+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 2008/2 for Windows + + Copyright(C) 2008 Bruker-AXS All Rights Reserved + + 2010src0243 started at 10:20:20 on 23-Mar-2010 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 6.984 12.050 13.212 90.01 89.99 88.47 26099 Reflections read from file 2010src0243.hkl; mean (I/sigma) = 8.66 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 13088 13074 13130 13130 19646 17322 17352 26099 N (int>3sigma) = 0 10373 10219 10004 9285 15298 13616 13670 20605 Mean intensity = 0.0 54.4 55.0 53.5 41.8 54.3 55.6 56.4 56.3 Mean int/sigma = 0.0 8.7 8.6 8.5 7.8 8.6 8.7 8.7 8.7 Lattice type: P chosen Volume: 1111.34 ------------------------------------------------------------------------------- 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: 6.984 12.050 13.212 90.01 90.01 91.53 Niggli form: a.a = 48.77 b.b = 145.19 c.c = 174.55 b.c = -0.04 a.c = -0.02 a.b = -2.25 ------------------------------------------------------------------------------- Search for higher metric symmetry Identical indices and Friedel opposites combined before calculating R(sym) ------------------------------------------------------------------------------ Option A: FOM = 0.017 deg. MONOCLINIC P-lattice R(sym) = 0.026 [ 2426] Cell: 6.984 13.212 12.050 89.99 91.53 89.99 Volume: 1111.34 Matrix: 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 Option A selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 13088 13130 13074 13130 19646 17375 17322 26099 N (int>3sigma) = 0 10373 10004 10219 9285 15298 13774 13616 20605 Mean intensity = 0.0 54.4 53.5 55.0 41.8 54.3 55.2 55.6 56.3 Mean int/sigma = 0.0 8.7 8.5 8.6 7.8 8.6 8.7 8.7 8.7 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.940 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 49 686 689 769 N I>3s 0 257 257 0 0.2 56.2 56.0 0.2 0.5 5.0 4.9 0.5 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 0.026 2426 0.5 / 4.9 2.36 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2010src0243.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) Rsigma Inf - 2.12 136 142 95.8 13.92 160.9 45.34 0.0556 0.0269 2.12 - 1.67 142 143 99.3 17.14 130.7 53.16 0.0437 0.0188 1.67 - 1.45 144 145 99.3 16.32 106.8 48.76 0.0440 0.0174 1.45 - 1.31 147 147 100.0 13.44 80.7 40.41 0.0428 0.0191 1.31 - 1.21 142 142 100.0 12.42 64.9 38.05 0.0458 0.0209 1.21 - 1.14 143 143 100.0 11.87 46.9 33.39 0.0501 0.0224 1.14 - 1.08 149 149 100.0 10.46 34.8 27.85 0.0588 0.0260 1.08 - 1.03 154 154 100.0 8.85 32.2 23.24 0.0572 0.0291 1.03 - 0.99 148 148 100.0 8.31 20.7 19.66 0.0664 0.0348 0.99 - 0.95 164 164 100.0 8.25 16.8 18.08 0.0722 0.0383 0.95 - 0.92 157 157 100.0 7.87 15.1 16.45 0.0844 0.0427 0.92 - 0.89 154 154 100.0 7.51 11.7 14.13 0.0849 0.0483 0.89 - 0.86 215 215 100.0 7.25 10.6 13.28 0.1005 0.0544 0.86 - 0.83 226 226 100.0 6.94 11.8 12.83 0.0909 0.0549 0.83 - 0.81 160 160 100.0 6.61 9.9 11.79 0.0910 0.0607 0.81 - 0.79 173 173 100.0 6.39 9.9 10.06 0.1115 0.0664 0.79 - 0.77 130 139 93.5 4.91 10.9 9.26 0.0992 0.0791 ------------------------------------------------------------------------------ 0.87 - 0.77 837 846 98.9 6.48 10.8 11.54 0.0971 0.0618 Inf - 0.77 2684 2701 99.4 9.66 42.3 24.52 0.0520 0.0269 Merged [A], lowest resolution = 6.98 Angstroms, 1277 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2010src0243.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C56H52F73NO12Si8 Formula weight = 2542.58 Tentative Z (number of formula units/cell) = 1.0 giving rho = 3.799, non-H atomic volume = 7.4 and following cell contents and analysis: C 56.00 26.45 % H 52.00 2.06 % N 1.00 0.55 % O 12.00 7.55 % F 73.00 54.55 % Si 8.00 8.84 % F(000) = 1260.0 Mo-K(alpha) radiation Mu (mm-1) = 0.66 ------------------------------------------------------------------------------- File p21n.ins set up as follows: TITL p21n in P2(1)/n CELL 0.71073 6.9836 13.2116 12.0495 90.000 91.532 90.000 ZERR 1.00 0.0001 0.0002 0.0002 0.000 0.001 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N O F SI UNIT 56 52 1 12 73 8 TEMP 0.28 TREF HKLF 4 END 26099 Reflections written to new reflection file p21n.hkl -------------------------------------------------------------------------------