++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION - Version 2005/2 + + COPYRIGHT(c) 2005 Bruker-AXS All Rights Reserved + + klat0831 started at 11:28:47 on 06-Apr-2005 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 23.515 25.962 24.331 90.00 105.27 90.00 40656 Reflections read from file klat0831.raw; mean (I/sigma) = 2.47 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 20289 20332 20335 20321 30478 27114 27096 40656 N (int>3sigma) = 0 5089 5253 5198 5175 7770 6984 6977 10408 Mean intensity = .0 13.0 12.3 13.4 12.3 12.9 13.3 13.1 13.3 Mean int/sigma = .0 2.6 2.6 2.6 2.5 2.6 2.6 2.6 2.6 Lattice type: P chosen Volume: 14329.68 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 1.0000 .0000 .0000 .0000 .0000 1.0000 .0000 -1.0000 .0000 Unitcell: 23.515 24.331 25.962 90.00 90.00 105.27 Niggli form: a.a = 552.96 b.b = 591.99 c.c = 674.03 b.c = .00 a.c = .00 a.b = -150.68 ------------------------------------------------------------------------------- Search for higher metric symmetry Identical indices and Friedel opposites combined before calculating R(sym) ------------------------------------------------------------------------------ Option A: FOM = .000 deg. MONOCLINIC P-lattice R(sym) = .185 [ 11283] Cell: 23.515 25.962 24.331 90.00 105.27 90.00 Volume: 14329.68 Matrix: 1.0000 .0000 .0000 .0000 1.0000 .0000 .0000 .0000 1.0000 ------------------------------------------------------------------------------ Option B: FOM = .000 deg. TRICLINIC P-lattice R(sym) = .000 [ 0] Cell: 23.515 24.331 25.962 90.00 90.00 105.27 Volume: 14329.69 Matrix:-1.0000 .0000 .0000 .0000 .0000 -1.0000 .0000 -1.0000 .0000 Option A selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 20289 20332 20335 20321 30478 27114 27096 40656 N (int>3sigma) = 0 5089 5253 5198 5175 7770 6984 6977 10408 Mean intensity = .0 13.0 12.3 13.4 12.3 12.9 13.3 13.1 13.3 Mean int/sigma = .0 2.6 2.6 2.6 2.5 2.6 2.6 2.6 2.6 Crystal system M and Lattice type P selected Mean |E*E-1| = .711 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 11 524 519 525 N I>3s 0 141 23 144 1.8 16.2 3.3 16.2 .8 2.9 .9 2.9 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 1 19410 .185 11283 .9 / 2.6 12.44 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 klat0831.raw Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) Rsigma Inf - 2.22 1472 1476 99.7 1.83 62.7 12.97 .0604 .0485 2.22 - 1.76 1471 1471 100.0 1.87 24.3 7.24 .0878 .1101 1.76 - 1.53 1518 1518 100.0 1.81 15.6 4.82 .1200 .1850 1.53 - 1.39 1473 1473 100.0 1.68 10.5 2.99 .1774 .3132 1.39 - 1.29 1490 1490 100.0 1.56 8.3 2.20 .2326 .4372 1.29 - 1.21 1574 1578 99.7 1.46 9.3 2.20 .2241 .4345 1.21 - 1.14 1730 1753 98.7 1.39 8.3 2.03 .2590 .4917 1.14 - 1.09 1487 1531 97.1 1.32 8.6 2.07 .2978 .4816 1.09 - 1.04 1756 1850 94.9 1.25 8.8 2.07 .3341 .4818 1.04 - 1.00 1662 1791 92.8 1.20 8.2 1.99 .3741 .5113 1.00 - .96 1880 2070 90.8 1.15 8.2 1.96 .4515 .5241 .96 - .93 1592 1808 88.1 1.10 7.7 1.84 .4859 .5603 .93 - .90 1762 2052 85.9 1.06 7.9 1.86 .4893 .5550 .90 - .87 1948 2346 83.0 1.01 7.7 1.73 .5509 .5804 .87 - .84 2121 2672 79.4 .96 7.5 1.64 .5588 .6098 .84 - .82 1551 2009 77.2 .92 7.2 1.50 .5222 .6663 .82 - .80 1622 2256 71.9 .85 7.1 1.41 .5811 .7034 .80 - .75 1136 5071 22.4 .24 9.1 1.62 .5029 .6153 ------------------------------------------------------------------------------ .85 - .75 5768 11169 51.6 .60 7.6 1.53 .5424 .6529 Inf - .75 29245 36215 80.8 1.12 12.2 2.90 .1659 .3372 Merged [A], lowest resolution = 17.41 Angstroms, 508 outliers downweighted ------------------------------------------------------------------------------- Dataset # 2 created containing 23660 data restricted to range 1.000 < d < 9999.99 Angstroms ------------------------------------------------------------------------------- Current dataset is # 2 klat0831.raw ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C68H68F24N2CrB_C4H10O Formula weight = 1506.17 Tentative Z (number of formula units/cell) = 8.0 giving rho = 1.396, non-H atomic volume = 17.7 and following cell contents and analysis: C 576.00 57.42 % H 624.00 5.22 % B 8.00 .72 % N 16.00 1.86 % O 8.00 1.06 % F 192.00 30.27 % Cr 8.00 3.45 % F(000) = 6216.0 Mo-K(alpha) radiation Mu (mm-1) = .27 ------------------------------------------------------------------------------- File klat0831.ins set up as follows: TITL klat0831 in P2(1)/c CELL .71073 23.5152 25.9620 24.3309 90.000 105.269 90.000 ZERR 8.00 .0047 .0053 .0051 .000 .005 .000 LATT 1 SYMM -X, .5+Y, .5-Z SFAC C H B N O F CR UNIT 576 624 8 16 8 192 8 TEMP -153 SIZE 0.04 0.08 0.18 TREF HKLF 4 END 23660 Reflections written to new reflection file klat0831.hkl -------------------------------------------------------------------------------