++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 04src0437 started at 09:14:38 on 04-JUN-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 15.574 12.402 23.024 90.00 109.10 89.99 43879 Reflections read from file 04src0437.hkl; mean (I/sigma) = 12.95 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 21929 21948 21913 21941 32895 29257 29261 43879 N (int>3sigma) = 0 17488 17451 17093 17511 26016 23507 23363 35064 Mean intensity = 0.0 216.1 212.2 205.8 212.2 211.4 207.6 207.2 209.5 Mean int/sigma = 0.0 13.0 13.0 12.7 13.0 12.9 13.0 12.9 13.0 Lattice type: P chosen Volume: 4202.08 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 -1.0000 0.0000 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 Unitcell: 12.402 15.574 23.024 109.10 90.00 90.01 Niggli form: a.a = 153.81 b.b = 242.55 c.c = 530.09 b.c = -117.34 a.c = -0.02 a.b = -0.02 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.665 deg. ORTHORHOMBIC C-lattice R(int) = 0.530 [ 38530] Cell: 15.574 43.515 12.402 90.01 90.01 89.34 Volume: 8404.16 Matrix: 1.0000 0.0000 0.0000 1.0000 0.0000 2.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.010 deg. MONOCLINIC P-lattice R(int) = 0.032 [ 33765] Cell: 15.574 12.402 23.024 90.00 109.10 89.99 Volume: 4202.08 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option C: FOM = 0.665 deg. MONOCLINIC C-lattice R(int) = 0.509 [ 33841] Cell: 43.515 15.574 12.402 89.99 90.01 90.66 Volume: 8404.16 Matrix: 1.0000 0.0000 2.0000 -1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option D: FOM = 0.665 deg. MONOCLINIC C-lattice R(int) = 0.524 [ 34370] Cell: 15.574 43.515 12.402 90.01 90.01 89.34 Volume: 8404.16 Matrix: 1.0000 0.0000 0.0000 1.0000 0.0000 2.0000 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 21929 21948 21913 21941 32895 29257 29261 43879 N (int>3sigma) = 0 17488 17451 17093 17511 26016 23507 23363 35064 Mean intensity = 0.0 216.1 212.2 205.8 212.2 211.4 207.6 207.2 209.5 Mean int/sigma = 0.0 13.0 13.0 12.7 13.0 12.9 13.0 12.9 13.0 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.938 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 21 1368 1370 1358 N I>3s 0 3 608 609 1.1 1.4 273.6 276.0 0.7 0.6 8.6 8.7 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/c # 14 centro 4 19410 0.032 33765 0.7 / 8.6 1.34 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C30H52Cl2Fe1P2Pd2 Formula weight = 814.21 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.287, non-H atomic volume = 28.4 and following cell contents and analysis: C 120.00 44.25 % H 208.00 6.44 % P 8.00 7.61 % Cl 8.00 8.71 % Fe 4.00 6.86 % Pd 8.00 26.14 % F(000) = 1656.0 Mo-K(alpha) radiation Mu (mm-1) = 1.41 ------------------------------------------------------------------------------- File s93.ins set up as follows: TITL s93 in P2(1)/c CELL 0.71073 23.0236 12.4019 15.5740 90.000 109.102 90.000 ZERR 4.00 0.0022 0.0006 0.0010 0.000 0.007 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H P CL FE PD UNIT 120 208 8 8 4 8 TEMP 0.02 TREF HKLF 4 END 43879 Reflections written to new reflection file s93.hkl -------------------------------------------------------------------------------