++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + 2008src1307r started at 17:15:50 on 27-Jan-2009 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 9.025 11.272 14.477 90.00 102.35 90.00 16167 Reflections read from file 2008src1307r.hkl; mean (I/sigma) = 4.55 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 8114 8093 8073 8065 12140 10774 10714 16167 N (int>3sigma) = 0 3890 3858 3666 3816 5707 5119 5080 7662 Mean intensity = 0.0 9.6 10.3 8.2 9.6 9.4 9.4 9.7 9.4 Mean int/sigma = 0.0 4.7 4.7 4.4 4.7 4.6 4.7 4.7 4.7 Lattice type: P chosen Volume: 1438.70 ------------------------------------------------------------------------------- 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: 9.025 11.272 14.477 90.00 102.35 90.00 Niggli form: a.a = 81.46 b.b = 127.06 c.c = 209.58 b.c = 0.00 a.c = -27.95 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) = 0.064 [ 2799] Cell: 9.025 11.272 14.477 90.00 102.35 90.00 Volume: 1438.70 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 8114 8093 8073 8065 12140 10774 10714 16167 N (int>3sigma) = 0 3890 3858 3666 3816 5707 5119 5080 7662 Mean intensity = 0.0 9.6 10.3 8.2 9.6 9.4 9.4 9.7 9.4 Mean int/sigma = 0.0 4.7 4.7 4.4 4.7 4.6 4.7 4.7 4.7 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.922 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 22 466 503 497 N I>3s 0 3 175 174 0.7 0.6 10.1 10.2 0.6 0.7 4.2 4.3 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)/c # 14 centro 4 19410 0.064 2799 0.7 / 4.2 3.02 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2008src1307r.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) Inf - 2.10 178 187 95.2 6.64 47.2 24.28 0.0512 0.0331 2.10 - 1.65 191 191 100.0 7.03 16.0 21.35 0.0750 0.0320 1.65 - 1.40 224 224 100.0 7.04 8.6 16.68 0.1135 0.0446 1.40 - 1.25 240 240 100.0 6.88 7.4 13.81 0.1274 0.0478 1.25 - 1.15 228 228 100.0 6.73 6.7 13.73 0.1400 0.0519 1.15 - 1.05 332 334 99.4 5.54 6.3 12.20 0.1442 0.0591 1.05 - 1.00 210 210 100.0 4.98 3.7 8.50 0.2050 0.0933 1.00 - 0.95 260 260 100.0 4.61 2.7 6.74 0.2872 0.1316 0.95 - 0.90 302 305 99.0 4.02 2.7 5.85 0.2887 0.1559 0.90 - 0.85 413 418 98.8 3.17 2.0 3.97 0.4068 0.2581 0.85 - 0.80 485 501 96.8 2.64 1.8 3.09 0.4761 0.3733 0.80 - 0.76 386 451 85.6 1.89 1.7 2.14 0.5555 0.5533 ------------------------------------------------------------------------------ 0.90 - 0.76 1284 1370 93.7 2.55 1.9 3.09 0.4608 0.3824 Inf - 0.76 3449 3549 97.2 4.56 6.8 9.25 0.1121 0.0833 Merged [A], lowest resolution = 6.20 Angstroms, 241 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2008src1307r.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C13H20N2 Formula weight = 204.31 Tentative Z (number of formula units/cell) = 5.0 giving rho = 1.179, non-H atomic volume = 19.2 and following cell contents and analysis: C 65.00 76.42 % H 100.00 9.87 % N 10.00 13.71 % F(000) = 560.0 Mo-K(alpha) radiation Mu (mm-1) = 0.07 ------------------------------------------------------------------------------- File 2008src1307p21c.ins set up as follows: TITL 2008src1307p21c in P2(1)/c CELL 0.71073 14.4770 11.2719 9.0254 90.000 102.352 90.000 ZERR 5.00 0.0005 0.0004 0.0003 0.000 0.002 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N UNIT 65 100 10 TEMP 0.01 TREF HKLF 4 END -------------------------------------------------------------------------------