++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 12:51:21 on 19-JUL-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 14.634 7.746 35.875 90.00 91.07 90.00 7533 Reflections read from file s92.hkl; mean (I/sigma) = 3.65 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 3765 3765 0 3771 3765 5029 5011 7533 N (int>3sigma) = 0 1289 1289 0 1398 1289 1946 1927 2888 Mean intensity = 0.0 12.5 12.5 0.0 15.0 12.5 16.9 17.0 16.7 Mean int/sigma = 0.0 3.4 3.4 0.0 3.6 3.4 3.8 3.8 3.8 Lattice type: C chosen Volume: 4066.06 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 1.0000 0.0000 -0.5000 0.5000 0.0000 0.0000 0.0000 1.0000 Unitcell: 7.746 8.279 35.875 89.06 90.00 62.11 Niggli form: a.a = 60.01 b.b = 68.54 c.c = 1287.03 b.c = 4.88 a.c = 0.00 a.b = 30.00 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC C-lattice R(int) = 0.106 [ 3932] Cell: 14.634 7.746 35.875 90.00 91.07 90.00 Volume: 4066.06 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 3765 3765 0 3771 3765 5029 5011 7533 N (int>3sigma) = 0 1289 1289 0 1398 1289 1946 1927 2888 Mean intensity = 0.0 12.5 12.5 0.0 15.0 12.5 16.9 17.0 16.7 Mean int/sigma = 0.0 3.4 3.4 0.0 3.6 3.4 3.8 3.8 3.8 Crystal system M and Lattice type C selected Mean |E*E-1| = 0.902 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -c- N 322 N I>3s 0 1.0 0.5 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] C2/c # 15 centro 1 3696 0.106 3932 0.5 / 3.8 3.46 [B] Cc # 9 non-cen 1 566 0.106 3932 0.5 / 3.8 5.93 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: V20 H31 N1 O3 Si1 Formula weight = 1140.15 Tentative Z (number of formula units/cell) = 6.0 giving rho = 2.794, non-H atomic volume = 27.1 and following cell contents and analysis: N 6.00 1.23 % H 186.00 2.74 % O 18.00 4.21 % Si 6.00 2.46 % V 120.00 89.36 % F(000) = 3216.0 Mo-K(alpha) radiation Mu (mm-1) = 6.56 ------------------------------------------------------------------------------- File s92.ins set up as follows: TITL s92 in C2/c CELL 0.71073 14.6339 7.7463 35.8752 90.000 91.066 90.000 ZERR 6.00 0.0029 0.0015 0.0072 0.000 0.030 0.000 LATT 7 SYMM -X, Y, 0.5-Z SFAC N H O SI V UNIT 6 186 18 6 120 TREF HKLF 4 END -------------------------------------------------------------------------------