++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + s92 started at 12:35:53 on 16-Jun-2003 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 9.632 16.636 9.858 90.00 103.59 90.00 6915 Reflections read from file s92.hkl; mean (I/sigma) = 11.01 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 3459 3457 3462 3471 5189 4609 4613 6915 N (int>3sigma) = 0 2441 2309 2446 2466 3598 3266 3251 4878 Mean intensity = 0.0 151.3 108.2 159.7 129.6 139.7 154.9 151.2 151.6 Mean int/sigma = 0.0 11.1 10.1 11.1 10.9 10.8 11.1 11.1 11.1 Lattice type: P chosen Volume: 1535.53 ------------------------------------------------------------------------------- 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: 9.632 9.858 16.636 90.00 90.00 103.59 Niggli form: a.a = 92.79 b.b = 97.19 c.c = 276.75 b.c = 0.00 a.c = 0.00 a.b = -22.32 ------------------------------------------------------------------------------- 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) = 0.000 [ 0] Cell: 9.632 16.636 9.858 90.00 103.59 90.00 Volume: 1535.53 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 3459 3457 3462 3471 5189 4609 4613 6915 N (int>3sigma) = 0 2441 2309 2446 2466 3598 3266 3251 4878 Mean intensity = 0.0 151.3 108.2 159.7 129.6 139.7 154.9 151.2 151.6 Mean int/sigma = 0.0 11.1 10.1 11.1 10.9 10.8 11.1 11.1 11.1 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.982 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 19 119 117 120 N I>3s 9 53 50 11 12.0 340.4 346.2 1.6 3.6 9.6 9.7 1.2 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/n # 13 centro 1 292 0.000 0 1.2 / 3.6 4.45 [B] Pn # 7 non-cen 1 226 0.000 0 1.2 / 3.6 10.56 Option [A] chosen ------------------------------------------------------------------------------- Input space group symbol: P2(1)/n Number: 14 centrosymmetric CSD frequency: 19410 R(sym) = 0.000 0 reflections merged Systematic absence exceptions: -21- -a- -c- -n- N 19 119 117 120 N I>3s 9 53 50 11 12.0 340.4 346.2 1.6 3.6 9.6 9.7 1.2 ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 s92.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) Inf - 2.10 184 194 94.8 1.74 686.0 33.98 0.0194 0.0276 2.10 - 1.65 195 195 100.0 1.90 495.1 35.18 0.0166 0.0237 1.65 - 1.45 183 183 100.0 1.90 397.2 32.33 0.0189 0.0257 1.45 - 1.30 216 216 100.0 1.92 257.6 27.89 0.0202 0.0272 1.30 - 1.20 192 192 100.0 1.93 199.3 25.75 0.0204 0.0309 1.20 - 1.10 294 294 100.0 1.93 172.7 19.61 0.0253 0.0366 1.10 - 1.05 194 194 100.0 1.90 132.2 16.87 0.0308 0.0411 1.05 - 1.00 220 220 100.0 1.94 92.8 14.31 0.0453 0.0499 1.00 - 0.95 278 278 100.0 1.92 76.1 10.59 0.0415 0.0609 0.95 - 0.90 338 338 100.0 1.92 53.1 8.91 0.0639 0.0801 0.90 - 0.85 428 430 99.5 1.89 33.3 6.42 0.0897 0.1139 0.85 - 0.80 521 522 99.8 1.90 33.7 5.53 0.0925 0.1302 0.80 - 0.77 393 402 97.8 1.80 28.7 4.24 0.1396 0.1730 ------------------------------------------------------------------------------ 0.90 - 0.77 1342 1354 99.1 1.87 32.1 5.43 0.1030 0.1360 Inf - 0.77 3636 3658 99.4 1.89 156.3 15.25 0.0305 0.0402 Merged [A], lowest resolution = 6.96 Angstroms, 58 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 s92.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C13H19N2P1F6 Formula weight = 348.27 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.506, non-H atomic volume = 17.4 and following cell contents and analysis: C 52.00 44.83 % H 76.00 5.50 % N 8.00 8.05 % F 24.00 32.73 % P 4.00 8.89 % F(000) = 720.0 Mo-K(alpha) radiation Mu (mm-1) = 0.24 ------------------------------------------------------------------------------- File s92.ins set up as follows: TITL s92 in P2(1)/n CELL 0.71073 9.6325 16.6358 9.8585 90.000 103.591 90.000 ZERR 4.00 0.0003 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 F P UNIT 52 76 8 24 4 TREF HKLF 4 END -------------------------------------------------------------------------------