++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 07skc0018 started at 11:34:48 on 20-FEB-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 6.631 11.550 22.226 90.00 90.00 90.00 10325 Reflections read from file 07skc0018.hkl; mean (I/sigma) = 5.87 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 5137 5165 5206 5136 7754 6891 6898 10325 N (int>3sigma) = 0 3079 3059 3192 3067 4665 4218 4243 6310 Mean intensity = 0.0 215.5 188.5 215.8 211.7 206.6 209.8 212.3 212.7 Mean int/sigma = 0.0 5.8 5.7 6.0 5.9 5.8 5.9 5.9 5.9 Lattice type: P chosen Volume: 1702.31 ------------------------------------------------------------------------------- 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: 6.631 11.550 22.226 90.00 90.00 90.00 Niggli form: a.a = 43.97 b.b = 133.41 c.c = 494.01 b.c = 0.00 a.c = 0.00 a.b = 0.00 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. ORTHORHOMBIC P-lattice R(int) = 0.067 [ 8051] Cell: 6.631 11.550 22.226 90.00 90.00 90.00 Volume: 1702.31 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 5137 5165 5206 5136 7754 6891 6898 10325 N (int>3sigma) = 0 3079 3059 3192 3067 4665 4218 4243 6310 Mean intensity = 0.0 215.5 188.5 215.8 211.7 206.6 209.8 212.3 212.7 Mean int/sigma = 0.0 5.8 5.7 6.0 5.9 5.8 5.9 5.9 5.9 Crystal system O and Lattice type P selected Mean |E*E-1| = 0.756 [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 643 637 638 5 316 322 300 16 151 140 149 34 N I>3s 422 412 412 0 145 145 2 0 65 3 64 0 351.6 216.5 417.4 6.0 409.3 401.7 4.8 4.8 454.1 5.4 460.6 4.7 7.0 6.7 7.0 0.9 5.2 5.1 0.7 0.8 4.8 0.7 4.9 1.0 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] Pna2(1) # 33 non-cen 3 903 0.067 8051 1.0 / 4.8 2.57 [B] Pnma # 62 centro 2 894 0.067 8051 1.0 / 4.8 7.03 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C13H31O4N1 Formula weight = 265.39 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.036, non-H atomic volume = 23.6 and following cell contents and analysis: C 52.00 58.83 % H 124.00 11.77 % N 4.00 5.28 % O 16.00 24.12 % F(000) = 592.0 Mo-K(alpha) radiation Mu (mm-1) = 0.07 ------------------------------------------------------------------------------- File 07skc0018pna21.ins set up as follows: TITL 07skc0018pna21 in Pna2(1) CELL 0.71073 11.5504 22.2264 6.6309 90.000 90.000 90.000 ZERR 4.00 0.0007 0.0010 0.0004 0.000 0.000 0.000 LATT -1 SYMM -X, -Y, 0.5+Z SYMM 0.5+X, 0.5-Y, Z SYMM 0.5-X, 0.5+Y, 0.5+Z SFAC C H N O UNIT 52 124 4 16 TEMP 0.04 TREF HKLF 4 END 10325 Reflections written to new reflection file 07skc0018pna21.hkl -------------------------------------------------------------------------------