++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 2007src0927 started at 16:48:26 on 20-JUL-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 9.683 22.378 16.012 90.00 91.85 90.00 35250 Reflections read from file 2007src0927.hkl; mean (I/sigma) = 13.95 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 17632 17684 17660 17597 26488 23522 23444 35250 N (int>3sigma) = 0 16309 16311 16344 16234 24482 21752 21650 32585 Mean intensity = 0.0 314.0 328.1 311.7 323.4 317.9 322.6 320.7 317.2 Mean int/sigma = 0.0 13.9 14.0 14.0 13.9 14.0 14.0 14.0 14.0 Lattice type: P chosen Volume: 3467.69 ------------------------------------------------------------------------------- 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: 9.683 16.012 22.378 90.00 90.00 91.85 Niggli form: a.a = 93.75 b.b = 256.40 c.c = 500.76 b.c = 0.00 a.c = 0.00 a.b = -5.00 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.036 [ 27090] Cell: 9.683 22.378 16.012 90.00 91.85 90.00 Volume: 3467.69 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 17632 17684 17660 17597 26488 23522 23444 35250 N (int>3sigma) = 0 16309 16311 16344 16234 24482 21752 21650 32585 Mean intensity = 0.0 314.0 328.1 311.7 323.4 317.9 322.6 320.7 317.2 Mean int/sigma = 0.0 13.9 14.0 14.0 13.9 14.0 14.0 14.0 14.0 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.776 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 34 483 482 499 N I>3s 1 380 385 407 12.0 455.1 596.4 567.5 1.3 11.7 11.8 12.3 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1) # 4 chiral 1 3543 0.036 27090 1.3 / 11.7 1.12 [B] P2(1)/m # 11 centro 1 402 0.036 27090 1.3 / 11.7 4.85 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C10H15Cl3N5OP3 Formula weight = 420.53 Tentative Z (number of formula units/cell) = 8.0 giving rho = 1.611, non-H atomic volume = 19.7 and following cell contents and analysis: C 80.00 28.56 % H 120.00 3.60 % N 40.00 16.66 % O 8.00 3.80 % P 24.00 22.09 % Cl 24.00 25.29 % F(000) = 1712.0 Mo-K(alpha) radiation Mu (mm-1) = 0.81 ------------------------------------------------------------------------------- File 2007src0927.ins set up as follows: TITL 2007src0927 in P2(1) CELL 0.71073 9.6827 22.3776 16.0124 90.000 91.846 90.000 ZERR 8.00 0.0001 0.0002 0.0002 0.000 0.001 0.000 LATT -1 SYMM -X, 0.5+Y, -Z SFAC C H N O P CL UNIT 80 120 40 8 24 24 TEMP 0.04 TREF HKLF 4 END -------------------------------------------------------------------------------