++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 04src0333 started at 10:00:09 on 06-MAY-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 14.668 19.628 25.461 90.02 93.88 90.05 102552 Reflections read from file 04src0333.hkl; mean (I/sigma) = 7.56 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 51287 51267 51322 51288 76938 68293 68354 102552 N (int>3sigma) = 0 28131 28575 28746 28630 42726 38036 38041 57146 Mean intensity = 0.0 143.4 151.6 152.8 151.8 149.3 147.1 145.9 148.3 Mean int/sigma = 0.0 7.5 7.7 7.7 7.6 7.6 7.7 7.6 7.7 Lattice type: P chosen Volume: 7313.84 ------------------------------------------------------------------------------- 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: 14.668 19.628 25.461 90.02 93.88 90.05 Niggli form: a.a = 215.16 b.b = 385.27 c.c = 648.27 b.c = -0.16 a.c = -25.28 a.b = -0.27 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.058 deg. MONOCLINIC P-lattice R(int) = 0.063 [ 85184] Cell: 14.668 19.628 25.461 90.02 93.88 90.05 Volume: 7313.84 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) = 0.058 [ 71820] Cell: 14.668 19.628 25.461 90.02 93.88 90.05 Volume: 7313.84 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 51287 51267 51322 51288 76938 68293 68354 102552 N (int>3sigma) = 0 28131 28575 28746 28630 42726 38036 38041 57146 Mean intensity = 0.0 143.4 151.6 152.8 151.8 149.3 147.1 145.9 148.3 Mean int/sigma = 0.0 7.5 7.7 7.7 7.6 7.6 7.7 7.6 7.7 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.950 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 49 1880 1876 1904 N I>3s 0 740 5 737 1.8 257.6 3.4 254.1 0.4 6.9 0.5 6.8 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/c # 14 centro 1 19410 0.063 85184 0.5 / 6.8 1.62 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C72H66N36O32Cl8Fe4 Formula weight = 2454.61 Tentative Z (number of formula units/cell) = 3.0 giving rho = 1.672, non-H atomic volume = 16.0 and following cell contents and analysis: C 216.00 35.23 % H 198.00 2.71 % N 108.00 20.55 % O 96.00 20.86 % Cl 24.00 11.55 % Fe 12.00 9.10 % F(000) = 3738.0 Mo-K(alpha) radiation Mu (mm-1) = 0.90 ------------------------------------------------------------------------------- File 04src0333.ins set up as follows: TITL 04src0333 in P2(1)/c CELL 0.71073 14.6685 19.6282 25.4611 90.000 93.882 90.000 ZERR 3.00 0.0019 0.0028 0.0030 0.000 0.010 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O CL FE UNIT 216 198 108 96 24 12 TEMP 0.08 TREF HKLF 4 END -------------------------------------------------------------------------------