+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 2009/1 for Windows + + Copyright(C) 2009 Bruker-AXS All Rights Reserved + + 2009src0116 started at 11:38:18 on 13-Feb-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 9.351 14.516 10.467 90.00 90.78 90.00 16121 Reflections read from file 2009src0116.hkl; mean (I/sigma) = 10.17 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 8030 8049 8073 8074 12076 10758 10720 16121 N (int>3sigma) = 0 6235 6507 6576 6535 9659 8709 8690 13042 Mean intensity = 0.0 201.0 235.1 239.2 236.7 225.2 235.7 241.9 231.6 Mean int/sigma = 0.0 9.7 10.1 10.3 10.3 10.0 10.2 10.3 10.2 Lattice type: P chosen Volume: 1420.64 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 Unitcell: 9.351 10.467 14.516 90.00 90.00 90.78 Niggli form: a.a = 87.44 b.b = 109.56 c.c = 210.71 b.c = 0.00 a.c = 0.00 a.b = -1.33 ------------------------------------------------------------------------------- Search for higher metric symmetry Identical indices and Friedel opposites combined before calculating R(sym) ------------------------------------------------------------------------------ Option A: FOM = 0.778 deg. ORTHORHOMBIC P-lattice R(sym) = 0.557 [ 4229] Cell: 9.351 10.467 14.516 90.00 90.00 90.78 Volume: 1420.64 Matrix: 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.000 deg. MONOCLINIC P-lattice R(sym) = 0.022 [ 2748] Cell: 9.351 14.516 10.467 90.00 90.78 90.00 Volume: 1420.64 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option C: FOM = 0.778 deg. MONOCLINIC P-lattice R(sym) = 0.593 [ 2730] Cell: 9.351 10.467 14.516 90.00 90.00 90.78 Volume: 1420.64 Matrix:-1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option D: FOM = 0.778 deg. MONOCLINIC P-lattice R(sym) = 0.634 [ 2686] Cell: 10.467 9.351 14.516 90.00 90.00 89.22 Volume: 1420.64 Matrix: 0.0000 0.0000 -1.0000 1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 Option B selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 8030 8049 8073 8074 12076 10758 10720 16121 N (int>3sigma) = 0 6235 6507 6576 6535 9659 8709 8690 13042 Mean intensity = 0.0 201.0 235.1 239.2 236.7 225.2 235.7 241.9 231.6 Mean int/sigma = 0.0 9.7 10.1 10.3 10.3 10.0 10.2 10.3 10.2 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.967 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 16 480 461 469 N I>3s 0 216 3 217 0.9 419.6 1.0 429.5 0.6 7.1 0.7 7.3 Identical indices and Friedel opposites combined before calculating R(sym) Option Space Group No. Type Axes CSD R(sym) N(eq) Syst. Abs. CFOM [A] P2(1)/c # 14 centro 1 19410 0.022 2748 0.7 / 7.1 1.55 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2009src0116.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) Rsigma Inf - 2.11 174 182 95.6 6.98 936.5 43.79 0.0239 0.0197 2.11 - 1.68 170 170 100.0 7.65 526.8 40.41 0.0300 0.0193 1.68 - 1.47 170 170 100.0 7.59 277.4 35.48 0.0414 0.0210 1.47 - 1.33 171 171 100.0 7.60 169.0 32.60 0.0407 0.0229 1.33 - 1.23 190 190 100.0 6.98 191.1 30.67 0.0478 0.0249 1.23 - 1.15 193 193 100.0 5.77 179.2 23.94 0.0408 0.0282 1.15 - 1.09 176 176 100.0 5.45 206.2 25.15 0.0402 0.0294 1.09 - 1.04 186 186 100.0 5.10 161.2 21.48 0.0486 0.0340 1.04 - 1.00 186 186 100.0 4.95 106.9 19.29 0.0529 0.0367 1.00 - 0.96 195 195 100.0 4.45 87.4 16.29 0.0567 0.0434 0.96 - 0.93 193 193 100.0 3.66 65.3 13.15 0.0690 0.0521 0.93 - 0.90 214 214 100.0 3.45 54.9 12.03 0.0712 0.0601 0.90 - 0.87 220 220 100.0 3.15 53.9 10.77 0.0719 0.0679 0.87 - 0.85 182 182 100.0 3.02 47.8 9.50 0.0802 0.0722 0.85 - 0.83 189 189 100.0 2.98 36.5 8.88 0.0872 0.0861 0.83 - 0.81 223 225 99.1 2.80 37.7 7.79 0.0895 0.0927 0.81 - 0.79 220 223 98.7 2.72 44.1 8.30 0.0831 0.0883 0.79 - 0.77 133 136 97.8 2.49 49.0 7.52 0.0694 0.0948 ------------------------------------------------------------------------------ 0.87 - 0.77 1022 1030 99.2 2.85 43.5 8.65 0.0816 0.0845 Inf - 0.77 3385 3401 99.5 4.74 171.1 19.85 0.0375 0.0305 Merged [A], lowest resolution = 6.93 Angstroms, 438 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2009src0116.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C7H14N1B5O10 Formula weight = 326.24 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.525, non-H atomic volume = 15.4 and following cell contents and analysis: C 28.00 25.77 % H 56.00 4.33 % B 20.00 16.57 % N 4.00 4.29 % O 40.00 49.04 % F(000) = 672.0 Mo-K(alpha) radiation Mu (mm-1) = 0.13 ------------------------------------------------------------------------------- File 2009src0116.ins set up as follows: TITL 2009src0116 in P2(1)/c CELL 0.71073 9.3511 14.5157 10.4670 90.000 90.778 90.000 ZERR 4.00 0.0002 0.0004 0.0002 0.000 0.002 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H B N O UNIT 28 56 20 4 40 TEMP 0.14 TREF HKLF 4 END -------------------------------------------------------------------------------