++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 06skc0047 started at 12:59:43 on 19-SEP-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 8.128 9.130 13.739 89.78 89.17 79.78 18864 Reflections read from file 06skc0047.hkl; mean (I/sigma) = 3.75 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 9441 9417 9436 9444 14147 12552 12563 18864 N (int>3sigma) = 0 4644 4752 4546 4512 6971 5987 6026 9139 Mean intensity = 0.0 114.7 117.6 111.1 104.0 114.5 111.6 114.0 112.5 Mean int/sigma = 0.0 3.9 3.9 3.8 3.8 3.9 3.8 3.8 3.8 Lattice type: P chosen Volume: 1003.28 ------------------------------------------------------------------------------- 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: 8.128 9.130 13.739 89.78 89.17 79.78 Niggli form: a.a = 66.07 b.b = 83.35 c.c = 188.75 b.c = 0.48 a.c = 1.62 a.b = 13.16 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.834 deg. MONOCLINIC P-lattice R(int) = 0.299 [ 16402] Cell: 8.129 13.739 9.130 89.78 100.22 90.83 Volume: 1003.28 Matrix:-1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.000 deg. TRICLINIC P-lattice R(int) = 0.124 [ 14200] Cell: 8.129 9.130 13.739 89.78 89.17 79.78 Volume: 1003.28 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 Option B selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 9441 9417 9436 9444 14147 12552 12563 18864 N (int>3sigma) = 0 4644 4752 4546 4512 6971 5987 6026 9139 Mean intensity = 0.0 114.7 117.6 111.1 104.0 114.5 111.6 114.0 112.5 Mean int/sigma = 0.0 3.9 3.9 3.8 3.8 3.9 3.8 3.8 3.8 Crystal system A and Lattice type P selected Mean |E*E-1| = 0.897 [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 0.124 14200 0.0 / 3.8 3.13 [B] P1 # 1 chiral 1 700 0.124 14200 0.0 / 3.8 5.36 Option [B] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C9H14O4N2 Formula weight = 214.22 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.418, non-H atomic volume = 16.7 and following cell contents and analysis: C 36.00 50.46 % H 56.00 6.59 % N 8.00 13.08 % O 16.00 29.88 % F(000) = 456.0 Mo-K(alpha) radiation Mu (mm-1) = 0.11 ------------------------------------------------------------------------------- File 06skc0047p1.ins set up as follows: TITL 06skc0047p1 in P1 CELL 0.71073 8.1285 9.1297 13.7387 89.781 89.170 79.782 ZERR 4.00 0.0006 0.0007 0.0011 0.004 0.004 0.005 LATT -1 SFAC C H N O UNIT 36 56 8 16 TEMP 0.04 TREF HKLF 4 END 18864 Reflections written to new reflection file 06skc0047p1.hkl -------------------------------------------------------------------------------