+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 2009/1 for Windows + + Copyright(C) 2009 Bruker-AXS All Rights Reserved + + 2009src0647 started at 15:25:36 on 14-Jun-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 11.316 11.813 33.262 90.00 99.35 90.00 49377 Reflections read from file 2009src0647.hkl; mean (I/sigma) = 5.87 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 24716 24645 24609 24754 36985 32908 32897 49377 N (int>3sigma) = 0 14725 14021 14748 14116 21747 19646 19663 29317 Mean intensity = 0.0 19.2 17.9 19.7 18.6 18.9 19.3 19.6 19.2 Mean int/sigma = 0.0 6.0 5.7 6.0 5.7 5.9 6.0 6.0 5.9 Lattice type: P chosen Volume: 4387.18 ------------------------------------------------------------------------------- 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: 11.316 11.813 33.262 90.00 99.35 90.00 Niggli form: a.a = 128.06 b.b = 139.54 c.c = 1106.34 b.c = 0.00 a.c = -61.15 a.b = 0.00 ------------------------------------------------------------------------------- Search for higher metric symmetry Identical indices and Friedel opposites combined before calculating R(sym) ------------------------------------------------------------------------------ Option A: FOM = 0.444 deg. ORTHORHOMBIC C-lattice R(sym) = 0.597 [ 14049] Cell: 11.316 65.642 11.813 90.00 90.00 90.44 Volume: 8774.37 Matrix:-1.0000 0.0000 0.0000 1.0000 0.0000 2.0000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.000 deg. MONOCLINIC P-lattice R(sym) = 0.044 [ 9139] Cell: 11.316 11.813 33.262 90.00 99.35 90.00 Volume: 4387.18 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option C: FOM = 0.444 deg. MONOCLINIC C-lattice R(sym) = 0.641 [ 9062] Cell: 65.642 11.316 11.813 90.00 90.00 89.56 Volume: 8774.37 Matrix: 1.0000 0.0000 2.0000 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option D: FOM = 0.444 deg. MONOCLINIC C-lattice R(sym) = 0.601 [ 9478] Cell: 11.316 65.642 11.813 90.00 90.00 90.44 Volume: 8774.37 Matrix: 1.0000 0.0000 0.0000 -1.0000 0.0000 -2.0000 0.0000 1.0000 0.0000 Option B selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 24716 24645 24609 24754 36985 32908 32897 49377 N (int>3sigma) = 0 14725 14021 14748 14116 21747 19646 19663 29317 Mean intensity = 0.0 19.2 17.9 19.7 18.6 18.9 19.3 19.6 19.2 Mean int/sigma = 0.0 6.0 5.7 6.0 5.7 5.9 6.0 6.0 5.9 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.944 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 27 1198 1204 1226 N I>3s 0 445 446 1 0.3 26.9 26.8 0.5 0.6 4.8 4.8 0.6 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] P2(1)/n # 14 centro 1 19410 0.044 9139 0.6 / 4.8 2.44 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2009src0647.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) Rsigma Inf - 2.13 533 554 96.2 8.19 66.3 33.34 0.0457 0.0258 2.13 - 1.68 532 532 100.0 6.85 46.7 29.09 0.0463 0.0273 1.68 - 1.46 559 560 99.8 6.46 28.0 22.92 0.0542 0.0321 1.46 - 1.32 568 570 99.6 5.92 23.2 19.68 0.0568 0.0359 1.32 - 1.22 589 589 100.0 5.53 19.7 16.34 0.0645 0.0433 1.22 - 1.14 610 611 99.8 5.13 18.3 15.07 0.0663 0.0483 1.14 - 1.08 588 591 99.5 4.84 12.2 11.67 0.0840 0.0609 1.08 - 1.03 595 601 99.0 4.58 10.2 10.09 0.1021 0.0714 1.03 - 0.99 576 580 99.3 4.37 9.0 8.96 0.1150 0.0818 0.99 - 0.95 680 684 99.4 4.22 8.1 8.15 0.1231 0.0920 0.95 - 0.92 571 573 99.7 3.99 7.0 7.29 0.1368 0.1071 0.92 - 0.89 673 675 99.7 3.91 6.3 6.54 0.1467 0.1200 0.89 - 0.86 766 769 99.6 3.64 5.4 5.50 0.1799 0.1439 0.86 - 0.84 594 594 100.0 3.60 4.8 4.86 0.1865 0.1637 0.84 - 0.82 602 602 100.0 3.45 3.8 4.07 0.2355 0.2066 0.82 - 0.80 705 705 100.0 3.29 3.8 3.79 0.2303 0.2152 0.80 - 0.78 758 764 99.2 3.22 3.1 3.31 0.2756 0.2693 0.78 - 0.76 40 309 12.9 0.15 2.3 1.63 0.2373 0.6238 ------------------------------------------------------------------------------ 0.86 - 0.76 2968 3245 91.5 3.09 3.8 3.99 0.2287 0.2109 Inf - 0.76 10539 10863 97.0 4.55 15.0 11.67 0.0694 0.0577 Merged [A], lowest resolution = 6.95 Angstroms, 1308 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2009src0647.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C46H58Br2S3 Formula weight = 866.96 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.313, non-H atomic volume = 21.5 and following cell contents and analysis: C 184.00 63.73 % H 232.00 6.74 % S 12.00 11.10 % Br 8.00 18.43 % F(000) = 1808.0 Mo-K(alpha) radiation Mu (mm-1) = 2.02 ------------------------------------------------------------------------------- File 2009src0647.ins set up as follows: TITL 2009src0647 in P2(1)/n CELL 0.71073 11.3163 11.8126 33.2617 90.000 99.350 90.000 ZERR 4.00 0.0003 0.0002 0.0007 0.000 0.001 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H S BR UNIT 184 232 12 8 TEMP 0.04 TREF HKLF 4 END 49377 Reflections written to new reflection file 2009src0647.hkl -------------------------------------------------------------------------------