+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 2009/1 for Windows + + Copyright(C) 2009 Bruker-AXS All Rights Reserved + + 2009src0404 started at 17:27:47 on 08-Apr-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 10.115 10.986 15.088 72.77 72.93 73.22 34086 Reflections read from file 2009src0404.hkl; mean (I/sigma) = 3.86 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 17056 17057 17107 17056 25610 22703 22704 34086 N (int>3sigma) = 0 7645 6158 7661 7423 10732 10002 10367 15203 Mean intensity = 0.0 14.9 6.6 14.8 14.4 12.1 15.3 14.6 15.1 Mean int/sigma = 0.0 4.0 3.0 3.9 3.8 3.6 4.0 4.0 4.0 Lattice type: P chosen Volume: 1492.97 ------------------------------------------------------------------------------- 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: 10.115 10.986 15.088 72.77 72.93 73.22 Niggli form: a.a = 102.30 b.b = 120.69 c.c = 227.64 b.c = 49.08 a.c = 44.79 a.b = 32.07 ------------------------------------------------------------------------------- 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: 10.114 10.986 15.088 72.77 72.93 73.22 Volume: 1492.97 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 17056 17057 17107 17056 25610 22703 22704 34086 N (int>3sigma) = 0 7645 6158 7661 7423 10732 10002 10367 15203 Mean intensity = 0.0 14.9 6.6 14.8 14.4 12.1 15.3 14.6 15.1 Mean int/sigma = 0.0 4.0 3.0 3.9 3.8 3.6 4.0 4.0 4.0 Crystal system A and Lattice type P selected Mean |E*E-1| = 1.004 [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 / 4.0 2.66 [B] P1 # 1 chiral 1 700 0.000 0 0.0 / 4.0 9.86 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2009src0404.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) Rsigma Inf - 2.07 348 356 97.8 6.91 47.9 21.82 0.0432 0.0287 2.07 - 1.65 353 353 100.0 7.01 33.3 20.41 0.0565 0.0311 1.65 - 1.44 357 357 100.0 6.98 19.7 15.94 0.0781 0.0409 1.44 - 1.31 361 361 100.0 6.91 22.7 14.72 0.0749 0.0425 1.31 - 1.21 383 383 100.0 6.94 17.4 13.46 0.0982 0.0514 1.21 - 1.14 349 349 100.0 6.82 12.0 9.67 0.1275 0.0673 1.14 - 1.08 395 395 100.0 6.71 10.3 8.80 0.1504 0.0775 1.08 - 1.03 389 389 100.0 6.30 7.2 6.78 0.1864 0.1048 1.03 - 0.99 387 387 100.0 5.45 8.3 6.55 0.1796 0.1086 0.99 - 0.95 435 435 100.0 4.94 7.1 5.59 0.1909 0.1339 0.95 - 0.92 370 370 100.0 4.61 6.8 5.00 0.2285 0.1650 0.92 - 0.89 462 463 99.8 3.85 5.7 3.87 0.2340 0.1980 0.89 - 0.86 489 489 100.0 3.30 5.3 3.31 0.2609 0.2364 0.86 - 0.84 374 376 99.5 2.85 4.7 2.72 0.2872 0.2997 0.84 - 0.82 431 432 99.8 2.72 4.7 2.52 0.2823 0.3173 0.82 - 0.80 445 446 99.8 2.62 3.4 1.89 0.3596 0.4533 0.80 - 0.78 496 511 97.1 2.34 3.1 1.62 0.3889 0.5424 0.78 - 0.77 46 88 52.3 0.64 4.4 1.24 0.3587 0.5775 ------------------------------------------------------------------------------ 0.87 - 0.77 2112 2173 97.2 2.61 4.1 2.31 0.3106 0.3695 Inf - 0.77 6870 6940 99.0 4.91 12.0 7.93 0.1040 0.0951 Merged [A], lowest resolution = 7.11 Angstroms, 893 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2009src0404.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C12H24Cl8N6O6P6 Formula weight = 817.82 Tentative Z (number of formula units/cell) = 2.0 giving rho = 1.819, non-H atomic volume = 19.6 and following cell contents and analysis: C 24.00 17.62 % H 48.00 2.96 % N 12.00 10.28 % O 12.00 11.74 % P 12.00 22.72 % Cl 16.00 34.68 % F(000) = 824.0 Mo-K(alpha) radiation Mu (mm-1) = 1.12 ------------------------------------------------------------------------------- File 2009src0404.ins set up as follows: TITL 2009src0404 in P-1 CELL 0.71073 10.1145 10.9859 15.0878 72.775 72.933 73.224 ZERR 2.00 0.0004 0.0005 0.0006 0.003 0.003 0.003 LATT 1 SFAC C H N O P CL UNIT 24 48 12 12 12 16 TEMP 0.02 TREF HKLF 4 END 34086 Reflections written to new reflection file 2009src0404.hkl -------------------------------------------------------------------------------