++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + s92 started at 13:32:36 on 03-Mar-2003 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 17.133 10.965 17.449 89.97 114.25 90.04 16079 Reflections read from file s92.hkl; mean (I/sigma) = 5.64 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 8035 8081 8022 8098 12069 10695 10716 16079 N (int>3sigma) = 0 3951 4131 4060 4048 6071 5291 5338 8008 Mean intensity = 0.0 173.6 171.7 164.4 170.1 169.9 169.6 164.9 169.7 Mean int/sigma = 0.0 5.7 5.8 5.8 5.8 5.8 5.7 5.7 5.8 Lattice type: P chosen Volume: 2989.10 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 1.0000 0.0000 -1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 Unitcell: 10.965 17.133 17.449 65.75 89.97 89.96 Niggli form: a.a = 120.24 b.b = 293.55 c.c = 304.49 b.c = 122.78 a.c = 0.10 a.b = 0.15 ------------------------------------------------------------------------------- Search for higher metric symmetry Identical indices and Friedel opposites combined before calculating R(sym) ------------------------------------------------------------------------------ Option A: FOM = 0.046 deg. MONOCLINIC P-lattice R(sym) = 0.061 [ 2516] Cell: 17.133 10.965 17.449 89.97 114.25 90.04 Volume: 2989.10 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 8035 8081 8022 8098 12069 10695 10716 16079 N (int>3sigma) = 0 3951 4131 4060 4048 6071 5291 5338 8008 Mean intensity = 0.0 173.6 171.7 164.4 170.1 169.9 169.6 164.9 169.7 Mean int/sigma = 0.0 5.7 5.8 5.8 5.8 5.8 5.7 5.7 5.8 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.908 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 0 483 468 489 N I>3s 0 165 1 166 0.0 207.7 8.3 205.5 0.0 4.6 0.6 4.6 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/c # 13 centro 1 292 0.061 2516 0.6 / 4.6 3.16 [B] Pc # 7 non-cen 1 226 0.061 2516 0.6 / 4.6 5.87 [C] P2(1)/c # 14 centro 1 19410 0.061 2516 0.6 / 4.6 2.83 Option [C] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 s92.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) Inf - 2.60 827 356 232.3 2.32 644.3 13.75 0.0550 2.60 - 2.05 897 376 238.6 2.39 322.2 10.91 0.0624 2.05 - 1.80 880 353 249.3 2.49 354.3 10.19 0.0642 1.80 - 1.60 1013 451 224.6 2.25 332.6 10.09 0.0670 1.60 - 1.45 890 512 173.8 1.74 227.9 9.09 0.0795 1.45 - 1.35 827 492 168.1 1.68 217.1 8.19 0.0861 1.35 - 1.25 1157 678 170.6 1.71 153.8 6.97 0.1083 1.25 - 1.15 1362 902 151.0 1.51 147.0 5.83 0.1231 1.15 - 1.05 1654 1325 124.8 1.25 104.5 4.53 0.1748 1.05 - 1.00 832 809 102.8 1.03 66.3 2.99 0.3213 1.00 - 0.95 1080 1077 100.3 1.00 58.0 2.64 0.3442 0.95 - 0.90 1210 1267 95.5 0.96 50.5 2.12 0.4372 0.90 - 0.85 1294 1594 81.2 0.81 39.7 1.57 0.6138 0.85 - 0.80 1402 2053 68.3 0.68 28.9 1.05 0.9495 0.80 - 0.77 754 1587 47.5 0.48 21.7 0.69 1.4461 ------------------------------------------------------------------------------ 0.90 - 0.77 3450 5234 65.9 0.66 31.4 1.16 0.8654 Inf - 0.77 16079 13832 116.2 1.16 167.4 5.64 0.1320 Merged [N], lowest resolution = 4.21 Angstroms, 0 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 s92.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C14 H13 N3 Br3 Formula weight = 463.00 Tentative Z (number of formula units/cell) = 8.0 giving rho = 2.058, non-H atomic volume = 18.7 and following cell contents and analysis: C 112.00 36.32 % H 104.00 2.83 % N 24.00 9.08 % Br 24.00 51.78 % F(000) = 1784.0 Mo-K(alpha) radiation Mu (mm-1) = 8.09 ------------------------------------------------------------------------------- File s92.ins set up as follows: TITL s92 in P2(1)/c CELL 0.71073 17.1333 10.9654 17.4495 90.000 114.247 90.000 ZERR 8.00 0.0353 0.0079 0.0145 0.000 0.065 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N BR UNIT 112 104 24 24 TEMP 0 TREF HKLF 4 END -------------------------------------------------------------------------------