++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 15:54:05 on 08-AUG-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 7.133 20.699 7.146 90.00 116.17 90.00 10271 Reflections read from file s92.hkl; mean (I/sigma) = 13.27 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 5142 5150 5120 5141 7706 6806 6842 10271 N (int>3sigma) = 0 3208 4189 4107 4106 5752 5498 5516 8292 Mean intensity = 0.0 49.3 188.8 188.1 186.3 142.0 193.8 192.8 191.5 Mean int/sigma = 0.0 8.3 13.4 13.2 13.1 11.6 13.3 13.3 13.3 Lattice type: P chosen Volume: 946.81 ------------------------------------------------------------------------------- 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: 7.133 7.146 20.699 90.00 90.00 116.17 Niggli form: a.a = 50.88 b.b = 51.06 c.c = 428.45 b.c = 0.00 a.c = 0.00 a.b = -22.48 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.114 deg. ORTHORHOMBIC C-lattice R(int) = 0.545 [ 9017] Cell: 7.548 12.120 20.699 90.00 90.00 89.89 Volume: 1893.61 Matrix: 1.0000 0.0000 1.0000 -1.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.049 [ 8036] Cell: 7.133 20.699 7.146 90.00 116.17 90.00 Volume: 946.81 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option C: FOM = 0.114 deg. MONOCLINIC C-lattice R(int) = 0.537 [ 8004] Cell: 7.548 12.120 20.699 90.00 90.00 89.89 Volume: 1893.61 Matrix:-1.0000 0.0000 -1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option D: FOM = 0.114 deg. MONOCLINIC C-lattice R(int) = 0.536 [ 7938] Cell: 12.120 7.548 20.699 90.00 90.00 90.11 Volume: 1893.61 Matrix: 1.0000 0.0000 -1.0000 1.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 Option B selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 5142 5150 5120 5141 7706 6806 6842 10271 N (int>3sigma) = 0 3208 4189 4107 4106 5752 5498 5516 8292 Mean intensity = 0.0 49.3 188.8 188.1 186.3 142.0 193.8 192.8 191.5 Mean int/sigma = 0.0 8.3 13.4 13.2 13.1 11.6 13.3 13.3 13.3 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.881 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 42 137 138 137 N I>3s 2 65 2 65 0.7 268.7 1.0 268.8 0.8 9.4 0.7 9.4 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/c # 14 centro 1 19410 0.049 8036 0.8 / 9.4 1.91 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C12 H16 N4 O6 Pd1 Cl2 Formula weight = 489.59 Tentative Z (number of formula units/cell) = 2.0 giving rho = 1.717, non-H atomic volume = 18.9 and following cell contents and analysis: C 24.00 29.44 % H 32.00 3.29 % N 8.00 11.45 % O 12.00 19.61 % Cl 4.00 14.48 % Pd 2.00 21.73 % F(000) = 488.0 Mo-K(alpha) radiation Mu (mm-1) = 1.30 ------------------------------------------------------------------------------- File s92.ins set up as follows: TITL s92 in P2(1)/c CELL 0.71073 7.1328 20.6990 7.1455 90.000 116.173 90.000 ZERR 2.00 0.0014 0.0041 0.0014 0.000 0.030 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O CL PD UNIT 24 32 8 12 4 2 TREF HKLF 4 END -------------------------------------------------------------------------------