++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + 2006src1374 started at 14:58:59 on 07-Dec-2006 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 7.861 19.622 21.398 90.00 90.00 90.00 28729 Reflections read from file 2006src1374.hkl; mean (I/sigma) = 3.56 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 14338 14365 14407 14295 21555 19137 19232 28729 N (int>3sigma) = 0 5688 5201 5475 5532 8182 7442 7502 11308 Mean intensity = 0.0 104.8 101.1 104.9 106.4 103.6 105.6 105.4 107.9 Mean int/sigma = 0.0 3.8 3.5 3.6 3.7 3.6 3.7 3.7 3.7 Lattice type: P chosen Volume: 3300.63 ------------------------------------------------------------------------------- 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: 7.861 19.622 21.398 90.00 90.00 90.00 Niggli form: a.a = 61.79 b.b = 385.03 c.c = 457.88 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. ORTHORHOMBIC P-lattice R(sym) = 0.119 [ 9097] Cell: 7.861 19.622 21.398 90.00 90.00 90.00 Volume: 3300.63 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 14338 14365 14407 14295 21555 19137 19232 28729 N (int>3sigma) = 0 5688 5201 5475 5532 8182 7442 7502 11308 Mean intensity = 0.0 104.8 101.1 104.9 106.4 103.6 105.6 105.4 107.9 Mean int/sigma = 0.0 3.8 3.5 3.6 3.7 3.6 3.7 3.7 3.7 Crystal system O and Lattice type P selected Mean |E*E-1| = 0.944 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: b-- c-- n-- 21-- -c- -a- -n- -21- --a --b --n --21 N 1385 1347 1346 8 504 506 524 41 429 435 432 38 N I>3s 393 7 388 0 148 1 149 1 131 133 6 0 118.8 9.3 122.0 3.4 146.5 7.1 141.0 11.8 181.1 178.8 8.4 9.6 3.0 0.7 3.0 0.8 3.2 0.7 3.1 0.9 3.5 3.5 0.8 0.7 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] Pbcn # 60 centro 2 571 0.119 9097 0.9 / 3.0 4.68 Option [A] chosen ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 14365 14338 14407 14295 21555 19137 19232 28729 N (int>3sigma) = 0 5201 5688 5475 5532 8182 7442 7502 11308 Mean intensity = 0.0 101.1 104.8 104.9 106.4 103.6 105.6 105.4 107.9 Mean int/sigma = 0.0 3.5 3.8 3.6 3.7 3.6 3.7 3.7 3.7 Crystal system O and Lattice type P selected Mean |E*E-1| = 0.944 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: b-- c-- n-- 21-- -c- -a- -n- -21- --a --b --n --21 N 506 504 524 41 1347 1385 1346 8 435 429 432 38 N I>3s 1 148 149 1 7 393 388 0 133 131 6 0 7.1 146.5 141.0 11.8 9.3 118.8 122.0 3.4 178.8 181.1 8.4 9.6 0.7 3.2 3.1 0.9 0.7 3.0 3.0 0.8 3.5 3.5 0.8 0.7 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] Pbcn # 60 centro 1 571 0.119 9097 0.9 / 3.0 4.68 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2006src1374.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) Inf - 2.75 1447 174 831.6 8.32 537.8 7.81 0.0887 2.75 - 2.15 1479 184 803.8 8.04 223.3 6.24 0.1045 2.15 - 1.80 1714 248 691.1 6.91 222.4 6.55 0.1065 1.80 - 1.60 1533 252 608.3 6.08 227.8 6.42 0.1087 1.60 - 1.45 1664 300 554.7 5.55 162.3 5.73 0.1253 1.45 - 1.30 2217 428 518.0 5.18 89.1 4.22 0.1756 1.30 - 1.20 2132 439 485.6 4.86 69.1 3.87 0.2125 1.20 - 1.10 2483 590 420.8 4.21 58.2 3.35 0.2575 1.10 - 1.05 1557 408 381.6 3.82 49.1 2.75 0.3076 1.05 - 1.00 1677 451 371.8 3.72 42.3 2.48 0.3675 1.00 - 0.95 2009 589 341.1 3.41 40.4 2.21 0.3946 0.95 - 0.90 2284 712 320.8 3.21 31.9 1.79 0.5067 0.90 - 0.85 2472 881 280.6 2.81 24.8 1.48 0.6713 0.85 - 0.80 2652 1137 233.2 2.33 20.6 1.24 0.8564 0.80 - 0.77 1409 896 157.3 1.57 14.3 0.82 1.2588 ------------------------------------------------------------------------------ 0.90 - 0.77 6533 2914 224.2 2.24 20.8 1.24 0.8324 Inf - 0.77 28729 7689 373.6 3.74 105.7 3.56 0.1815 Merged [N], lowest resolution = 6.91 Angstroms, 0 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2006src1374.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C46H50O8B4Fe3 Formula weight = 941.65 Tentative Z (number of formula units/cell) = 3.0 giving rho = 1.421, non-H atomic volume = 18.0 and following cell contents and analysis: C 138.00 58.67 % H 150.00 5.35 % B 12.00 4.59 % O 24.00 13.59 % Fe 9.00 17.79 % F(000) = 1464.0 Mo-K(alpha) radiation Mu (mm-1) = 1.03 ------------------------------------------------------------------------------- File Test.ins set up as follows: TITL Test in Pbcn CELL 0.71073 19.6222 7.8609 21.3982 90.000 90.000 90.000 ZERR 3.00 0.0011 0.0003 0.0011 0.000 0.000 0.000 LATT 1 SYMM 0.5-X, 0.5-Y, 0.5+Z SYMM -X, Y, 0.5-Z SYMM 0.5+X, 0.5-Y, -Z SFAC C H B O FE UNIT 138 150 12 24 9 TEMP 0.01 TREF HKLF 4 END 28729 Reflections written to new reflection file Test.hkl -------------------------------------------------------------------------------