++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + 2007src0806 started at 12:14:01 on 02-Jul-2007 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 11.936 17.285 21.441 90.00 92.58 90.00 39822 Reflections read from file 2007src0806.hkl; mean (I/sigma) = 4.44 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 19812 19865 19939 19897 29808 26627 26574 39822 N (int>3sigma) = 0 8496 8926 9186 9180 13304 12200 12048 18133 Mean intensity = 0.0 50.7 57.5 63.1 61.5 57.1 65.0 61.4 63.9 Mean int/sigma = 0.0 4.3 4.5 4.7 4.6 4.5 4.6 4.5 4.6 Lattice type: P chosen Volume: 4418.84 ------------------------------------------------------------------------------- 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: 11.936 17.285 21.441 90.00 92.58 90.00 Niggli form: a.a = 142.47 b.b = 298.75 c.c = 459.70 b.c = 0.00 a.c = -11.53 a.b = 0.00 ------------------------------------------------------------------------------- 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) = 0.069 [ 7776] Cell: 11.936 17.285 21.441 90.00 92.58 90.00 Volume: 4418.84 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 19812 19865 19939 19897 29808 26627 26574 39822 N (int>3sigma) = 0 8496 8926 9186 9180 13304 12200 12048 18133 Mean intensity = 0.0 50.7 57.5 63.1 61.5 57.1 65.0 61.4 63.9 Mean int/sigma = 0.0 4.3 4.5 4.7 4.6 4.5 4.6 4.5 4.6 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.937 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 30 832 798 832 N I>3s 0 292 0 292 2.5 59.4 3.4 59.4 0.6 4.0 0.6 4.0 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)/c # 14 centro 1 19410 0.069 7776 0.6 / 4.0 3.08 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2007src0806.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) Inf - 2.10 526 544 96.7 6.43 249.4 25.00 0.0398 0.0291 2.10 - 1.65 562 562 100.0 6.83 129.9 21.62 0.0580 0.0317 1.65 - 1.40 690 690 100.0 6.56 78.0 16.95 0.0804 0.0418 1.40 - 1.25 708 708 100.0 5.16 51.5 12.13 0.1051 0.0625 1.25 - 1.15 703 703 100.0 4.46 40.0 9.26 0.1191 0.0814 1.15 - 1.05 977 978 99.9 4.10 27.0 6.89 0.1598 0.1149 1.05 - 1.00 639 640 99.8 3.82 22.1 6.02 0.1897 0.1457 1.00 - 0.95 792 798 99.2 3.06 19.7 4.20 0.2275 0.1972 0.95 - 0.90 983 992 99.1 2.78 17.0 3.51 0.2732 0.2486 0.90 - 0.85 1191 1204 98.9 2.64 13.4 2.73 0.3540 0.3304 0.85 - 0.80 1516 1537 98.6 2.44 10.7 2.01 0.4809 0.4492 0.80 - 0.77 1158 1234 93.8 2.11 8.5 1.49 0.6348 0.6212 ------------------------------------------------------------------------------ 0.90 - 0.77 3865 3975 97.2 2.40 10.9 2.08 0.4561 0.4441 Inf - 0.77 10445 10590 98.6 3.76 41.9 7.42 0.0918 0.1004 Merged [A], lowest resolution = 7.00 Angstroms, 458 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2007src0806.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C29H31Fe1B1N1 Formula weight = 460.21 Tentative Z (number of formula units/cell) = 8.0 giving rho = 1.384, non-H atomic volume = 17.3 and following cell contents and analysis: C 232.00 75.68 % H 248.00 6.79 % B 8.00 2.35 % N 8.00 3.04 % Fe 8.00 12.14 % F(000) = 1944.0 Mo-K(alpha) radiation Mu (mm-1) = 0.70 ------------------------------------------------------------------------------- File 2007src0806.ins set up as follows: TITL 2007src0806 in P2(1)/c CELL 0.71073 11.9359 17.2845 21.4406 90.000 92.581 90.000 ZERR 8.00 0.0003 0.0005 0.0006 0.000 0.002 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H B N FE UNIT 232 248 8 8 8 TEMP 0.02 TREF HKLF 4 END -------------------------------------------------------------------------------