+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 2009/1 for Windows + + Copyright(C) 2009 Bruker-AXS All Rights Reserved + + 2009src1247 started at 10:40:47 on 24-Nov-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 15.296 15.296 43.217 90.00 90.00 90.00 52099 Reflections read from file 2009src1247.hkl; mean (I/sigma) = 5.96 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 26120 26027 25935 26020 39041 34747 34761 52099 N (int>3sigma) = 0 15168 15117 15019 15265 22652 20158 20116 30275 Mean intensity = 0.0 19.1 18.9 19.0 19.5 19.0 19.1 18.9 19.0 Mean int/sigma = 0.0 6.0 6.0 6.0 6.0 6.0 6.0 6.0 6.0 Lattice type: P chosen Volume: 10111.29 ------------------------------------------------------------------------------- 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: 15.296 15.296 43.217 90.00 90.00 90.00 Niggli form: a.a = 233.96 b.b = 233.96 c.c = 1867.73 b.c = 0.00 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. TETRAGONAL P-lattice R(sym) = 0.055 [ 18226] Cell: 15.296 15.296 43.217 90.00 90.00 90.00 Volume: 10111.29 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 26120 26027 25935 26020 39041 34747 34761 52099 N (int>3sigma) = 0 15168 15117 15019 15265 22652 20158 20116 30275 Mean intensity = 0.0 19.1 18.9 19.0 19.5 19.0 19.1 18.9 19.0 Mean int/sigma = 0.0 6.0 6.0 6.0 6.0 6.0 6.0 6.0 6.0 Crystal system T and Lattice type P selected Mean |E*E-1| = 0.800 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: 41/43 42 n-- -b- -c- -n- -21- --c N 100 67 410 2493 2448 2453 26 1574 N I>3s 2 2 94 1602 1555 1577 0 1093 0.4 0.5 4.4 25.7 17.9 26.2 0.6 25.0 0.8 0.9 2.9 7.0 6.9 7.0 0.8 7.7 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] P4(1)2(1)2 # 92 chiral 1 245 0.067 23324 0.9 / 2.9 6.30 [B] P4(3)2(1)2 # 96 chiral 1 245 0.067 23324 0.9 / 2.9 6.30 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2009src1247.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) Rsigma Inf - 2.21 333 354 94.1 11.02 83.6 43.23 0.0414 0.0227 2.21 - 1.73 338 339 99.7 11.47 57.8 41.22 0.0452 0.0225 1.73 - 1.50 343 344 99.7 10.51 32.8 34.12 0.0554 0.0238 1.50 - 1.35 358 358 100.0 9.23 21.7 27.19 0.0659 0.0297 1.35 - 1.24 375 375 100.0 8.68 17.1 22.78 0.0759 0.0337 1.24 - 1.16 357 357 100.0 8.23 15.8 20.22 0.0874 0.0385 1.16 - 1.10 340 341 99.7 7.86 12.9 17.77 0.0984 0.0448 1.10 - 1.05 355 355 100.0 7.64 9.9 14.61 0.1134 0.0544 1.05 - 1.01 334 334 100.0 7.53 7.9 12.55 0.1473 0.0664 1.01 - 0.97 392 392 100.0 7.46 6.9 10.98 0.1605 0.0756 0.97 - 0.94 334 334 100.0 7.42 5.5 9.05 0.1842 0.0922 0.94 - 0.91 351 352 99.7 7.23 4.6 7.73 0.2206 0.1117 0.91 - 0.88 459 459 100.0 7.43 4.3 6.59 0.2393 0.1313 0.88 - 0.85 495 496 99.8 7.21 3.4 5.37 0.2867 0.1630 0.85 - 0.83 364 364 100.0 7.12 2.7 4.11 0.3942 0.2213 0.83 - 0.81 403 406 99.3 5.67 2.5 3.29 0.4164 0.2809 0.81 - 0.79 444 446 99.6 5.07 2.0 2.60 0.4491 0.3680 0.79 - 0.77 258 267 96.6 4.51 1.7 2.03 0.5124 0.4835 ------------------------------------------------------------------------------ 0.86 - 0.77 1814 1829 99.2 5.93 2.5 3.49 0.3917 0.2762 Inf - 0.77 6633 6673 99.4 7.81 15.4 15.25 0.0743 0.0460 Merged [A], lowest resolution = 6.84 Angstroms, 2326 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2009src1247.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C36H81N3O12P3Ho1 Formula weight = 1005.89 Tentative Z (number of formula units/cell) = 8.0 giving rho = 1.322, non-H atomic volume = 23.0 and following cell contents and analysis: C 288.00 42.99 % H 648.00 8.12 % N 24.00 4.18 % O 96.00 19.09 % P 24.00 9.24 % Ho 8.00 16.40 % F(000) = 4208.0 Mo-K(alpha) radiation Mu (mm-1) = 1.71 ------------------------------------------------------------------------------- File 2009src1247.ins set up as follows: TITL 2009src1247 in P4(1)2(1)2 CELL 0.71073 15.2959 15.2959 43.2172 90.000 90.000 90.000 ZERR 8.00 0.0006 0.0006 0.0020 0.000 0.000 0.000 LATT -1 SYMM -X, -Y, 0.5+Z SYMM 0.5-Y, 0.5+X, 0.25+Z SYMM 0.5+Y, 0.5-X, 0.75+Z SYMM 0.5-X, 0.5+Y, 0.25-Z SYMM 0.5+X, 0.5-Y, 0.75-Z SYMM Y, X, -Z SYMM -Y, -X, 0.5-Z SFAC C H N O P HO UNIT 288 648 24 96 24 8 TEMP 0.12 TREF HKLF 4 END -------------------------------------------------------------------------------