++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION - Version 2014/2 + + COPYRIGHT(c) 2014 Bruker-AXS All Rights Reserved + + cu_marc004_0m started at 10:04:00 on 13-Jan-2020 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 19.903 11.314 22.098 90.00 89.98 90.00 36740 Reflections read from file cu_marc004_0m.hkl; mean (I/sigma) = 12.82 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 18395 18395 0 18405 18395 24490 24460 36740 N (int>3sigma) = 0 14258 14258 0 14123 14258 19262 19315 28969 Mean intensity = 0.0 2.7 2.7 0.0 2.8 2.7 3.0 3.0 3.1 Mean int/sigma = 0.0 12.7 12.7 0.0 12.4 12.7 12.8 12.9 12.9 Lattice type: C chosen Volume: 4976.04 ------------------------------------------------------------------------------- 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: 11.314 11.447 22.098 89.98 90.00 60.38 Niggli form: a.a = 128.01 b.b = 131.03 c.c = 488.30 b.c = 0.07 a.c = 0.00 a.b = 64.00 ------------------------------------------------------------------------------- Search for higher metric symmetry Identical indices and Friedel opposites combined before calculating R(sym) ------------------------------------------------------------------------------ Option A: FOM = 0.770 deg. HEXAGONAL P-lattice R(sym) = 0.771 [ 6166] Cell: 11.447 11.314 22.098 90.00 90.02 119.62 Volume: 2488.02 Matrix:-0.5000 0.5000 0.0000 0.0000 -1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.020 deg. ORTHORHOMBIC C-lattice R(sym) = 0.657 [ 6774] Cell: 11.314 19.903 22.098 89.98 90.00 90.00 Volume: 4976.04 Matrix: 0.0000 -1.0000 0.0000 -1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option C: FOM = 0.770 deg. ORTHORHOMBIC C-lattice R(sym) = 0.827 [ 6757] Cell: 11.447 19.674 22.098 89.99 89.98 89.23 Volume: 4976.04 Matrix:-0.5000 -0.5000 0.0000 -0.5000 1.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option D: FOM = 0.770 deg. ORTHORHOMBIC C-lattice R(sym) = 0.829 [ 6758] Cell: 11.447 19.674 22.098 89.99 90.02 90.77 Volume: 4976.04 Matrix: 0.5000 -0.5000 0.0000 -0.5000 -1.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option E: FOM = 0.000 deg. MONOCLINIC C-lattice R(sym) = 0.017 [ 4262] Cell: 19.903 11.314 22.098 90.00 90.02 90.00 Volume: 4976.04 Matrix: 1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option F: FOM = 0.020 deg. MONOCLINIC P-lattice R(sym) = 0.689 [ 4363] Cell: 11.314 22.098 11.447 90.02 119.62 90.00 Volume: 2488.02 Matrix: 0.0000 -1.0000 0.0000 0.0000 0.0000 1.0000 -0.5000 0.5000 0.0000 ------------------------------------------------------------------------------ Option G: FOM = 0.020 deg. MONOCLINIC C-lattice R(sym) = 0.677 [ 4424] Cell: 11.314 19.903 22.098 90.02 90.00 90.00 Volume: 4976.04 Matrix: 0.0000 1.0000 0.0000 1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 Option E selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 18395 18395 0 18405 18395 24468 24467 36740 N (int>3sigma) = 0 14258 14258 0 14123 14258 19277 19240 28969 Mean intensity = 0.0 2.7 2.7 0.0 2.8 2.7 3.0 3.0 3.1 Mean int/sigma = 0.0 12.7 12.7 0.0 12.4 12.7 12.8 12.8 12.9 Crystal system M and Lattice type C selected Mean |E*E-1| = 1.032 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -c- N 911 N I>3s 21 0.0 0.6 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 0.017 4262 0.6 / 12.9 1.25 [B] Cc # 9 non-cen 1 566 0.017 4262 0.6 / 12.9 9.74 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: 11.314 11.447 22.098 89.98 90.00 60.38 Niggli form: a.a = 128.01 b.b = 131.03 c.c = 488.30 b.c = 0.07 a.c = 0.00 a.b = 64.00 ------------------------------------------------------------------------------- Search for higher metric symmetry Identical indices and Friedel opposites combined before calculating R(sym) ------------------------------------------------------------------------------ Option A: FOM = 0.770 deg. HEXAGONAL P-lattice R(sym) = 0.771 [ 6166] Cell: 11.447 11.314 22.098 90.00 90.02 119.62 Volume: 2488.02 Matrix:-0.5000 0.5000 0.0000 0.0000 -1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.020 deg. ORTHORHOMBIC C-lattice R(sym) = 0.657 [ 6774] Cell: 11.314 19.903 22.098 89.98 90.00 90.00 Volume: 4976.04 Matrix: 0.0000 -1.0000 0.0000 -1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option C: FOM = 0.770 deg. ORTHORHOMBIC C-lattice R(sym) = 0.827 [ 6757] Cell: 11.447 19.674 22.098 89.99 89.98 89.23 Volume: 4976.04 Matrix:-0.5000 -0.5000 0.0000 -0.5000 1.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option D: FOM = 0.770 deg. ORTHORHOMBIC C-lattice R(sym) = 0.829 [ 6758] Cell: 11.447 19.674 22.098 89.99 90.02 90.77 Volume: 4976.04 Matrix: 0.5000 -0.5000 0.0000 -0.5000 -1.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option E: FOM = 0.000 deg. MONOCLINIC C-lattice R(sym) = 0.017 [ 4262] Cell: 19.903 11.314 22.098 90.00 90.02 90.00 Volume: 4976.04 Matrix: 1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option F: FOM = 0.020 deg. MONOCLINIC P-lattice R(sym) = 0.689 [ 4363] Cell: 11.314 22.098 11.447 90.02 119.62 90.00 Volume: 2488.02 Matrix: 0.0000 -1.0000 0.0000 0.0000 0.0000 1.0000 -0.5000 0.5000 0.0000 ------------------------------------------------------------------------------ Option G: FOM = 0.020 deg. MONOCLINIC C-lattice R(sym) = 0.677 [ 4424] Cell: 11.314 19.903 22.098 90.02 90.00 90.00 Volume: 4976.04 Matrix: 0.0000 1.0000 0.0000 1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 Option E selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 18395 18395 0 18405 18395 24468 24467 36740 N (int>3sigma) = 0 14258 14258 0 14123 14258 19277 19240 28969 Mean intensity = 0.0 2.7 2.7 0.0 2.8 2.7 3.0 3.0 3.1 Mean int/sigma = 0.0 12.7 12.7 0.0 12.4 12.7 12.8 12.8 12.9 Crystal system M and Lattice type C selected Mean |E*E-1| = 1.032 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -c- N 911 N I>3s 21 0.0 0.6 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 0.017 4262 0.6 / 12.9 1.25 [B] Cc # 9 non-cen 1 566 0.017 4262 0.6 / 12.9 9.74 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 cu_marc004_0m.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s Rmerge Rsigma Inf - 3.44 82 82 100.0 1.80 48.15 31.17 0.0348 0.0298 3.44 - 2.22 191 191 100.0 2.92 16.08 33.22 0.0278 0.0261 2.22 - 1.75 273 276 98.9 5.17 13.08 45.17 0.0231 0.0182 1.75 - 1.53 259 262 98.9 5.33 5.82 39.17 0.0221 0.0196 1.53 - 1.37 292 295 99.0 4.77 3.17 35.59 0.0278 0.0213 1.37 - 1.27 266 268 99.3 4.80 2.90 33.17 0.0305 0.0216 1.27 - 1.20 267 268 99.6 5.01 5.82 35.10 0.0312 0.0191 1.20 - 1.13 289 291 99.3 4.73 4.70 31.33 0.0237 0.0209 1.13 - 1.09 229 229 100.0 7.29 3.71 36.85 0.0400 0.0196 1.09 - 1.04 305 305 100.0 11.58 2.88 44.36 0.0320 0.0146 1.04 - 1.01 234 234 100.0 11.09 2.70 43.64 0.0318 0.0156 1.01 - 0.97 345 345 100.0 10.32 2.03 38.70 0.0382 0.0180 0.97 - 0.94 280 280 100.0 8.76 1.65 31.24 0.0368 0.0200 0.94 - 0.92 228 228 100.0 8.55 1.38 29.27 0.0395 0.0218 0.92 - 0.90 236 236 100.0 8.44 1.34 30.27 0.0433 0.0224 0.90 - 0.88 257 257 100.0 8.13 0.84 24.84 0.0523 0.0271 0.88 - 0.86 288 289 99.7 7.21 1.15 28.36 0.0418 0.0239 0.86 - 0.84 329 330 99.7 6.81 1.02 27.35 0.0451 0.0250 0.84 - 0.82 300 303 99.0 6.08 0.96 25.72 0.0507 0.0254 0.82 - 0.81 190 193 98.4 5.23 0.77 24.15 0.0590 0.0288 0.81 - 0.80 235 271 86.7 2.86 0.97 21.43 0.0595 0.0340 ------------------------------------------------------------------------------ 0.90 - 0.80 1599 1643 97.3 6.12 0.96 25.57 0.0488 0.0268 Inf - 0.80 5375 5433 98.9 6.76 4.17 33.12 0.0319 0.0225 Merged [A], lowest resolution = 22.10 Angstroms ------------------------------------------------------------------------------- Current dataset is # 1 cu_marc004_0m.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C29 H20 O3 Formula weight = 416.47 Tentative Z (number of formula units/cell) = 8.0 giving rho = 1.112, non-H atomic volume = 19.4 and following cell contents and analysis: C 232.00 83.63 % H 160.00 4.84 % O 24.00 11.53 % F(000) = 1744.0 Cu-K(alpha) radiation Mu (mm-1) = 0.57 ------------------------------------------------------------------------------- File marc004a.ins set up as follows: TITL marc004a in C2/c CELL 1.54178 19.90300 11.31410 22.09760 90.0000 90.0195 90.0000 ZERR 8.00 0.00080 0.00050 0.00090 0.0000 0.0016 0.0000 LATT 7 SYMM -X, Y, 0.5-Z SFAC C H O UNIT 232 160 24 TEMP -173.160 SIZE 0.18 0.184 0.195 TREF HKLF 4 END 36740 Reflections written to new reflection file marc004a.hkl -------------------------------------------------------------------------------