++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 2005sjc0007 started at 19:30:00 on 17-APR-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 8.848 10.644 13.480 89.99 89.99 89.98 16478 Reflections read from file 2005sjc0007.hkl; mean (I/sigma) = 9.84 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 8300 8230 8248 8228 12389 10976 10984 16478 N (int>3sigma) = 0 6113 6653 6402 6440 9584 8802 8805 13203 Mean intensity = 0.0 122.8 325.8 314.7 377.6 254.1 369.0 373.7 369.6 Mean int/sigma = 0.0 8.0 9.9 9.4 9.8 9.1 9.9 9.9 9.9 Lattice type: P chosen Volume: 1269.57 ------------------------------------------------------------------------------- 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: 8.848 10.644 13.480 89.99 89.99 89.98 Niggli form: a.a = 78.29 b.b = 113.30 c.c = 181.72 b.c = 0.04 a.c = 0.03 a.b = 0.04 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.028 deg. ORTHORHOMBIC P-lattice R(int) = 0.043 [ 14796] Cell: 8.848 10.644 13.480 89.99 89.99 89.98 Volume: 1269.57 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 8300 8230 8248 8228 12389 10976 10984 16478 N (int>3sigma) = 0 6113 6653 6402 6440 9584 8802 8805 13203 Mean intensity = 0.0 122.8 325.8 314.7 377.6 254.1 369.0 373.7 369.6 Mean int/sigma = 0.0 8.0 9.9 9.4 9.8 9.1 9.9 9.9 9.9 Crystal system O and Lattice type P selected Mean |E*E-1| = 0.886 [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 506 500 512 13 432 444 428 19 411 407 394 19 N I>3s 415 411 386 0 4 202 200 4 203 207 20 1 420.3 471.2 254.5 3.9 2.3 663.5 688.2 7.9 189.9 192.0 4.0 7.5 10.7 10.9 9.4 1.0 0.6 7.3 7.5 1.9 7.3 7.4 1.0 1.6 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] Pna2(1) # 33 non-cen 4 903 0.043 14796 1.9 / 7.3 3.94 [B] Pnma # 62 centro 5 894 0.043 14796 1.9 / 7.3 2.37 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C5H10Cl4N4P3 Formula weight = 360.88 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.888, non-H atomic volume = 19.8 and following cell contents and analysis: C 20.00 16.64 % H 40.00 2.79 % N 16.00 15.53 % P 12.00 25.75 % Cl 16.00 39.29 % F(000) = 724.0 Mo-K(alpha) radiation Mu (mm-1) = 1.29 ------------------------------------------------------------------------------- File 1.ins set up as follows: TITL 1 in Pna2(1) CELL 0.71073 13.4804 10.6442 8.8479 90.000 90.000 90.000 ZERR 4.00 0.0014 0.0009 0.0007 0.000 0.000 0.000 LATT -1 SYMM -X, -Y, 0.5+Z SYMM 0.5+X, 0.5-Y, Z SYMM 0.5-X, 0.5+Y, 0.5+Z SFAC C H N P CL UNIT 20 40 16 12 16 TEMP 0.1 TREF HKLF 4 END -------------------------------------------------------------------------------