++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 07skc0017 started at 07:45:30 on 18-FEB-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 5.068 5.592 7.247 91.98 103.96 99.50 3187 Reflections read from file 07skc0017.hkl; mean (I/sigma) = 11.29 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 1613 1587 1584 1610 2392 2129 2116 3187 N (int>3sigma) = 0 1407 1348 1383 1374 2069 1874 1839 2786 Mean intensity = 0.0 595.4 440.7 535.6 499.2 524.3 554.2 556.5 540.1 Mean int/sigma = 0.0 11.4 10.8 11.2 11.1 11.2 11.4 11.3 11.3 Lattice type: P chosen Volume: 195.97 ------------------------------------------------------------------------------- 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: 5.068 5.592 7.247 91.98 103.96 99.50 Niggli form: a.a = 25.68 b.b = 31.27 c.c = 52.52 b.c = -1.40 a.c = -8.86 a.b = -4.68 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. TRICLINIC P-lattice R(int) = 0.046 [ 2284] Cell: 5.068 5.592 7.247 91.98 103.96 99.50 Volume: 195.97 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 1613 1587 1584 1610 2392 2129 2116 3187 N (int>3sigma) = 0 1407 1348 1383 1374 2069 1874 1839 2786 Mean intensity = 0.0 595.4 440.7 535.6 499.2 524.3 554.2 556.5 540.1 Mean int/sigma = 0.0 11.4 10.8 11.2 11.1 11.2 11.4 11.3 11.3 Crystal system A and Lattice type P selected Mean |E*E-1| = 0.941 [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 0.046 2284 0.0 / 11.3 0.97 [B] P1 # 1 chiral 1 700 0.046 2284 0.0 / 11.3 5.22 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C6H12O4N2 Formula weight = 176.18 Tentative Z (number of formula units/cell) = 1.0 giving rho = 1.493, non-H atomic volume = 16.3 and following cell contents and analysis: C 6.00 40.90 % H 12.00 6.87 % N 2.00 15.90 % O 4.00 36.33 % F(000) = 94.0 Mo-K(alpha) radiation Mu (mm-1) = 0.13 ------------------------------------------------------------------------------- File e.ins set up as follows: TITL e in P-1 CELL 0.71073 5.0677 5.5917 7.2473 91.984 103.960 99.504 ZERR 1.00 0.0003 0.0004 0.0004 0.003 0.004 0.003 LATT 1 SFAC C H N O UNIT 6 12 2 4 TEMP 0.04 TREF HKLF 4 END ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C6H12O4N2 Formula weight = 176.18 Tentative Z (number of formula units/cell) = 2.0 giving rho = 2.986, non-H atomic volume = 8.2 and following cell contents and analysis: C 12.00 40.90 % H 24.00 6.87 % N 4.00 15.90 % O 8.00 36.33 % F(000) = 188.0 Mo-K(alpha) radiation Mu (mm-1) = 0.25 ------------------------------------------------------------------------------- File 07skc0017p-1.ins set up as follows: TITL 07skc0017p-1 in P-1 CELL 0.71073 5.0677 5.5917 7.2473 91.984 103.960 99.504 ZERR 2.00 0.0003 0.0004 0.0004 0.003 0.004 0.003 LATT 1 SFAC C H N O UNIT 12 24 4 8 TEMP 0.04 TREF HKLF 4 END 3187 Reflections written to new reflection file 07skc0017p-1.hkl -------------------------------------------------------------------------------