++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 07skc0022 started at 15:47:51 on 20-FEB-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 7.648 11.204 11.673 90.00 90.02 86.45 15730 Reflections read from file 07skc0022.hkl; mean (I/sigma) = 3.77 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 7817 7805 7886 7841 11754 10515 10417 15730 N (int>3sigma) = 0 3257 3246 3229 3348 4866 4469 4453 6601 Mean intensity = 0.0 27.2 21.8 24.1 30.2 24.4 29.2 29.3 31.7 Mean int/sigma = 0.0 3.9 3.8 3.7 4.0 3.8 4.0 4.0 3.9 Lattice type: P chosen Volume: 998.32 ------------------------------------------------------------------------------- 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: 7.648 11.204 11.673 90.00 89.98 86.45 Niggli form: a.a = 58.49 b.b = 125.52 c.c = 136.26 b.c = 0.00 a.c = 0.03 a.b = 5.30 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.020 deg. MONOCLINIC P-lattice R(int) = 0.124 [ 13291] Cell: 7.648 11.673 11.204 90.00 93.55 90.02 Volume: 998.32 Matrix: 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.000 deg. TRICLINIC P-lattice R(int) = 0.106 [ 11143] Cell: 7.648 11.204 11.673 90.00 89.98 86.45 Volume: 998.32 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 7817 7886 7805 7841 11754 10455 10515 15730 N (int>3sigma) = 0 3257 3229 3246 3348 4866 4412 4469 6601 Mean intensity = 0.0 27.2 24.1 21.8 30.2 24.4 33.2 29.2 31.7 Mean int/sigma = 0.0 3.9 3.7 3.8 4.0 3.8 3.9 4.0 3.9 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.951 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 28 401 416 405 N I>3s 0 116 114 4 1.9 23.9 23.0 2.0 0.8 3.1 3.0 0.6 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/n # 14 centro 1 19410 0.124 13291 0.8 / 3.0 4.21 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C9H12O4N2 Formula weight = 212.21 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.412, non-H atomic volume = 16.6 and following cell contents and analysis: C 36.00 50.94 % H 48.00 5.70 % N 8.00 13.20 % O 16.00 30.16 % F(000) = 448.0 Mo-K(alpha) radiation Mu (mm-1) = 0.11 ------------------------------------------------------------------------------- File 07skc0022p21n.ins set up as follows: TITL 07skc0022p21n in P2(1)/n CELL 0.71073 7.6481 11.6731 11.2037 90.000 93.547 90.000 ZERR 4.00 0.0007 0.0009 0.0011 0.000 0.004 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N O UNIT 36 48 8 16 TEMP 0.01 TREF HKLF 4 END 15730 Reflections written to new reflection file 07skc0022p21n.hkl -------------------------------------------------------------------------------