++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 2007src0218r started at 11:37:30 on 02-MAR-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 9.324 9.325 9.819 79.08 79.06 75.83 13485 Reflections read from file 2007src0218r.hkl; mean (I/sigma) = 8.96 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 6737 6761 6720 6782 10109 8959 8936 13485 N (int>3sigma) = 0 4870 4901 4861 4943 7316 6419 6434 9703 Mean intensity = 0.0 94.9 97.3 91.6 106.1 94.6 97.1 97.1 103.8 Mean int/sigma = 0.0 9.0 9.0 9.0 9.2 9.0 9.0 9.0 9.0 Lattice type: P chosen Volume: 803.48 ------------------------------------------------------------------------------- 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: 9.324 9.325 9.819 79.08 79.06 75.83 Niggli form: a.a = 86.93 b.b = 86.95 c.c = 96.42 b.c = 17.35 a.c = 17.38 a.b = 21.28 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.018 deg. MONOCLINIC C-lattice R(int) = 0.043 [ 11536] Cell: 14.712 11.460 9.819 89.99 103.91 89.99 Volume: 1606.96 Matrix:-1.0000 -1.0000 0.0000 1.0000 -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 6782 6782 0 6738 6782 8990 8966 13485 N (int>3sigma) = 0 4943 4943 0 4936 4943 6456 6475 9703 Mean intensity = 0.0 106.1 106.1 0.0 89.2 106.1 106.2 106.5 103.8 Mean int/sigma = 0.0 9.2 9.2 0.0 9.1 9.2 9.1 9.0 9.0 Crystal system M and Lattice type C selected Mean |E*E-1| = 1.012 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -c- N 371 N I>3s 324 301.6 13.1 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] C2 # 5 chiral 1 552 0.043 11536 0.0 / 9.0 8.92 [B] C2/m # 12 centro 1 310 0.043 11536 0.0 / 9.0 1.63 [C] Cm # 8 non-cen 1 32 0.043 11536 0.0 / 9.0 11.77 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C4H14N1O11B5 Formula weight = 306.21 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.266, non-H atomic volume = 19.1 and following cell contents and analysis: C 16.00 15.69 % H 56.00 4.61 % B 20.00 17.65 % N 4.00 4.58 % O 44.00 57.48 % F(000) = 632.0 Mo-K(alpha) radiation Mu (mm-1) = 0.12 ------------------------------------------------------------------------------- File c2.ins set up as follows: TITL c2 in C2 CELL 0.71073 14.7118 11.4599 9.8194 90.000 103.911 90.000 ZERR 4.00 0.0003 0.0003 0.0003 0.000 0.002 0.000 LATT -7 SYMM -X, Y, -Z SFAC C H B N O UNIT 16 56 20 4 44 TEMP 0.04 TREF HKLF 4 END 13485 Reflections written to new reflection file c2.hkl -------------------------------------------------------------------------------