++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 14:06:39 on 05-FEB-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 7.228 9.246 33.461 89.92 89.96 90.01 7443 Reflections read from file s92.hkl; mean (I/sigma) = 8.35 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 3718 3719 3749 0 5593 4980 4969 7443 N (int>3sigma) = 0 2568 2618 2480 0 3833 3498 3480 5226 Mean intensity = 0.0 171.8 171.4 154.0 0.0 165.7 166.9 164.7 168.2 Mean int/sigma = 0.0 8.4 8.5 8.0 0.0 8.3 8.4 8.4 8.4 Lattice type: I chosen Volume: 2236.43 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 -0.5000 -0.5000 0.5000 Unitcell: 7.228 9.246 17.721 105.05 101.72 90.01 Niggli form: a.a = 52.25 b.b = 85.49 c.c = 314.04 b.c = -42.53 a.c = -26.03 a.b = -0.02 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.087 deg. ORTHORHOMBIC I-lattice R(int) = 0.080 [ 5964] Cell: 7.228 9.246 33.461 89.92 89.96 90.01 Volume: 2236.43 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.045 deg. MONOCLINIC C-lattice R(int) = 0.070 [ 4713] Cell: 34.703 7.228 9.246 90.01 105.38 89.96 Volume: 2236.43 Matrix: 0.0000 -1.0000 1.0000 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option C: FOM = 0.045 deg. MONOCLINIC I-lattice R(int) = 0.070 [ 4713] Cell: 9.246 7.228 33.461 89.96 90.08 89.99 Volume: 2236.43 Matrix: 0.0000 -1.0000 0.0000 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option D: FOM = 0.077 deg. MONOCLINIC C-lattice R(int) = 0.076 [ 4812] Cell: 34.228 9.246 7.228 89.99 102.15 90.08 Volume: 2236.43 Matrix:-1.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option E: FOM = 0.077 deg. MONOCLINIC I-lattice R(int) = 0.076 [ 4812] Cell: 7.228 9.246 33.461 90.08 90.04 90.01 Volume: 2236.43 Matrix:-1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option F: FOM = 0.087 deg. MONOCLINIC C-lattice R(int) = 0.072 [ 4956] Cell: 11.735 33.461 7.228 90.04 128.01 89.91 Volume: 2236.43 Matrix:-1.0000 -1.0000 0.0000 0.0000 0.0000 -1.0000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option G: FOM = 0.087 deg. MONOCLINIC I-lattice R(int) = 0.072 [ 4956] Cell: 7.228 33.461 9.246 89.92 90.01 89.96 Volume: 2236.43 Matrix:-1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 Option A selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 3718 3719 3749 0 5593 4980 4969 7443 N (int>3sigma) = 0 2568 2618 2480 0 3833 3498 3480 5226 Mean intensity = 0.0 171.8 171.4 154.0 0.0 165.7 166.9 164.7 168.2 Mean int/sigma = 0.0 8.4 8.5 8.0 0.0 8.3 8.4 8.4 8.4 Crystal system O and Lattice type I selected Mean |E*E-1| = 0.846 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: b-- c-- -c- -a- --a --b N 303 303 311 311 68 68 N I>3s 195 195 6 6 0 0 125.0 125.0 1.6 1.6 1.9 1.9 6.9 6.9 0.6 0.6 0.5 0.5 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] Iba2 # 45 non-cen 3 54 0.080 5964 0.6 / 6.9 4.61 [B] Ibam # 72 centro 3 35 0.080 5964 0.6 / 6.9 5.84 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C14H13NO Formula weight = 211.25 Tentative Z (number of formula units/cell) = 8.0 giving rho = 1.255, non-H atomic volume = 17.5 and following cell contents and analysis: C 112.00 79.59 % H 104.00 6.20 % N 8.00 6.63 % O 8.00 7.57 % F(000) = 896.0 Mo-K(alpha) radiation Mu (mm-1) = 0.08 ------------------------------------------------------------------------------- File 1.ins set up as follows: TITL 1 in Iba2 CELL 0.71073 9.2463 33.4610 7.2285 90.000 90.000 90.000 ZERR 8.00 0.0018 0.0067 0.0014 0.000 0.000 0.000 LATT -2 SYMM -X, -Y, Z SYMM 0.5+X, 0.5-Y, Z SYMM 0.5-X, 0.5+Y, Z SFAC C H N O UNIT 112 104 8 8 TREF HKLF 4 END -------------------------------------------------------------------------------