++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 06skc0082 started at 16:49:31 on 05-FEB-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 7.053 7.519 18.931 79.45 90.04 89.99 28732 Reflections read from file 06skc0082.hkl; mean (I/sigma) = 6.23 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 14392 14383 14277 14272 21526 19140 19190 28732 N (int>3sigma) = 0 8248 8583 8325 7878 12578 11384 11361 17102 Mean intensity = 0.0 258.5 269.6 270.6 224.5 266.3 268.7 271.5 264.2 Mean int/sigma = 0.0 6.0 6.3 6.1 5.8 6.1 6.3 6.3 6.3 Lattice type: P chosen Volume: 987.03 ------------------------------------------------------------------------------- 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: 7.053 7.519 18.931 100.55 90.04 90.01 Niggli form: a.a = 49.75 b.b = 56.54 c.c = 358.37 b.c = -26.07 a.c = -0.09 a.b = -0.01 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.902 deg. ORTHORHOMBIC C-lattice R(int) = 0.580 [ 27368] Cell: 7.519 37.226 7.053 90.04 90.01 89.10 Volume: 1974.05 Matrix: 0.0000 1.0000 0.0000 0.0000 1.0000 -2.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.043 deg. MONOCLINIC P-lattice R(int) = 0.067 [ 26251] Cell: 7.519 7.053 18.931 89.96 100.55 89.99 Volume: 987.03 Matrix: 0.0000 1.0000 0.0000 1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option C: FOM = 0.901 deg. MONOCLINIC C-lattice R(int) = 0.577 [ 26247] Cell: 37.226 7.519 7.053 89.99 90.04 90.90 Volume: 1974.05 Matrix: 0.0000 1.0000 -2.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option D: FOM = 0.902 deg. MONOCLINIC C-lattice R(int) = 0.576 [ 26379] Cell: 7.519 37.226 7.053 90.04 90.01 89.10 Volume: 1974.05 Matrix: 0.0000 1.0000 0.0000 0.0000 1.0000 -2.0000 -1.0000 0.0000 0.0000 Option B selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 14383 14392 14277 14272 21526 19140 19190 28732 N (int>3sigma) = 0 8583 8248 8325 7878 12578 11384 11361 17102 Mean intensity = 0.0 269.6 258.5 270.6 224.5 266.3 268.7 271.5 264.2 Mean int/sigma = 0.0 6.3 6.0 6.1 5.8 6.1 6.3 6.3 6.3 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.923 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 30 1200 1211 1151 N I>3s 0 543 533 20 6.4 413.9 409.5 6.7 0.8 5.9 5.8 0.9 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/n # 14 centro 1 19410 0.067 26251 0.9 / 5.8 2.24 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C8H612O4N2 Formula weight = 805.00 Tentative Z (number of formula units/cell) = 2.0 giving rho = 2.709, non-H atomic volume = 35.3 and following cell contents and analysis: C 16.00 11.94 % H 1224.00 76.63 % N 4.00 3.48 % O 8.00 7.95 % F(000) = 1412.0 Mo-K(alpha) radiation Mu (mm-1) = 0.13 ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C8H612O4N2 Formula weight = 805.00 Tentative Z (number of formula units/cell) = 2.0 giving rho = 2.709, non-H atomic volume = 35.3 and following cell contents and analysis: C 16.00 11.94 % H 1224.00 76.63 % N 4.00 3.48 % O 8.00 7.95 % F(000) = 1412.0 Mo-K(alpha) radiation Mu (mm-1) = 0.13 ------------------------------------------------------------------------------- File 06skc0082p21n.ins set up as follows: TITL 06skc0082p21n in P2(1)/n CELL 0.71073 7.5192 7.0534 18.9307 90.000 100.552 90.000 ZERR 2.00 0.0003 0.0003 0.0008 0.000 0.002 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N O UNIT 16 1224 4 8 TEMP 0.05 TREF HKLF 4 END 28732 Reflections written to new reflection file 06skc0082p21n.hkl -------------------------------------------------------------------------------