++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 04src0951_90 started at 23:15:46 on 15-DEC-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 7.294 7.294 17.104 90.05 89.99 120.02 7403 Reflections read from file 04src0951_90.hkl; mean (I/sigma) = 2.81 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 3698 3703 3709 3710 5555 4959 4931 7403 N (int>3sigma) = 0 944 944 904 947 1396 6 1295 1954 Mean intensity = 0.0 16.7 16.4 13.7 16.6 15.6 0.4 22.2 22.9 Mean int/sigma = 0.0 3.0 2.9 2.8 3.0 2.9 0.5 3.2 3.2 Lattice type: O chosen Volume: 787.89 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.6667 0.3333 0.3333 -0.3333 0.3333 0.3333 -0.3333 -0.6667 0.3333 Unitcell: 7.086 7.086 7.091 61.92 61.91 61.95 Niggli form: a.a = 50.22 b.b = 50.22 c.c = 50.28 b.c = 23.65 a.c = 23.66 a.b = 23.62 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.052 deg. RHOMBOHEDRAL O-lattice R(int) = 0.040 [ 2036] Cell: 7.294 7.294 17.104 90.05 89.99 120.02 Volume: 787.89 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.052 deg. RHOMBOHEDRAL P-lattice R(int) = 0.040 [ 2036] Cell: 7.086 7.086 7.091 61.92 61.91 61.95 Volume: 262.63 Matrix: 0.6667 0.3333 0.3333 -0.3333 0.3333 0.3333 -0.3333 -0.6667 0.3333 ------------------------------------------------------------------------------ Option C: FOM = 0.018 deg. MONOCLINIC C-lattice R(int) = 0.036 [ 1797] Cell: 12.152 7.294 7.091 89.98 123.30 90.00 Volume: 525.26 Matrix:-0.3333 -0.6667 -0.6667 1.0000 0.0000 0.0000 -0.3333 -0.6667 0.3333 ------------------------------------------------------------------------------ Option D: FOM = 0.018 deg. MONOCLINIC I-lattice R(int) = 0.036 [ 1797] Cell: 7.091 7.294 10.165 89.99 92.36 90.02 Volume: 525.26 Matrix: 0.3333 0.6667 -0.3333 1.0000 0.0000 0.0000 -0.6667 -1.3333 -0.3333 ------------------------------------------------------------------------------ Option E: FOM = 0.042 deg. MONOCLINIC C-lattice R(int) = 0.037 [ 1794] Cell: 12.158 7.292 7.086 89.96 123.27 90.04 Volume: 525.26 Matrix:-0.3333 0.3333 -0.6667 -1.0000 -1.0000 0.0000 -0.3333 0.3333 0.3333 ------------------------------------------------------------------------------ Option F: FOM = 0.042 deg. MONOCLINIC I-lattice R(int) = 0.037 [ 1794] Cell: 7.086 7.292 10.174 90.02 92.35 90.04 Volume: 525.26 Matrix: 0.3333 -0.3333 -0.3333 -1.0000 -1.0000 0.0000 -0.6667 0.6667 -0.3333 ------------------------------------------------------------------------------ Option G: FOM = 0.052 deg. MONOCLINIC C-lattice R(int) = 0.036 [ 1811] Cell: 12.157 7.294 7.086 90.05 123.28 89.96 Volume: 525.26 Matrix: 0.6667 0.3333 -0.6667 0.0000 1.0000 0.0000 0.6667 0.3333 0.3333 ------------------------------------------------------------------------------ Option H: FOM = 0.052 deg. MONOCLINIC I-lattice R(int) = 0.036 [ 1811] Cell: 7.086 7.294 10.171 89.99 92.34 89.95 Volume: 525.26 Matrix:-0.6667 -0.3333 -0.3333 0.0000 1.0000 0.0000 1.3333 0.6667 -0.3333 Option A selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 3698 3703 3709 3710 5555 4959 4931 7403 N (int>3sigma) = 0 944 944 904 947 1396 6 1295 1954 Mean intensity = 0.0 16.7 16.4 13.7 16.6 15.6 0.4 22.2 22.9 Mean int/sigma = 0.0 3.0 2.9 2.8 3.0 2.9 0.5 3.2 3.2 Crystal system H and Lattice type O selected Mean |E*E-1| = 0.912 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: 61/65 62=31 63 -c- --c N 10 0 10 319 175 N I>3s 10 0 10 276 163 173.4 0.0 173.4 99.9 91.8 16.7 0.0 16.7 10.5 11.7 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] R-3 #148 centro 1 232 0.040 2036 0.0 / 3.2 4.71 [B] R3 #146 chiral 1 85 0.040 2036 0.0 / 3.2 8.23 [C] R3m #160 non-cen 1 39 0.042 2188 0.0 / 3.2 8.78 [D] R32 #155 chiral 1 29 0.042 2188 0.0 / 3.2 9.61 [E] R-3m #166 centro 1 28 0.042 2188 0.0 / 3.2 6.93 Option [A] chosen ------------------------------------------------------------------------------- ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: KFe3S2O14H6 Formula weight = 500.82 Tentative Z (number of formula units/cell) = 1.0 giving rho = 1.056, non-H atomic volume = 39.4 and following cell contents and analysis: O 14.00 44.73 % H 6.00 1.21 % S 2.00 12.80 % K 1.00 7.81 % Fe 3.00 33.46 % F(000) = 247.0 Mo-K(alpha) radiation Mu (mm-1) = 1.66 ------------------------------------------------------------------------------- File 04src0951_90.ins set up as follows: TITL 04src0951_90 in R-3 CELL 0.71073 7.2938 7.2938 17.1045 90.000 90.000 120.000 ZERR 1.00 0.0010 0.0010 0.0034 0.000 0.000 0.000 LATT 3 SYMM -Y, X-Y, Z SYMM -X+Y, -X, Z SFAC O H S K FE UNIT 14 6 2 1 3 TEMP 0.08 TREF HKLF 4 END -------------------------------------------------------------------------------