SHELXL-97 2006-09-19 2006-12-13 Acta Crystallographica, Section B 2007 63 2 319 327 FA BK5043 Monoclinic -C 2yc 8447.0 1.0 27.5 190.0 prism colorless 0.44 0.38 0.3 1.412 not measured 848.0 0.359 multi-scan HKL Scalepack (Otwinowski & Minor, 1997) 0.858 0.8999 190.0 MoK\a 0.71069 fine-focus sealed tube graphite Nonius KappaCCD CCD \f and \w scans 9.0 32179.0 0.0303 0.027 3.6 27.5 27.5 0.998 0.998 -22.0 23.0 -7.0 7.0 -23.0 23.0 0.0 Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Late refinement difference maps suggested a minor disorder of 180\o rotation about the >C1 - C1'< bond of the C1' - C6' phenyl ring. The relative occupancy refined to 0.9774(16):0.0226(16) with the sum constrained to 1.0. Also U(iso)(F2) = 1.2*U(iso,eq)(C2') and the C2" - F2 was constrained to be the same as C2' - F1. 2217.0 1708.0 I>2u(I) Fsqd full 0.0497 0.0344 0.0876 0.0965 1.045 1.045 2217.0 131.0 1.0 constr calc calc w=1/[\s^2^(Fo^2^)+(0.0509P)^2^+0.6778P] where P=(Fo^2^+2Fc^2^)/3 direct difmap 0.012 0.0020 0.203 -0.261 none Collect (Nonius BV, 1997 - 2000) HKL Scalepack (Otwinowski & Minor, 1997) HKL Denzo, Scalepack (Otwinowski & Minor, 1997 SHELXTL v6.1 (Sheldrick, 2001) SHELXTL v6.1 (Sheldrick, 2001) SHELXTL v6.1 (Sheldrick, 2001) SHELXTL v6.1 (Sheldrick, 2001) All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. 206.63 geom |C|H|F|Cl| |C|H|F|Cl| |0.0033|0.0|0.0171|0.1484| |0.0016|0.0|0.0103|0.1585| |International Tables Vol C Tables 4.2.6.8 and 6.1.1.4|International Tables Vol C Tables 4.2.6.8 and 6.1.1.4|International Tables Vol C Tables 4.2.6.8 and 6.1.1.4|International Tables Vol C Tables 4.2.6.8 and 6.1.1.4| 17.9426 6.0863 18.3206 90.0 103.701 90.0 1.0 0.0 0.0 0.0 0.0 1.0 0.0 0.0 0.0 0.0 1.0 0.0 0.0 0.0 0.0 1.0 -1.0 0.0 0.0 0.0 0.0 1.0 0.0 0.0 0.0 0.0 -1.0 0.5 0.0 0.0 0.0 1.0 1.0 0.0 0.0 0.5 0.0 1.0 0.0 0.5 0.0 0.0 1.0 0.0 0.0 0.0 0.0 1.0 -1.0 0.0 0.0 0.5 0.0 1.0 0.0 0.5 0.0 0.0 -1.0 0.5 0.0 0.0 0.0 1.0 -1.0 0.0 0.0 0.0 0.0 -1.0 0.0 0.0 0.0 0.0 -1.0 0.0 0.0 0.0 0.0 1.0 1.0 0.0 0.0 0.0 0.0 -1.0 0.0 0.0 0.0 0.0 1.0 0.5 0.0 0.0 0.0 1.0 -1.0 0.0 0.0 0.5 0.0 -1.0 0.0 0.5 0.0 0.0 -1.0 0.0 0.0 0.0 0.0 1.0 1.0 0.0 0.0 0.5 0.0 -1.0 0.0 0.5 0.0 0.0 1.0 0.5 0.0 0.0 0.0 1.0 0.05558 Uani A 1 Cl1 . 0.0281 Uani A 1 C1 . 0.0317 Uani A 1 C2 . 0.038 Uiso calc A 1 H2 R 0.0359 Uani A 1 C3 . 0.043 Uiso calc A 1 H3 R 0.0351 Uani A 1 C4 . 0.0368 Uani A 1 C5 . 0.044 Uiso calc A 1 H5 R 0.0331 Uani A 1 C6 . 0.04 Uiso calc A 1 H6 R 0.0276 Uani A 1 C1' P 0.0313 Uani A 1 C2' PD 0.0437 Uani A 1 F1 PD 0.0398 Uani A 1 C3' . 0.048 Uiso calc A 1 H3' R 0.0403 Uani A 1 C4' . 0.048 Uiso calc A 1 H4' R 0.0381 Uani A 1 C5' P 0.046 Uiso calc A 1 H5' R 0.0333 Uani A 1 C6' P 0.04 Uiso calc A 1 H6' PR 0.0333 Uani A 2 C2" PD 0.04 Uiso A 2 F2 PD 0.0313 Uani A 2 C6" P 0.038 Uiso calc A 2 H6" PR |Cl1|C1|C2|C3|C4|C5|C6|C1'|C2'|F1|C3'|C4'|C5'|C6'|C2"|C1"|C6"|C5"| |0.0481|0.0267|0.0325|0.0307|0.0315|0.04|0.0333|0.0253|0.0316|0.0452|0.0321|0.0295|0.0331|0.0303|0.0303|0.0253|0.0316|0.0321| |0.0746|0.0307|0.0314|0.0407|0.0461|0.0378|0.0297|0.0291|0.0291|0.0319|0.0415|0.0536|0.0449|0.0336|0.0336|0.0291|0.0291|0.0415| |0.0349|0.0278|0.0309|0.0356|0.0261|0.0332|0.0372|0.0293|0.033|0.0484|0.0441|0.0344|0.0355|0.0357|0.0357|0.0293|0.033|0.0441| |-0.0194|6.0E-4|0.0036|0.0047|-0.0086|-0.0074|0.0010|0.0037|0.0032|-0.0044|-0.0039|0.0025|0.0042|8.0E-4|8.0E-4|0.0037|0.0032|-0.0039| |-0.00848|0.0084|0.0066|0.0067|0.0037|0.0098|0.01|0.0080|0.0074|3.0E-4|0.0053|9.0E-4|0.0068|0.0075|0.0075|0.0080|0.0074|0.0053| |0.00921|0.0021|-1.0E-4|0.0084|0.0039|-0.0067|-9.0E-4|-5.0E-4|0.0040|0.0115|-0.0032|0.0034|0.0122|0.0053|0.0053|-5.0E-4|0.0040|-0.0032| |Cl1|C1|C1|C1|C2|C2|C3|C3|C4|C5|C5|C6|C1'|C1'|C2'|C2'|C3'|C3'|C4'|C4'|C5'|C5'|C6'|C2"| |C4|C6|C2|C1'|C3|H2|C4|H3|C5|C6|H5|H6|C2'|C6'|F1|C3'|C4'|H3'|C5'|H4'|C6'|H5'|H6'|F2| |1.7417|1.3922|1.3981|1.485|1.3881|0.95|1.382|0.95|1.379|1.3861|0.95|0.95|1.3879|1.4008|1.3613|1.375|1.387|0.95|1.383|0.95|1.3855|0.95|0.95|1.36| |yes|yes|yes|yes|yes|?|yes|?|yes|yes|?|?|yes|yes|yes|yes|yes|?|yes|?|yes|?|?|?| |C6|C6|C2|C3|C3|C1|C4|C4|C2|C5|C5|C3|C4|C4|C6|C5|C5|C1|C2'|C2'|C6'|F1|F1|C3'|C2'|C2'|C4'|C5'|C5'|C3'|C4'|C4'|C6'|C5'|C5'|C1'| |C1|C1|C1|C2|C2|C2|C3|C3|C3|C4|C4|C4|C5|C5|C5|C6|C6|C6|C1'|C1'|C1'|C2'|C2'|C2'|C3'|C3'|C3'|C4'|C4'|C4'|C5'|C5'|C5'|C6'|C6'|C6'| |C2|C1'|C1'|C1|H2|H2|C2|H3|H3|C3|Cl1|Cl1|C6|H5|H5|C1|H6|H6|C6'|C1|C1|C3'|C1'|C1'|C4'|H3'|H3'|C3'|H4'|H4'|C6'|H5'|H5'|C1'|H6'|H6'| |118.23|120.16|121.59|121.05|119.5|119.5|118.99|120.5|120.5|121.38|119.09|119.53|119.11|120.4|120.4|121.24|119.4|119.4|115.68|122.94|121.37|117.55|118.29|124.15|118.55|120.7|120.7|119.68|120.2|120.2|120.35|119.8|119.8|121.58|119.2|119.2| |yes|yes|yes|yes|?|?|yes|?|?|yes|yes|yes|yes|?|?|yes|?|?|yes|yes|yes|yes|yes|yes|yes|?|?|yes|?|?|yes|?|?|yes|?|?|