++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 06skc0048 started at 20:13:07 on 07-SEP-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 4.639 10.406 22.888 90.00 90.00 90.00 7004 Reflections read from file 06skc0048.hkl; mean (I/sigma) = 2.97 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 3504 3515 3505 3448 5262 4665 4656 7004 N (int>3sigma) = 0 1278 1223 1267 1143 1884 1741 1735 2592 Mean intensity = 0.0 97.8 86.4 104.4 80.9 96.2 99.6 98.9 99.5 Mean int/sigma = 0.0 3.0 2.9 3.0 2.8 3.0 3.1 3.1 3.1 Lattice type: P chosen Volume: 1104.91 ------------------------------------------------------------------------------- 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: 4.639 10.406 22.888 90.00 90.00 90.00 Niggli form: a.a = 21.52 b.b = 108.28 c.c = 523.88 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) = 0.152 [ 5530] Cell: 4.639 10.406 22.888 90.00 90.00 90.00 Volume: 1104.91 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.138 [ 4658] Cell: 4.639 22.888 10.406 90.00 90.00 90.00 Volume: 1104.91 Matrix: 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option C: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.135 [ 4427] Cell: 10.406 4.639 22.888 90.00 90.00 90.00 Volume: 1104.91 Matrix: 0.0000 -1.0000 0.0000 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option D: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.136 [ 4585] Cell: 4.639 10.406 22.888 90.00 90.00 90.00 Volume: 1104.91 Matrix:-1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option E: FOM = 0.000 deg. TRICLINIC P-lattice R(int) = 0.106 [ 2992] Cell: 4.639 10.406 22.888 90.00 90.00 90.00 Volume: 1104.91 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 3504 3515 3505 3448 5262 4665 4656 7004 N (int>3sigma) = 0 1278 1223 1267 1143 1884 1741 1735 2592 Mean intensity = 0.0 97.8 86.4 104.4 80.9 96.2 99.6 98.9 99.5 Mean int/sigma = 0.0 3.0 2.9 3.0 2.8 3.0 3.1 3.1 3.1 Crystal system O and Lattice type P selected Mean |E*E-1| = 0.773 [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 547 545 534 6 255 265 256 13 90 90 88 26 N I>3s 242 230 218 0 89 89 0 0 27 0 27 0 102.0 82.6 89.9 9.8 113.6 108.6 9.3 3.6 489.9 7.1 500.1 15.1 3.8 3.7 3.5 1.1 3.0 2.8 0.6 0.5 2.8 0.7 2.8 0.9 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] Pna2(1) # 33 non-cen 3 903 0.152 5530 1.1 / 2.8 4.83 [B] Pnma # 62 centro 2 894 0.152 5530 1.1 / 2.8 8.48 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C10H16O4N2 Formula weight = 228.25 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.372, non-H atomic volume = 17.3 and following cell contents and analysis: C 40.00 52.62 % H 64.00 7.07 % N 8.00 12.28 % O 16.00 28.04 % F(000) = 488.0 Mo-K(alpha) radiation Mu (mm-1) = 0.11 ------------------------------------------------------------------------------- File 06skc0048pna21.ins set up as follows: TITL 06skc0048pna21 in Pna2(1) CELL 0.71073 10.4056 22.8884 4.6392 90.000 90.000 90.000 ZERR 4.00 0.0016 0.0040 0.0009 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 40 64 8 16 TEMP 0.06 TREF HKLF 4 END 7004 Reflections written to new reflection file 06skc0048pna21.hkl -------------------------------------------------------------------------------