++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION - Version 2014/2 + + COPYRIGHT(c) 2014 Bruker-AXS All Rights Reserved + + mo_marc003_0m started at 14:36:12 on 17-Aug-2015 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 17.280 6.938 21.121 90.00 104.01 90.00 25603 Reflections read from file mo_marc003_0m.raw; mean (I/sigma) = 4.61 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 12777 12808 12807 12777 19196 17063 17093 25603 N (int>3sigma) = 0 3667 4077 3926 4077 5835 5359 5467 8106 Mean intensity = 0.0 45.0 58.1 57.3 58.2 53.5 58.4 58.0 58.4 Mean int/sigma = 0.0 4.0 4.7 4.6 4.6 4.4 4.7 4.7 4.7 Lattice type: P chosen Volume: 2456.84 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 -1.0000 0.0000 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 Unitcell: 6.938 17.280 21.121 104.01 90.00 90.00 Niggli form: a.a = 48.14 b.b = 298.59 c.c = 446.08 b.c = -88.37 a.c = 0.00 a.b = 0.00 ------------------------------------------------------------------------------- Search for higher metric symmetry Identical indices and Friedel opposites combined before calculating R(sym) ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC P-lattice R(sym) = 0.047 [ 4991] Cell: 17.280 6.938 21.121 90.00 104.01 90.00 Volume: 2456.84 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 12777 12808 12807 12777 19196 17063 17093 25603 N (int>3sigma) = 0 3667 4077 3926 4077 5835 5359 5467 8106 Mean intensity = 0.0 45.0 58.1 57.3 58.2 53.5 58.4 58.0 58.4 Mean int/sigma = 0.0 4.0 4.7 4.6 4.6 4.4 4.7 4.7 4.7 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.960 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 19 1119 1118 1113 N I>3s 0 329 0 329 1.0 126.9 1.1 127.6 0.3 6.8 0.3 6.8 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 0.047 4991 0.3 / 4.7 2.30 Option [A] chosen ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 -1.0000 0.0000 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 Unitcell: 6.938 17.280 21.121 104.01 90.00 90.00 Niggli form: a.a = 48.14 b.b = 298.59 c.c = 446.08 b.c = -88.37 a.c = 0.00 a.b = 0.00 ------------------------------------------------------------------------------- Search for higher metric symmetry Identical indices and Friedel opposites combined before calculating R(sym) ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC P-lattice R(sym) = 0.047 [ 4991] Cell: 17.280 6.938 21.121 90.00 104.01 90.00 Volume: 2456.84 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 12777 12808 12807 12777 19196 17063 17093 25603 N (int>3sigma) = 0 3667 4077 3926 4077 5835 5359 5467 8106 Mean intensity = 0.0 45.0 58.1 57.3 58.2 53.5 58.4 58.0 58.4 Mean int/sigma = 0.0 4.0 4.7 4.6 4.6 4.4 4.7 4.7 4.7 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.960 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 19 1119 1118 1113 N I>3s 0 329 0 329 1.0 126.9 1.1 127.6 0.3 6.8 0.3 6.8 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 0.047 4991 0.3 / 4.7 2.30 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 mo_marc003_0m.raw Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s Rmerge Rsigma Inf - 3.36 93 93 100.0 6.19 621.81 134.72 0.0351 0.0060 3.36 - 2.18 215 215 100.0 6.18 263.11 42.10 0.0281 0.0124 2.18 - 1.70 308 308 100.0 6.03 124.20 25.04 0.0382 0.0234 1.70 - 1.48 309 309 100.0 6.09 69.12 15.64 0.0566 0.0384 1.48 - 1.33 322 322 100.0 5.76 39.71 10.45 0.0762 0.0635 1.33 - 1.23 324 324 100.0 5.06 42.64 8.84 0.0783 0.0742 1.23 - 1.16 275 275 100.0 4.66 53.56 9.52 0.0679 0.0697 1.16 - 1.10 321 321 100.0 4.65 39.19 7.25 0.0914 0.0943 1.10 - 1.05 314 314 100.0 4.24 27.71 5.47 0.1048 0.1325 1.05 - 1.00 363 363 100.0 3.90 23.26 4.38 0.1185 0.1666 1.00 - 0.97 271 271 100.0 4.04 16.07 3.30 0.1542 0.2221 0.97 - 0.94 309 309 100.0 3.75 11.47 2.44 0.2059 0.3160 0.94 - 0.91 347 347 100.0 3.63 9.28 2.01 0.1974 0.3841 0.91 - 0.88 357 357 100.0 3.30 8.91 1.79 0.2462 0.4366 0.88 - 0.86 289 289 100.0 3.34 8.61 1.66 0.2549 0.4648 0.86 - 0.84 326 326 100.0 3.40 6.06 1.28 0.3234 0.6337 0.84 - 0.82 337 337 100.0 3.17 6.51 1.33 0.3103 0.6424 0.82 - 0.81 195 195 100.0 2.99 7.64 1.36 0.2852 0.5899 0.81 - 0.79 387 387 100.0 2.89 6.25 1.19 0.3112 0.7116 0.79 - 0.78 208 208 100.0 2.83 5.75 1.10 0.3641 0.7969 0.78 - 0.77 292 294 99.3 2.80 6.50 1.20 0.3080 0.7389 ------------------------------------------------------------------------------ 0.87 - 0.77 1893 1895 99.9 3.06 6.70 1.30 0.3055 0.6491 Inf - 0.77 6162 6164 100.0 4.15 44.31 8.80 0.0605 0.0837 Merged [A], lowest resolution = 20.49 Angstroms ------------------------------------------------------------------------------- Current dataset is # 1 mo_marc003_0m.raw ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C28 H30 O7 Formula weight = 478.53 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.294, non-H atomic volume = 17.5 and following cell contents and analysis: C 112.00 70.28 % H 120.00 6.32 % O 28.00 23.40 % F(000) = 1016.0 Mo-K(alpha) radiation Mu (mm-1) = 0.09 ------------------------------------------------------------------------------- File marc003.ins set up as follows: TITL marc003 in P2(1)/c CELL 0.71073 17.27970 6.93830 21.12070 90.0000 104.0129 90.0000 ZERR 4.00 0.00260 0.00110 0.00330 0.0000 0.0024 0.0000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H O UNIT 112 120 28 TEMP -73.150 SIZE 0.287 0.31 0.322 TREF HKLF 4 END 25603 Reflections written to new reflection file marc003.hkl -------------------------------------------------------------------------------