++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + 2007src0196 started at 22:46:24 on 18-Mar-2007 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 9.298 18.463 18.980 90.00 99.32 90.00 24005 Reflections read from file 2007src0196.hkl; mean (I/sigma) = 5.35 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 12052 12036 12016 12007 18052 16008 16001 24005 N (int>3sigma) = 0 7393 7182 7303 7192 10939 9706 9745 14513 Mean intensity = 0.0 260.0 271.0 272.1 255.8 267.7 265.2 263.4 261.5 Mean int/sigma = 0.0 5.5 5.4 5.5 5.4 5.5 5.5 5.5 5.4 Lattice type: P chosen Volume: 3215.19 ------------------------------------------------------------------------------- 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: 9.298 18.463 18.980 90.00 99.32 90.00 Niggli form: a.a = 86.45 b.b = 340.89 c.c = 360.23 b.c = 0.00 a.c = -28.59 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) = 0.053 [ 5215] Cell: 9.298 18.463 18.980 90.00 99.32 90.00 Volume: 3215.19 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 Current cell not changed ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 12052 12036 12016 12007 18052 16008 16001 24005 N (int>3sigma) = 0 7393 7182 7303 7192 10939 9706 9745 14513 Mean intensity = 0.0 260.0 271.0 272.1 255.8 267.7 265.2 263.4 261.5 Mean int/sigma = 0.0 5.5 5.4 5.5 5.4 5.5 5.5 5.5 5.4 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.950 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 18 384 377 371 N I>3s 0 154 153 7 9.2 408.6 415.9 8.5 0.7 4.2 4.3 0.8 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)/n # 14 centro 1 19410 0.053 5215 0.8 / 4.2 2.96 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2007src0196.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) Inf - 2.10 376 401 93.8 3.48 993.2 17.72 0.0468 0.0446 2.10 - 1.65 400 408 98.0 3.36 747.4 16.97 0.0552 0.0459 1.65 - 1.40 480 496 96.8 3.34 358.2 14.00 0.0640 0.0533 1.40 - 1.25 502 514 97.7 3.87 371.0 14.45 0.0689 0.0532 1.25 - 1.15 490 499 98.2 4.33 264.2 13.02 0.0772 0.0558 1.15 - 1.05 712 721 98.8 4.25 191.8 11.18 0.0878 0.0637 1.05 - 1.00 464 476 97.5 3.88 158.9 10.13 0.0970 0.0726 1.00 - 0.95 569 574 99.1 3.71 117.7 8.59 0.1177 0.0886 0.95 - 0.90 688 698 98.6 3.28 98.8 7.00 0.1353 0.1112 0.90 - 0.85 863 889 97.1 2.62 75.0 5.03 0.1620 0.1613 0.85 - 0.80 1076 1122 95.9 2.13 64.1 3.91 0.1966 0.2138 0.80 - 0.77 761 943 80.7 1.47 49.6 2.64 0.2627 0.3171 ------------------------------------------------------------------------------ 0.90 - 0.77 2700 2954 91.4 2.07 63.5 3.91 0.1888 0.2167 Inf - 0.77 7381 7741 95.3 3.10 227.2 9.04 0.0771 0.0724 Merged [A], lowest resolution = 6.67 Angstroms, 232 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2007src0196.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C27 H37 Ga1 I3 Mo1 O2 P1 Formula weight = 970.90 Tentative Z (number of formula units/cell) = 4.0 giving rho = 2.006, non-H atomic volume = 23.0 and following cell contents and analysis: C 108.00 33.40 % H 148.00 3.84 % O 8.00 3.30 % P 4.00 3.19 % Ga 4.00 7.18 % Mo 4.00 9.88 % I 12.00 39.21 % F(000) = 1848.0 Mo-K(alpha) radiation Mu (mm-1) = 4.18 ------------------------------------------------------------------------------- File 2007src0196.ins set up as follows: TITL 2007src0196 in P2(1)/n CELL 0.71073 9.2979 18.4632 18.9798 90.000 99.325 90.000 ZERR 4.00 0.0005 0.0008 0.0009 0.000 0.003 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H O P GA MO I UNIT 108 148 8 4 4 4 12 TEMP 0.02 TREF HKLF 4 END -------------------------------------------------------------------------------