++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 2007src0719 started at 18:12:44 on 13-JUN-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 9.318 15.156 18.965 90.00 99.59 90.00 32693 Reflections read from file 2007src0719.hkl; mean (I/sigma) = 9.90 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 16355 16322 16301 16328 24489 21775 21822 32693 N (int>3sigma) = 0 12008 11420 11720 11604 17574 15730 15786 23652 Mean intensity = 0.0 22.8 20.9 23.0 21.6 22.2 23.0 23.2 23.1 Mean int/sigma = 0.0 10.1 9.6 9.9 9.8 9.9 10.0 10.0 10.0 Lattice type: P chosen Volume: 2640.96 ------------------------------------------------------------------------------- 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: 9.318 15.156 18.965 90.00 99.59 90.00 Niggli form: a.a = 86.83 b.b = 229.70 c.c = 359.68 b.c = 0.00 a.c = -29.43 a.b = 0.00 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.038 [ 26407] Cell: 9.318 15.156 18.965 90.00 99.59 90.00 Volume: 2640.96 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 16355 16322 16301 16328 24489 21775 21822 32693 N (int>3sigma) = 0 12008 11420 11720 11604 17574 15730 15786 23652 Mean intensity = 0.0 22.8 20.9 23.0 21.6 22.2 23.0 23.2 23.1 Mean int/sigma = 0.0 10.1 9.6 9.9 9.8 9.9 10.0 10.0 10.0 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.973 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 29 752 765 759 N I>3s 0 325 319 8 0.2 33.4 32.9 0.2 0.5 7.5 7.4 0.6 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/n # 14 centro 1 19410 0.038 26407 0.6 / 7.4 1.49 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C32H31O2NB Formula weight = 472.39 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.188, non-H atomic volume = 18.3 and following cell contents and analysis: C 128.00 81.36 % H 124.00 6.61 % B 4.00 2.29 % N 4.00 2.97 % O 8.00 6.77 % F(000) = 1004.0 Mo-K(alpha) radiation Mu (mm-1) = 0.07 ------------------------------------------------------------------------------- File 2007src0719.ins set up as follows: TITL 2007src0719 in P2(1)/n CELL 0.71073 9.3182 15.1558 18.9653 90.000 99.587 90.000 ZERR 4.00 0.0001 0.0002 0.0002 0.000 0.001 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H B N O UNIT 128 124 4 4 8 TEMP 0.2 TREF HKLF 4 END -------------------------------------------------------------------------------