++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 12:53:37 on 14-DEC-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 26.798 6.091 12.637 90.00 108.97 90.00 5588 Reflections read from file s92.hkl; mean (I/sigma) = 5.34 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 2797 2797 0 2805 2797 3731 3708 5588 N (int>3sigma) = 0 1012 1012 0 1353 1012 1885 1889 2846 Mean intensity = 0.0 25.1 25.1 0.0 51.3 25.1 54.2 54.2 54.3 Mean int/sigma = 0.0 3.9 3.9 0.0 5.2 3.9 5.4 5.4 5.5 Lattice type: C chosen Volume: 1950.66 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 -1.0000 0.0000 0.0000 0.0000 -1.0000 0.5000 -0.5000 0.0000 Unitcell: 6.091 12.637 13.741 71.52 77.20 90.00 Niggli form: a.a = 37.10 b.b = 159.70 c.c = 188.81 b.c = 55.04 a.c = 18.55 a.b = 0.00 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC C-lattice R(int) = 0.064 [ 3300] Cell: 26.798 6.091 12.637 90.00 108.97 90.00 Volume: 1950.66 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. MONOCLINIC I-lattice R(int) = 0.064 [ 3300] Cell: 12.637 6.091 25.646 90.00 98.81 90.00 Volume: 1950.66 Matrix: 0.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 0.0000 1.0000 Option A selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 2797 2797 0 2805 2797 3731 3708 5588 N (int>3sigma) = 0 1012 1012 0 1353 1012 1885 1889 2846 Mean intensity = 0.0 25.1 25.1 0.0 51.3 25.1 54.2 54.2 54.3 Mean int/sigma = 0.0 3.9 3.9 0.0 5.2 3.9 5.4 5.4 5.5 Crystal system M and Lattice type C selected Mean |E*E-1| = 0.914 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -c- N 302 N I>3s 1 2.1 0.6 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] C2/c # 15 centro 1 3696 0.064 3300 0.6 / 5.5 2.36 [B] Cc # 9 non-cen 1 566 0.064 3300 0.6 / 5.5 5.40 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C7 H9 N2 B1 Br2 Formula weight = 291.79 Tentative Z (number of formula units/cell) = 8.0 giving rho = 1.987, non-H atomic volume = 20.3 and following cell contents and analysis: C 56.00 28.81 % H 72.00 3.11 % B 8.00 3.70 % N 16.00 9.60 % Br 16.00 54.77 % F(000) = 1120.0 Mo-K(alpha) radiation Mu (mm-1) = 8.26 ------------------------------------------------------------------------------- File s92.ins set up as follows: TITL s92 in C2/c CELL 0.71073 26.7983 6.0907 12.6373 90.000 108.968 90.000 ZERR 8.00 0.0023 0.0006 0.0015 0.000 0.003 0.000 LATT 7 SYMM -X, Y, 0.5-Z SFAC C H B N BR UNIT 56 72 8 16 16 TREF HKLF 4 END -------------------------------------------------------------------------------