++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + 2007may0002 started at 16:50:24 on 08-Jun-2007 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 22.550 22.550 6.358 90.00 90.00 90.00 13907 Reflections read from file 2007may0002.hkl; mean (I/sigma) = 4.70 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 6960 6955 7023 0 10469 9253 9281 13907 N (int>3sigma) = 0 3608 3581 4099 0 5644 5100 5175 7715 Mean intensity = 0.0 9.2 9.1 11.6 0.0 10.0 11.4 11.4 11.2 Mean int/sigma = 0.0 4.5 4.5 5.1 0.0 4.7 4.8 4.8 4.8 Lattice type: I chosen Volume: 3233.00 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 0.0000 1.0000 0.5000 0.5000 0.5000 -0.5000 0.5000 0.5000 Unitcell: 6.358 16.259 16.259 87.81 78.72 78.72 Niggli form: a.a = 40.43 b.b = 264.35 c.c = 264.35 b.c = 10.11 a.c = 20.21 a.b = 20.21 ------------------------------------------------------------------------------- Search for higher metric symmetry Identical indices and Friedel opposites combined before calculating R(sym) ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. TETRAGONAL I-lattice R(sym) = 0.054 [ 4432] Cell: 22.550 22.550 6.358 90.00 90.00 90.00 Volume: 3233.00 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 6960 6955 7023 0 10469 9253 9281 13907 N (int>3sigma) = 0 3608 3581 4099 0 5644 5100 5175 7715 Mean intensity = 0.0 9.2 9.1 11.6 0.0 10.0 11.4 11.4 11.2 Mean int/sigma = 0.0 4.5 4.5 5.1 0.0 4.7 4.8 4.8 4.8 Crystal system T and Lattice type I selected Mean |E*E-1| = 0.962 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: 41/43 a-- -c- --d N 6 719 399 293 N I>3s 0 2 278 128 0.2 0.2 17.2 8.7 0.4 0.6 6.3 3.7 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] I4(1)/a # 88 centro 1 176 0.054 4432 0.6 / 3.7 3.72 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2007may0002.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) Inf - 2.15 103 108 95.4 9.21 60.6 29.69 0.0305 0.0282 2.15 - 1.65 120 120 100.0 10.93 26.1 29.74 0.0400 0.0230 1.65 - 1.40 138 138 100.0 11.00 9.3 20.25 0.0754 0.0342 1.40 - 1.25 128 128 100.0 10.86 8.4 16.80 0.0838 0.0391 1.25 - 1.15 140 140 100.0 9.19 10.6 17.44 0.0827 0.0409 1.15 - 1.05 188 188 100.0 7.90 7.8 12.72 0.0989 0.0526 1.05 - 1.00 132 132 100.0 7.38 5.0 11.19 0.1375 0.0659 1.00 - 0.95 152 152 100.0 5.78 3.9 7.67 0.1536 0.0900 0.95 - 0.90 171 171 100.0 4.84 2.4 5.30 0.2377 0.1388 0.90 - 0.85 251 251 100.0 4.70 2.5 4.57 0.2616 0.1492 0.85 - 0.80 276 276 100.0 4.16 1.7 3.34 0.3506 0.2279 0.80 - 0.77 229 229 100.0 3.98 1.3 2.67 0.4641 0.3060 ------------------------------------------------------------------------------ 0.90 - 0.77 756 756 100.0 4.29 1.8 3.55 0.3317 0.2100 Inf - 0.77 2028 2033 99.8 6.84 8.7 11.16 0.0702 0.0517 Merged [A], lowest resolution = 6.12 Angstroms, 595 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2007may0002.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C9H10O3 Formula weight = 166.17 Tentative Z (number of formula units/cell) = 14.0 giving rho = 1.195, non-H atomic volume = 19.2 and following cell contents and analysis: C 126.00 65.05 % H 140.00 6.07 % O 42.00 28.89 % F(000) = 1232.0 Mo-K(alpha) radiation Mu (mm-1) = 0.09 ------------------------------------------------------------------------------- File 2007may0002.ins set up as follows: TITL 2007may0002 in I4(1)/a CELL 0.71073 22.5496 22.5496 6.3581 90.000 90.000 90.000 ZERR 14.00 0.0004 0.0004 0.0002 0.000 0.000 0.000 LATT 2 SYMM 0.5-X, -Y, 0.5+Z SYMM 0.75-Y, 0.25+X, 0.25+Z SYMM 0.75+Y, 0.75-X, 0.75+Z SFAC C H O UNIT 126 140 42 TEMP 0.12 TREF HKLF 4 END -------------------------------------------------------------------------------