++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 2007src0260 started at 22:27:23 on 19-MAR-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 9.420 9.420 42.348 90.00 90.00 90.00 28882 Reflections read from file 2007src0260.hkl; mean (I/sigma) = 4.80 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 14432 14442 14442 14472 21658 19262 19266 28882 N (int>3sigma) = 0 8842 8752 9116 8741 13355 11835 11859 17660 Mean intensity = 0.0 413.2 407.9 414.8 438.1 411.9 417.8 413.4 417.7 Mean int/sigma = 0.0 4.8 4.8 5.0 4.8 4.9 4.9 4.9 4.9 Lattice type: P chosen Volume: 3757.57 ------------------------------------------------------------------------------- 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: 9.420 9.420 42.348 90.00 90.00 90.00 Niggli form: a.a = 88.73 b.b = 88.73 c.c = 1793.35 b.c = 0.00 a.c = 0.00 a.b = 0.00 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. TETRAGONAL P-lattice R(int) = 0.106 [ 24438] Cell: 9.420 9.420 42.348 90.00 90.00 90.00 Volume: 3757.57 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 14432 14442 14442 14472 21658 19262 19266 28882 N (int>3sigma) = 0 8842 8752 9116 8741 13355 11835 11859 17660 Mean intensity = 0.0 413.2 407.9 414.8 438.1 411.9 417.8 413.4 417.7 Mean int/sigma = 0.0 4.8 4.8 5.0 4.8 4.9 4.9 4.9 4.9 Crystal system T and Lattice type P selected Mean |E*E-1| = 0.796 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: 41/43 42 n-- -b- -c- -n- -21- --c N 94 66 306 1866 1848 1836 33 1440 N I>3s 0 0 157 1168 1143 1093 0 874 3.2 3.5 463.5 657.6 543.5 677.9 6.8 757.4 0.5 0.6 4.5 5.3 5.1 5.0 0.7 5.3 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P4(1)2(1)2 # 92 chiral 1 245 0.110 26189 0.7 / 4.5 7.75 [B] P4(3)2(1)2 # 96 chiral 1 245 0.110 26189 0.7 / 4.5 7.75 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C15H17Cl2N4OP3 Formula weight = 433.14 Tentative Z (number of formula units/cell) = 8.0 giving rho = 1.531, non-H atomic volume = 18.8 and following cell contents and analysis: C 120.00 41.59 % H 136.00 3.96 % N 32.00 12.94 % O 8.00 3.69 % P 24.00 21.45 % Cl 16.00 16.37 % F(000) = 1776.0 Mo-K(alpha) radiation Mu (mm-1) = 0.61 ------------------------------------------------------------------------------- File 2007src0260.ins set up as follows: TITL 2007src0260 in P4(1)2(1)2 CELL 0.71073 9.4197 9.4197 42.3480 90.000 90.000 90.000 ZERR 8.00 0.0001 0.0001 0.0009 0.000 0.000 0.000 LATT -1 SYMM -X, -Y, 0.5+Z SYMM 0.5-Y, 0.5+X, 0.25+Z SYMM 0.5+Y, 0.5-X, 0.75+Z SYMM 0.5-X, 0.5+Y, 0.25-Z SYMM 0.5+X, 0.5-Y, 0.75-Z SYMM Y, X, -Z SYMM -Y, -X, 0.5-Z SFAC C H N O P CL UNIT 120 136 32 8 24 16 TEMP 0.12 TREF HKLF 4 END -------------------------------------------------------------------------------