++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + 2008src1016 started at 00:05:51 on 25-Sep-2008 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 7.667 10.842 12.641 79.32 73.44 73.22 19490 Reflections read from file 2008src1016.hkl; mean (I/sigma) = 10.34 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 9761 9717 9690 9785 14584 12986 12998 19490 N (int>3sigma) = 0 7350 7134 7194 7176 10839 9562 9671 14449 Mean intensity = 0.0 23.3 23.2 23.3 22.4 23.2 22.4 23.6 23.0 Mean int/sigma = 0.0 10.5 10.4 10.3 10.2 10.4 10.3 10.4 10.4 Lattice type: P chosen Volume: 958.24 ------------------------------------------------------------------------------- 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: 7.667 10.842 12.641 79.32 73.44 73.22 Niggli form: a.a = 58.78 b.b = 117.56 c.c = 159.79 b.c = 25.40 a.c = 27.63 a.b = 23.99 ------------------------------------------------------------------------------- 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: 7.667 10.842 12.641 79.32 73.44 73.22 Volume: 958.24 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 9761 9717 9690 9785 14584 12986 12998 19490 N (int>3sigma) = 0 7350 7134 7194 7176 10839 9562 9671 14449 Mean intensity = 0.0 23.3 23.2 23.3 22.4 23.2 22.4 23.6 23.0 Mean int/sigma = 0.0 10.5 10.4 10.3 10.2 10.4 10.3 10.4 10.4 Crystal system A and Lattice type P selected Mean |E*E-1| = 0.965 [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 / 10.4 0.98 [B] P1 # 1 chiral 1 700 0.000 0 0.0 / 10.4 6.35 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2008src1016.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) Inf - 2.05 229 235 97.4 5.89 82.6 53.34 0.0232 0.0154 2.05 - 1.60 254 254 100.0 6.09 50.0 46.80 0.0292 0.0156 1.60 - 1.40 240 240 100.0 5.97 33.2 37.36 0.0333 0.0191 1.40 - 1.25 294 294 100.0 5.92 26.8 32.74 0.0363 0.0222 1.25 - 1.15 298 298 100.0 5.91 22.0 26.20 0.0416 0.0254 1.15 - 1.05 408 408 100.0 5.88 17.3 23.83 0.0498 0.0296 1.05 - 1.00 274 274 100.0 5.57 12.5 19.17 0.0623 0.0369 1.00 - 0.95 338 338 100.0 4.74 11.3 16.57 0.0718 0.0440 0.95 - 0.90 403 403 100.0 4.19 8.8 12.98 0.0847 0.0556 0.90 - 0.85 518 518 100.0 3.35 8.8 10.64 0.0883 0.0690 0.85 - 0.80 662 663 99.8 2.45 5.9 6.98 0.1021 0.1113 0.80 - 0.77 483 506 95.5 2.08 5.3 5.94 0.1163 0.1385 ------------------------------------------------------------------------------ 0.90 - 0.77 1663 1687 98.6 2.61 6.7 7.82 0.0976 0.1001 Inf - 0.77 4401 4431 99.3 4.40 18.8 20.29 0.0413 0.0336 Merged [A], lowest resolution = 6.92 Angstroms, 608 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2008src1016.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C13H14Cl2N2O2Si Formula weight = 329.25 Tentative Z (number of formula units/cell) = 3.0 giving rho = 1.712, non-H atomic volume = 16.0 and following cell contents and analysis: C 39.00 47.42 % H 42.00 4.29 % N 6.00 8.51 % O 6.00 9.72 % Si 3.00 8.53 % Cl 6.00 21.53 % F(000) = 510.0 Mo-K(alpha) radiation Mu (mm-1) = 0.60 ------------------------------------------------------------------------------- File 2008src1016.ins set up as follows: TITL 2008src1016 in P-1 CELL 0.71073 7.6668 10.8424 12.6410 79.319 73.438 73.223 ZERR 3.00 0.0002 0.0004 0.0005 0.002 0.002 0.002 LATT 1 SFAC C H N O SI CL UNIT 39 42 6 6 3 6 TEMP 0.2 TREF HKLF 4 END -------------------------------------------------------------------------------