++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION - Version 2014/2 + + COPYRIGHT(c) 2014 Bruker-AXS All Rights Reserved + + cu_marc002_0m started at 11:42:18 on 27-Feb-2015 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 6.835 7.367 18.326 90.00 100.59 90.00 19617 Reflections read from file cu_marc002_0m.hkl; mean (I/sigma) = 6.40 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 9792 9822 9896 9768 14755 13152 13086 19617 N (int>3sigma) = 0 7083 7089 7202 7122 10687 9581 9441 14300 Mean intensity = 0.0 22.6 22.8 22.5 22.6 22.6 22.7 22.0 22.4 Mean int/sigma = 0.0 6.3 6.4 6.4 6.4 6.4 6.4 6.4 6.4 Lattice type: P chosen Volume: 907.04 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): -1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 -1.0000 Unitcell: 6.835 7.367 18.326 90.00 100.59 90.00 Niggli form: a.a = 46.72 b.b = 54.28 c.c = 335.82 b.c = 0.00 a.c = -23.03 a.b = 0.00 ------------------------------------------------------------------------------- Search for higher metric symmetry Identical indices and Friedel opposites combined before calculating R(sym) ------------------------------------------------------------------------------ Option A: FOM = 0.155 deg. ORTHORHOMBIC C-lattice R(sym) = 0.430 [ 2433] Cell: 6.835 36.027 7.367 90.00 90.00 90.15 Volume: 1814.07 Matrix:-1.0000 0.0000 0.0000 1.0000 0.0000 2.0000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.000 deg. MONOCLINIC P-lattice R(sym) = 0.034 [ 1531] Cell: 6.835 7.367 18.326 90.00 100.59 90.00 Volume: 907.04 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option C: FOM = 0.155 deg. MONOCLINIC C-lattice R(sym) = 0.437 [ 1659] Cell: 6.835 36.027 7.367 90.00 90.00 90.15 Volume: 1814.07 Matrix: 1.0000 0.0000 0.0000 -1.0000 0.0000 -2.0000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option D: FOM = 0.155 deg. MONOCLINIC C-lattice R(sym) = 0.496 [ 1519] Cell: 36.027 6.835 7.367 90.00 90.00 89.85 Volume: 1814.07 Matrix: 1.0000 0.0000 2.0000 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 9792 9822 9896 9768 14755 13152 13086 19617 N (int>3sigma) = 0 7083 7089 7202 7122 10687 9581 9441 14300 Mean intensity = 0.0 22.6 22.8 22.5 22.6 22.6 22.7 22.0 22.4 Mean int/sigma = 0.0 6.3 6.4 6.4 6.4 6.4 6.4 6.4 6.4 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.709 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 29 743 751 754 N I>3s 0 472 434 478 0.2 31.5 23.3 32.7 0.5 6.4 5.8 6.7 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) # 4 chiral 1 3543 0.034 1531 0.5 / 5.8 1.87 [B] P2(1)/m # 11 centro 1 402 0.034 1531 0.5 / 5.8 8.74 Option [A] chosen ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): -1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 -1.0000 Unitcell: 6.835 7.367 18.326 90.00 100.59 90.00 Niggli form: a.a = 46.72 b.b = 54.28 c.c = 335.82 b.c = 0.00 a.c = -23.03 a.b = 0.00 ------------------------------------------------------------------------------- Search for higher metric symmetry Identical indices and Friedel opposites combined before calculating R(sym) ------------------------------------------------------------------------------ Option A: FOM = 0.155 deg. ORTHORHOMBIC C-lattice R(sym) = 0.430 [ 2433] Cell: 6.835 36.027 7.367 90.00 90.00 90.15 Volume: 1814.07 Matrix:-1.0000 0.0000 0.0000 1.0000 0.0000 2.0000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.000 deg. MONOCLINIC P-lattice R(sym) = 0.034 [ 1531] Cell: 6.835 7.367 18.326 90.00 100.59 90.00 Volume: 907.04 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option C: FOM = 0.155 deg. MONOCLINIC C-lattice R(sym) = 0.437 [ 1659] Cell: 6.835 36.027 7.367 90.00 90.00 90.15 Volume: 1814.07 Matrix: 1.0000 0.0000 0.0000 -1.0000 0.0000 -2.0000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option D: FOM = 0.155 deg. MONOCLINIC C-lattice R(sym) = 0.496 [ 1519] Cell: 36.027 6.835 7.367 90.00 90.00 89.85 Volume: 1814.07 Matrix: 1.0000 0.0000 2.0000 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 9792 9822 9896 9768 14755 13152 13086 19617 N (int>3sigma) = 0 7083 7089 7202 7122 10687 9581 9441 14300 Mean intensity = 0.0 22.6 22.8 22.5 22.6 22.6 22.7 22.0 22.4 Mean int/sigma = 0.0 6.3 6.4 6.4 6.4 6.4 6.4 6.4 6.4 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.709 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 29 743 751 754 N I>3s 0 472 434 478 0.2 31.5 23.3 32.7 0.5 6.4 5.8 6.7 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) # 4 chiral 1 3543 0.034 1531 0.5 / 5.8 1.87 [B] P2(1)/m # 11 centro 1 402 0.034 1531 0.5 / 5.8 8.74 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 cu_marc002_0m.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s Rmerge Rsigma Inf - 3.41 31 31 100.0 4.48 203.32 30.82 0.0573 0.0289 3.41 - 2.26 72 72 100.0 7.25 159.38 40.06 0.0648 0.0233 2.26 - 1.77 101 101 100.0 6.06 102.17 35.27 0.0766 0.0261 1.77 - 1.55 98 98 100.0 5.48 65.94 32.04 0.0726 0.0281 1.55 - 1.38 106 106 100.0 5.89 41.80 28.10 0.0737 0.0329 1.38 - 1.28 108 108 100.0 4.86 33.67 23.74 0.0766 0.0382 1.28 - 1.21 87 87 100.0 5.64 34.93 24.76 0.0855 0.0349 1.21 - 1.14 112 112 100.0 5.58 29.61 24.46 0.0753 0.0365 1.14 - 1.09 105 105 100.0 10.50 23.62 23.66 0.1135 0.0378 1.09 - 1.05 95 95 100.0 15.16 16.88 22.39 0.0983 0.0367 1.05 - 1.01 100 100 100.0 14.74 13.49 21.22 0.1090 0.0408 1.01 - 0.98 96 96 100.0 14.99 11.89 20.11 0.1158 0.0412 0.98 - 0.95 112 112 100.0 13.80 11.30 19.48 0.1263 0.0431 0.95 - 0.92 109 109 100.0 13.64 9.40 18.33 0.1228 0.0445 0.92 - 0.90 88 88 100.0 13.35 8.23 17.00 0.1390 0.0489 0.90 - 0.88 105 105 100.0 12.65 7.09 16.66 0.1550 0.0516 0.88 - 0.86 100 100 100.0 12.02 5.69 14.06 0.1796 0.0585 0.86 - 0.84 113 113 100.0 10.62 5.22 13.61 0.1600 0.0595 0.84 - 0.82 131 132 99.2 9.17 4.07 11.99 0.1867 0.0703 0.82 - 0.81 67 67 100.0 8.01 3.35 10.64 0.1935 0.0789 0.81 - 0.80 83 87 95.4 4.62 3.16 8.58 0.2088 0.1026 ------------------------------------------------------------------------------ 0.90 - 0.80 599 604 99.2 9.73 4.88 12.83 0.1708 0.0646 Inf - 0.80 2019 2024 99.8 9.69 30.46 21.30 0.0891 0.0324 Merged [A], lowest resolution = 18.01 Angstroms ------------------------------------------------------------------------------- Current dataset is # 1 cu_marc002_0m.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C20 H18 Br O4 Formula weight = 402.26 Tentative Z (number of formula units/cell) = 2.0 giving rho = 1.473, non-H atomic volume = 18.1 and following cell contents and analysis: C 40.00 59.72 % H 36.00 4.51 % O 8.00 15.91 % Br 2.00 19.86 % F(000) = 410.0 Cu-K(alpha) radiation Mu (mm-1) = 3.27 ------------------------------------------------------------------------------- File marc002.ins set up as follows: TITL marc002 in P2(1) CELL 1.54178 6.83490 7.36720 18.32550 90.0000 100.5931 90.0000 ZERR 2.00 0.00030 0.00030 0.00080 0.0000 0.0022 0.0000 LATT -1 SYMM -X, 0.5+Y, -Z SFAC C H O BR UNIT 40 36 8 2 TEMP -73.150 SIZE 0.086 0.371 0.453 TREF HKLF 4 END 19617 Reflections written to new reflection file marc002.hkl -------------------------------------------------------------------------------