++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + 2009src0685 started at 14:46:29 on 22-Jul-2009 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 9.357 25.933 11.100 90.00 89.99 90.00 28928 Reflections read from file 2009src0685.hkl; mean (I/sigma) = 8.24 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 14491 14438 14457 14493 21693 19269 19290 28928 N (int>3sigma) = 0 10780 10706 10646 10766 16066 14352 14382 21507 Mean intensity = 0.0 199.0 205.9 216.3 194.8 207.1 207.7 207.4 201.7 Mean int/sigma = 0.0 8.3 8.2 8.2 8.2 8.2 8.3 8.3 8.3 Lattice type: P chosen Volume: 2693.55 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): -1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 Unitcell: 9.357 11.100 25.933 90.00 90.00 89.99 Niggli form: a.a = 87.56 b.b = 123.21 c.c = 672.54 b.c = 0.00 a.c = 0.00 a.b = 0.01 ------------------------------------------------------------------------------- Search for higher metric symmetry Identical indices and Friedel opposites combined before calculating R(sym) ------------------------------------------------------------------------------ Option A: FOM = 0.008 deg. ORTHORHOMBIC P-lattice R(sym) = 0.043 [ 7992] Cell: 9.357 11.100 25.933 90.00 90.00 89.99 Volume: 2693.55 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 14491 14457 14438 14493 21693 19269 19291 28928 N (int>3sigma) = 0 10780 10646 10706 10766 16066 14352 14380 21507 Mean intensity = 0.0 199.0 216.3 205.9 194.8 207.1 207.7 207.8 201.7 Mean int/sigma = 0.0 8.3 8.2 8.2 8.2 8.2 8.3 8.3 8.3 Crystal system O and Lattice type P selected Mean |E*E-1| = 0.732 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: b-- c-- n-- 21-- -c- -a- -n- -21- --a --b --n --21 N 969 963 958 18 879 886 871 22 466 471 469 45 N I>3s 707 684 687 3 614 652 542 0 348 314 288 0 336.3 282.7 299.0 3.3 231.5 286.5 212.0 2.0 479.7 276.7 337.1 2.8 9.0 8.7 8.7 1.3 8.2 8.8 7.4 0.6 9.1 8.3 7.4 0.8 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)2(1)2(1) # 19 chiral 1 5917 0.043 7992 1.3 / 7.4 1.54 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2009src0685.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) Inf - 2.20 180 190 94.7 13.84 928.9 58.17 0.0232 0.0150 2.20 - 1.70 195 195 100.0 15.55 389.0 52.80 0.0383 0.0160 1.70 - 1.45 205 205 100.0 12.27 184.2 39.31 0.0538 0.0207 1.45 - 1.30 207 207 100.0 11.14 132.5 33.76 0.0704 0.0251 1.30 - 1.20 196 196 100.0 10.44 122.7 29.76 0.0709 0.0272 1.20 - 1.10 282 282 100.0 9.73 118.8 28.22 0.0757 0.0290 1.10 - 1.00 396 396 100.0 8.10 80.1 20.09 0.0983 0.0400 1.00 - 0.95 263 263 100.0 7.11 51.6 14.52 0.1356 0.0566 0.95 - 0.90 323 323 100.0 6.55 34.1 10.36 0.1807 0.0799 0.90 - 0.85 386 386 100.0 5.80 26.1 7.72 0.2270 0.1107 0.85 - 0.80 510 513 99.4 5.00 19.6 5.51 0.2869 0.1581 0.80 - 0.75 411 644 63.8 2.56 15.1 3.79 0.3712 0.2573 0.75 - 0.74 6 120 5.0 0.06 13.7 1.70 0.0062 0.5338 ------------------------------------------------------------------------------ 0.85 - 0.74 927 1277 72.6 3.31 17.6 4.72 0.3146 0.1979 Inf - 0.74 3560 3920 90.8 7.38 126.0 20.25 0.0497 0.0314 Merged [A], lowest resolution = 6.90 Angstroms, 1513 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2009src0685.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C274H32O15 Formula weight = 3563.00 Tentative Z (number of formula units/cell) = 1.0 giving rho = 2.197, non-H atomic volume = 9.3 and following cell contents and analysis: C 274.00 92.36 % H 32.00 0.91 % O 15.00 6.74 % F(000) = 1796.0 Mo-K(alpha) radiation Mu (mm-1) = 0.14 ------------------------------------------------------------------------------- File 2009src0685a.ins set up as follows: TITL 2009src0685a in P2(1)2(1)2(1) CELL 0.71073 9.3572 11.0999 25.9334 90.000 90.000 90.000 ZERR 1.00 0.0001 0.0002 0.0005 0.000 0.000 0.000 LATT -1 SYMM 0.5-X, -Y, 0.5+Z SYMM -X, 0.5+Y, 0.5-Z SYMM 0.5+X, 0.5-Y, -Z SFAC C H O UNIT 274 32 15 TEMP 0.1 TREF HKLF 4 END 28928 Reflections written to new reflection file 2009src0685a.hkl -------------------------------------------------------------------------------