++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 07skc0019 started at 18:43:34 on 18-FEB-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 11.889 6.218 21.946 90.00 104.85 90.00 13653 Reflections read from file 07skc0019.hkl; mean (I/sigma) = 5.54 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 6822 6838 6790 6839 10225 9099 9137 13653 N (int>3sigma) = 0 3400 3758 3700 3771 5429 4963 5028 7466 Mean intensity = 0.0 89.3 108.3 107.6 96.0 101.7 105.9 106.7 103.9 Mean int/sigma = 0.0 5.1 5.7 5.8 5.6 5.5 5.7 5.7 5.7 Lattice type: P chosen Volume: 1568.07 ------------------------------------------------------------------------------- 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: 6.218 11.889 21.946 104.85 90.00 90.00 Niggli form: a.a = 38.66 b.b = 141.34 c.c = 481.62 b.c = -66.88 a.c = 0.00 a.b = 0.00 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.861 deg. ORTHORHOMBIC C-lattice R(int) = 0.587 [ 11547] Cell: 11.889 42.430 6.218 90.00 90.00 89.14 Volume: 3136.15 Matrix: 1.0000 0.0000 0.0000 1.0000 0.0000 2.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.060 [ 9754] Cell: 11.889 6.218 21.946 90.00 104.85 90.00 Volume: 1568.07 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option C: FOM = 0.861 deg. MONOCLINIC C-lattice R(int) = 0.574 [ 9926] Cell: 42.430 11.889 6.218 90.00 90.00 90.86 Volume: 3136.15 Matrix:-1.0000 0.0000 -2.0000 1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option D: FOM = 0.861 deg. MONOCLINIC C-lattice R(int) = 0.570 [ 10015] Cell: 11.889 42.430 6.218 90.00 90.00 89.14 Volume: 3136.15 Matrix:-1.0000 0.0000 0.0000 -1.0000 0.0000 -2.0000 0.0000 -1.0000 0.0000 Option B selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 6822 6838 6790 6839 10225 9099 9137 13653 N (int>3sigma) = 0 3400 3758 3700 3771 5429 4963 5028 7466 Mean intensity = 0.0 89.3 108.3 107.6 96.0 101.7 105.9 106.7 103.9 Mean int/sigma = 0.0 5.1 5.7 5.8 5.6 5.5 5.7 5.7 5.7 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.947 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 12 821 807 836 N I>3s 0 323 1 324 3.0 166.0 2.4 163.3 1.1 4.9 0.7 4.9 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/c # 14 centro 1 19410 0.060 9754 1.1 / 4.9 2.40 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C12H27O4N1 Formula weight = 249.35 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.056, non-H atomic volume = 23.1 and following cell contents and analysis: C 48.00 57.80 % H 108.00 10.91 % N 4.00 5.62 % O 16.00 25.67 % F(000) = 552.0 Mo-K(alpha) radiation Mu (mm-1) = 0.08 ------------------------------------------------------------------------------- File 07skc0019.ins set up as follows: TITL 07skc0019 in P2(1)/c CELL 0.71073 11.8885 6.2179 21.9459 90.000 104.852 90.000 ZERR 4.00 0.0005 0.0003 0.0009 0.000 0.002 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O UNIT 48 108 4 16 TEMP 0.02 TREF HKLF 4 END ------------------------------------------------------------------------------- File o7skc0019p21c.ins set up as follows: TITL o7skc0019p21c in P2(1)/c CELL 0.71073 11.8885 6.2179 21.9459 90.000 104.852 90.000 ZERR 4.00 0.0005 0.0003 0.0009 0.000 0.002 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O UNIT 48 108 4 16 TEMP 0.02 TREF HKLF 4 END ------------------------------------------------------------------------------- File 07skc0019p21c.ins set up as follows: TITL 07skc0019p21c in P2(1)/c CELL 0.71073 11.8885 6.2179 21.9459 90.000 104.852 90.000 ZERR 4.00 0.0005 0.0003 0.0009 0.000 0.002 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O UNIT 48 108 4 16 TEMP 0.02 TREF HKLF 4 END 13653 Reflections written to new reflection file 07skc0019p21c.hkl -------------------------------------------------------------------------------