++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 04src1114 started at 17:17:00 on 02-DEC-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 11.019 13.230 16.983 110.04 93.94 109.79 42164 Reflections read from file 04src1114.hkl; mean (I/sigma) = 7.64 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 21092 21083 21069 21024 31622 28106 28106 42164 N (int>3sigma) = 0 13859 13875 14002 13969 20868 18761 18464 27920 Mean intensity = 0.0 20.1 18.9 20.5 20.1 19.9 20.0 20.5 20.1 Mean int/sigma = 0.0 7.7 7.7 7.7 7.7 7.7 7.7 7.7 7.7 Lattice type: P chosen Volume: 2140.28 ------------------------------------------------------------------------------- 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: 11.019 13.230 16.983 110.04 93.94 109.79 Niggli form: a.a = 121.43 b.b = 175.02 c.c = 288.44 b.c = -76.99 a.c = -12.86 a.b = -49.36 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. TRICLINIC P-lattice R(int) = 0.054 [ 32288] Cell: 11.019 13.230 16.983 110.04 93.94 109.79 Volume: 2140.28 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 21092 21083 21069 21024 31622 28106 28106 42164 N (int>3sigma) = 0 13859 13875 14002 13969 20868 18761 18464 27920 Mean intensity = 0.0 20.1 18.9 20.5 20.1 19.9 20.0 20.5 20.1 Mean int/sigma = 0.0 7.7 7.7 7.7 7.7 7.7 7.7 7.7 7.7 Crystal system A and Lattice type P selected Mean |E*E-1| = 0.951 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absences not required for triclinic Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P-1 # 2 centro 1 8646 0.054 32288 0.0 / 7.7 1.34 [B] P1 # 1 chiral 1 700 0.054 32288 0.0 / 7.7 6.06 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C102H84N42O32Cl8Mn4 Formula weight = 2913.47 Tentative Z (number of formula units/cell) = 1.0 giving rho = 2.260, non-H atomic volume = 11.4 and following cell contents and analysis: C 102.00 42.05 % H 84.00 2.91 % N 42.00 20.20 % O 32.00 17.57 % Cl 8.00 9.73 % Mn 4.00 7.54 % F(000) = 1482.0 Mo-K(alpha) radiation Mu (mm-1) = 0.96 ------------------------------------------------------------------------------- File 04src1114.ins set up as follows: TITL 04src1114 in P-1 CELL 0.71073 11.0194 13.2296 16.9834 110.038 93.940 109.791 ZERR 1.00 0.0006 0.0021 0.0040 0.011 0.010 0.012 LATT 1 SFAC C H N O CL MN UNIT 102 84 42 32 8 4 TEMP 0.04 TREF HKLF 4 END -------------------------------------------------------------------------------