++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 04src1119 started at 09:23:21 on 03-DEC-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 20.455 25.332 25.134 89.95 111.54 90.05 170588 Reflections read from file 04src1119.hkl; mean (I/sigma) = 5.96 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 85350 85297 85285 85587 127966 113780 113753 170588 N (int>3sigma) = 0 45585 45041 44792 44730 67709 60297 60495 90621 Mean intensity = 0.0 143.2 145.1 144.1 119.5 144.1 145.9 144.0 144.2 Mean int/sigma = 0.0 6.1 6.0 6.0 5.9 6.0 6.0 6.0 6.0 Lattice type: P chosen Volume: 12113.80 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): -1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 0.0000 1.0000 0.0000 Unitcell: 20.455 25.134 25.332 89.95 89.95 68.46 Niggli form: a.a = 418.40 b.b = 631.70 c.c = 641.71 b.c = 0.52 a.c = 0.48 a.b = 188.75 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.061 deg. MONOCLINIC P-lattice R(int) = 0.078 [141924] Cell: 20.455 25.332 25.134 89.95 111.54 90.05 Volume: 12113.80 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) = 0.067 [115391] Cell: 20.455 25.134 25.332 89.95 89.95 68.46 Volume: 12113.80 Matrix:-1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 0.0000 1.0000 0.0000 Option A selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 85350 85297 85285 85587 127966 113780 113753 170588 N (int>3sigma) = 0 45585 45041 44792 44730 67709 60297 60495 90621 Mean intensity = 0.0 143.2 145.1 144.1 119.5 144.1 145.9 144.0 144.2 Mean int/sigma = 0.0 6.1 6.0 6.0 5.9 6.0 6.0 6.0 6.0 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.922 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 67 2124 2090 2120 N I>3s 13 146 910 808 18.8 11.0 177.4 169.3 1.8 1.0 5.5 5.1 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/c # 14 centro 4 19410 0.078141924 1.8 / 5.1 3.09 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C72H64N36O32Cl8Mn4 Formula weight = 2448.95 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.343, non-H atomic volume = 19.9 and following cell contents and analysis: C 288.00 35.31 % H 256.00 2.63 % N 144.00 20.59 % O 128.00 20.91 % Cl 32.00 11.58 % Mn 16.00 8.97 % F(000) = 4960.0 Mo-K(alpha) radiation Mu (mm-1) = 0.66 ------------------------------------------------------------------------------- File s93.ins set up as follows: TITL s93 in P2(1)/c CELL 0.71073 25.1337 25.3319 20.4549 90.000 111.540 90.000 ZERR 4.00 0.0061 0.0089 0.0089 0.000 0.014 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O CL MN UNIT 288 256 144 128 32 16 TEMP 0.08 TREF HKLF 4 END 170588 Reflections written to new reflection file s93.hkl -------------------------------------------------------------------------------