++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 2007src0259 started at 13:28:50 on 23-FEB-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 9.783 10.042 11.598 90.00 109.23 90.00 15417 Reflections read from file 2007src0259.hkl; mean (I/sigma) = 20.98 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 7747 7731 7730 7713 11604 10271 10298 15417 N (int>3sigma) = 0 7514 7471 7467 7447 11226 9943 9986 14914 Mean intensity = 0.0 645.5 632.1 643.8 593.6 640.5 636.7 625.9 629.4 Mean int/sigma = 0.0 21.3 21.1 21.0 20.7 21.1 21.1 21.0 21.0 Lattice type: P chosen Volume: 1075.89 ------------------------------------------------------------------------------- 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: 9.783 10.042 11.598 90.00 109.23 90.00 Niggli form: a.a = 95.71 b.b = 100.84 c.c = 134.52 b.c = 0.00 a.c = -37.37 a.b = 0.00 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.025 [ 12817] Cell: 9.783 10.042 11.598 90.00 109.23 90.00 Volume: 1075.89 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 7747 7731 7730 7713 11604 10271 10298 15417 N (int>3sigma) = 0 7514 7471 7467 7447 11226 9943 9986 14914 Mean intensity = 0.0 645.5 632.1 643.8 593.6 640.5 636.7 625.9 629.4 Mean int/sigma = 0.0 21.3 21.1 21.0 20.7 21.1 21.1 21.0 21.0 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.697 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 13 543 558 539 N I>3s 2 492 519 497 2.0 669.1 726.7 734.5 1.1 19.5 21.7 21.8 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1) # 4 chiral 1 3543 0.025 12817 1.1 / 19.5 0.71 [B] P2(1)/m # 11 centro 1 402 0.025 12817 1.1 / 19.5 8.13 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C18H25ClN5O2P3 Formula weight = 471.79 Tentative Z (number of formula units/cell) = 2.0 giving rho = 1.456, non-H atomic volume = 18.5 and following cell contents and analysis: C 36.00 45.82 % H 50.00 5.34 % N 10.00 14.85 % O 4.00 6.78 % P 6.00 19.69 % Cl 2.00 7.51 % F(000) = 492.0 Mo-K(alpha) radiation Mu (mm-1) = 0.43 ------------------------------------------------------------------------------- File 2007src0259.ins set up as follows: TITL 2007src0259 in P2(1) CELL 0.71073 9.7832 10.0420 11.5984 90.000 109.228 90.000 ZERR 2.00 0.0002 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 36 50 10 4 6 2 TEMP 0.2 TREF HKLF 4 END -------------------------------------------------------------------------------