++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 2007src0655 started at 14:37:26 on 13-JUN-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 8.201 9.066 12.813 83.34 84.01 72.53 37351 Reflections read from file 2007src0655.hkl; mean (I/sigma) = 11.23 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 18652 18639 18699 18653 27995 24891 24937 37351 N (int>3sigma) = 0 16152 16078 16258 16122 24244 21498 21586 32278 Mean intensity = 0.0 58.9 59.4 60.1 60.3 59.5 59.7 59.1 58.7 Mean int/sigma = 0.0 11.3 11.2 11.4 11.3 11.3 11.2 11.3 11.2 Lattice type: P chosen Volume: 900.23 ------------------------------------------------------------------------------- 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: 8.201 9.066 12.813 83.34 84.01 72.53 Niggli form: a.a = 67.26 b.b = 82.20 c.c = 164.18 b.c = 13.47 a.c = 10.96 a.b = 22.32 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. TRICLINIC P-lattice R(int) = 0.035 [ 33209] Cell: 8.201 9.066 12.813 83.34 84.01 72.53 Volume: 900.23 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 18652 18639 18699 18653 27995 24891 24937 37351 N (int>3sigma) = 0 16152 16078 16258 16122 24244 21498 21586 32278 Mean intensity = 0.0 58.9 59.4 60.1 60.3 59.5 59.7 59.1 58.7 Mean int/sigma = 0.0 11.3 11.2 11.4 11.3 11.3 11.2 11.3 11.2 Crystal system A and Lattice type P selected Mean |E*E-1| = 0.946 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absences not required for triclinic Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P-1 # 2 centro 1 8646 0.035 33209 0.0 / 11.2 0.95 [B] P1 # 1 chiral 1 700 0.035 33209 0.0 / 11.2 5.43 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C9H18Cl4N3O2P3 Formula weight = 434.97 Tentative Z (number of formula units/cell) = 2.0 giving rho = 1.605, non-H atomic volume = 21.4 and following cell contents and analysis: C 18.00 24.85 % H 36.00 4.17 % N 6.00 9.66 % O 4.00 7.36 % P 6.00 21.36 % Cl 8.00 32.60 % F(000) = 444.0 Mo-K(alpha) radiation Mu (mm-1) = 0.93 ------------------------------------------------------------------------------- File 2007src0655.ins set up as follows: TITL 2007src0655 in P-1 CELL 0.71073 8.2012 9.0665 12.8131 83.344 84.013 72.530 ZERR 2.00 0.0001 0.0001 0.0001 0.001 0.001 0.001 LATT 1 SFAC C H N O P CL UNIT 18 36 6 4 6 8 TEMP 0.05 TREF HKLF 4 END -------------------------------------------------------------------------------