++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 2005src1659 started at 09:22:25 on 09-JAN-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 7.031 19.820 19.831 87.99 79.78 79.78 15089 Reflections read from file 2005src1659.hkl; mean (I/sigma) = 6.79 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 7542 7528 7534 7553 11302 10076 10034 15089 N (int>3sigma) = 0 5161 5188 5181 5160 7765 6922 6936 10380 Mean intensity = 0.0 118.2 126.3 120.9 123.9 121.8 122.0 122.9 122.4 Mean int/sigma = 0.0 6.8 6.9 6.8 6.8 6.8 6.8 6.8 6.8 Lattice type: P chosen Volume: 2676.70 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 1.0000 0.0000 0.0000 1.0000 -1.0000 0.0000 1.0000 0.0000 -1.0000 Unitcell: 7.031 19.820 19.830 88.00 79.80 79.79 Niggli form: a.a = 49.44 b.b = 392.82 c.c = 393.24 b.c = 13.73 a.c = 24.70 a.b = 24.71 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.104 deg. TETRAGONAL I-lattice R(int) = 0.106 [ 11745] Cell: 27.543 27.643 7.031 89.99 90.00 89.97 Volume: 5353.40 Matrix: 0.0000 1.0000 -1.0000 1.0000 -1.0000 -1.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.034 deg. ORTHORHOMBIC I-lattice R(int) = 0.694 [ 11622] Cell: 7.031 27.543 27.643 89.97 89.99 90.00 Volume: 5353.40 Matrix:-1.0000 0.0000 0.0000 0.0000 1.0000 -1.0000 1.0000 -1.0000 -1.0000 ------------------------------------------------------------------------------ Option C: FOM = 0.010 deg. MONOCLINIC C-lattice R(int) = 0.078 [ 8640] Cell: 39.011 7.031 27.543 90.00 134.88 90.00 Volume: 5353.40 Matrix: 1.0000 -2.0000 0.0000 -1.0000 0.0000 0.0000 0.0000 1.0000 -1.0000 ------------------------------------------------------------------------------ Option D: FOM = 0.010 deg. MONOCLINIC I-lattice R(int) = 0.078 [ 8640] Cell: 27.543 7.031 27.643 89.99 90.03 90.00 Volume: 5353.40 Matrix: 0.0000 -1.0000 1.0000 -1.0000 0.0000 0.0000 1.0000 -1.0000 -1.0000 ------------------------------------------------------------------------------ Option E: FOM = 0.033 deg. MONOCLINIC C-lattice R(int) = 0.669 [ 9528] Cell: 28.522 27.543 7.031 90.00 104.26 89.97 Volume: 5353.40 Matrix:-2.0000 1.0000 1.0000 0.0000 -1.0000 1.0000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option F: FOM = 0.033 deg. MONOCLINIC I-lattice R(int) = 0.669 [ 9528] Cell: 7.031 27.543 27.643 89.97 90.01 90.00 Volume: 5353.40 Matrix:-1.0000 0.0000 0.0000 0.0000 -1.0000 1.0000 -1.0000 1.0000 1.0000 ------------------------------------------------------------------------------ Option G: FOM = 0.034 deg. MONOCLINIC C-lattice R(int) = 0.669 [ 9291] Cell: 28.426 27.643 7.031 90.01 104.32 90.03 Volume: 5353.40 Matrix:-1.0000 -1.0000 1.0000 1.0000 -1.0000 -1.0000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option H: FOM = 0.034 deg. MONOCLINIC I-lattice R(int) = 0.669 [ 9291] Cell: 7.031 27.643 27.543 90.03 90.00 89.99 Volume: 5353.40 Matrix:-1.0000 0.0000 0.0000 1.0000 -1.0000 -1.0000 0.0000 -1.0000 1.0000 Option A selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 7542 7553 7523 0 11309 10042 10039 15089 N (int>3sigma) = 0 5161 5160 5309 0 7815 6931 6931 10380 Mean intensity = 0.0 118.2 123.9 120.4 0.0 120.8 123.8 123.0 122.4 Mean int/sigma = 0.0 6.8 6.8 7.0 0.0 6.8 6.8 6.9 6.8 Crystal system T and Lattice type I selected Mean |E*E-1| = 1.064 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: 41/43 a-- -c- --d N 2 841 333 267 N I>3s 2 515 242 213 1244.4 135.4 85.5 227.2 12.7 6.2 7.2 9.0 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] I-4 # 82 non-cen 1 99 0.106 11745 0.0 / 6.2 13.39 [B] I4/m # 87 centro 1 46 0.106 11745 0.0 / 6.2 4.67 [C] I4 # 79 chiral 1 19 0.106 11745 0.0 / 6.2 17.39 [D] I4(1) # 80 chiral 1 16 0.106 11745 0.0 / 6.2 18.27 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C24H28B3P1 Formula weight = 379.86 Tentative Z (number of formula units/cell) = 10.0 giving rho = 1.178, non-H atomic volume = 19.1 and following cell contents and analysis: C 240.00 75.88 % H 280.00 7.43 % B 30.00 8.54 % P 10.00 8.15 % F(000) = 2020.0 Mo-K(alpha) radiation Mu (mm-1) = 0.14 ------------------------------------------------------------------------------- File s93.ins set up as follows: TITL s93 in I-4 CELL 0.71073 27.5929 27.5929 7.0313 90.000 90.000 90.000 ZERR 10.00 0.0020 0.0020 0.0005 0.000 0.000 0.000 LATT -2 SYMM -X, -Y, Z SYMM Y, -X, -Z SYMM -Y, X, -Z SFAC C H B P UNIT 240 280 30 10 TEMP 0.08 TREF HKLF 4 END 15089 Reflections written to new reflection file s93.hkl -------------------------------------------------------------------------------