++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 06skc0073 started at 11:14:57 on 23-NOV-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 8.643 6.071 18.947 90.00 102.76 90.00 15359 Reflections read from file 06skc0073.hkl; mean (I/sigma) = 3.10 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 7720 7670 7724 7702 11557 10249 10231 15359 N (int>3sigma) = 0 2709 2517 2720 2687 3973 3654 3578 5493 Mean intensity = 0.0 170.1 157.2 189.4 155.1 172.3 183.5 178.1 176.9 Mean int/sigma = 0.0 3.2 2.9 3.3 3.1 3.1 3.2 3.2 3.2 Lattice type: P chosen Volume: 969.63 ------------------------------------------------------------------------------- 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: 6.071 8.643 18.947 102.76 90.00 90.00 Niggli form: a.a = 36.86 b.b = 74.69 c.c = 358.98 b.c = -36.18 a.c = 0.00 a.b = 0.00 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.419 deg. ORTHORHOMBIC C-lattice R(int) = 0.592 [ 14030] Cell: 8.643 36.958 6.071 90.00 90.00 89.58 Volume: 1939.26 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) = 0.145 [ 12913] Cell: 8.643 6.071 18.947 90.00 102.76 90.00 Volume: 969.63 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option C: FOM = 0.419 deg. MONOCLINIC C-lattice R(int) = 0.579 [ 12969] Cell: 36.958 8.643 6.071 90.00 90.00 90.42 Volume: 1939.26 Matrix:-1.0000 0.0000 -2.0000 1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option D: FOM = 0.419 deg. MONOCLINIC C-lattice R(int) = 0.579 [ 13070] Cell: 8.643 36.958 6.071 90.00 90.00 89.58 Volume: 1939.26 Matrix:-1.0000 0.0000 0.0000 -1.0000 0.0000 -2.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option E: FOM = 0.000 deg. TRICLINIC P-lattice R(int) = 0.133 [ 10933] Cell: 6.071 8.643 18.947 77.24 90.00 90.00 Volume: 969.63 Matrix: 0.0000 1.0000 0.0000 -1.0000 0.0000 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 7720 7670 7724 7702 11557 10249 10231 15359 N (int>3sigma) = 0 2709 2517 2720 2687 3973 3654 3578 5493 Mean intensity = 0.0 170.1 157.2 189.4 155.1 172.3 183.5 178.1 176.9 Mean int/sigma = 0.0 3.2 2.9 3.3 3.1 3.1 3.2 3.2 3.2 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.923 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 16 727 722 727 N I>3s 0 218 220 2 11.0 199.3 200.5 9.7 0.6 3.1 3.1 0.5 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/n # 14 centro 1 19410 0.145 12913 0.6 / 3.1 4.07 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C7H16O4N2 Formula weight = 192.22 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.317, non-H atomic volume = 18.6 and following cell contents and analysis: C 28.00 43.74 % H 64.00 8.39 % N 8.00 14.58 % O 16.00 33.30 % F(000) = 416.0 Mo-K(alpha) radiation Mu (mm-1) = 0.11 ------------------------------------------------------------------------------- File 06skc0073p21n.ins set up as follows: TITL 06skc0073p21n in P2(1)/n CELL 0.71073 8.6426 6.0715 18.9467 90.000 102.765 90.000 ZERR 4.00 0.0005 0.0005 0.0014 0.000 0.005 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N O UNIT 28 64 8 16 TEMP 0.03 TREF HKLF 4 END 15359 Reflections written to new reflection file 06skc0073p21n.hkl -------------------------------------------------------------------------------