++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 09:41:29 on 26-SEP-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 10.988 11.970 22.466 90.01 89.99 90.00 16596 Reflections read from file s92.hkl; mean (I/sigma) = 1.81 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 8299 8250 8297 8306 12423 11096 11056 16596 N (int>3sigma) = 0 1789 1646 1689 1688 2562 2262 2223 3431 Mean intensity = 0.0 4.7 4.4 5.0 5.1 4.7 4.9 4.9 5.0 Mean int/sigma = 0.0 2.1 1.9 2.0 2.0 2.0 2.0 2.0 2.0 Lattice type: P chosen Volume: 2954.90 ------------------------------------------------------------------------------- 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: 10.988 11.970 22.466 90.01 90.01 90.00 Niggli form: a.a = 120.73 b.b = 143.29 c.c = 504.73 b.c = -0.04 a.c = -0.04 a.b = -0.01 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.013 deg. ORTHORHOMBIC P-lattice R(int) = 0.290 [ 13127] Cell: 10.988 11.970 22.466 90.01 89.99 90.00 Volume: 2954.90 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.010 deg. MONOCLINIC P-lattice R(int) = 0.251 [ 10599] Cell: 10.988 11.970 22.466 90.01 90.01 90.00 Volume: 2954.90 Matrix: 1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option C: FOM = 0.011 deg. MONOCLINIC P-lattice R(int) = 0.252 [ 10809] Cell: 11.970 10.988 22.466 89.99 90.01 90.00 Volume: 2954.90 Matrix: 0.0000 -1.0000 0.0000 -1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option D: FOM = 0.013 deg. MONOCLINIC P-lattice R(int) = 0.252 [ 10706] Cell: 10.988 22.466 11.970 89.99 90.00 89.99 Volume: 2954.90 Matrix: 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option E: FOM = 0.000 deg. TRICLINIC P-lattice R(int) = 0.178 [ 6793] Cell: 10.988 11.970 22.466 90.01 90.01 90.00 Volume: 2954.90 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 8299 8250 8297 8306 12423 11096 11056 16596 N (int>3sigma) = 0 1789 1646 1689 1688 2562 2262 2223 3431 Mean intensity = 0.0 4.7 4.4 5.0 5.1 4.7 4.9 4.9 5.0 Mean int/sigma = 0.0 2.1 1.9 2.0 2.0 2.0 2.0 2.0 2.0 Crystal system O and Lattice type P selected Mean |E*E-1| = 0.758 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: b-- c-- n-- 21-- -c- -a- -n- -21- --a --b --n --21 N 567 546 541 5 440 438 436 8 218 226 224 24 N I>3s 183 122 139 0 86 129 89 0 72 97 73 0 9.9 6.7 6.4 0.5 5.3 8.0 7.6 1.4 6.9 10.9 9.5 0.6 2.9 2.2 2.3 0.3 1.9 2.5 1.8 0.7 2.9 3.5 3.0 0.4 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)2(1)2(1) # 19 chiral 1 5917 0.290 13127 0.7 / 1.8 5.66 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C33 H45 O6 S1 N2 Formula weight = 597.77 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.344, non-H atomic volume = 17.6 and following cell contents and analysis: C 132.00 66.30 % H 180.00 7.59 % N 8.00 4.69 % O 24.00 16.06 % S 4.00 5.36 % F(000) = 1284.0 Mo-K(alpha) radiation Mu (mm-1) = 0.16 ------------------------------------------------------------------------------- File s92.ins set up as follows: TITL s92 in P2(1)2(1)2(1) CELL 0.71073 10.9877 11.9703 22.4663 90.000 90.000 90.000 ZERR 4.00 0.0007 0.0008 0.0018 0.000 0.000 0.000 LATT -1 SYMM 0.5-X, -Y, 0.5+Z SYMM -X, 0.5+Y, 0.5-Z SYMM 0.5+X, 0.5-Y, -Z SFAC C H N O S UNIT 132 180 8 24 4 TREF HKLF 4 END -------------------------------------------------------------------------------