+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 2009/1 for Windows + + Copyright(C) 2009 Bruker-AXS All Rights Reserved + + 2009src1135 started at 10:21:48 on 25-Nov-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 10.455 14.653 18.114 90.00 94.09 90.00 25224 Reflections read from file 2009src1135.hkl; mean (I/sigma) = 7.47 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 12609 12638 12591 12546 18919 16778 16821 25224 N (int>3sigma) = 0 8788 8803 8581 8740 13086 11690 11796 17567 Mean intensity = 0.0 110.6 107.4 107.7 103.5 108.6 109.6 104.4 108.2 Mean int/sigma = 0.0 7.6 7.5 7.4 7.5 7.5 7.5 7.5 7.5 Lattice type: P chosen Volume: 2767.89 ------------------------------------------------------------------------------- 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: 10.455 14.653 18.114 90.00 94.09 90.00 Niggli form: a.a = 109.31 b.b = 214.72 c.c = 328.10 b.c = 0.00 a.c = -13.52 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) = 0.036 [ 5518] Cell: 10.455 14.653 18.114 90.00 94.09 90.00 Volume: 2767.89 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 12609 12638 12591 12546 18919 16778 16821 25224 N (int>3sigma) = 0 8788 8803 8581 8740 13086 11690 11796 17567 Mean intensity = 0.0 110.6 107.4 107.7 103.5 108.6 109.6 104.4 108.2 Mean int/sigma = 0.0 7.6 7.5 7.4 7.5 7.5 7.5 7.5 7.5 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.976 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 20 649 664 667 N I>3s 0 228 403 399 2.3 10.8 188.7 188.4 0.9 3.3 7.4 7.3 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 0.036 5518 0.9 / 3.3 9.26 [B] P2(1)/m # 11 centro 1 402 0.036 5518 0.9 / 3.3 3.73 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2009src1135.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) Rsigma Inf - 2.11 333 346 96.2 5.87 401.8 31.52 0.0257 0.0268 2.11 - 1.68 331 332 99.7 5.55 221.8 27.05 0.0336 0.0254 1.68 - 1.47 330 330 100.0 5.43 152.1 25.06 0.0408 0.0295 1.47 - 1.33 339 339 100.0 5.12 140.7 22.70 0.0431 0.0303 1.33 - 1.23 357 357 100.0 4.66 119.9 19.78 0.0482 0.0345 1.23 - 1.15 368 368 100.0 4.28 80.8 16.36 0.0550 0.0406 1.15 - 1.09 365 366 99.7 4.19 70.0 16.04 0.0637 0.0454 1.09 - 1.04 362 362 100.0 3.82 51.4 11.96 0.0754 0.0574 1.04 - 1.00 350 351 99.7 3.65 45.7 11.07 0.0867 0.0650 1.00 - 0.96 387 387 100.0 3.50 44.9 10.61 0.0861 0.0688 0.96 - 0.93 367 367 100.0 3.42 37.7 8.88 0.0922 0.0799 0.93 - 0.90 395 396 99.7 3.19 38.6 8.62 0.0994 0.0849 0.90 - 0.87 446 448 99.6 3.05 34.5 7.97 0.1061 0.0958 0.87 - 0.85 366 368 99.5 3.00 37.9 7.91 0.1023 0.0940 0.85 - 0.83 357 359 99.4 2.84 30.8 7.00 0.1134 0.1137 0.83 - 0.81 417 418 99.8 2.78 22.6 5.42 0.1485 0.1485 0.81 - 0.79 456 458 99.6 2.69 21.2 4.87 0.1550 0.1646 0.79 - 0.77 250 267 93.6 2.36 18.5 4.45 0.1709 0.1947 ------------------------------------------------------------------------------ 0.87 - 0.77 1996 2022 98.7 2.77 26.6 6.06 0.1271 0.1305 Inf - 0.77 6576 6619 99.4 3.81 83.4 13.36 0.0487 0.0471 Merged [A], lowest resolution = 6.79 Angstroms, 411 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2009src1135.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C37H27NO14NaCr Formula weight = 784.59 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.883, non-H atomic volume = 12.8 and following cell contents and analysis: C 148.00 56.64 % H 108.00 3.47 % N 4.00 1.79 % O 56.00 28.55 % Na 4.00 2.93 % Cr 4.00 6.63 % F(000) = 1612.0 Mo-K(alpha) radiation Mu (mm-1) = 0.52 ------------------------------------------------------------------------------- File 2009src1135.ins set up as follows: TITL 2009src1135 in P2(1) CELL 0.71073 10.4550 14.6532 18.1135 90.000 94.095 90.000 ZERR 4.00 0.0004 0.0008 0.0010 0.000 0.002 0.000 LATT -1 SYMM -X, 0.5+Y, -Z SFAC C H N O NA CR UNIT 148 108 4 56 4 4 TEMP 0.01 TREF HKLF 4 END -------------------------------------------------------------------------------