++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION - Version 2013/1 + + COPYRIGHT(c) 2013 Bruker-AXS All Rights Reserved + + marc_0m started at 16:55:44 on 10-Jul-2013 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 24.445 7.241 17.657 90.00 101.42 90.00 10106 Reflections read from file marc_0m.hkl; mean (I/sigma) = 12.61 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 5055 5055 0 5052 5055 6736 6737 10106 N (int>3sigma) = 0 3427 3427 0 3402 3427 4795 4782 7150 Mean intensity = 0.0 19.1 19.1 0.0 16.9 19.1 20.5 20.0 20.9 Mean int/sigma = 0.0 11.9 11.9 0.0 11.9 11.9 12.8 12.7 12.7 Lattice type: C chosen Volume: 3063.33 ------------------------------------------------------------------------------- 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: 7.241 12.747 17.657 79.05 90.00 73.50 Niggli form: a.a = 52.43 b.b = 162.49 c.c = 311.78 b.c = 42.75 a.c = 0.00 a.b = 26.21 ------------------------------------------------------------------------------- Search for higher metric symmetry Identical indices and Friedel opposites combined before calculating R(sym) ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC C-lattice R(sym) = 0.020 [ 2819] Cell: 24.445 7.241 17.657 90.00 101.42 90.00 Volume: 3063.33 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 5055 5055 0 5052 5055 6736 6737 10106 N (int>3sigma) = 0 3427 3427 0 3402 3427 4795 4782 7150 Mean intensity = 0.0 19.1 19.1 0.0 16.9 19.1 20.5 20.0 20.9 Mean int/sigma = 0.0 11.9 11.9 0.0 11.9 11.9 12.8 12.7 12.7 Crystal system M and Lattice type C selected Mean |E*E-1| = 0.935 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -c- N 391 N I>3s 1 0.1 0.5 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] C2/c # 15 centro 1 3696 0.020 2819 0.5 / 12.7 0.95 [B] Cc # 9 non-cen 1 566 0.020 2819 0.5 / 12.7 4.94 Option [A] chosen ------------------------------------------------------------------------------- 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: 7.241 12.747 17.657 79.05 90.00 73.50 Niggli form: a.a = 52.43 b.b = 162.49 c.c = 311.78 b.c = 42.75 a.c = 0.00 a.b = 26.21 ------------------------------------------------------------------------------- Search for higher metric symmetry Identical indices and Friedel opposites combined before calculating R(sym) ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC C-lattice R(sym) = 0.020 [ 2819] Cell: 24.445 7.241 17.657 90.00 101.42 90.00 Volume: 3063.33 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 5055 5055 0 5052 5055 6736 6737 10106 N (int>3sigma) = 0 3427 3427 0 3402 3427 4795 4782 7150 Mean intensity = 0.0 19.1 19.1 0.0 16.9 19.1 20.5 20.0 20.9 Mean int/sigma = 0.0 11.9 11.9 0.0 11.9 11.9 12.8 12.7 12.7 Crystal system M and Lattice type C selected Mean |E*E-1| = 0.935 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -c- N 391 N I>3s 1 0.1 0.5 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] C2/c # 15 centro 1 3696 0.020 2819 0.5 / 12.7 0.95 [B] Cc # 9 non-cen 1 566 0.020 2819 0.5 / 12.7 4.94 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 marc_0m.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s Rmerge Rsigma Inf - 3.21 58 63 92.1 2.52 160.5 55.08 0.0143 0.0137 3.21 - 2.15 134 134 100.0 3.33 99.7 59.79 0.0134 0.0113 2.15 - 1.71 187 187 100.0 3.36 63.2 48.72 0.0157 0.0127 1.71 - 1.47 193 193 100.0 3.42 27.1 36.01 0.0188 0.0165 1.47 - 1.33 205 205 100.0 3.35 22.0 33.48 0.0227 0.0196 1.33 - 1.23 187 187 100.0 3.27 17.4 26.99 0.0293 0.0240 1.23 - 1.16 179 179 100.0 3.03 22.2 25.75 0.0249 0.0232 1.16 - 1.10 200 200 100.0 2.94 20.8 24.64 0.0284 0.0260 1.10 - 1.05 185 185 100.0 2.76 14.0 18.80 0.0357 0.0341 1.05 - 1.01 193 194 99.5 2.72 11.7 17.57 0.0389 0.0386 1.01 - 0.97 209 210 99.5 2.61 8.8 14.03 0.0461 0.0487 0.97 - 0.94 181 182 99.5 2.51 6.9 11.29 0.0615 0.0600 0.94 - 0.91 194 197 98.5 2.32 4.4 8.44 0.0769 0.0846 0.91 - 0.89 169 172 98.3 2.39 4.9 8.84 0.0809 0.0821 0.89 - 0.86 256 260 98.5 2.27 5.1 8.41 0.0771 0.0842 0.86 - 0.84 192 199 96.5 2.18 4.3 7.32 0.0741 0.0999 0.84 - 0.82 204 211 96.7 2.14 3.8 6.47 0.0873 0.1093 0.82 - 0.81 110 115 95.7 2.00 3.3 5.57 0.0757 0.1329 0.81 - 0.79 237 247 96.0 2.04 3.4 5.63 0.1039 0.1317 0.79 - 0.78 127 133 95.5 2.01 3.4 5.46 0.1167 0.1395 0.78 - 0.77 193 208 92.8 1.90 3.6 5.30 0.1060 0.1312 ------------------------------------------------------------------------------ 0.87 - 0.77 1149 1201 95.7 2.06 3.7 6.16 0.0914 0.1181 Inf - 0.77 3793 3861 98.2 2.62 18.6 19.04 0.0254 0.0276 Merged [A], lowest resolution = 17.31 Angstroms ------------------------------------------------------------------------------- Current dataset is # 1 marc_0m.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C16 H20 O4 Formula weight = 276.33 Tentative Z (number of formula units/cell) = 8.0 giving rho = 1.198, non-H atomic volume = 19.1 and following cell contents and analysis: C 128.00 69.54 % H 160.00 7.30 % O 32.00 23.16 % F(000) = 1184.0 Mo-K(alpha) radiation Mu (mm-1) = 0.09 ------------------------------------------------------------------------------- File marc.ins set up as follows: TITL marc in C2/c CELL 0.71073 24.4446 7.2407 17.6572 90.000 101.424 90.000 ZERR 8.00 0.0074 0.0023 0.0054 0.000 0.004 0.000 LATT 7 SYMM -X, Y, 0.5-Z SFAC C H O UNIT 128 160 32 TEMP 23.000 SIZE 0.44 0.557 0.60 TREF HKLF 4 END 10106 Reflections written to new reflection file marc.hkl -------------------------------------------------------------------------------