+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 01src322 started at 11:46:27 on 21-Jul-2004 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL SHELXL INS file, from DIRDIF output for S92 REM P21/c pseudo-orthorhmbic C-centered CELL 0.71073 9.91080 29.93160 9.90750 90.0000 104.1960 90.0000 ZERR 4 0.00200 0.00600 0.00200 0.0000 0.0300 0.0000 LATT 1 SYMM -X , 1/2+Y , 1/2-Z SFAC C H N O F P PD UNIT 132 100 4 8 12 4 4 V = 2849.27 F(000) = 1336.0 Mu = 0.76 mm-1 Cell Wt = 2647.64 Rho = 1.543 TEMP -123 SIZE .5 .15 .02 REM PLATE OMIT 0 52 OMIT 0 7 5 OMIT 0 4 1 OMIT -3 2 2 OMIT -1 3 6 OMIT -1 2 2 OMIT -6 4 2 OMIT -5 0 4 OMIT -3 8 5 OMIT -3 5 1 OMIT 6 23 4 OMIT 1 32 0 OMIT 1 3 1 OMIT 7 1 4 OMIT 6 3 5 HTAB BOND $H L.S. 4 BOND FMAP 2 PLAN 10 WGHT 0.058000 1.794700 EXTI 0.001023 FVAR 0.37093 PD1 7 0.208734 0.164766 0.437633 11.00000 0.01828 0.01226 = 0.01796 -0.00121 0.00686 0.00130 P1 6 0.309910 0.097132 0.474559 11.00000 0.01708 0.01299 = 0.01789 -0.00064 0.00815 0.00128 F1 5 -0.168410 0.150834 0.032418 11.00000 0.06304 0.11823 = 0.10672 -0.07261 -0.05276 0.05596 F2 5 -0.124156 0.084352 0.078665 11.00000 0.09980 0.09540 = 0.05092 0.01224 -0.01520 -0.06708 F3 5 -0.049197 0.114551 -0.077697 11.00000 0.06364 0.11220 = 0.02661 -0.02104 0.01175 -0.02135 O1 4 0.043162 0.140772 0.274913 11.00000 0.02607 0.02047 = 0.02018 -0.00287 0.00858 0.00140 O2 4 0.171412 0.139965 0.116499 11.00000 0.02927 0.03093 = 0.02913 0.00266 0.01459 -0.00085 N1 3 0.128701 0.230844 0.415449 11.00000 0.02287 0.01664 = 0.02214 -0.00035 0.00957 0.00167 C1 1 0.195814 0.256169 0.515008 11.00000 0.02958 0.01236 = 0.02981 -0.00237 0.00831 0.00260 AFIX 43 H1 2 0.168636 0.286376 0.521442 11.00000 0.02491 AFIX 0 C2 1 0.312608 0.237833 0.616161 11.00000 0.02346 0.01801 = 0.02366 -0.00183 0.00893 -0.00098 C3 1 0.347791 0.193048 0.595712 11.00000 0.02123 0.02007 = 0.02215 0.00081 0.01152 0.00123 C4 1 0.467198 0.176902 0.689496 11.00000 0.02512 0.01772 = 0.02722 -0.00329 -0.00147 0.00434 AFIX 43 H4 2 0.498369 0.147466 0.677851 11.00000 0.02464 AFIX 0 C5 1 0.541503 0.202843 0.799406 11.00000 0.02352 0.03135 = 0.03070 -0.00265 -0.00287 -0.00224 AFIX 43 H5 2 0.622493 0.190887 0.860754 11.00000 0.02724 AFIX 0 C6 1 0.499342 0.245653 0.820624 11.00000 0.03294 0.03000 = 0.03068 -0.01262 -0.00078 -0.00647 AFIX 43 H6 2 0.548104 0.262563 0.898526 11.00000 0.02803 AFIX 0 C7 1 0.385551 0.263611 0.727391 11.00000 0.03192 0.02060 = 0.03765 -0.00772 0.00939 -0.00092 AFIX 43 H7 2 0.357085 0.293380 0.738953 11.00000 0.02501 AFIX 0 C8 1 0.063355 0.135528 0.155535 11.00000 0.02609 0.00940 = 0.02580 0.00108 0.00783 0.00127 C9 1 -0.068541 0.122058 0.046210 11.00000 0.03454 0.02453 = 0.02379 -0.00128 0.00758 0.00440 C10 1 0.021818 0.251093 0.308392 11.00000 0.02234 0.01829 = 0.02208 -0.00091 0.00910 0.00703 C11 1 -0.105381 0.230113 0.261314 11.00000 0.02615 0.02047 = 0.02785 -0.00146 0.00826 0.00001 AFIX 43 H11 2 -0.122038 0.201902 0.298087 11.00000 0.01048 AFIX 0 C12 1 -0.207676 0.250439 0.160726 11.00000 0.02599 0.03143 = 0.03288 -0.00083 0.00136 0.00353 AFIX 43 H12 2 -0.295010 0.236020 0.128191 11.00000 0.04251 AFIX 0 C13 1 -0.184964 0.291864 0.105938 11.00000 0.03091 0.03529 = 0.03106 0.00197 0.00269 0.00955 AFIX 43 H13 2 -0.256377 0.305910 0.037455 11.00000 0.05500 AFIX 0 C14 1 -0.056863 0.312135 0.152924 11.00000 0.04215 0.02571 = 0.03376 0.00858 0.01306 0.00477 AFIX 43 H14 2 -0.039653 0.340224 0.115741 11.00000 0.05846 AFIX 0 C15 1 0.046027 0.291999 0.253109 11.00000 0.02765 0.02175 = 0.03214 0.00321 0.01034 0.00301 AFIX 43 H15 2 0.133921 0.306167 0.284499 11.00000 0.02324 AFIX 0 C20 1 0.210239 0.053654 0.364839 11.00000 0.02084 0.01541 = 0.01939 0.00322 0.00905 0.00239 C21 1 0.256756 0.030238 0.264353 11.00000 0.02721 0.02057 = 0.02965 -0.00673 0.01724 -0.00555 AFIX 43 H21 2 0.345258 0.036804 0.248191 11.00000 0.03761 AFIX 0 C22 1 0.174149 -0.002766 0.187427 11.00000 0.04170 0.03025 = 0.03242 -0.01179 0.01910 -0.00938 AFIX 43 H22 2 0.206564 -0.018779 0.118791 11.00000 0.06020 AFIX 0 C23 1 0.044630 -0.012627 0.209718 11.00000 0.03779 0.02495 = 0.03380 -0.00546 0.00906 -0.01169 AFIX 43 H23 2 -0.011558 -0.035208 0.156293 11.00000 0.03491 AFIX 0 C24 1 -0.002321 0.010453 0.309690 11.00000 0.02265 0.02874 = 0.03697 -0.00113 0.01163 -0.00654 AFIX 43 H24 2 -0.090936 0.003762 0.325374 11.00000 0.02585 AFIX 0 C25 1 0.079277 0.043197 0.386763 11.00000 0.02148 0.02526 = 0.02607 -0.00301 0.01056 -0.00091 AFIX 43 H25 2 0.046481 0.058919 0.455702 11.00000 0.02450 AFIX 0 C30 1 0.481055 0.097060 0.437591 11.00000 0.01751 0.01119 = 0.02738 -0.00429 0.01189 -0.00136 C31 1 0.601890 0.081330 0.529164 11.00000 0.02399 0.01837 = 0.02576 0.00193 0.00893 0.00123 AFIX 43 H31 2 0.597179 0.068208 0.615198 11.00000 0.02568 AFIX 0 C32 1 0.729399 0.084854 0.494515 11.00000 0.01914 0.02396 = 0.03740 0.00029 0.00698 0.00189 AFIX 43 H32 2 0.811180 0.073800 0.556872 11.00000 0.04854 AFIX 0 C33 1 0.738335 0.104313 0.370046 11.00000 0.02501 0.02385 = 0.04643 -0.00192 0.01937 -0.00064 AFIX 43 H33 2 0.825815 0.106936 0.347528 11.00000 0.05881 AFIX 0 C34 1 0.618945 0.119840 0.279151 11.00000 0.03128 0.02447 = 0.03271 0.00508 0.01730 0.00027 AFIX 43 H34 2 0.624576 0.133096 0.193580 11.00000 0.04258 AFIX 0 C35 1 0.489806 0.116280 0.311583 11.00000 0.02504 0.01679 = 0.03183 0.00350 0.01299 0.00336 AFIX 43 H35 2 0.408170 0.126915 0.248032 11.00000 0.03030 AFIX 0 C40 1 0.327387 0.072032 0.645267 11.00000 0.01706 0.01843 = 0.01776 0.00194 0.00710 -0.00018 C41 1 0.282946 0.094556 0.749821 11.00000 0.02564 0.01884 = 0.02568 -0.00449 0.00924 0.00016 AFIX 43 H41 2 0.245908 0.123871 0.732946 11.00000 0.02092 AFIX 0 C42 1 0.292185 0.074727 0.877500 11.00000 0.02977 0.04081 = 0.02152 -0.00416 0.01511 -0.00110 AFIX 43 H42 2 0.262685 0.090412 0.948560 11.00000 0.02633 AFIX 0 C43 1 0.344765 0.031802 0.901319 11.00000 0.02668 0.04630 = 0.02069 0.01161 0.00647 -0.00103 AFIX 43 H43 2 0.352115 0.018163 0.989410 11.00000 0.02054 AFIX 0 C44 1 0.386552 0.008695 0.798121 11.00000 0.02614 0.02336 = 0.02841 0.00795 0.00744 0.00139 AFIX 43 H44 2 0.422014 -0.020805 0.815133 11.00000 0.02319 AFIX 0 C45 1 0.376813 0.028518 0.669478 11.00000 0.02258 0.02136 = 0.02223 0.00094 0.00916 0.00245 AFIX 43 H45 2 0.403912 0.012368 0.597875 11.00000 0.02098 HKLF 4 Covalent radii and connectivity table for SHELXL INS file, from DIRDIF output for S92 C 0.770 H 0.320 N 0.700 O 0.660 F 0.640 P 1.100 PD 1.380 Pd1 - C3 N1 O1 P1 P1 - C40 C30 C20 Pd1 F1 - C9 F2 - C9 F3 - C9 O1 - C8 Pd1 O2 - C8 N1 - C1 C10 Pd1 C1 - N1 C2 C2 - C7 C3 C1 C3 - C4 C2 Pd1 C4 - C5 C3 C5 - C6 C4 C6 - C7 C5 C7 - C6 C2 C8 - O2 O1 C9 C9 - F1 F3 F2 C8 C10 - C11 C15 N1 C11 - C12 C10 C12 - C11 C13 C13 - C14 C12 C14 - C15 C13 C15 - C14 C10 C20 - C21 C25 P1 C21 - C20 C22 C22 - C21 C23 C23 - C24 C22 C24 - C25 C23 C25 - C24 C20 C30 - C31 C35 P1 C31 - C32 C30 C32 - C33 C31 C33 - C34 C32 C34 - C33 C35 C35 - C30 C34 C40 - C45 C41 P1 C41 - C42 C40 C42 - C41 C43 C43 - C44 C42 C44 - C43 C45 C45 - C44 C40 h k l Fo^2 Sigma Why rejected -2 0 5 11.41 2.06 observed but should be systematically absent -1 0 3 5.18 1.18 observed but should be systematically absent 0 5 0 3.22 0.60 observed but should be systematically absent -3 0 3 12.71 1.89 observed but should be systematically absent -2 0 1 3.53 0.46 observed but should be systematically absent -1 0 3 11.70 1.64 observed but should be systematically absent 1 0 1 1.72 0.29 observed but should be systematically absent 2 0 3 5.32 1.30 observed but should be systematically absent 2 0 3 4.67 1.10 observed but should be systematically absent 15793 Reflections read, of which 1318 rejected -10 =< h =< 12, -33 =< k =< 36, -12 =< l =< 9, Max. 2-theta = 52.00 9 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 6 9 0 375.77 10.95 2 68.42 7 9 0 116.21 3.79 3 19.25 7 10 0 1043.71 28.25 2 223.02 6 11 0 1541.05 45.33 2 311.36 7 11 0 337.90 8.96 3 45.68 6 12 0 122.95 4.10 3 22.90 7 13 0 125.05 5.91 2 33.66 8 13 0 572.27 16.44 3 86.11 7 14 0 301.01 8.42 3 57.90 6 15 0 123.76 5.45 2 31.76 6 17 0 529.26 17.42 2 118.26 7 18 0 596.55 21.11 2 166.11 6 19 0 215.43 8.61 2 54.16 5 22 0 1018.39 34.16 2 177.49 6 23 0 1058.70 38.10 2 215.71 5 24 0 1095.51 39.71 2 212.21 7 2 1 1249.92 29.15 3 222.51 -6 10 1 752.61 16.99 3 98.22 6 10 1 453.67 10.87 4 55.76 7 10 1 528.52 17.60 3 94.62 6 11 1 149.67 4.43 3 28.86 -5 12 1 116.80 3.50 3 19.00 -7 13 1 216.80 6.17 3 38.31 -6 13 1 559.50 14.27 3 71.73 6 13 1 251.63 8.83 2 55.49 7 13 1 157.18 6.50 2 34.13 6 14 1 174.18 6.76 2 40.14 7 14 1 351.14 12.04 2 80.57 -9 15 1 320.55 11.46 3 58.13 -7 15 1 217.47 8.07 2 52.45 6 15 1 154.18 6.62 2 41.92 7 15 1 683.46 24.54 2 152.29 -9 16 1 133.14 5.86 3 32.86 6 16 1 511.48 19.22 2 121.94 6 17 1 176.55 7.71 2 46.67 -6 20 1 1736.30 56.96 2 355.72 -7 21 1 467.75 19.48 2 114.34 -7 22 1 199.48 10.08 2 61.29 -6 22 1 397.32 13.93 2 74.18 6 0 2 950.69 21.40 3 113.52 7 0 2 121.58 4.94 2 30.19 7 1 2 301.49 7.58 4 40.68 7 3 2 290.62 6.99 4 41.30 1 4 2 848.79 8.61 9 45.62 5 10 2 1665.99 35.10 3 265.11 6 10 2 437.16 11.75 3 88.64 6 11 2 881.19 22.70 3 168.33 -9 12 2 335.35 14.11 2 103.81 -6 12 2 750.32 16.34 3 95.68 6 12 2 383.60 12.82 2 64.99 ** etc. ** 108 Inconsistent equivalents 5317 Unique reflections, of which 0 suppressed R(int) = 0.0868 R(sigma) = 0.0683 Friedel opposites merged Maximum memory for data reduction = 3348 / 53321 Default effective X-H distances for T = -123.0 C AFIX m = 1 2 3 4 4[N] 3[N] 15[B] 8[O] 9 9[N] 16 d(X-H) = 1.00 0.99 0.98 0.95 0.88 0.91 1.12 0.84 0.95 0.88 0.95 Note that these distances are chosen to give the best fit to the X-ray data and so avoid the introduction of systematic error. The true internuclear distances are longer and do not vary with temperature ! The apparent variation with temperature is caused by libration. Least-squares cycle 1 Maximum vector length = 511 Memory required = 4344 / 510171 wR2 = 0.1188 before cycle 1 for 5317 data and 396 / 396 parameters GooF = S = 1.098; Restrained GooF = 1.098 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0580 * P )^2 + 1.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.37093 0.00080 0.000 OSF 2 0.00102 0.00048 -0.002 EXTI Mean shift/esd = 0.001 Maximum = -0.041 for U23 Pd1 Max. shift = 0.000 A for F2 Max. dU = 0.000 for H22 Least-squares cycle 2 Maximum vector length = 511 Memory required = 4344 / 510171 wR2 = 0.1187 before cycle 2 for 5317 data and 396 / 396 parameters GooF = S = 1.098; Restrained GooF = 1.098 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0580 * P )^2 + 1.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.37093 0.00080 0.000 OSF 2 0.00102 0.00048 0.000 EXTI Mean shift/esd = 0.001 Maximum = -0.015 for U23 Pd1 Max. shift = 0.000 A for F2 Max. dU = 0.000 for H13 Least-squares cycle 3 Maximum vector length = 511 Memory required = 4344 / 510171 wR2 = 0.1187 before cycle 3 for 5317 data and 396 / 396 parameters GooF = S = 1.098; Restrained GooF = 1.098 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0580 * P )^2 + 1.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.37093 0.00080 0.002 OSF 2 0.00102 0.00048 0.001 EXTI Mean shift/esd = 0.000 Maximum = 0.002 for OSF Max. shift = 0.000 A for F1 Max. dU = 0.000 for H32 Least-squares cycle 4 Maximum vector length = 511 Memory required = 4344 / 510171 wR2 = 0.1187 before cycle 4 for 5317 data and 396 / 396 parameters GooF = S = 1.098; Restrained GooF = 1.098 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0580 * P )^2 + 1.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.37093 0.00080 0.001 OSF 2 0.00102 0.00048 0.001 EXTI Mean shift/esd = 0.000 Maximum = 0.001 for OSF Max. shift = 0.000 A for C7 Max. dU = 0.000 for H13 Largest correlation matrix elements 0.634 U33 Pd1 / OSF 0.585 U11 Pd1 / OSF -0.513 U23 F1 / U33 F1 0.620 U22 Pd1 / OSF 0.576 EXTI / OSF -0.503 U23 F1 / U22 F1 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1 0.1686 0.2864 0.5214 43 0.950 0.000 C1 N1 C2 H4 0.4984 0.1475 0.6779 43 0.950 0.000 C4 C5 C3 H5 0.6225 0.1909 0.8608 43 0.950 0.000 C5 C6 C4 H6 0.5481 0.2626 0.8985 43 0.950 0.000 C6 C7 C5 H7 0.3571 0.2934 0.7390 43 0.950 0.000 C7 C6 C2 H11 -0.1220 0.2019 0.2981 43 0.950 0.000 C11 C12 C10 H12 -0.2950 0.2360 0.1282 43 0.950 0.000 C12 C11 C13 H13 -0.2564 0.3059 0.0375 43 0.950 0.000 C13 C14 C12 H14 -0.0397 0.3402 0.1157 43 0.950 0.000 C14 C15 C13 H15 0.1339 0.3062 0.2845 43 0.950 0.000 C15 C14 C10 H21 0.3453 0.0368 0.2482 43 0.950 0.000 C21 C20 C22 H22 0.2066 -0.0188 0.1188 43 0.950 0.000 C22 C21 C23 H23 -0.0116 -0.0352 0.1563 43 0.950 0.000 C23 C24 C22 H24 -0.0909 0.0038 0.3254 43 0.950 0.000 C24 C25 C23 H25 0.0465 0.0589 0.4557 43 0.950 0.000 C25 C24 C20 H31 0.5972 0.0682 0.6152 43 0.950 0.000 C31 C32 C30 H32 0.8112 0.0738 0.5569 43 0.950 0.000 C32 C33 C31 H33 0.8258 0.1069 0.3475 43 0.950 0.000 C33 C34 C32 H34 0.6246 0.1331 0.1936 43 0.950 0.000 C34 C33 C35 H35 0.4082 0.1269 0.2480 43 0.950 0.000 C35 C30 C34 H41 0.2459 0.1239 0.7329 43 0.950 0.000 C41 C42 C40 H42 0.2627 0.0904 0.9486 43 0.950 0.000 C42 C41 C43 H43 0.3521 0.0182 0.9894 43 0.950 0.000 C43 C44 C42 H44 0.4220 -0.0208 0.8151 43 0.950 0.000 C44 C43 C45 H45 0.4039 0.0124 0.5979 43 0.950 0.000 C45 C44 C40 SHELXL INS file, from DIRDIF output for S92 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq Pd1 0.20873 0.16477 0.43763 1.00000 0.01828 0.01226 0.01796 -0.00121 0.00686 0.00130 0.01575 0.00044 0.00002 0.00001 0.00002 0.00000 0.00018 0.00018 0.00017 0.00009 0.00011 0.00009 0.00012 P1 0.30991 0.09713 0.47456 1.00000 0.01708 0.01299 0.01789 -0.00064 0.00815 0.00128 0.01532 0.00155 0.00009 0.00003 0.00008 0.00000 0.00042 0.00042 0.00039 0.00031 0.00032 0.00032 0.00019 F1 -0.16841 0.15083 0.03242 1.00000 0.06304 0.11823 0.10672 -0.07260 -0.05276 0.05595 0.10880 0.00608 0.00037 0.00014 0.00039 0.00000 0.00215 0.00293 0.00262 0.00237 0.00195 0.00224 0.00161 F2 -0.12415 0.08435 0.07867 1.00000 0.09980 0.09539 0.05091 0.01224 -0.01520 -0.06708 0.08789 0.00508 0.00038 0.00012 0.00029 0.00000 0.00270 0.00248 0.00167 0.00163 0.00162 0.00219 0.00121 F3 -0.04920 0.11455 -0.07770 1.00000 0.06364 0.11220 0.02661 -0.02104 0.01175 -0.02136 0.06737 0.00491 0.00029 0.00012 0.00024 0.00000 0.00182 0.00248 0.00123 0.00140 0.00116 0.00177 0.00086 O1 0.04316 0.14077 0.27491 1.00000 0.02607 0.02047 0.02018 -0.00287 0.00858 0.00140 0.02173 0.00420 0.00024 0.00008 0.00021 0.00000 0.00131 0.00127 0.00112 0.00094 0.00095 0.00100 0.00051 O2 0.17141 0.13996 0.11650 1.00000 0.02927 0.03093 0.02913 0.00266 0.01458 -0.00085 0.02849 0.00468 0.00025 0.00008 0.00024 0.00000 0.00140 0.00146 0.00126 0.00106 0.00106 0.00114 0.00057 N1 0.12870 0.23084 0.41545 1.00000 0.02287 0.01664 0.02214 -0.00035 0.00957 0.00167 0.01985 0.00518 0.00028 0.00009 0.00027 0.00000 0.00150 0.00141 0.00134 0.00112 0.00112 0.00119 0.00058 C1 0.19581 0.25617 0.51501 1.00000 0.02958 0.01236 0.02981 -0.00237 0.00831 0.00260 0.02374 0.00645 0.00036 0.00011 0.00034 0.00000 0.00195 0.00168 0.00180 0.00135 0.00148 0.00145 0.00074 H1 0.16864 0.28638 0.52144 1.00000 0.02492 0.00000 0.00934 C2 0.31261 0.23783 0.61616 1.00000 0.02346 0.01801 0.02365 -0.00183 0.00893 -0.00098 0.02116 0.00641 0.00035 0.00011 0.00034 0.00000 0.00179 0.00172 0.00162 0.00135 0.00133 0.00142 0.00070 C3 0.34779 0.19305 0.59571 1.00000 0.02123 0.02007 0.02215 0.00081 0.01152 0.00123 0.02007 0.00643 0.00035 0.00011 0.00032 0.00000 0.00173 0.00172 0.00157 0.00135 0.00132 0.00142 0.00069 C4 0.46720 0.17690 0.68950 1.00000 0.02512 0.01772 0.02722 -0.00329 -0.00147 0.00433 0.02473 0.00660 0.00037 0.00012 0.00035 0.00000 0.00193 0.00171 0.00176 0.00142 0.00145 0.00154 0.00076 H4 0.49837 0.14747 0.67785 1.00000 0.02464 0.00000 0.00935 C5 0.54150 0.20284 0.79941 1.00000 0.02351 0.03135 0.03070 -0.00265 -0.00287 -0.00224 0.03018 0.00668 0.00038 0.00013 0.00037 0.00000 0.00192 0.00214 0.00187 0.00156 0.00150 0.00160 0.00084 H5 0.62249 0.19089 0.86076 1.00000 0.02723 0.00000 0.00973 C6 0.49934 0.24565 0.82062 1.00000 0.03294 0.03000 0.03068 -0.01262 -0.00078 -0.00647 0.03270 0.00676 0.00040 0.00013 0.00038 0.00000 0.00217 0.00210 0.00190 0.00163 0.00161 0.00175 0.00088 H6 0.54810 0.26256 0.89852 1.00000 0.02802 0.00000 0.00970 C7 0.38555 0.26361 0.72739 1.00000 0.03192 0.02060 0.03765 -0.00772 0.00939 -0.00092 0.02991 0.00681 0.00038 0.00012 0.00037 0.00000 0.00211 0.00189 0.00201 0.00155 0.00165 0.00161 0.00083 H7 0.35709 0.29338 0.73895 1.00000 0.02501 0.00000 0.00936 C8 0.06336 0.13553 0.15554 1.00000 0.02608 0.00940 0.02580 0.00108 0.00783 0.00127 0.02017 0.00623 0.00035 0.00010 0.00033 0.00000 0.00185 0.00154 0.00168 0.00127 0.00137 0.00139 0.00069 C9 -0.06854 0.12206 0.04621 1.00000 0.03454 0.02453 0.02379 -0.00129 0.00758 0.00440 0.02754 0.00693 0.00039 0.00012 0.00035 0.00000 0.00212 0.00194 0.00177 0.00142 0.00150 0.00166 0.00081 C10 0.02182 0.25109 0.30839 1.00000 0.02234 0.01829 0.02208 -0.00091 0.00910 0.00704 0.02027 0.00637 0.00034 0.00011 0.00032 0.00000 0.00179 0.00170 0.00159 0.00133 0.00135 0.00141 0.00070 C11 -0.10538 0.23011 0.26131 1.00000 0.02615 0.02047 0.02786 -0.00146 0.00826 0.00001 0.02454 0.00643 0.00035 0.00012 0.00034 0.00000 0.00189 0.00181 0.00174 0.00142 0.00142 0.00149 0.00074 H11 -0.12204 0.20190 0.29809 1.00000 0.01048 0.00000 0.00783 C12 -0.20768 0.25044 0.16073 1.00000 0.02599 0.03143 0.03288 -0.00083 0.00136 0.00353 0.03112 0.00725 0.00040 0.00013 0.00037 0.00000 0.00201 0.00207 0.00193 0.00163 0.00155 0.00168 0.00083 H12 -0.29501 0.23602 0.12819 1.00000 0.04251 0.00000 0.01171 C13 -0.18496 0.29186 0.10594 1.00000 0.03091 0.03529 0.03106 0.00197 0.00269 0.00955 0.03328 0.00769 0.00041 0.00013 0.00039 0.00000 0.00210 0.00224 0.00185 0.00168 0.00159 0.00178 0.00088 H13 -0.25638 0.30591 0.03746 1.00000 0.05503 0.00000 0.01333 C14 -0.05686 0.31214 0.15292 1.00000 0.04215 0.02571 0.03376 0.00858 0.01306 0.00477 0.03322 0.00773 0.00042 0.00013 0.00038 0.00000 0.00242 0.00210 0.00199 0.00163 0.00174 0.00177 0.00089 H14 -0.03965 0.34022 0.11574 1.00000 0.05844 0.00000 0.01465 C15 0.04603 0.29200 0.25311 1.00000 0.02765 0.02175 0.03214 0.00321 0.01034 0.00300 0.02666 0.00714 0.00038 0.00012 0.00036 0.00000 0.00198 0.00184 0.00184 0.00147 0.00153 0.00154 0.00078 H15 0.13392 0.30617 0.28450 1.00000 0.02324 0.00000 0.00921 C20 0.21024 0.05365 0.36484 1.00000 0.02085 0.01541 0.01938 0.00322 0.00905 0.00239 0.01783 0.00618 0.00034 0.00011 0.00031 0.00000 0.00172 0.00160 0.00154 0.00126 0.00127 0.00136 0.00067 C21 0.25676 0.03024 0.26435 1.00000 0.02721 0.02057 0.02965 -0.00673 0.01724 -0.00555 0.02402 0.00645 0.00037 0.00011 0.00034 0.00000 0.00190 0.00177 0.00176 0.00141 0.00149 0.00150 0.00075 H21 0.34526 0.03680 0.24819 1.00000 0.03761 0.00000 0.01103 C22 0.17415 -0.00277 0.18743 1.00000 0.04169 0.03025 0.03243 -0.01179 0.01910 -0.00938 0.03305 0.00714 0.00042 0.00013 0.00038 0.00000 0.00233 0.00211 0.00193 0.00162 0.00173 0.00178 0.00089 H22 0.20656 -0.01878 0.11879 1.00000 0.06017 0.00000 0.01418 C23 0.04463 -0.01263 0.20972 1.00000 0.03779 0.02495 0.03380 -0.00546 0.00906 -0.01169 0.03213 0.00709 0.00041 0.00013 0.00037 0.00000 0.00228 0.00199 0.00198 0.00159 0.00168 0.00173 0.00087 H23 -0.01156 -0.03521 0.15629 1.00000 0.03492 0.00000 0.01061 C24 -0.00232 0.01045 0.30969 1.00000 0.02265 0.02874 0.03697 -0.00113 0.01163 -0.00654 0.02870 0.00687 0.00038 0.00012 0.00037 0.00000 0.00189 0.00197 0.00195 0.00160 0.00156 0.00162 0.00080 H24 -0.09094 0.00376 0.32537 1.00000 0.02586 0.00000 0.00940 C25 0.07928 0.04320 0.38676 1.00000 0.02149 0.02526 0.02607 -0.00301 0.01056 -0.00091 0.02345 0.00640 0.00035 0.00012 0.00034 0.00000 0.00178 0.00190 0.00170 0.00143 0.00140 0.00148 0.00074 H25 0.04648 0.05892 0.45570 1.00000 0.02451 0.00000 0.00942 C30 0.48106 0.09706 0.43759 1.00000 0.01751 0.01119 0.02738 -0.00429 0.01189 -0.00136 0.01759 0.00596 0.00033 0.00010 0.00032 0.00000 0.00164 0.00156 0.00163 0.00125 0.00134 0.00126 0.00066 C31 0.60189 0.08133 0.52916 1.00000 0.02399 0.01837 0.02576 0.00193 0.00893 0.00123 0.02221 0.00645 0.00035 0.00011 0.00035 0.00000 0.00182 0.00170 0.00170 0.00136 0.00139 0.00144 0.00072 H31 0.59718 0.06821 0.61520 1.00000 0.02568 0.00000 0.00950 C32 0.72940 0.08485 0.49451 1.00000 0.01914 0.02396 0.03740 0.00029 0.00698 0.00189 0.02683 0.00695 0.00036 0.00012 0.00039 0.00000 0.00181 0.00188 0.00197 0.00156 0.00150 0.00151 0.00077 H32 0.81118 0.07380 0.55687 1.00000 0.04855 0.00000 0.01312 C33 0.73833 0.10431 0.37005 1.00000 0.02501 0.02385 0.04642 -0.00192 0.01936 -0.00064 0.02992 0.00726 0.00038 0.00012 0.00039 0.00000 0.00194 0.00194 0.00214 0.00165 0.00167 0.00158 0.00082 H33 0.82582 0.10694 0.34753 1.00000 0.05882 0.00000 0.01388 C34 0.61894 0.11984 0.27915 1.00000 0.03128 0.02447 0.03271 0.00508 0.01730 0.00027 0.02784 0.00718 0.00038 0.00012 0.00037 0.00000 0.00206 0.00190 0.00193 0.00151 0.00159 0.00161 0.00081 H34 0.62458 0.13310 0.19358 1.00000 0.04258 0.00000 0.01162 C35 0.48981 0.11628 0.31158 1.00000 0.02504 0.01679 0.03183 0.00350 0.01299 0.00336 0.02351 0.00671 0.00036 0.00011 0.00035 0.00000 0.00185 0.00168 0.00182 0.00142 0.00148 0.00147 0.00074 H35 0.40817 0.12692 0.24803 1.00000 0.03029 0.00000 0.01014 C40 0.32739 0.07203 0.64527 1.00000 0.01707 0.01843 0.01776 0.00194 0.00710 -0.00018 0.01726 0.00607 0.00033 0.00011 0.00031 0.00000 0.00163 0.00165 0.00150 0.00125 0.00122 0.00131 0.00066 C41 0.28295 0.09456 0.74982 1.00000 0.02564 0.01884 0.02568 -0.00449 0.00924 0.00016 0.02288 0.00630 0.00036 0.00011 0.00033 0.00000 0.00185 0.00176 0.00169 0.00135 0.00141 0.00144 0.00073 H41 0.24591 0.12387 0.73295 1.00000 0.02091 0.00000 0.00907 C42 0.29218 0.07473 0.87750 1.00000 0.02977 0.04081 0.02152 -0.00416 0.01511 -0.00110 0.02916 0.00703 0.00038 0.00013 0.00035 0.00000 0.00201 0.00228 0.00169 0.00157 0.00148 0.00172 0.00083 H42 0.26268 0.09041 0.94856 1.00000 0.02634 0.00000 0.00951 C43 0.34477 0.03180 0.90132 1.00000 0.02668 0.04630 0.02069 0.01161 0.00647 -0.00103 0.03110 0.00711 0.00038 0.00014 0.00035 0.00000 0.00198 0.00241 0.00167 0.00162 0.00144 0.00177 0.00086 H43 0.35212 0.01816 0.98941 1.00000 0.02054 0.00000 0.00884 C44 0.38655 0.00869 0.79812 1.00000 0.02614 0.02336 0.02841 0.00795 0.00744 0.00139 0.02584 0.00679 0.00036 0.00012 0.00034 0.00000 0.00191 0.00187 0.00179 0.00146 0.00145 0.00156 0.00076 H44 0.42201 -0.02080 0.81513 1.00000 0.02320 0.00000 0.00931 C45 0.37681 0.02852 0.66948 1.00000 0.02257 0.02136 0.02223 0.00095 0.00916 0.00245 0.02142 0.00639 0.00035 0.00011 0.00033 0.00000 0.00177 0.00174 0.00162 0.00135 0.00134 0.00144 0.00071 H45 0.40391 0.01237 0.59788 1.00000 0.02098 0.00000 0.00894 Final Structure Factor Calculation for SHELXL INS file, from DIRDIF output for S92 Total number of l.s. parameters = 396 Maximum vector length = 511 Memory required = 3948 / 26061 wR2 = 0.1187 before cycle 5 for 5317 data and 0 / 396 parameters GooF = S = 1.098; Restrained GooF = 1.098 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0580 * P )^2 + 1.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0429 for 4675 Fo > 4sig(Fo) and 0.0493 for all 5317 data wR2 = 0.1187, GooF = S = 1.098, Restrained GooF = 1.098 for all data Occupancy sum of asymmetric unit = 41.00 for non-hydrogen and 25.00 for hydrogen atoms Principal mean square atomic displacements U 0.0201 0.0160 0.0111 Pd1 0.0206 0.0143 0.0111 P1 0.2622 0.0421 0.0220 F1 may be split into -0.1740 0.1462 0.0494 and -0.1628 0.1555 0.0154 0.1860 0.0495 0.0281 F2 0.1223 0.0582 0.0217 F3 0.0267 0.0230 0.0155 O1 0.0355 0.0313 0.0187 O2 0.0259 0.0185 0.0152 N1 0.0305 0.0293 0.0114 C1 0.0265 0.0196 0.0174 C2 0.0269 0.0199 0.0134 C3 0.0385 0.0200 0.0157 C4 0.0405 0.0319 0.0181 C5 0.0455 0.0381 0.0145 C6 0.0406 0.0315 0.0176 C7 0.0273 0.0240 0.0093 C8 0.0364 0.0251 0.0211 C9 0.0279 0.0220 0.0109 C10 0.0287 0.0248 0.0201 C11 0.0393 0.0311 0.0230 C12 0.0441 0.0337 0.0221 C13 0.0454 0.0340 0.0203 C14 0.0342 0.0254 0.0204 C15 0.0248 0.0153 0.0134 C20 0.0399 0.0175 0.0147 C21 0.0533 0.0270 0.0188 C22 0.0448 0.0339 0.0177 C23 0.0380 0.0314 0.0167 C24 0.0298 0.0237 0.0168 C25 0.0302 0.0128 0.0098 C30 0.0277 0.0210 0.0179 C31 0.0377 0.0246 0.0182 C32 0.0489 0.0237 0.0171 C33 0.0404 0.0258 0.0173 C34 0.0351 0.0198 0.0156 C35 0.0206 0.0181 0.0131 C40 0.0290 0.0238 0.0158 C41 0.0420 0.0328 0.0127 C42 0.0512 0.0266 0.0155 C43 0.0342 0.0258 0.0175 C44 0.0263 0.0208 0.0172 C45 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.024 0.045 0.069 0.095 0.126 0.158 0.194 0.237 0.314 1.000 Number in group 546. 529. 535. 516. 532. 532. 543. 519. 531. 534. GooF 1.016 0.997 1.093 1.094 1.150 1.247 1.186 1.159 1.108 0.887 K 2.021 1.069 1.024 1.001 0.988 1.001 1.016 1.017 1.021 1.010 Resolution(A) 0.81 0.84 0.88 0.92 0.98 1.04 1.12 1.23 1.40 1.75 inf Number in group 545. 531. 523. 538. 526. 533. 539. 517. 534. 531. GooF 1.100 1.013 1.076 1.111 1.093 1.098 1.017 1.007 1.186 1.252 K 0.993 1.008 1.006 1.029 1.044 1.047 1.027 1.012 1.008 0.997 R1 0.094 0.080 0.069 0.062 0.055 0.050 0.042 0.038 0.033 0.029 Recommended weighting scheme: WGHT 0.0529 2.5354 Note that in most cases convergence will be faster if fixed weights (e.g. the default WGHT 0.1) are retained until the refinement is virtually complete, and only then should the above recommended values be used. Most Disagreeable Reflections (* if suppressed or used for Rfree) h k l Fo^2 Fc^2 Delta(F^2)/esd Fc/Fc(max) Resolution(A) 5 1 6 1850.99 1271.75 4.52 0.150 1.10 -5 1 1 1213.83 878.18 4.09 0.125 1.98 5 4 7 4125.21 3082.02 3.93 0.234 1.00 5 3 7 2723.86 2020.34 3.76 0.189 1.00 -2 13 2 88.62 18.14 3.74 0.018 1.98 6 2 5 4994.85 3836.05 3.53 0.261 1.10 2 1 2 1047.18 1405.47 3.50 0.158 3.03 6 1 6 5213.03 3778.64 3.49 0.259 1.01 5 0 8 4645.39 3368.17 3.41 0.245 0.92 -6 25 2 2486.69 1808.30 3.37 0.179 0.97 -5 1 6 338.76 485.54 3.37 0.093 1.41 -7 4 4 90.89 38.48 3.35 0.026 1.32 7 3 5 1329.36 941.80 3.34 0.129 1.00 -8 3 4 339.56 487.18 3.31 0.093 1.19 7 8 2 580.73 385.68 3.30 0.083 1.18 7 7 4 2953.78 2175.11 3.28 0.197 1.05 6 2 7 5212.56 3936.00 3.27 0.264 0.93 -1 4 2 722.76 550.96 3.24 0.099 4.04 7 11 4 3095.50 2314.37 3.23 0.203 1.01 -7 1 5 310.58 207.79 3.20 0.061 1.27 7 8 3 7083.15 5536.65 3.18 0.314 1.11 4 12 1 243.91 148.77 3.17 0.051 1.65 6 21 6 47.39 247.91 3.16 0.066 0.83 4 4 7 2789.82 2186.18 3.15 0.197 1.07 -2 2 4 62.45 28.53 3.15 0.023 2.37 4 21 2 1250.49 1614.56 3.14 0.169 1.15 8 22 2 901.88 1329.38 3.11 0.154 0.86 3 19 2 531.67 713.94 3.08 0.113 1.32 6 6 4 12750.73 10137.78 3.05 0.424 1.17 -4 30 3 747.88 450.12 3.05 0.089 0.91 -1 3 4 2535.11 2038.68 3.03 0.190 2.40 9 1 4 1438.83 1873.97 3.00 0.182 0.90 -1 17 3 237.41 345.17 2.99 0.078 1.55 -3 6 5 63.38 24.57 2.98 0.021 1.74 -2 0 4 1431.35 1799.24 2.96 0.179 2.40 7 26 3 1602.00 2147.24 2.94 0.195 0.82 5 0 6 1836.14 1396.65 2.93 0.157 1.10 -6 0 6 610.50 444.73 2.93 0.089 1.30 0 18 0 474.98 641.49 2.92 0.107 1.66 -3 7 1 399.86 546.98 2.90 0.099 2.61 -5 27 1 2538.71 1852.20 2.90 0.181 0.97 -7 25 1 1716.14 1246.37 2.88 0.149 0.91 -10 1 2 6030.66 4884.02 2.88 0.294 0.99 0 31 1 6392.21 5159.99 2.87 0.303 0.96 7 0 4 3298.71 2559.06 2.86 0.213 1.08 9 2 1 3220.89 2566.75 2.86 0.213 1.03 6 24 1 1581.86 2066.24 2.85 0.192 0.96 -6 25 3 10168.01 7934.73 2.85 0.375 0.96 -5 12 2 836.44 1062.59 2.84 0.137 1.54 -6 3 4 1724.61 1337.84 2.83 0.154 1.50 Bond lengths and angles Pd1 - Distance Angles C3 2.0025 (0.0034) N1 2.1222 (0.0027) 81.67 (0.12) O1 2.1237 (0.0023) 172.80 (0.11) 92.12 (0.10) P1 2.2489 (0.0009) 93.41 (0.10) 175.00 (0.08) 92.85 (0.07) Pd1 - C3 N1 O1 P1 - Distance Angles C40 1.8197 (0.0031) C30 1.8210 (0.0032) 107.78 (0.15) C20 1.8233 (0.0034) 100.00 (0.15) 105.93 (0.14) Pd1 2.2489 (0.0009) 117.38 (0.11) 111.62 (0.10) 113.00 (0.11) P1 - C40 C30 C20 F1 - Distance Angles C9 1.2938 (0.0046) F1 - F2 - Distance Angles C9 1.3296 (0.0046) F2 - F3 - Distance Angles C9 1.3076 (0.0039) F3 - O1 - Distance Angles C8 1.2568 (0.0038) Pd1 2.1237 (0.0023) 119.01 (0.21) O1 - C8 O2 - Distance Angles C8 1.2318 (0.0039) O2 - N1 - Distance Angles C1 1.2916 (0.0042) C10 1.4364 (0.0041) 117.69 (0.28) Pd1 2.1222 (0.0027) 111.01 (0.22) 131.22 (0.21) N1 - C1 C10 C1 - Distance Angles N1 1.2916 (0.0042) C2 1.4410 (0.0048) 118.88 (0.30) H1 0.9500 120.56 120.56 C1 - N1 C2 C2 - Distance Angles C7 1.3934 (0.0048) C3 1.4122 (0.0046) 122.73 (0.32) C1 1.4410 (0.0048) 120.77 (0.31) 116.50 (0.30) C2 - C7 C3 C3 - Distance Angles C4 1.3993 (0.0047) C2 1.4122 (0.0046) 115.53 (0.30) Pd1 2.0025 (0.0034) 132.93 (0.26) 111.51 (0.24) C3 - C4 C2 C4 - Distance Angles C5 1.3920 (0.0048) C3 1.3993 (0.0047) 121.72 (0.33) H4 0.9500 119.14 119.14 C4 - C5 C3 C5 - Distance Angles C6 1.3798 (0.0053) C4 1.3920 (0.0048) 121.02 (0.35) H5 0.9500 119.49 119.49 C5 - C6 C4 C6 - Distance Angles C7 1.3795 (0.0053) C5 1.3798 (0.0053) 119.22 (0.33) H6 0.9500 120.39 120.39 C6 - C7 C5 C7 - Distance Angles C6 1.3795 (0.0053) C2 1.3934 (0.0048) 119.62 (0.33) H7 0.9500 120.19 120.19 C7 - C6 C2 C8 - Distance Angles O2 1.2318 (0.0039) O1 1.2568 (0.0038) 129.30 (0.32) C9 1.5330 (0.0048) 117.57 (0.29) 113.13 (0.29) C8 - O2 O1 C9 - Distance Angles F1 1.2938 (0.0046) F3 1.3076 (0.0039) 107.44 (0.34) F2 1.3296 (0.0046) 103.82 (0.39) 104.25 (0.32) C8 1.5330 (0.0048) 113.41 (0.31) 114.37 (0.31) 112.62 (0.29) C9 - F1 F3 F2 C10 - Distance Angles C11 1.3830 (0.0047) C15 1.3861 (0.0048) 119.98 (0.32) N1 1.4364 (0.0041) 120.24 (0.29) 119.78 (0.31) C10 - C11 C15 C11 - Distance Angles C12 1.3768 (0.0048) C10 1.3830 (0.0047) 119.47 (0.33) H11 0.9500 120.27 120.27 C11 - C12 C10 C12 - Distance Angles C11 1.3768 (0.0048) C13 1.3938 (0.0055) 120.96 (0.36) H12 0.9500 119.52 119.52 C12 - C11 C13 C13 - Distance Angles C14 1.3809 (0.0056) C12 1.3938 (0.0055) 118.85 (0.36) H13 0.9500 120.57 120.57 C13 - C14 C12 C14 - Distance Angles C15 1.3755 (0.0051) C13 1.3809 (0.0056) 120.55 (0.35) H14 0.9500 119.72 119.72 C14 - C15 C13 C15 - Distance Angles C14 1.3755 (0.0051) C10 1.3861 (0.0048) 120.18 (0.35) H15 0.9500 119.91 119.91 C15 - C14 C10 C20 - Distance Angles C21 1.3857 (0.0043) C25 1.4029 (0.0044) 118.81 (0.30) P1 1.8233 (0.0034) 124.22 (0.25) 116.97 (0.23) C20 - C21 C25 C21 - Distance Angles C20 1.3857 (0.0043) C22 1.3860 (0.0049) 119.99 (0.32) H21 0.9500 120.00 120.00 C21 - C20 C22 C22 - Distance Angles C21 1.3860 (0.0049) C23 1.3866 (0.0052) 120.61 (0.32) H22 0.9500 119.69 119.69 C22 - C21 C23 C23 - Distance Angles C24 1.3787 (0.0050) C22 1.3866 (0.0052) 119.77 (0.34) H23 0.9500 120.12 120.12 C23 - C24 C22 C24 - Distance Angles C25 1.3765 (0.0048) C23 1.3787 (0.0050) 119.96 (0.33) H24 0.9500 120.02 120.02 C24 - C25 C23 C25 - Distance Angles C24 1.3765 (0.0048) C20 1.4029 (0.0044) 120.86 (0.30) H25 0.9500 119.57 119.57 C25 - C24 C20 C30 - Distance Angles C31 1.3950 (0.0047) C35 1.3965 (0.0044) 119.26 (0.29) P1 1.8210 (0.0032) 124.26 (0.24) 116.39 (0.25) C30 - C31 C35 C31 - Distance Angles C32 1.3924 (0.0046) C30 1.3950 (0.0046) 120.02 (0.31) H31 0.9500 119.99 119.99 C31 - C32 C30 C32 - Distance Angles C33 1.3861 (0.0051) C31 1.3924 (0.0046) 120.73 (0.34) H32 0.9500 119.63 119.63 C32 - C33 C31 C33 - Distance Angles C34 1.3800 (0.0052) C32 1.3861 (0.0051) 119.37 (0.32) H33 0.9500 120.32 120.32 C33 - C34 C32 C34 - Distance Angles C33 1.3800 (0.0053) C35 1.3980 (0.0046) 120.74 (0.32) H34 0.9500 119.63 119.63 C34 - C33 C35 C35 - Distance Angles C30 1.3965 (0.0044) C34 1.3980 (0.0046) 119.86 (0.32) H35 0.9500 120.07 120.07 C35 - C30 C34 C40 - Distance Angles C45 1.3915 (0.0046) C41 1.3947 (0.0044) 119.10 (0.28) P1 1.8197 (0.0031) 119.73 (0.23) 121.02 (0.25) C40 - C45 C41 C41 - Distance Angles C42 1.3799 (0.0047) C40 1.3947 (0.0044) 120.72 (0.32) H41 0.9500 119.64 119.64 C41 - C42 C40 C42 - Distance Angles C41 1.3799 (0.0047) C43 1.3848 (0.0054) 119.53 (0.31) H42 0.9500 120.23 120.23 C42 - C41 C43 C43 - Distance Angles C44 1.3795 (0.0050) C42 1.3848 (0.0054) 120.51 (0.31) H43 0.9500 119.74 119.74 C43 - C44 C42 C44 - Distance Angles C43 1.3795 (0.0050) C45 1.3876 (0.0045) 120.03 (0.33) H44 0.9500 119.98 119.98 C44 - C43 C45 C45 - Distance Angles C44 1.3876 (0.0045) C40 1.3915 (0.0046) 120.05 (0.30) H45 0.9500 119.97 119.97 C45 - C44 C40 FMAP and GRID set by program FMAP 2 2 35 GRID -0.781 -2 -2 0.781 2 2 R1 = 0.0488 for 5317 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 1.07 at 0.8391 0.1155 0.0820 [ 1.00 A from F2 ] Deepest hole -1.30 at 0.1427 0.1590 0.3793 [ 0.78 A from PD1 ] Mean = 0.00, Rms deviation from mean = 0.10 e/A^3, Highest memory used = 3653 / 24515 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.1609 0.1155 0.0820 1.00000 0.05 1.07 1.00 F2 1.08 C9 1.16 F1 2.14 F3 Q2 1 -0.1032 0.1645 -0.0210 1.00000 0.05 0.97 1.02 F1 1.44 C9 1.73 F3 2.26 C8 Q3 1 0.3040 0.1628 0.4395 1.00000 0.05 0.81 0.94 PD1 1.75 C3 1.99 P1 2.54 H7 Q4 1 0.3221 0.1882 0.5135 1.00000 0.05 0.77 0.80 C3 1.38 PD1 1.82 C2 2.00 C4 Q5 1 0.2625 0.1658 0.5601 1.00000 0.05 0.66 1.17 C3 1.20 PD1 2.14 C4 2.16 H41 Q6 1 0.2151 0.1960 0.4582 1.00000 0.05 0.64 0.96 PD1 1.35 N1 1.65 C3 1.91 C1 Q7 1 0.1153 0.1641 0.4384 1.00000 0.05 0.63 0.93 PD1 1.75 O1 2.02 N1 2.59 C3 Q8 1 0.0975 0.1883 0.3598 1.00000 0.05 0.62 1.37 PD1 1.39 N1 1.67 O1 2.04 C10 Q9 1 0.2060 0.1335 0.4223 1.00000 0.05 0.62 0.95 PD1 1.50 P1 1.91 O1 2.46 C20 Q10 1 -0.1972 0.1502 0.0433 1.00000 0.05 0.60 0.33 F1 1.52 C9 2.10 F2 2.36 F3 Shortest distances between peaks (including symmetry equivalents) 3 4 1.04 7 8 1.05 4 5 1.07 4 6 1.09 1 10 1.13 3 9 1.29 7 9 1.32 2 10 1.32 6 8 1.34 5 6 1.35 6 7 1.35 3 5 1.36 3 6 1.37 5 7 1.65 5 9 1.65 3 7 1.87 6 9 1.90 1 2 1.95 8 9 1.98 4 9 2.08 4 7 2.13 3 8 2.14 5 8 2.34 4 8 2.37 Time profile in seconds ----------------------- 0.17: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.02: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 2.39: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.05: Set up l.s. refinement 0.00: Generate idealized H-atoms 3.06: Structure factors and derivatives 5.78: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.95: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.09: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.09: Fourier summations 0.08: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 01src322 finished at 11:46:40 Total CPU time: 12.8 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++