++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 2005src1310 started at 13:26:46 on 08-FEB-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 17.969 20.827 20.857 69.21 83.49 83.54 85014 Reflections read from file 2005src1310.hkl; mean (I/sigma) = 4.88 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 42512 42502 42494 42489 63754 56697 56746 85014 N (int>3sigma) = 0 20342 19928 20024 20033 30147 26770 26806 40106 Mean intensity = 0.0 81.6 80.3 81.2 81.4 81.0 81.6 83.0 80.6 Mean int/sigma = 0.0 5.0 5.0 5.0 5.0 5.0 5.0 5.0 5.0 Lattice type: P chosen Volume: 7228.33 ------------------------------------------------------------------------------- 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: 17.969 20.827 20.857 69.21 83.49 83.54 Niggli form: a.a = 322.90 b.b = 433.77 c.c = 435.02 b.c = 154.22 a.c = 42.52 a.b = 42.10 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.099 deg. MONOCLINIC C-lattice R(int) = 0.082 [ 68073] Cell: 34.311 23.672 17.969 90.06 97.89 89.91 Volume: 14456.66 Matrix: 0.0000 -1.0000 -1.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.000 deg. TRICLINIC P-lattice R(int) = 0.066 [ 54731] Cell: 17.969 20.827 20.857 69.21 83.49 83.54 Volume: 7228.33 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 42489 42489 0 42711 42489 56661 56668 85014 N (int>3sigma) = 0 20033 20033 0 18815 20033 26817 26700 40106 Mean intensity = 0.0 81.4 81.4 0.0 40.4 81.4 79.8 80.2 80.6 Mean int/sigma = 0.0 5.0 5.0 0.0 4.2 5.0 5.0 5.0 5.0 Crystal system M and Lattice type C selected Mean |E*E-1| = 1.082 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -c- N 1299 N I>3s 453 60.1 3.5 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] C2 # 5 chiral 1 552 0.082 68073 0.0 / 3.5 15.00 [B] C2/m # 12 centro 1 310 0.082 68073 0.0 / 3.5 4.47 [C] Cm # 8 non-cen 1 32 0.082 68073 0.0 / 3.5 17.85 Option [B] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C38H22N10S4Co1Ni1 Formula weight = 864.54 Tentative Z (number of formula units/cell) = 16.0 giving rho = 1.589, non-H atomic volume = 16.7 and following cell contents and analysis: C 608.00 52.79 % H 352.00 2.57 % N 160.00 16.21 % S 64.00 14.83 % Co 16.00 6.82 % Ni 16.00 6.79 % F(000) = 7024.0 Mo-K(alpha) radiation Mu (mm-1) = 1.26 ------------------------------------------------------------------------------- File s94.ins set up as follows: TITL s94 in C2/m CELL 0.71073 34.3107 23.6718 17.9695 90.000 97.888 90.000 ZERR 16.00 0.0019 0.0019 0.0012 0.000 0.004 0.000 LATT 7 SYMM -X, Y, -Z SFAC C H N S CO NI UNIT 608 352 160 64 16 16 TEMP 0.08 TREF HKLF 4 END 85014 Reflections written to new reflection file s94.hkl -------------------------------------------------------------------------------