+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 2005/1 for Windows + + Copyright(C) 2005 Bruker-AXS All Rights Reserved + + jsib001 started at 13:55:01 on 02-Nov-2005 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 10.010 12.463 16.423 90.00 90.00 90.00 17529 Reflections read from file jsib001.hkl; mean (I/sigma) = 6.49 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 8797 8770 8777 8779 13172 11671 11686 17529 N (int>3sigma) = 0 5125 5233 5282 5176 7820 6938 6946 10445 Mean intensity = 0.0 292.6 305.9 302.3 318.2 300.3 308.1 308.3 313.0 Mean int/sigma = 0.0 6.4 6.6 6.6 6.5 6.5 6.5 6.5 6.5 Lattice type: P chosen Volume: 2048.81 ------------------------------------------------------------------------------- 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: 10.010 12.463 16.423 90.00 90.00 90.00 Niggli form: a.a = 100.19 b.b = 155.33 c.c = 269.71 b.c = 0.00 a.c = 0.00 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. ORTHORHOMBIC P-lattice R(sym) = 0.057 [ 6305] Cell: 10.010 12.463 16.423 90.00 90.00 90.00 Volume: 2048.81 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 8797 8770 8777 8779 13172 11671 11686 17529 N (int>3sigma) = 0 5125 5233 5282 5176 7820 6938 6946 10445 Mean intensity = 0.0 292.6 305.9 302.3 318.2 300.3 308.1 308.3 313.0 Mean int/sigma = 0.0 6.4 6.6 6.6 6.5 6.5 6.5 6.5 6.5 Crystal system O and Lattice type P selected Mean |E*E-1| = 0.714 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: b-- c-- n-- 21-- -c- -a- -n- -21- --a --b --n --21 N 527 524 525 15 435 431 436 20 368 368 372 19 N I>3s 299 276 267 0 236 240 204 0 213 179 172 0 340.5 340.5 429.3 3.5 459.5 417.7 457.5 4.5 354.4 274.2 362.5 2.2 7.0 6.9 6.7 0.5 7.2 7.6 6.3 0.5 7.4 5.5 6.1 0.3 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)2(1)2(1) # 19 chiral 1 5917 0.057 6305 0.5 / 5.5 1.89 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 jsib001.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) Rsigma Inf - 2.25 139 139 100.0 7.95 1545.7 48.71 0.0254 0.0153 2.25 - 1.73 143 143 100.0 9.54 680.5 43.74 0.0378 0.0180 1.73 - 1.49 144 144 100.0 9.10 509.1 35.98 0.0488 0.0223 1.49 - 1.35 139 139 100.0 8.29 384.4 27.06 0.0655 0.0287 1.35 - 1.24 148 148 100.0 7.90 258.3 19.98 0.0882 0.0398 1.24 - 1.16 146 146 100.0 7.62 252.1 18.34 0.0893 0.0439 1.16 - 1.10 143 143 100.0 7.14 208.5 14.84 0.1022 0.0531 1.10 - 1.04 170 170 100.0 6.83 183.6 13.35 0.1188 0.0617 1.04 - 1.00 140 140 100.0 6.39 149.2 10.91 0.1330 0.0774 1.00 - 0.96 166 166 100.0 6.36 109.2 9.10 0.1673 0.0952 0.96 - 0.92 185 185 100.0 6.04 65.8 6.00 0.2220 0.1422 0.92 - 0.89 171 172 99.4 5.65 49.1 4.52 0.2873 0.1914 0.89 - 0.86 189 189 100.0 5.47 43.4 4.16 0.3037 0.2200 0.86 - 0.84 140 141 99.3 5.45 39.8 3.62 0.3571 0.2490 0.84 - 0.82 163 167 97.6 5.07 49.1 4.21 0.3109 0.2217 0.82 - 0.80 166 168 98.8 4.95 44.0 3.67 0.3692 0.2584 0.80 - 0.78 154 186 82.8 2.60 47.8 2.94 0.3310 0.3286 0.78 - 0.75 95 215 44.2 0.62 50.3 2.06 0.3160 0.4395 ------------------------------------------------------------------------------ 0.84 - 0.75 652 811 80.4 3.30 47.1 3.40 0.3356 0.2930 Inf - 0.75 2741 2901 94.5 6.04 246.5 14.65 0.0676 0.0487 Merged [A], lowest resolution = 16.42 Angstroms, 535 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 jsib001.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: NaPF6O3N2C16H26 Formula weight = 462.34 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.499, non-H atomic volume = 17.7 and following cell contents and analysis: C 64.00 41.56 % H 104.00 5.67 % N 8.00 6.06 % O 12.00 10.38 % F 24.00 24.65 % Na 4.00 4.97 % P 4.00 6.70 % F(000) = 960.0 Mo-K(alpha) radiation Mu (mm-1) = 0.23 ------------------------------------------------------------------------------- File jsib001.ins set up as follows: TITL jsib001 in P2(1)2(1)2(1) CELL 0.71073 10.0096 12.4633 16.4230 90.000 90.000 90.000 ZERR 4.00 0.0041 0.0050 0.0065 0.000 0.000 0.000 LATT -1 SYMM 0.5-X, -Y, 0.5+Z SYMM -X, 0.5+Y, 0.5-Z SYMM 0.5+X, 0.5-Y, -Z SFAC C H N O F NA P UNIT 64 104 8 12 24 4 4 TEMP -153 SIZE 0.08 0.10 0.20 TREF HKLF 4 END 17529 Reflections written to new reflection file jsib001.hkl -------------------------------------------------------------------------------