++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 13:51:37 on 11-FEB-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 18.449 9.660 30.586 90.00 94.60 90.00 12864 Reflections read from file s92.hkl; mean (I/sigma) = 2.47 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 6421 6425 6454 6424 9650 8556 8592 12864 N (int>3sigma) = 0 1717 1714 1563 1675 2497 2255 2249 3382 Mean intensity = 0.0 23.8 24.0 24.4 25.7 24.1 23.3 23.8 24.0 Mean int/sigma = 0.0 2.6 2.6 2.5 2.6 2.6 2.6 2.6 2.6 Lattice type: P chosen Volume: 5433.15 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 -1.0000 0.0000 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 Unitcell: 9.660 18.449 30.586 94.60 90.00 90.00 Niggli form: a.a = 93.31 b.b = 340.37 c.c = 935.50 b.c = -45.25 a.c = 0.00 a.b = 0.00 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.141 [ 6130] Cell: 18.449 9.660 30.586 90.00 94.60 90.00 Volume: 5433.15 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. TRICLINIC P-lattice R(int) = 0.124 [ 3528] Cell: 9.660 18.449 30.586 85.40 90.00 90.00 Volume: 5433.15 Matrix: 0.0000 1.0000 0.0000 -1.0000 0.0000 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 6421 6425 6454 6424 9650 8556 8592 12864 N (int>3sigma) = 0 1717 1714 1563 1675 2497 2255 2249 3382 Mean intensity = 0.0 23.8 24.0 24.4 25.7 24.1 23.3 23.8 24.0 Mean int/sigma = 0.0 2.6 2.6 2.5 2.6 2.6 2.6 2.6 2.6 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.811 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 2 706 709 711 N I>3s 0 10 197 195 2.1 2.7 25.5 25.2 1.0 0.8 3.1 3.1 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2/c # 13 centro 4 292 0.141 6130 0.8 / 2.6 8.36 [B] Pc # 7 non-cen 4 226 0.141 6130 0.8 / 2.6 6.57 [C] P2(1)/c # 14 centro 4 19410 0.141 6130 0.8 / 2.6 8.03 Option [C] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C42H86N18P6 Formula weight = 1029.11 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.258, non-H atomic volume = 20.6 and following cell contents and analysis: C 168.00 49.02 % H 344.00 8.42 % N 72.00 24.50 % P 24.00 18.06 % F(000) = 2216.0 Mo-K(alpha) radiation Mu (mm-1) = 0.25 ------------------------------------------------------------------------------- File 1.ins set up as follows: TITL 1 in P2(1)/c CELL 0.71073 30.5860 9.6595 18.4491 90.000 94.599 90.000 ZERR 4.00 0.0097 0.0023 0.0052 0.000 0.010 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N P UNIT 168 344 72 24 TREF HKLF 4 END -------------------------------------------------------------------------------