+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 2009/1 for Windows + + Copyright(C) 2009 Bruker-AXS All Rights Reserved + + 2009src0117 started at 13:59:19 on 17-Feb-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 20.211 10.160 29.683 90.00 91.34 90.00 53981 Reflections read from file 2009src0117.hkl; mean (I/sigma) = 7.58 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 27000 27002 26922 26968 40462 36013 35935 53981 N (int>3sigma) = 0 19612 19724 19128 19659 29232 26366 26256 39403 Mean intensity = 0.0 132.0 129.5 116.1 134.1 125.9 133.1 132.9 132.7 Mean int/sigma = 0.0 7.6 7.6 7.4 7.6 7.5 7.7 7.6 7.6 Lattice type: P chosen Volume: 6093.86 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 -1.0000 0.0000 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 Unitcell: 10.160 20.211 29.683 91.34 90.00 90.00 Niggli form: a.a = 103.23 b.b = 408.50 c.c = 881.06 b.c = -13.99 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. MONOCLINIC P-lattice R(sym) = 0.034 [ 9803] Cell: 20.211 10.160 29.683 90.00 91.34 90.00 Volume: 6093.86 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 27000 27002 26922 26968 40462 36013 35935 53981 N (int>3sigma) = 0 19612 19724 19128 19659 29232 26366 26256 39403 Mean intensity = 0.0 132.0 129.5 116.1 134.1 125.9 133.1 132.9 132.7 Mean int/sigma = 0.0 7.6 7.6 7.4 7.6 7.5 7.7 7.6 7.6 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.907 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 17 1835 1877 1888 N I>3s 0 7 786 793 1.2 1.5 207.0 205.8 0.7 0.7 5.2 5.2 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)/c # 14 centro 4 19410 0.034 9803 0.7 / 5.2 2.58 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2009src0117.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) Rsigma Inf - 2.14 741 769 96.4 5.70 435.5 28.00 0.0353 0.0281 2.14 - 1.69 736 739 99.6 5.42 259.6 25.78 0.0414 0.0297 1.69 - 1.47 762 762 100.0 5.19 176.7 22.86 0.0480 0.0323 1.47 - 1.33 783 785 99.7 4.81 144.4 20.86 0.0503 0.0349 1.33 - 1.23 795 797 99.7 4.37 152.9 19.05 0.0531 0.0371 1.23 - 1.15 809 810 99.9 4.13 114.9 16.75 0.0578 0.0415 1.15 - 1.09 814 818 99.5 3.84 93.4 14.95 0.0666 0.0478 1.09 - 1.04 795 797 99.7 3.63 77.0 13.08 0.0679 0.0533 1.04 - 1.00 777 778 99.9 3.44 72.5 12.36 0.0724 0.0567 1.00 - 0.96 921 923 99.8 3.26 64.9 11.40 0.0784 0.0630 0.96 - 0.93 750 754 99.5 3.21 56.6 9.79 0.0845 0.0683 0.93 - 0.90 914 918 99.6 3.10 51.0 9.48 0.0884 0.0753 0.90 - 0.87 1040 1045 99.5 2.90 48.5 8.40 0.0926 0.0829 0.87 - 0.84 1163 1166 99.7 2.84 39.2 7.59 0.1000 0.0963 0.84 - 0.82 872 876 99.5 2.75 33.2 6.64 0.1175 0.1111 0.82 - 0.80 961 966 99.5 2.64 34.1 6.37 0.1103 0.1146 0.80 - 0.78 1052 1075 97.9 2.55 28.8 5.57 0.1268 0.1327 0.78 - 0.77 7 54 13.0 0.13 25.9 3.61 0.2463 ------------------------------------------------------------------------------ 0.87 - 0.77 4434 4517 98.2 2.68 35.1 6.69 0.1092 0.1091 Inf - 0.77 14692 14832 99.1 3.64 102.6 13.36 0.0539 0.0473 Merged [A], lowest resolution = 6.99 Angstroms, 843 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2009src0117.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C36H30B5N1O10P2 Formula weight = 752.63 Tentative Z (number of formula units/cell) = 6.0 giving rho = 1.231, non-H atomic volume = 18.8 and following cell contents and analysis: C 216.00 57.45 % H 180.00 4.02 % B 30.00 7.18 % N 6.00 1.86 % O 60.00 21.26 % P 12.00 8.23 % F(000) = 2328.0 Mo-K(alpha) radiation Mu (mm-1) = 0.16 ------------------------------------------------------------------------------- File p21c.ins set up as follows: TITL p21c in P2(1)/c CELL 0.71073 29.6827 10.1604 20.2114 90.000 91.337 90.000 ZERR 6.00 0.0006 0.0002 0.0004 0.000 0.001 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H B N O P UNIT 216 180 30 6 60 12 TEMP 0.05 TREF HKLF 4 END 53981 Reflections written to new reflection file p21c.hkl -------------------------------------------------------------------------------