++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 04src0553 started at 16:20:16 on 09-JUL-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 16.812 19.229 22.968 90.00 89.98 89.99 45408 Reflections read from file 04src0553.hkl; mean (I/sigma) = 10.69 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 22703 22706 22763 22702 34086 30293 30278 45408 N (int>3sigma) = 0 14905 15127 15086 15299 22559 20486 20474 30591 Mean intensity = 0.0 290.6 289.2 285.0 290.2 288.2 283.6 284.7 289.0 Mean int/sigma = 0.0 10.6 10.7 10.7 10.8 10.7 10.8 10.8 10.8 Lattice type: P chosen Volume: 7425.34 ------------------------------------------------------------------------------- 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: 16.812 19.229 22.968 90.00 89.98 89.99 Niggli form: a.a = 282.65 b.b = 369.77 c.c = 527.55 b.c = 0.01 a.c = 0.13 a.b = 0.05 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.021 deg. ORTHORHOMBIC P-lattice R(int) = 0.038 [ 36156] Cell: 16.812 19.229 22.968 90.00 89.98 89.99 Volume: 7425.34 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 22703 22706 22763 22702 34086 30293 30278 45408 N (int>3sigma) = 0 14905 15127 15086 15299 22559 20486 20474 30591 Mean intensity = 0.0 290.6 289.2 285.0 290.2 288.2 283.6 284.7 289.0 Mean int/sigma = 0.0 10.6 10.7 10.7 10.8 10.7 10.8 10.8 10.8 Crystal system O and Lattice type P selected Mean |E*E-1| = 1.031 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: b-- c-- n-- 21-- -c- -a- -n- -21- --a --b --n --21 N 883 870 869 17 585 582 585 20 635 640 639 18 N I>3s 1 320 321 0 3 221 222 0 2 243 241 0 3.0 358.8 359.1 0.9 2.6 341.0 339.4 3.0 2.6 330.2 330.5 1.7 0.4 7.8 7.8 0.3 0.4 7.6 7.6 0.4 0.5 8.3 8.2 0.3 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] Pbca # 61 centro 1 2293 0.038 36156 0.5 / 7.6 1.84 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C37H58ClFeO4P2Rh Formula weight = 822.98 Tentative Z (number of formula units/cell) = 8.0 giving rho = 1.472, non-H atomic volume = 20.2 and following cell contents and analysis: C 296.00 53.99 % H 464.00 7.10 % O 32.00 7.78 % P 16.00 7.53 % Cl 8.00 4.31 % Fe 8.00 6.79 % Rh 8.00 12.50 % F(000) = 3440.0 Mo-K(alpha) radiation Mu (mm-1) = 1.03 ------------------------------------------------------------------------------- File 04src0553.ins set up as follows: TITL 04src0553 in Pbca CELL 0.71073 16.8121 19.2293 22.9684 90.000 90.000 90.000 ZERR 8.00 0.0012 0.0024 0.0027 0.000 0.000 0.000 LATT 1 SYMM 0.5-X, -Y, 0.5+Z SYMM -X, 0.5+Y, 0.5-Z SYMM 0.5+X, 0.5-Y, -Z SFAC C H O P CL FE RH UNIT 296 464 32 16 8 8 8 TEMP 0.25 TREF HKLF 4 END -------------------------------------------------------------------------------