++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 06skc0065 started at 16:45:53 on 07-NOV-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 17.308 9.009 18.932 90.00 105.31 90.00 53588 Reflections read from file 06skc0065.hkl; mean (I/sigma) = 1.11 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 26719 26823 26744 26802 40143 35742 35787 53588 N (int>3sigma) = 0 3221 3038 3263 2820 4761 4364 4447 6392 Mean intensity = 0.0 39.8 37.1 40.5 36.1 39.1 40.9 41.4 40.8 Mean int/sigma = 0.0 1.4 1.3 1.4 1.3 1.4 1.4 1.4 1.4 Lattice type: P chosen Volume: 2847.23 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 -1.0000 0.0000 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 Unitcell: 9.009 17.308 18.932 105.31 90.00 90.00 Niggli form: a.a = 81.16 b.b = 299.56 c.c = 358.42 b.c = -86.49 a.c = 0.00 a.b = 0.00 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.367 [ 46604] Cell: 17.308 9.009 18.932 90.00 105.31 90.00 Volume: 2847.23 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.000 deg. TRICLINIC P-lattice R(int) = 0.341 [ 41005] Cell: 9.009 17.308 18.932 74.69 90.00 90.00 Volume: 2847.23 Matrix: 0.0000 1.0000 0.0000 -1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 Option A selected ------------------------------------------------------------------------------- Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 26719 26823 26744 26802 40143 35742 35787 53588 N (int>3sigma) = 0 3221 3038 3263 2820 4761 4364 4447 6392 Mean intensity = 0.0 39.8 37.1 40.5 36.1 39.1 40.9 41.4 40.8 Mean int/sigma = 0.0 1.4 1.3 1.4 1.3 1.4 1.4 1.4 1.4 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.917 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 18 2214 2230 2220 N I>3s 0 243 246 9 3.9 87.9 87.2 8.3 0.5 1.4 1.4 0.6 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM No acceptable space group - change tolerances or unset chiral flag or possibly change input lattice type, then recheck cell using H-option Input space group symbol: P2(1)/n Number: 14 centrosymmetric CSD frequency: 19410 R(int) = 0.367 46604 reflections merged Systematic absence exceptions: -21- -a- -c- -n- N 18 2214 2230 2220 N I>3s 0 243 246 9 3.9 87.9 87.2 8.3 0.5 1.4 1.4 0.6 ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C11H24O4N2 Formula weight = 248.32 Tentative Z (number of formula units/cell) = 8.0 giving rho = 1.159, non-H atomic volume = 20.9 and following cell contents and analysis: C 88.00 53.20 % H 192.00 9.74 % N 16.00 11.28 % O 32.00 25.77 % F(000) = 1088.0 Mo-K(alpha) radiation Mu (mm-1) = 0.09 ------------------------------------------------------------------------------- File 06skc0065p21n.ins set up as follows: TITL 06skc0065p21n in P2(1)/n CELL 0.71073 17.3078 9.0088 18.9320 90.000 105.305 90.000 ZERR 8.00 0.0022 0.0014 0.0026 0.000 0.007 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N O UNIT 88 192 16 32 TEMP 0.07 TREF HKLF 4 END 53588 Reflections written to new reflection file 06skc0065p21n.hkl -------------------------------------------------------------------------------