++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION - Version 2008/2 + + COPYRIGHT(c) 2008 Bruker-AXS All Rights Reserved + + mo_uqam001_0m started at 10:58:06 on 22-Mar-2013 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 10.363 11.222 11.500 117.74 107.59 95.62 14411 Reflections read from file mo_uqam001_0m.hkl; mean (I/sigma) = 21.46 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 7190 7191 7215 7211 10798 9605 9623 14411 N (int>3sigma) = 0 6931 6941 6948 6935 10410 9265 9281 13892 Mean intensity = 0.0 27.9 27.8 27.4 27.6 27.7 27.2 27.8 27.3 Mean int/sigma = 0.0 21.6 21.5 21.5 21.4 21.5 21.4 21.5 21.5 Lattice type: P chosen Volume: 1082.24 ------------------------------------------------------------------------------- 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: 10.363 11.222 11.500 117.74 107.59 95.62 Niggli form: a.a = 107.40 b.b = 125.93 c.c = 132.26 b.c = -60.08 a.c = -36.01 a.b = -11.39 ------------------------------------------------------------------------------- Search for higher metric symmetry Identical indices and Friedel opposites combined before calculating R(sym) ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. TRICLINIC P-lattice R(sym) = 0.000 [ 0] Cell: 10.363 11.222 11.500 117.74 107.59 95.62 Volume: 1082.24 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 7190 7191 7215 7211 10798 9605 9623 14411 N (int>3sigma) = 0 6931 6941 6948 6935 10410 9265 9281 13892 Mean intensity = 0.0 27.9 27.8 27.4 27.6 27.7 27.2 27.8 27.3 Mean int/sigma = 0.0 21.6 21.5 21.5 21.4 21.5 21.4 21.5 21.5 Crystal system A and Lattice type P selected Mean |E*E-1| = 0.588 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absences not required for triclinic 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] P-1 # 2 centro 1 8646 0.000 0 0.0 / 21.5 14.90 [B] P1 # 1 chiral 1 700 0.000 0 0.0 / 21.5 2.79 Option [B] 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: 10.363 11.222 11.500 117.74 107.59 95.62 Niggli form: a.a = 107.40 b.b = 125.93 c.c = 132.26 b.c = -60.08 a.c = -36.01 a.b = -11.39 ------------------------------------------------------------------------------- Search for higher metric symmetry Identical indices and Friedel opposites combined before calculating R(sym) ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. TRICLINIC P-lattice R(sym) = 0.000 [ 0] Cell: 10.363 11.222 11.500 117.74 107.59 95.62 Volume: 1082.24 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 7190 7191 7215 7211 10798 9605 9623 14411 N (int>3sigma) = 0 6931 6941 6948 6935 10410 9265 9281 13892 Mean intensity = 0.0 27.9 27.8 27.4 27.6 27.7 27.2 27.8 27.3 Mean int/sigma = 0.0 21.6 21.5 21.5 21.4 21.5 21.4 21.5 21.5 Crystal system A and Lattice type P selected Mean |E*E-1| = 0.588 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absences not required for triclinic 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] P-1 # 2 centro 1 8646 0.000 0 0.0 / 21.5 14.90 [B] P1 # 1 chiral 1 700 0.000 0 0.0 / 21.5 2.79 Option [B] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 mo_uqam001_0m.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) Rsigma Inf - 2.10 249 249 100.0 4.00 109.6 93.54 0.0187 0.0088 2.10 - 1.66 252 252 100.0 3.88 60.4 80.42 0.0226 0.0109 1.66 - 1.45 256 256 100.0 3.80 41.6 66.49 0.0217 0.0130 1.45 - 1.31 267 267 100.0 3.71 31.2 55.84 0.0281 0.0155 1.31 - 1.22 261 261 100.0 3.48 26.1 45.59 0.0291 0.0184 1.22 - 1.14 286 286 100.0 3.29 23.6 40.81 0.0287 0.0208 1.14 - 1.08 277 277 100.0 3.15 20.9 36.27 0.0322 0.0238 1.08 - 1.03 279 279 100.0 2.95 18.4 32.00 0.0364 0.0274 1.03 - 0.99 281 281 100.0 2.90 16.2 29.37 0.0383 0.0308 0.99 - 0.95 312 312 100.0 2.74 13.3 24.40 0.0427 0.0368 0.95 - 0.92 292 292 100.0 2.59 11.7 20.78 0.0470 0.0416 0.92 - 0.89 307 307 100.0 2.53 10.4 18.54 0.0511 0.0469 0.89 - 0.86 372 372 100.0 2.42 9.1 16.39 0.0554 0.0538 0.86 - 0.84 278 278 100.0 2.34 8.9 15.58 0.0564 0.0570 0.84 - 0.82 297 297 100.0 2.27 7.9 14.01 0.0627 0.0638 0.82 - 0.80 340 340 100.0 2.20 7.0 12.32 0.0678 0.0714 0.80 - 0.78 357 360 99.2 2.08 6.4 11.15 0.0735 0.0803 0.78 - 0.77 5 18 27.8 0.28 4.3 6.44 0.1436 ------------------------------------------------------------------------------ 0.87 - 0.77 1528 1544 99.0 2.22 7.6 13.49 0.0638 0.0659 Inf - 0.77 4968 4984 99.7 2.89 23.0 33.91 0.0287 0.0231 Merged [A], lowest resolution = 9.65 Angstroms, 883 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 mo_uqam001_0m.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C51 H38 O6 P2 Ru S2 Formula weight = 973.99 Tentative Z (number of formula units/cell) = 1.0 giving rho = 1.494, non-H atomic volume = 17.5 and following cell contents and analysis: C 51.00 62.89 % H 38.00 3.93 % O 6.00 9.86 % P 2.00 6.36 % S 2.00 6.58 % Ru 1.00 10.38 % F(000) = 498.0 Mo-K(alpha) radiation Mu (mm-1) = 0.58 ------------------------------------------------------------------------------- File clav002.ins set up as follows: TITL clav002 in P1 CELL 0.71073 10.3632 11.2217 11.5003 117.744 107.588 95.622 ZERR 1.00 0.0008 0.0009 0.0009 0.001 0.001 0.001 LATT -1 SFAC C H O P S RU UNIT 51 38 6 2 2 1 TEMP -23.150 SIZE 0.151 0.218 0.331 TREF HKLF 4 END 14411 Reflections written to new reflection file clav002.hkl -------------------------------------------------------------------------------