+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 2009/1 for Windows + + Copyright(C) 2009 Bruker-AXS All Rights Reserved + + 2009src0837r started at 10:13:45 on 29-Sep-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 10.409 14.752 18.228 90.00 94.74 90.00 25739 Reflections read from file 2009src0837r.hkl; mean (I/sigma) = 4.09 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 12913 12873 12816 12853 19301 17091 17159 25739 N (int>3sigma) = 0 5646 5613 5527 5572 8393 7462 7410 11211 Mean intensity = 0.0 124.9 123.9 126.0 119.0 124.9 123.3 121.3 123.7 Mean int/sigma = 0.0 4.3 4.2 4.2 4.2 4.2 4.2 4.2 4.2 Lattice type: P chosen Volume: 2789.34 ------------------------------------------------------------------------------- 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: 10.409 14.752 18.228 90.00 94.74 90.00 Niggli form: a.a = 108.34 b.b = 217.63 c.c = 332.24 b.c = 0.00 a.c = -15.68 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) = 0.086 [ 5491] Cell: 10.409 14.752 18.228 90.00 94.74 90.00 Volume: 2789.34 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 12913 12873 12816 12853 19301 17091 17159 25739 N (int>3sigma) = 0 5646 5613 5527 5572 8393 7462 7410 11211 Mean intensity = 0.0 124.9 123.9 126.0 119.0 124.9 123.3 121.3 123.7 Mean int/sigma = 0.0 4.3 4.2 4.2 4.2 4.2 4.2 4.2 4.2 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.941 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 19 748 783 777 N I>3s 0 173 376 361 6.1 24.0 233.5 236.4 1.0 2.1 5.1 5.1 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 0.086 5491 1.0 / 2.1 10.29 [B] P2(1)/m # 11 centro 1 402 0.086 5491 1.0 / 2.1 6.39 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2009src0837r.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) Rsigma Inf - 2.11 336 349 96.3 7.88 458.8 23.98 0.0548 0.0294 2.11 - 1.67 345 345 100.0 6.36 236.2 18.57 0.0650 0.0356 1.67 - 1.46 338 338 100.0 5.27 135.7 14.38 0.0847 0.0496 1.46 - 1.32 352 354 99.4 4.91 146.8 13.01 0.0776 0.0509 1.32 - 1.22 371 371 100.0 4.72 107.9 11.33 0.0982 0.0618 1.22 - 1.14 387 387 100.0 4.33 67.9 8.61 0.1271 0.0893 1.14 - 1.08 382 382 100.0 3.85 55.9 6.97 0.1479 0.1201 1.08 - 1.03 374 374 100.0 3.66 38.7 4.97 0.2151 0.1712 1.03 - 0.99 357 359 99.4 3.42 37.1 4.50 0.2252 0.1924 0.99 - 0.95 425 425 100.0 3.36 34.2 4.09 0.2420 0.2204 0.95 - 0.92 378 380 99.5 3.17 31.2 3.43 0.2402 0.2583 0.92 - 0.89 419 423 99.1 3.02 31.4 3.52 0.2603 0.2745 0.89 - 0.86 482 487 99.0 2.90 28.3 3.07 0.2839 0.3129 0.86 - 0.84 359 363 98.9 2.82 28.0 2.85 0.3090 0.3459 0.84 - 0.82 383 389 98.5 2.71 19.9 2.05 0.4138 0.4995 0.82 - 0.80 439 451 97.3 2.58 18.7 1.91 0.4271 0.5690 0.80 - 0.78 477 493 96.8 2.38 18.5 1.67 0.4836 0.6470 0.78 - 0.76 47 190 24.7 0.27 18.5 0.67 0.4256 1.2948 ------------------------------------------------------------------------------ 0.86 - 0.76 1883 2064 91.2 2.43 21.6 2.16 0.3834 0.4983 Inf - 0.76 6651 6860 97.0 3.75 80.8 7.07 0.0975 0.1073 Merged [A], lowest resolution = 6.83 Angstroms, 242 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2009src0837r.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C38H27NO12S24NaCr Formula weight = 1534.19 Tentative Z (number of formula units/cell) = 2.0 giving rho = 1.827, non-H atomic volume = 18.1 and following cell contents and analysis: C 76.00 29.75 % H 54.00 1.77 % N 2.00 0.91 % O 24.00 12.51 % Na 2.00 1.50 % S 48.00 50.16 % Cr 2.00 3.39 % F(000) = 1554.0 Mo-K(alpha) radiation Mu (mm-1) = 1.17 ------------------------------------------------------------------------------- File 2009src0837r.ins set up as follows: TITL 2009src0837r in P2(1) CELL 0.71073 10.4088 14.7524 18.2275 90.000 94.741 90.000 ZERR 2.00 0.0004 0.0008 0.0008 0.000 0.003 0.000 LATT -1 SYMM -X, 0.5+Y, -Z SFAC C H N O NA S CR UNIT 76 54 2 24 2 48 2 TEMP 0.01 TREF HKLF 4 END -------------------------------------------------------------------------------