++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + 2008src0391 started at 12:26:32 on 28-Mar-2008 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 8.088 8.445 9.307 104.52 101.38 114.95 11632 Reflections read from file 2008src0391.hkl; mean (I/sigma) = 16.26 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 5830 5776 5832 5790 8719 7777 7742 11632 N (int>3sigma) = 0 5152 5134 5170 5116 7728 6991 6901 10391 Mean intensity = 0.0 83.3 81.2 82.6 82.7 82.3 81.6 82.3 81.2 Mean int/sigma = 0.0 16.2 16.3 16.2 16.3 16.2 16.4 16.4 16.3 Lattice type: P chosen Volume: 523.64 ------------------------------------------------------------------------------- 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: 8.088 8.445 9.307 104.52 101.38 114.95 Niggli form: a.a = 65.41 b.b = 71.32 c.c = 86.62 b.c = -19.70 a.c = -14.85 a.b = -28.81 ------------------------------------------------------------------------------- Search for higher metric symmetry Identical indices and Friedel opposites combined before calculating R(sym) ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. TRICLINIC P-lattice R(sym) = 0.000 [ 0] Cell: 8.088 8.445 9.307 104.52 101.38 114.95 Volume: 523.64 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 5830 5776 5832 5790 8719 7777 7742 11632 N (int>3sigma) = 0 5152 5134 5170 5116 7728 6991 6901 10391 Mean intensity = 0.0 83.3 81.2 82.6 82.7 82.3 81.6 82.3 81.2 Mean int/sigma = 0.0 16.2 16.3 16.2 16.3 16.2 16.4 16.4 16.3 Crystal system A and Lattice type P selected Mean |E*E-1| = 0.913 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absences not required for triclinic Identical indices and Friedel opposites combined before calculating R(sym) Option Space Group No. Type Axes CSD R(sym) N(eq) Syst. Abs. CFOM [A] P-1 # 2 centro 1 8646 0.000 0 0.0 / 16.3 0.93 [B] P1 # 1 chiral 1 700 0.000 0 0.0 / 16.3 3.88 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2008src0391.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) Inf - 2.05 124 126 98.4 6.17 184.7 60.95 0.0353 0.0155 2.05 - 1.60 142 142 100.0 6.51 138.8 61.06 0.0265 0.0133 1.60 - 1.40 125 125 100.0 6.50 114.1 56.31 0.0279 0.0138 1.40 - 1.25 168 169 99.4 6.56 116.6 53.32 0.0255 0.0145 1.25 - 1.15 162 162 100.0 6.46 87.0 46.48 0.0269 0.0167 1.15 - 1.05 228 228 100.0 6.39 66.3 38.91 0.0312 0.0194 1.05 - 1.00 145 145 100.0 6.19 46.4 33.66 0.0348 0.0218 1.00 - 0.95 184 184 100.0 5.20 51.9 28.67 0.0345 0.0246 0.95 - 0.90 214 214 100.0 4.65 55.8 27.70 0.0364 0.0285 0.90 - 0.85 284 284 100.0 3.70 42.4 21.65 0.0422 0.0353 0.85 - 0.80 360 360 100.0 2.74 41.5 17.92 0.0384 0.0419 0.80 - 0.77 261 268 97.4 2.31 29.3 13.53 0.0402 0.0534 ------------------------------------------------------------------------------ 0.90 - 0.77 905 912 99.2 2.91 38.3 17.82 0.0403 0.0421 Inf - 0.77 2397 2407 99.6 4.83 70.3 33.73 0.0313 0.0226 Merged [A], lowest resolution = 6.96 Angstroms, 385 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2008src0391.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C7H16Cl3N4O2P3 Formula weight = 387.50 Tentative Z (number of formula units/cell) = 1.0 giving rho = 1.229, non-H atomic volume = 27.6 and following cell contents and analysis: C 7.00 21.70 % H 16.00 4.16 % N 4.00 14.46 % O 2.00 8.26 % P 3.00 23.98 % Cl 3.00 27.45 % F(000) = 198.0 Mo-K(alpha) radiation Mu (mm-1) = 0.67 ------------------------------------------------------------------------------- File 2008src0391.ins set up as follows: TITL 2008src0391 in P-1 CELL 0.71073 8.0877 8.4452 9.3069 104.517 101.380 114.951 ZERR 1.00 0.0002 0.0002 0.0002 0.001 0.001 0.001 LATT 1 SFAC C H N O P CL UNIT 7 16 4 2 3 3 TEMP 0.2 TREF HKLF 4 END -------------------------------------------------------------------------------