++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + 2007src0831 started at 12:51:06 on 05-Jul-2007 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 7.820 19.169 11.384 90.00 100.73 90.00 22137 Reflections read from file 2007src0831.hkl; mean (I/sigma) = 6.38 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 11042 11047 11065 11079 16577 14740 14758 22137 N (int>3sigma) = 0 7006 6752 7130 7004 10444 9476 9514 14187 Mean intensity = 0.0 29.7 25.3 28.8 26.5 27.9 28.5 28.7 28.4 Mean int/sigma = 0.0 6.4 6.2 6.5 6.4 6.4 6.5 6.5 6.5 Lattice type: P chosen Volume: 1676.72 ------------------------------------------------------------------------------- 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: 7.820 11.384 19.169 90.00 90.00 100.73 Niggli form: a.a = 61.16 b.b = 129.59 c.c = 367.45 b.c = 0.00 a.c = 0.00 a.b = -16.57 ------------------------------------------------------------------------------- Search for higher metric symmetry Identical indices and Friedel opposites combined before calculating R(sym) ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC P-lattice R(sym) = 0.037 [ 3616] Cell: 7.820 19.169 11.384 90.00 100.73 90.00 Volume: 1676.72 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 11042 11047 11065 11079 16577 14740 14758 22137 N (int>3sigma) = 0 7006 6752 7130 7004 10444 9476 9514 14187 Mean intensity = 0.0 29.7 25.3 28.8 26.5 27.9 28.5 28.7 28.4 Mean int/sigma = 0.0 6.4 6.2 6.5 6.4 6.4 6.5 6.5 6.5 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.972 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 33 338 334 336 N I>3s 0 136 136 0 0.3 36.5 36.9 0.4 0.4 5.0 5.1 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 0.037 3616 0.5 / 5.0 2.19 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2007src0831.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) Inf - 2.10 200 208 96.2 7.17 98.2 35.83 0.0276 0.0256 2.10 - 1.65 213 213 100.0 7.69 72.2 35.79 0.0364 0.0229 1.65 - 1.40 261 261 100.0 7.73 45.7 28.88 0.0451 0.0253 1.40 - 1.25 266 266 100.0 7.69 31.7 22.43 0.0563 0.0315 1.25 - 1.15 257 257 100.0 7.76 22.6 18.10 0.0745 0.0384 1.15 - 1.05 381 381 100.0 7.53 18.6 14.58 0.0875 0.0467 1.05 - 1.00 246 246 100.0 6.54 15.6 12.09 0.1069 0.0577 1.00 - 0.95 297 297 100.0 5.88 16.5 11.20 0.1063 0.0630 0.95 - 0.90 377 377 100.0 5.19 11.7 8.79 0.1387 0.0809 0.90 - 0.85 462 463 99.8 3.84 10.3 6.62 0.1559 0.1121 0.85 - 0.80 581 581 100.0 3.10 6.8 4.57 0.1913 0.1682 0.80 - 0.77 420 432 97.2 2.75 5.1 3.30 0.2659 0.2455 ------------------------------------------------------------------------------ 0.90 - 0.77 1463 1476 99.1 3.23 7.4 4.85 0.1866 0.1589 Inf - 0.77 3961 3982 99.5 5.56 23.3 13.94 0.0631 0.0497 Merged [A], lowest resolution = 6.97 Angstroms, 805 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2007src0831.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C17H18N1O3Fe1 Formula weight = 340.17 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.348, non-H atomic volume = 19.1 and following cell contents and analysis: C 68.00 60.02 % H 72.00 5.33 % N 4.00 4.12 % O 12.00 14.11 % Fe 4.00 16.42 % F(000) = 708.0 Mo-K(alpha) radiation Mu (mm-1) = 0.91 ------------------------------------------------------------------------------- File 2007src0831.ins set up as follows: TITL 2007src0831 in P2(1)/n CELL 0.71073 7.8204 19.1689 11.3839 90.000 100.727 90.000 ZERR 4.00 0.0002 0.0006 0.0003 0.000 0.002 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N O FE UNIT 68 72 4 12 4 TEMP 0.08 TREF HKLF 4 END -------------------------------------------------------------------------------