++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + 07skc0031 started at 17:41:08 on 22-Jul-2007 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 7.653 6.969 10.560 90.00 104.62 90.00 7450 Reflections read from file 07skc0031.hkl; mean (I/sigma) = 5.06 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 3719 3721 3728 3706 5584 4967 4978 7450 N (int>3sigma) = 0 2095 2188 2105 2181 3194 2876 2930 4321 Mean intensity = 0.0 11.9 13.4 12.0 12.9 12.4 13.5 14.1 13.6 Mean int/sigma = 0.0 5.0 5.3 4.9 5.2 5.0 5.1 5.2 5.1 Lattice type: P chosen Volume: 545.04 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 -1.0000 0.0000 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 Unitcell: 6.969 7.653 10.560 104.62 90.00 90.00 Niggli form: a.a = 48.57 b.b = 58.57 c.c = 111.52 b.c = -20.40 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. MONOCLINIC P-lattice R(sym) = 0.061 [ 1123] Cell: 7.653 6.969 10.560 90.00 104.62 90.00 Volume: 545.04 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 3719 3721 3728 3706 5584 4967 4978 7450 N (int>3sigma) = 0 2095 2188 2105 2181 3194 2876 2930 4321 Mean intensity = 0.0 11.9 13.4 12.0 12.9 12.4 13.5 14.1 13.6 Mean int/sigma = 0.0 5.0 5.3 4.9 5.2 5.0 5.1 5.2 5.1 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.793 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 14 375 375 368 N I>3s 0 212 227 249 0.3 24.1 19.2 28.2 0.6 5.4 5.7 6.7 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) # 4 chiral 1 3543 0.061 1123 0.6 / 5.1 2.31 [B] P2(1)/m # 11 centro 1 402 0.061 1123 0.6 / 5.1 5.27 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C9H14O6N2 Formula weight = 246.22 Tentative Z (number of formula units/cell) = 2.0 giving rho = 1.500, non-H atomic volume = 16.0 and following cell contents and analysis: C 18.00 43.90 % H 28.00 5.73 % N 4.00 11.38 % O 12.00 38.99 % F(000) = 260.0 Mo-K(alpha) radiation Mu (mm-1) = 0.13 ------------------------------------------------------------------------------- File 07skc0031p21.ins set up as follows: TITL 07skc0031p21 in P2(1) CELL 0.71073 7.6534 6.9693 10.5603 90.000 104.616 90.000 ZERR 2.00 0.0008 0.0007 0.0010 0.000 0.005 0.000 LATT -1 SYMM -X, 0.5+Y, -Z SFAC C H N O UNIT 18 28 4 12 TEMP 0.02 TREF HKLF 4 END 7450 Reflections written to new reflection file 07skc0031p21.hkl -------------------------------------------------------------------------------