++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 2005src0328 started at 14:16:05 on 19-MAY-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 7.747 15.519 25.745 89.96 89.98 89.96 14544 Reflections read from file 2005src0328.hkl; mean (I/sigma) = 2.83 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 7286 7266 7272 7265 10912 9690 9709 14544 N (int>3sigma) = 0 2382 2307 2339 2383 3514 3202 3179 4805 Mean intensity = 0.0 164.0 145.1 155.3 147.5 154.8 157.8 159.4 159.9 Mean int/sigma = 0.0 3.0 2.9 2.9 2.9 2.9 3.0 2.9 3.0 Lattice type: P chosen Volume: 3095.28 ------------------------------------------------------------------------------- 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: 7.747 15.519 25.745 89.96 89.98 89.96 Niggli form: a.a = 60.02 b.b = 240.85 c.c = 662.80 b.c = 0.29 a.c = 0.06 a.b = 0.08 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.057 deg. ORTHORHOMBIC P-lattice R(int) = 0.171 [ 10694] Cell: 7.747 15.519 25.745 89.96 89.98 89.96 Volume: 3095.28 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.043 deg. MONOCLINIC P-lattice R(int) = 0.142 [ 7625] Cell: 15.519 7.747 25.745 90.02 90.04 89.96 Volume: 3095.28 Matrix: 0.0000 1.0000 0.0000 1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option C: FOM = 0.045 deg. MONOCLINIC P-lattice R(int) = 0.144 [ 8020] Cell: 7.747 25.745 15.519 90.04 90.04 89.98 Volume: 3095.28 Matrix: 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option D: FOM = 0.057 deg. MONOCLINIC P-lattice R(int) = 0.152 [ 8436] Cell: 7.747 15.519 25.745 90.04 90.02 89.96 Volume: 3095.28 Matrix:-1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option E: FOM = 0.000 deg. TRICLINIC P-lattice R(int) = 0.101 [ 4226] Cell: 7.747 15.519 25.745 89.96 89.98 89.96 Volume: 3095.28 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 Option E selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 7286 7266 7272 7265 10912 9690 9709 14544 N (int>3sigma) = 0 2382 2307 2339 2383 3514 3202 3179 4805 Mean intensity = 0.0 164.0 145.1 155.3 147.5 154.8 157.8 159.4 159.9 Mean int/sigma = 0.0 3.0 2.9 2.9 2.9 2.9 3.0 2.9 3.0 Crystal system A and Lattice type P selected Mean |E*E-1| = 0.923 [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 0.101 4226 0.0 / 3.0 3.60 [B] P1 # 1 chiral 1 700 0.101 4226 0.0 / 3.0 7.04 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C16H24N2Ru1 Formula weight = 345.44 Tentative Z (number of formula units/cell) = 8.0 giving rho = 1.483, non-H atomic volume = 20.4 and following cell contents and analysis: C 128.00 55.63 % H 192.00 7.00 % N 16.00 8.11 % Ru 8.00 29.26 % F(000) = 1424.0 Mo-K(alpha) radiation Mu (mm-1) = 1.00 ------------------------------------------------------------------------------- File s93.ins set up as follows: TITL s93 in P-1 CELL 0.71073 7.7470 15.5194 25.7449 89.959 89.982 89.961 ZERR 8.00 0.0089 0.0179 0.0081 0.072 0.057 0.079 LATT 1 SFAC C H N RU UNIT 128 192 16 8 TEMP 0.02 TREF HKLF 4 END 14544 Reflections written to new reflection file s93.hkl -------------------------------------------------------------------------------