------- File 04skc0004p-1.ins set up as follows: TITL 04skc0004p-1 in P-1 CELL 0.71073 7.6152 8.2002 10.1113 98.680 106.417 105.156 ZERR 4.00 0.0007 0.0011 0.0012 0.010 0.008 0.008 LATT 1 SFAC C H N O UNIT 32 60 4 28 TEMP 0.4 TREF HKLF 4 END 12526 Reflections written to new reflection file 04skc0004p-1.hkl -------------------------------------------------------------------------------