+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 2007/1 for Windows + + Copyright(C) 2007 Bruker-AXS All Rights Reserved + + 2007src1313 started at 10:00:21 on 09-Oct-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 8.401 10.711 20.792 90.00 94.92 90.00 31015 Reflections read from file 2007src1313.hkl; mean (I/sigma) = 6.08 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 15495 15522 15635 15487 23326 20663 20672 31015 N (int>3sigma) = 0 9868 9999 9189 10005 14528 13343 13315 19909 Mean intensity = 0.0 18.3 18.8 13.4 19.2 16.9 18.8 18.9 18.6 Mean int/sigma = 0.0 6.2 6.2 5.6 6.2 6.0 6.2 6.2 6.2 Lattice type: P chosen Volume: 1864.19 ------------------------------------------------------------------------------- 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: 8.401 10.711 20.792 90.00 94.92 90.00 Niggli form: a.a = 70.58 b.b = 114.73 c.c = 432.32 b.c = 0.00 a.c = -14.99 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) = 0.038 [ 3978] Cell: 8.401 10.711 20.792 90.00 94.92 90.00 Volume: 1864.19 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 15495 15522 15635 15487 23326 20663 20672 31015 N (int>3sigma) = 0 9868 9999 9189 10005 14528 13343 13315 19909 Mean intensity = 0.0 18.3 18.8 13.4 19.2 16.9 18.8 18.9 18.6 Mean int/sigma = 0.0 6.2 6.2 5.6 6.2 6.0 6.2 6.2 6.2 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.979 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 26 930 926 922 N I>3s 0 6 326 330 0.2 0.2 21.7 21.8 0.9 0.6 4.0 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 4 19410 0.038 3978 0.9 / 4.0 2.98 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2007src1313.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) Rsigma Inf - 2.11 228 238 95.8 9.94 82.7 31.83 0.0477 0.0351 2.11 - 1.68 226 226 100.0 11.04 39.4 33.96 0.0498 0.0238 1.68 - 1.47 231 231 100.0 11.25 34.3 33.10 0.0462 0.0221 1.47 - 1.33 234 234 100.0 11.15 20.4 27.67 0.0614 0.0283 1.33 - 1.23 232 232 100.0 10.66 20.6 27.79 0.0641 0.0285 1.23 - 1.16 229 229 100.0 8.55 14.1 20.65 0.0754 0.0359 1.16 - 1.10 244 244 100.0 8.16 11.7 17.91 0.0861 0.0416 1.10 - 1.04 289 289 100.0 7.45 10.9 15.75 0.0970 0.0477 1.04 - 1.00 234 234 100.0 6.85 7.7 13.72 0.1088 0.0503 1.00 - 0.96 273 273 100.0 5.77 5.4 10.27 0.1180 0.0669 0.96 - 0.93 238 238 100.0 4.92 3.8 8.27 0.1439 0.0909 0.93 - 0.90 284 284 100.0 4.77 3.0 6.83 0.1707 0.1058 0.90 - 0.87 314 314 100.0 4.73 2.7 6.65 0.1822 0.1143 0.87 - 0.84 341 341 100.0 4.44 2.2 5.33 0.2136 0.1473 0.84 - 0.82 288 288 100.0 4.38 1.8 4.30 0.2485 0.1861 0.82 - 0.80 297 297 100.0 4.11 2.4 5.05 0.2396 0.1630 0.80 - 0.78 307 310 99.0 3.77 1.7 3.48 0.2761 0.2399 0.78 - 0.77 14 31 45.2 0.74 1.8 2.39 0.4487 0.3153 ------------------------------------------------------------------------------ 0.87 - 0.77 1364 1384 98.6 4.13 2.0 4.64 0.2384 0.1767 Inf - 0.77 4503 4533 99.3 6.84 14.0 14.84 0.0633 0.0417 Merged [A], lowest resolution = 6.91 Angstroms, 1081 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2007src1313.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C16H20N2PF9 Formula weight = 442.30 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.576, non-H atomic volume = 16.6 and following cell contents and analysis: C 64.00 43.45 % H 80.00 4.56 % N 8.00 6.33 % F 36.00 38.66 % P 4.00 7.00 % F(000) = 904.0 Mo-K(alpha) radiation Mu (mm-1) = 0.24 ------------------------------------------------------------------------------- File 1.ins set up as follows: TITL 1 in P2(1)/c CELL 0.71073 20.7923 10.7114 8.4013 90.000 94.923 90.000 ZERR 4.00 0.0009 0.0005 0.0003 0.000 0.003 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N F P UNIT 64 80 8 36 4 TEMP 0.04 TREF HKLF 4 END 31015 Reflections written to new reflection file 1.hkl -------------------------------------------------------------------------------