++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 04skc0009 started at 10:48:44 on 03-SEP-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 9.411 8.736 12.448 89.97 102.10 90.01 8284 Reflections read from file 04skc0009.hkl; mean (I/sigma) = 5.53 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 4162 4130 4132 4145 6212 5503 5539 8284 N (int>3sigma) = 0 2290 2241 2289 2300 3410 3074 3098 4615 Mean intensity = 0.0 187.2 164.8 167.8 175.4 173.3 173.9 171.0 176.3 Mean int/sigma = 0.0 5.5 5.4 5.6 5.7 5.5 5.6 5.6 5.6 Lattice type: P chosen Volume: 1000.70 ------------------------------------------------------------------------------- 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: 8.736 9.411 12.448 77.90 89.97 89.99 Niggli form: a.a = 76.33 b.b = 88.57 c.c = 154.95 b.c = 24.55 a.c = 0.06 a.b = 0.01 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.030 deg. MONOCLINIC P-lattice R(int) = 0.083 [ 5821] Cell: 9.411 8.736 12.448 89.97 102.10 90.01 Volume: 1000.70 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 4162 4130 4132 4145 6212 5503 5539 8284 N (int>3sigma) = 0 2290 2241 2289 2300 3410 3074 3098 4615 Mean intensity = 0.0 187.2 164.8 167.8 175.4 173.3 173.9 171.0 176.3 Mean int/sigma = 0.0 5.5 5.4 5.6 5.7 5.5 5.6 5.6 5.6 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.750 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 12 313 310 311 N I>3s 0 177 173 162 2.9 251.3 260.3 164.3 0.5 6.3 6.4 6.1 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1) # 4 chiral 1 3543 0.083 5821 0.5 / 5.6 1.84 [B] P2(1)/m # 11 centro 1 402 0.083 5821 0.5 / 5.6 6.79 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C7H16O6N2 Formula weight = 224.22 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.488, non-H atomic volume = 16.7 and following cell contents and analysis: C 28.00 37.49 % H 64.00 7.19 % N 8.00 12.50 % O 24.00 42.82 % F(000) = 480.0 Mo-K(alpha) radiation Mu (mm-1) = 0.13 ------------------------------------------------------------------------------- File o4skc0009p21.ins set up as follows: TITL o4skc0009p21 in P2(1) CELL 0.71073 9.4109 8.7365 12.4478 90.000 102.099 90.000 ZERR 4.00 0.0012 0.0011 0.0014 0.000 0.009 0.000 LATT -1 SYMM -X, 0.5+Y, -Z SFAC C H N O UNIT 28 64 8 24 TEMP 0.04 TREF HKLF 4 END 8284 Reflections written to new reflection file o4skc0009p21.hkl ------------------------------------------------------------------------------- File 04skc0009p21.ins set up as follows: TITL 04skc0009p21 in P2(1) CELL 0.71073 9.4109 8.7365 12.4478 90.000 102.099 90.000 ZERR 4.00 0.0012 0.0011 0.0014 0.000 0.009 0.000 LATT -1 SYMM -X, 0.5+Y, -Z SFAC C H N O UNIT 28 64 8 24 TEMP 0.04 TREF HKLF 4 END 8284 Reflections written to new reflection file 04skc0009p21.hkl -------------------------------------------------------------------------------