++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + 2009src1074 started at 10:11:32 on 30-Sep-2009 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 10.538 31.372 15.934 90.00 89.99 90.00 64350 Reflections read from file 2009src1074.hkl; mean (I/sigma) = 2.44 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 32111 32174 32091 32196 48188 42837 42877 64350 N (int>3sigma) = 0 9333 9443 9368 9304 14072 12581 12473 18807 Mean intensity = 0.0 6.1 5.8 6.0 6.1 6.0 5.8 5.8 5.9 Mean int/sigma = 0.0 2.6 2.6 2.5 2.5 2.6 2.6 2.6 2.6 Lattice type: P chosen Volume: 5267.42 ------------------------------------------------------------------------------- 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: 10.538 15.934 31.372 90.00 90.00 89.99 Niggli form: a.a = 111.04 b.b = 253.88 c.c = 984.22 b.c = 0.00 a.c = 0.00 a.b = 0.02 ------------------------------------------------------------------------------- Search for higher metric symmetry Identical indices and Friedel opposites combined before calculating R(sym) ------------------------------------------------------------------------------ Option A: FOM = 0.006 deg. ORTHORHOMBIC P-lattice R(sym) = 0.234 [ 15540] Cell: 10.538 15.934 31.372 90.00 90.00 89.99 Volume: 5267.42 Matrix:-1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.000 deg. MONOCLINIC P-lattice R(sym) = 0.180 [ 10219] Cell: 10.538 31.372 15.934 90.00 90.01 90.00 Volume: 5267.42 Matrix: 1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option C: FOM = 0.006 deg. MONOCLINIC P-lattice R(sym) = 0.197 [ 9972] Cell: 10.538 15.934 31.372 90.00 90.00 89.99 Volume: 5267.42 Matrix: 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option D: FOM = 0.006 deg. MONOCLINIC P-lattice R(sym) = 0.206 [ 9745] Cell: 15.934 10.538 31.372 90.00 90.00 90.01 Volume: 5267.42 Matrix: 0.0000 0.0000 1.0000 -1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option E: FOM = 0.000 deg. TRICLINIC P-lattice R(sym) = 0.000 [ 0] Cell: 10.538 15.934 31.372 90.00 90.00 89.99 Volume: 5267.42 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 32111 32091 32174 32196 48188 42837 42851 64350 N (int>3sigma) = 0 9333 9368 9443 9304 14072 12581 12474 18807 Mean intensity = 0.0 6.1 6.0 5.8 6.1 6.0 5.8 5.8 5.9 Mean int/sigma = 0.0 2.6 2.5 2.6 2.5 2.6 2.6 2.6 2.6 Crystal system O and Lattice type P selected Mean |E*E-1| = 0.759 [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 2126 2132 2130 23 1295 1276 1299 45 676 688 688 61 N I>3s 443 654 673 0 383 514 419 0 342 338 314 2 3.4 12.5 12.9 0.4 3.9 6.4 6.1 0.5 7.3 17.6 15.3 1.1 2.0 2.6 2.7 0.6 2.5 3.1 2.9 0.7 4.0 4.2 3.8 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 0.234 15540 0.8 / 2.0 7.34 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2009src1074.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) Inf - 2.15 350 368 95.1 20.78 24.8 28.84 0.0723 0.0288 2.15 - 1.70 343 343 100.0 16.72 9.6 19.10 0.1335 0.0437 1.70 - 1.45 387 387 100.0 15.42 5.3 13.45 0.2073 0.0648 1.45 - 1.30 400 400 100.0 14.01 4.7 11.04 0.2469 0.0788 1.30 - 1.20 382 382 100.0 12.00 4.0 8.52 0.3036 0.1040 1.20 - 1.10 532 532 100.0 10.49 3.4 6.55 0.3727 0.1380 1.10 - 1.00 750 750 100.0 8.92 2.4 4.38 0.5236 0.2186 1.00 - 0.95 491 492 99.8 7.99 1.8 2.84 0.7301 0.3441 0.95 - 0.90 618 626 98.7 7.23 1.5 2.10 0.9261 0.4764 0.90 - 0.85 769 781 98.5 6.65 1.3 1.66 1.0226 0.6246 0.85 - 0.80 929 946 98.2 6.01 0.9 1.15 1.2997 0.8975 0.80 - 0.77 725 790 91.8 4.06 0.5 0.55 1.8969 1.8782 ------------------------------------------------------------------------------ 0.90 - 0.77 2423 2517 96.3 5.60 0.9 1.13 1.2385 0.9265 Inf - 0.77 6676 6797 98.2 9.47 3.8 6.25 0.2292 0.1707 Merged [A], lowest resolution = 7.04 Angstroms, 2822 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2009src1074.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C28H36O5Si1 Formula weight = 480.66 Tentative Z (number of formula units/cell) = 8.0 giving rho = 1.212, non-H atomic volume = 19.4 and following cell contents and analysis: C 224.00 69.96 % H 288.00 7.55 % O 40.00 16.64 % Si 8.00 5.84 % F(000) = 2064.0 Mo-K(alpha) radiation Mu (mm-1) = 0.12 ------------------------------------------------------------------------------- File 2009src1074a.ins set up as follows: TITL 2009src1074a in P2(1)2(1)2(1) CELL 0.71073 10.5375 15.9336 31.3723 90.000 90.000 90.000 ZERR 8.00 0.0007 0.0012 0.0024 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 SI UNIT 224 288 40 8 TEMP 0.03 TREF HKLF 4 END 64350 Reflections written to new reflection file 2009src1074a.hkl -------------------------------------------------------------------------------