++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 14:29:03 on 17-JAN-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 10.125 10.579 17.772 89.93 89.96 93.54 5854 Reflections read from file s92.hkl; mean (I/sigma) = 1.79 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 2914 2929 2913 2929 4378 3909 3906 5854 N (int>3sigma) = 0 586 597 595 545 889 818 822 1202 Mean intensity = 0.0 50.5 45.9 52.5 42.7 49.6 51.8 52.3 51.1 Mean int/sigma = 0.0 2.0 2.0 2.0 1.9 2.0 2.1 2.1 2.0 Lattice type: P chosen Volume: 1900.03 ------------------------------------------------------------------------------- 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: 10.125 10.579 17.772 90.07 90.04 93.54 Niggli form: a.a = 102.52 b.b = 111.92 c.c = 315.84 b.c = -0.24 a.c = -0.13 a.b = -6.62 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.087 deg. MONOCLINIC P-lattice R(int) = 0.206 [ 3387] Cell: 10.125 17.772 10.579 89.93 93.54 89.96 Volume: 1900.03 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) = 0.139 [ 1640] Cell: 10.125 10.579 17.772 90.07 90.04 93.54 Volume: 1900.03 Matrix:-1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 0.0000 0.0000 1.0000 Option A selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 2914 2913 2929 2929 4378 3909 3911 5854 N (int>3sigma) = 0 586 595 597 545 889 818 818 1202 Mean intensity = 0.0 50.5 52.5 45.9 42.7 49.6 51.8 48.2 51.1 Mean int/sigma = 0.0 2.0 2.0 2.0 1.9 2.0 2.1 2.0 2.0 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.839 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 13 128 119 123 N I>3s 0 1 24 25 4.3 5.7 60.6 58.5 0.4 0.5 2.1 2.0 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/c # 14 centro 4 19410 0.206 3387 0.5 / 2.0 8.07 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C44 H50 N2 O6 Formula weight = 702.86 Tentative Z (number of formula units/cell) = 2.0 giving rho = 1.229, non-H atomic volume = 18.3 and following cell contents and analysis: C 88.00 75.18 % H 100.00 7.17 % N 4.00 3.99 % O 12.00 13.66 % F(000) = 752.0 Mo-K(alpha) radiation Mu (mm-1) = 0.08 ------------------------------------------------------------------------------- File s93.ins set up as follows: TITL s93 in P2(1)/c CELL 0.71073 10.5790 17.7720 10.1254 90.000 93.545 90.000 ZERR 2.00 0.0021 0.0036 0.0020 0.000 0.030 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O UNIT 88 100 4 12 TREF HKLF 4 END 5854 Reflections written to new reflection file s93.hkl -------------------------------------------------------------------------------