++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 06skc0036 started at 10:20:40 on 24-AUG-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 9.687 6.546 10.821 90.00 102.70 90.00 7124 Reflections read from file 06skc0036.hkl; mean (I/sigma) = 12.50 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 3569 3582 3545 3566 5348 4744 4744 7124 N (int>3sigma) = 0 2560 2660 2602 2650 3911 3436 3543 5272 Mean intensity = 0.0 264.6 267.3 272.8 254.6 268.2 268.1 257.0 260.2 Mean int/sigma = 0.0 12.1 12.3 12.6 12.8 12.3 12.5 12.5 12.6 Lattice type: P chosen Volume: 669.41 ------------------------------------------------------------------------------- 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: 6.546 9.687 10.821 102.70 90.00 90.00 Niggli form: a.a = 42.85 b.b = 93.84 c.c = 117.09 b.c = -23.04 a.c = 0.00 a.b = 0.00 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.032 [ 6063] Cell: 9.687 6.546 10.821 90.00 102.70 90.00 Volume: 669.41 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 3569 3582 3545 3566 5348 4744 4744 7124 N (int>3sigma) = 0 2560 2660 2602 2650 3911 3436 3543 5272 Mean intensity = 0.0 264.6 267.3 272.8 254.6 268.2 268.1 257.0 260.2 Mean int/sigma = 0.0 12.1 12.3 12.6 12.8 12.3 12.5 12.5 12.6 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.990 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 15 391 403 392 N I>3s 2 175 2 175 1.4 294.4 1.7 293.7 1.1 9.1 0.5 9.1 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/c # 14 centro 1 19410 0.032 6063 1.1 / 9.1 1.23 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C6H10O5N1 Formula weight = 176.15 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.748, non-H atomic volume = 13.9 and following cell contents and analysis: C 24.00 40.91 % H 40.00 5.72 % N 4.00 7.95 % O 20.00 45.42 % F(000) = 372.0 Mo-K(alpha) radiation Mu (mm-1) = 0.15 ------------------------------------------------------------------------------- File 06skc0036p21c.ins set up as follows: TITL 06skc0036p21c in P2(1)/c CELL 0.71073 9.6872 6.5461 10.8209 90.000 102.698 90.000 ZERR 4.00 0.0005 0.0003 0.0005 0.000 0.003 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O UNIT 24 40 4 20 TEMP 0.1 TREF HKLF 4 END 7124 Reflections written to new reflection file 06skc0036p21c.hkl -------------------------------------------------------------------------------