+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + non-dis started at 13:23:14 on 30-Mar-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2009src0268p21c in P2(1)/c CELL 0.71073 9.4839 11.0427 26.0770 90.000 95.022 90.000 ZERR 4.00 0.0001 0.0002 0.0004 0.000 0.001 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O P S PD CL UNIT 128 124 4 8 4 4 4 0 V = 2720.50 F(000) = 1292.0 Mu = 0.85 mm-1 Cell Wt = 2524.03 Rho = 1.541 MERG 2 OMIT -3.00 55.00 SHEL 7 0.77 SADI C41 C42 C42 C43 DFIX 1.55 0.005 C41 C42 ISOR 0.005 C41 C42 FMAP 2 PLAN 10 SIZE 0.03 0.18 0.23 ACTA 50.00 BOND $H WGHT 0.04930 24.32690 L.S. 4 TEMP -153.00 FVAR 0.32033 MOLE 1 C2 1 -0.236254 0.214293 0.086257 11.00000 0.02106 0.01977 = 0.02105 -0.00106 -0.00187 0.00049 AFIX 43 H2 2 -0.257149 0.221913 0.121081 11.00000 -1.20000 AFIX 0 C3 1 -0.330339 0.231730 0.049214 11.00000 0.01637 0.02843 = 0.02980 -0.00035 -0.00616 0.00381 AFIX 43 H3 2 -0.424902 0.253241 0.054600 11.00000 -1.20000 AFIX 0 C4 1 -0.283218 0.216473 -0.002006 11.00000 0.02658 0.02830 = 0.02302 0.00079 -0.01198 -0.00014 AFIX 43 H4 2 -0.352978 0.228353 -0.029978 11.00000 -1.20000 AFIX 0 C5 1 -0.143708 0.185563 -0.015407 11.00000 0.02567 0.02763 = 0.01529 -0.00015 -0.00696 -0.00402 AFIX 43 H5 2 -0.120789 0.177084 -0.049967 11.00000 -1.20000 AFIX 0 C6 1 -0.053216 0.170517 0.023493 11.00000 0.01971 0.01783 = 0.01582 0.00056 -0.00331 -0.00193 C7 1 0.096355 0.141161 0.017235 11.00000 0.01988 0.01607 = 0.01497 -0.00117 -0.00325 0.00021 C9 1 0.344937 0.096754 -0.009571 11.00000 0.01537 0.03131 = 0.02306 -0.00017 0.00032 0.00295 AFIX 43 H9 2 0.432898 0.081421 -0.023187 11.00000 -1.20000 AFIX 0 C10 1 0.318471 0.102948 0.043087 11.00000 0.01778 0.02053 = 0.02281 0.00227 -0.00639 -0.00031 AFIX 43 H10 2 0.394506 0.090346 0.068743 11.00000 -1.20000 AFIX 0 C11 1 0.174155 0.128769 0.059252 11.00000 0.01744 0.01642 = 0.01297 -0.00153 -0.00213 -0.00161 C13 1 -0.149876 0.059785 0.202349 11.00000 0.01289 0.02396 = 0.01532 0.00405 -0.00694 0.00008 C14 1 -0.244764 0.058037 0.251956 11.00000 0.02276 0.02964 = 0.02381 0.00500 -0.00049 -0.00338 AFIX 137 H14A 2 -0.316423 -0.005883 0.247299 11.00000 -1.50000 H14B 2 -0.291530 0.136580 0.254831 11.00000 -1.50000 H14C 2 -0.183062 0.042371 0.283393 11.00000 -1.50000 AFIX 66 C15 1 0.347629 0.241842 0.174930 11.00000 0.01461 0.01513 = 0.01837 -0.00325 -0.00152 -0.00101 C16 1 0.455820 0.246598 0.214441 11.00000 0.02006 0.02202 = 0.01935 -0.00230 -0.00758 0.00186 AFIX 43 H16 2 0.460479 0.187648 0.241070 11.00000 -1.20000 AFIX 65 C17 1 0.557196 0.337604 0.214992 11.00000 0.02538 0.01975 = 0.03465 -0.00628 0.00435 -0.00147 AFIX 43 H17 2 0.631139 0.340854 0.241996 11.00000 -1.20000 AFIX 65 C18 1 0.550380 0.423856 0.176031 11.00000 0.01983 0.01739 = 0.03149 -0.00415 -0.00193 -0.00286 AFIX 43 H18 2 0.619666 0.486055 0.176407 11.00000 -1.20000 AFIX 65 C19 1 0.442190 0.419103 0.136519 11.00000 0.02466 0.01974 = 0.02615 0.00251 -0.00191 -0.00247 AFIX 43 H19 2 0.437533 0.478053 0.109891 11.00000 -1.20000 AFIX 65 C20 1 0.340814 0.328097 0.135968 11.00000 0.03046 0.01358 = 0.02561 -0.00130 0.00629 -0.00030 AFIX 43 H20 2 0.266871 0.324847 0.108964 11.00000 -1.20000 AFIX 0 C21 1 0.330637 -0.022177 0.160107 11.00000 0.02048 0.01363 = 0.01479 -0.00048 -0.00524 0.00119 C22 1 0.258299 -0.127180 0.148219 11.00000 0.02086 0.01977 = 0.01797 -0.00101 -0.00731 -0.00269 AFIX 43 H22 2 0.157885 -0.128149 0.146908 11.00000 -1.20000 AFIX 0 C23 1 0.332577 -0.234137 0.137892 11.00000 0.03361 0.01925 = 0.01878 -0.00183 -0.00493 -0.00235 AFIX 43 H23 2 0.280615 -0.306416 0.130241 11.00000 -1.20000 AFIX 0 C24 1 0.478789 -0.236932 0.138571 11.00000 0.03052 0.01937 = 0.01934 -0.00099 -0.00378 0.00676 AFIX 43 H24 2 0.526872 -0.309767 0.131592 11.00000 -1.20000 AFIX 0 C25 1 0.551682 -0.132671 0.149490 11.00000 0.01992 0.02427 = 0.02117 0.00020 -0.00307 0.00394 AFIX 43 H25 2 0.651939 -0.131864 0.149894 11.00000 -1.20000 AFIX 0 C26 1 0.478225 -0.025519 0.160237 11.00000 0.02099 0.01657 = 0.01539 0.00084 -0.00350 -0.00066 AFIX 43 H26 2 0.530698 0.046542 0.167789 11.00000 -1.20000 AFIX 66 C27 1 0.158059 0.091323 0.247073 11.00000 0.01474 0.01878 = 0.02040 0.00015 -0.00892 0.00150 C28 1 0.141730 0.192628 0.277632 11.00000 0.02021 0.01631 = 0.02301 0.00090 -0.00455 -0.00070 AFIX 43 H28 2 0.164691 0.270720 0.265541 11.00000 -1.20000 AFIX 65 C29 1 0.091807 0.179673 0.325883 11.00000 0.02586 0.02496 = 0.02335 -0.00550 -0.00298 0.00359 AFIX 43 H29 2 0.080647 0.248911 0.346768 11.00000 -1.20000 AFIX 65 C30 1 0.058212 0.065413 0.343574 11.00000 0.02948 0.03202 = 0.02305 0.00275 -0.00131 0.00318 AFIX 43 H30 2 0.024092 0.056559 0.376552 11.00000 -1.20000 AFIX 65 C31 1 0.074540 -0.035894 0.313016 11.00000 0.02472 0.01990 = 0.02900 0.00901 -0.00420 0.00010 AFIX 43 H31 2 0.051580 -0.113985 0.325107 11.00000 -1.20000 AFIX 65 C32 1 0.124464 -0.022940 0.264765 11.00000 0.01365 0.01755 = 0.02558 -0.00097 -0.00751 0.00229 AFIX 43 H32 2 0.135623 -0.092179 0.243879 11.00000 -1.20000 AFIX 0 N1 3 -0.101423 0.183582 0.073595 11.00000 0.01472 0.01685 = 0.01799 -0.00147 -0.00622 -0.00126 O12A 4 -0.098538 0.163654 0.188742 11.00000 0.01889 0.01875 = 0.01536 0.00183 -0.00383 -0.00115 O12B 4 -0.123317 -0.035480 0.178308 11.00000 0.03548 0.01789 = 0.03122 -0.00166 -0.00259 -0.00532 P1 5 0.225187 0.113283 0.176327 11.00000 0.01447 0.01307 = 0.01352 0.00049 -0.00467 -0.00047 S8 6 0.195810 0.120972 -0.041055 11.00000 0.02054 0.03167 = 0.01449 0.00005 -0.00189 0.00140 PD1 7 0.051196 0.145522 0.125250 11.00000 0.01302 0.01311 = 0.01281 -0.00052 -0.00370 0.00001 MOLE 2 C41 1 0.314846 0.441123 -0.004489 11.00000 0.14642 0.12137 = 0.13647 0.00341 0.01061 -0.00132 AFIX 137 H41A 2 0.290904 0.453125 -0.041463 11.00000 -1.50000 H41B 2 0.343403 0.356805 0.001931 11.00000 -1.50000 H41C 2 0.392997 0.495068 0.007424 11.00000 -1.50000 AFIX 0 C42 1 0.183006 0.470387 0.025203 11.00000 0.06240 0.04675 = 0.09425 0.01577 -0.00796 -0.00030 AFIX 23 H42A 2 0.165112 0.403718 0.049173 11.00000 -1.20000 H42B 2 0.198581 0.546007 0.045296 11.00000 -1.20000 AFIX 0 C43 1 0.065504 0.483993 -0.012737 11.00000 0.06546 0.02161 = 0.04129 0.00071 -0.00614 -0.00458 AFIX 23 H43A 2 0.050005 0.407467 -0.032194 11.00000 -1.20000 H43B 2 0.086264 0.548540 -0.037327 11.00000 -1.20000 AFIX 0 HKLF 4 Covalent radii and connectivity table for 2009src0268p21c in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 P 1.100 S 1.030 PD 1.380 CL 0.990 C2 - C3 N1 C3 - C2 C4 C4 - C5 C3 C5 - C6 C4 C6 - C5 N1 C7 C7 - C11 C6 S8 C9 - C10 S8 C10 - C9 C11 C11 - C7 C10 Pd1 C13 - O12B O12A C14 C14 - C13 C15 - C16 C20 P1 C16 - C15 C17 C17 - C18 C16 C18 - C19 C17 C19 - C18 C20 C20 - C19 C15 C21 - C22 C26 P1 C22 - C21 C23 C23 - C24 C22 C24 - C25 C23 C25 - C24 C26 C26 - C21 C25 C27 - C28 C32 P1 C28 - C29 C27 C29 - C28 C30 C30 - C31 C29 C31 - C30 C32 C32 - C31 C27 N1 - C2 C6 Pd1 O12A - C13 Pd1 O12B - C13 P1 - C15 C21 C27 Pd1 S8 - C9 C7 Pd1 - N1 P1 C11 O12A C41 - C42 C42 - C43 C41 C43 - C42 C43_$1 Operators for generating equivalent atoms: $1 -x, -y+1, -z 58067 Reflections read, of which 3667 rejected -12 =< h =< 12, -14 =< k =< 14, -33 =< l =< 33, Max. 2-theta = 54.95 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Su of mean(Fo^2) 4 11 1 155.70 9.85 6 53.58 4 11 2 35.20 6.80 4 36.50 9 5 8 53.77 6.38 5 42.88 5 3 14 47.99 1.26 12 6.46 4 Inconsistent equivalents 5891 Unique reflections, of which 0 suppressed R(int) = 0.0688 R(sigma) = 0.0418 Friedel opposites merged Maximum memory for data reduction = 3456 / 59567 Default effective X-H distances for T = -153.0 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 = 4419 / 407468 wR2 = 0.1427 before cycle 1 for 5891 data and 321 / 321 parameters Disagreeable restraints before cycle 1 Observed Target Error Sigma Restraint 0.1292 0.0200 SAME/SADI C41 C42 C42 C43 0.0219 0.0050 ISOR U22 C42 -0.0256 0.0050 ISOR U33 C42 -0.0158 0.0050 ISOR U23 C42 Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 1. 0. 0. 0. 0. 0. 12. 0. rms sigma 0.000 0.005 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.005 0.000 rms deviation 0.000 0.011 0.000 0.129 0.000 0.000 0.000 0.000 0.000 0.013 0.000 GooF = S = 1.041; Restrained GooF = 1.051 for 14 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0493 * P )^2 + 24.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.32031 0.00063 -0.037 OSF Mean shift/su = 0.007 Maximum = 0.056 for U22 C41 Max. shift = 0.001 A for H41C Max. dU = 0.000 for C41 Least-squares cycle 2 Maximum vector length = 511 Memory required = 4419 / 407468 wR2 = 0.1427 before cycle 2 for 5891 data and 321 / 321 parameters Disagreeable restraints before cycle 2 Observed Target Error Sigma Restraint 0.1292 0.0200 SAME/SADI C41 C42 C42 C43 0.0219 0.0050 ISOR U22 C42 -0.0256 0.0050 ISOR U33 C42 -0.0158 0.0050 ISOR U23 C42 Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 1. 0. 0. 0. 0. 0. 12. 0. rms sigma 0.000 0.005 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.005 0.000 rms deviation 0.000 0.011 0.000 0.129 0.000 0.000 0.000 0.000 0.000 0.013 0.000 GooF = S = 1.041; Restrained GooF = 1.051 for 14 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0493 * P )^2 + 24.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.32030 0.00063 -0.006 OSF Mean shift/su = 0.003 Maximum = 0.047 for U22 C41 Max. shift = 0.001 A for H41B Max. dU = 0.000 for C41 Least-squares cycle 3 Maximum vector length = 511 Memory required = 4419 / 407468 wR2 = 0.1427 before cycle 3 for 5891 data and 321 / 321 parameters Disagreeable restraints before cycle 3 Observed Target Error Sigma Restraint 0.1292 0.0200 SAME/SADI C41 C42 C42 C43 0.0219 0.0050 ISOR U22 C42 -0.0256 0.0050 ISOR U33 C42 -0.0159 0.0050 ISOR U23 C42 Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 1. 0. 0. 0. 0. 0. 12. 0. rms sigma 0.000 0.005 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.005 0.000 rms deviation 0.000 0.011 0.000 0.129 0.000 0.000 0.000 0.000 0.000 0.013 0.000 GooF = S = 1.041; Restrained GooF = 1.051 for 14 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0493 * P )^2 + 24.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.32030 0.00063 0.001 OSF Mean shift/su = 0.001 Maximum = 0.023 for U22 C41 Max. shift = 0.001 A for H41B Max. dU = 0.000 for C41 Least-squares cycle 4 Maximum vector length = 511 Memory required = 4419 / 407468 wR2 = 0.1427 before cycle 4 for 5891 data and 321 / 321 parameters Disagreeable restraints before cycle 4 Observed Target Error Sigma Restraint 0.1292 0.0200 SAME/SADI C41 C42 C42 C43 0.0219 0.0050 ISOR U22 C42 -0.0257 0.0050 ISOR U33 C42 -0.0159 0.0050 ISOR U23 C42 Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 1. 0. 0. 0. 0. 0. 12. 0. rms sigma 0.000 0.005 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.005 0.000 rms deviation 0.000 0.011 0.000 0.129 0.000 0.000 0.000 0.000 0.000 0.013 0.000 GooF = S = 1.041; Restrained GooF = 1.051 for 14 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0493 * P )^2 + 24.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.32030 0.00063 0.002 OSF Mean shift/su = 0.000 Maximum = 0.012 for U22 C41 Max. shift = 0.000 A for H41B Max. dU = 0.000 for C41 Largest correlation matrix elements -0.748 x C27 / rotY C27 0.592 y C27 / rotX C27 0.523 U22 Pd1 / OSF 0.641 x C15 / rotZ C15 0.545 U11 Pd1 / OSF -0.640 y C15 / rotZ C15 0.543 U33 Pd1 / OSF Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 -0.2572 0.2219 0.1211 43 0.950 0.000 C2 C3 N1 H3 -0.4249 0.2533 0.0546 43 0.950 0.000 C3 C2 C4 H4 -0.3530 0.2284 -0.0300 43 0.950 0.000 C4 C5 C3 H5 -0.1208 0.1771 -0.0500 43 0.950 0.000 C5 C6 C4 H9 0.4329 0.0814 -0.0232 43 0.950 0.000 C9 C10 S8 H10 0.3945 0.0904 0.0687 43 0.950 0.000 C10 C9 C11 H14A -0.3165 -0.0058 0.2473 137 0.980 0.000 C14 C13 H14A H14B -0.2914 0.1366 0.2549 137 0.980 0.000 C14 C13 H14A H14C -0.1831 0.0422 0.2834 137 0.980 0.000 C14 C13 H14A H16 0.4605 0.1876 0.2411 43 0.950 0.000 C16 C15 C17 H17 0.6311 0.3409 0.2420 43 0.950 0.000 C17 C18 C16 H18 0.6197 0.4861 0.1764 43 0.950 0.000 C18 C19 C17 H19 0.4375 0.4781 0.1099 43 0.950 0.000 C19 C18 C20 H20 0.2669 0.3248 0.1090 43 0.950 0.000 C20 C19 C15 H22 0.1579 -0.1282 0.1469 43 0.950 0.000 C22 C21 C23 H23 0.2806 -0.3064 0.1302 43 0.950 0.000 C23 C24 C22 H24 0.5269 -0.3098 0.1316 43 0.950 0.000 C24 C25 C23 H25 0.6519 -0.1319 0.1499 43 0.950 0.000 C25 C24 C26 H26 0.5307 0.0465 0.1678 43 0.950 0.000 C26 C21 C25 H28 0.1647 0.2707 0.2655 43 0.950 0.000 C28 C29 C27 H29 0.0806 0.2489 0.3468 43 0.950 0.000 C29 C28 C30 H30 0.0241 0.0566 0.3766 43 0.950 0.000 C30 C31 C29 H31 0.0516 -0.1140 0.3251 43 0.950 0.000 C31 C30 C32 H32 0.1356 -0.0922 0.2439 43 0.950 0.000 C32 C31 C27 H41A 0.2907 0.4532 -0.0415 137 0.980 0.000 C41 C42 H41A H41B 0.3433 0.3568 0.0019 137 0.980 0.000 C41 C42 H41A H41C 0.3929 0.4951 0.0074 137 0.980 0.000 C41 C42 H41A H42A 0.1650 0.4037 0.0492 23 0.990 0.000 C42 C43 C41 H42B 0.1985 0.5460 0.0453 23 0.990 0.000 C42 C43 C41 H43A 0.0500 0.4075 -0.0322 23 0.990 0.000 C43 C42 C43_$1 H43B 0.0863 0.5485 -0.0373 23 0.990 0.000 C43 C42 C43_$1 2009src0268p21c in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C2 -0.23626 0.21429 0.08626 1.00000 0.02106 0.01973 0.02108 -0.00107 -0.00188 0.00047 0.02084 0.00882 0.00054 0.00046 0.00020 0.00000 0.00248 0.00250 0.00249 0.00198 0.00201 0.00200 0.00104 H2 -0.25716 0.22189 0.12108 1.00000 0.02501 0.00000 0.00000 C3 -0.33033 0.23173 0.04921 1.00000 0.01634 0.02842 0.02976 -0.00034 -0.00617 0.00383 0.02532 0.00940 0.00056 0.00051 0.00021 0.00000 0.00243 0.00283 0.00285 0.00228 0.00213 0.00210 0.00116 H3 -0.42489 0.25325 0.05460 1.00000 0.03039 0.00000 0.00000 C4 -0.28322 0.21648 -0.00201 1.00000 0.02657 0.02831 0.02302 0.00080 -0.01201 -0.00013 0.02680 0.00928 0.00059 0.00052 0.00021 0.00000 0.00276 0.00288 0.00265 0.00220 0.00219 0.00227 0.00120 H4 -0.35299 0.22836 -0.02998 1.00000 0.03216 0.00000 0.00000 C5 -0.14370 0.18556 -0.01541 1.00000 0.02567 0.02759 0.01530 -0.00012 -0.00700 -0.00402 0.02337 0.00882 0.00057 0.00050 0.00020 0.00000 0.00267 0.00272 0.00236 0.00203 0.00203 0.00218 0.00111 H5 -0.12078 0.17708 -0.04997 1.00000 0.02804 0.00000 0.00000 C6 -0.05321 0.17052 0.02349 1.00000 0.01970 0.01781 0.01581 0.00054 -0.00331 -0.00192 0.01806 0.00837 0.00053 0.00044 0.00019 0.00000 0.00238 0.00238 0.00228 0.00183 0.00187 0.00189 0.00099 C7 0.09636 0.14116 0.01723 1.00000 0.01983 0.01610 0.01498 -0.00118 -0.00327 0.00020 0.01725 0.00827 0.00052 0.00044 0.00018 0.00000 0.00235 0.00225 0.00220 0.00182 0.00185 0.00189 0.00096 C9 0.34494 0.09676 -0.00957 1.00000 0.01536 0.03127 0.02302 -0.00017 0.00031 0.00295 0.02330 0.00937 0.00054 0.00052 0.00020 0.00000 0.00237 0.00288 0.00259 0.00220 0.00200 0.00210 0.00110 H9 0.43290 0.08142 -0.02319 1.00000 0.02796 0.00000 0.00000 C10 0.31848 0.10295 0.04309 1.00000 0.01780 0.02053 0.02273 0.00233 -0.00639 -0.00028 0.02083 0.00878 0.00053 0.00047 0.00020 0.00000 0.00237 0.00244 0.00251 0.00201 0.00199 0.00196 0.00105 H10 0.39451 0.09036 0.06874 1.00000 0.02500 0.00000 0.00000 C11 0.17415 0.12877 0.05926 1.00000 0.01745 0.01644 0.01293 -0.00153 -0.00215 -0.00161 0.01581 0.00801 0.00050 0.00043 0.00018 0.00000 0.00226 0.00231 0.00213 0.00174 0.00179 0.00182 0.00094 C13 -0.14988 0.05979 0.20235 1.00000 0.01288 0.02394 0.01531 0.00406 -0.00694 0.00007 0.01786 0.00836 0.00049 0.00047 0.00018 0.00000 0.00214 0.00249 0.00223 0.00193 0.00178 0.00191 0.00099 C14 -0.24476 0.05804 0.25196 1.00000 0.02275 0.02963 0.02381 0.00501 -0.00053 -0.00338 0.02555 0.00978 0.00057 0.00053 0.00021 0.00000 0.00260 0.00287 0.00267 0.00223 0.00214 0.00225 0.00115 H14A -0.31652 -0.00579 0.24728 1.00000 0.03833 0.00000 0.00000 H14B -0.29140 0.13663 0.25487 1.00000 0.03833 0.00000 0.00000 H14C -0.18308 0.04224 0.28339 1.00000 0.03833 0.00000 0.00000 C15 0.34762 0.24184 0.17493 1.00000 0.01459 0.01512 0.01838 -0.00327 -0.00152 -0.00102 0.01621 0.00441 0.00030 0.00025 0.00012 0.00000 0.00221 0.00224 0.00232 0.00183 0.00185 0.00178 0.00095 C16 0.45582 0.24660 0.21444 1.00000 0.02006 0.02201 0.01935 -0.00230 -0.00760 0.00187 0.02102 0.00530 0.00034 0.00026 0.00011 0.00000 0.00246 0.00253 0.00242 0.00199 0.00199 0.00200 0.00106 H16 0.46048 0.18765 0.24107 1.00000 0.02523 0.00000 0.00000 C17 0.55719 0.33760 0.21499 1.00000 0.02536 0.01972 0.03467 -0.00634 0.00436 -0.00153 0.02648 0.00430 0.00031 0.00030 0.00011 0.00000 0.00273 0.00265 0.00304 0.00223 0.00231 0.00213 0.00117 H17 0.63114 0.34085 0.24199 1.00000 0.03178 0.00000 0.00000 C18 0.55037 0.42385 0.17603 1.00000 0.01975 0.01742 0.03153 -0.00421 -0.00194 -0.00287 0.02314 0.00467 0.00031 0.00026 0.00013 0.00000 0.00246 0.00246 0.00281 0.00210 0.00214 0.00198 0.00110 H18 0.61966 0.48605 0.17641 1.00000 0.02777 0.00000 0.00000 C19 0.44218 0.41910 0.13652 1.00000 0.02473 0.01974 0.02610 0.00252 -0.00190 -0.00243 0.02377 0.00561 0.00036 0.00027 0.00011 0.00000 0.00264 0.00259 0.00266 0.00210 0.00215 0.00209 0.00111 H19 0.43752 0.47805 0.10989 1.00000 0.02852 0.00000 0.00000 C20 0.34080 0.32810 0.13597 1.00000 0.03045 0.01358 0.02561 -0.00126 0.00632 -0.00026 0.02299 0.00441 0.00031 0.00029 0.00011 0.00000 0.00282 0.00237 0.00268 0.00196 0.00222 0.00203 0.00110 H20 0.26686 0.32485 0.10897 1.00000 0.02758 0.00000 0.00000 C21 0.33065 -0.02218 0.16010 1.00000 0.02050 0.01360 0.01476 -0.00049 -0.00527 0.00120 0.01669 0.00818 0.00052 0.00043 0.00018 0.00000 0.00236 0.00219 0.00222 0.00176 0.00185 0.00184 0.00097 C22 0.25830 -0.12718 0.14822 1.00000 0.02082 0.01978 0.01797 -0.00103 -0.00731 -0.00271 0.02005 0.00834 0.00055 0.00046 0.00019 0.00000 0.00242 0.00250 0.00234 0.00190 0.00193 0.00197 0.00104 H22 0.15789 -0.12815 0.14692 1.00000 0.02406 0.00000 0.00000 C23 0.33258 -0.23414 0.13789 1.00000 0.03358 0.01923 0.01876 -0.00183 -0.00493 -0.00234 0.02428 0.00918 0.00060 0.00049 0.00020 0.00000 0.00297 0.00252 0.00246 0.00198 0.00217 0.00219 0.00114 H23 0.28061 -0.30642 0.13024 1.00000 0.02914 0.00000 0.00000 C24 0.47879 -0.23693 0.13857 1.00000 0.03054 0.01934 0.01933 -0.00099 -0.00377 0.00677 0.02342 0.00940 0.00059 0.00048 0.00020 0.00000 0.00286 0.00251 0.00245 0.00199 0.00213 0.00215 0.00112 H24 0.52688 -0.30977 0.13159 1.00000 0.02810 0.00000 0.00000 C25 0.55168 -0.13267 0.14949 1.00000 0.01990 0.02426 0.02114 0.00018 -0.00309 0.00391 0.02205 0.00918 0.00056 0.00048 0.00020 0.00000 0.00244 0.00266 0.00251 0.00205 0.00198 0.00207 0.00107 H25 0.65193 -0.13186 0.14990 1.00000 0.02647 0.00000 0.00000 C26 0.47823 -0.02552 0.16024 1.00000 0.02098 0.01658 0.01539 0.00084 -0.00351 -0.00068 0.01795 0.00849 0.00052 0.00045 0.00018 0.00000 0.00241 0.00232 0.00227 0.00181 0.00189 0.00190 0.00099 H26 0.53070 0.04653 0.16779 1.00000 0.02154 0.00000 0.00000 C27 0.15806 0.09132 0.24707 1.00000 0.01471 0.01880 0.02039 0.00014 -0.00892 0.00151 0.01858 0.00538 0.00033 0.00027 0.00009 0.00000 0.00223 0.00240 0.00237 0.00192 0.00187 0.00184 0.00101 C28 0.14174 0.19263 0.27763 1.00000 0.02024 0.01630 0.02297 0.00092 -0.00456 -0.00071 0.02022 0.00527 0.00036 0.00021 0.00012 0.00000 0.00243 0.00234 0.00252 0.00196 0.00199 0.00193 0.00103 H28 0.16470 0.27072 0.26554 1.00000 0.02426 0.00000 0.00000 C29 0.09181 0.17967 0.32588 1.00000 0.02587 0.02493 0.02331 -0.00552 -0.00299 0.00360 0.02500 0.00533 0.00038 0.00025 0.00011 0.00000 0.00271 0.00271 0.00266 0.00213 0.00216 0.00218 0.00115 H29 0.08065 0.24891 0.34677 1.00000 0.03000 0.00000 0.00000 C30 0.05821 0.06541 0.34357 1.00000 0.02940 0.03207 0.02300 0.00274 -0.00130 0.00318 0.02837 0.00621 0.00038 0.00031 0.00010 0.00000 0.00289 0.00304 0.00270 0.00231 0.00225 0.00242 0.00121 H30 0.02409 0.05656 0.37655 1.00000 0.03404 0.00000 0.00000 C31 0.07453 -0.03589 0.31302 1.00000 0.02469 0.01989 0.02892 0.00898 -0.00417 0.00010 0.02488 0.00574 0.00037 0.00023 0.00012 0.00000 0.00266 0.00258 0.00282 0.00215 0.00221 0.00209 0.00115 H31 0.05157 -0.11398 0.32511 1.00000 0.02986 0.00000 0.00000 C32 0.12446 -0.02294 0.26477 1.00000 0.01364 0.01756 0.02552 -0.00098 -0.00751 0.00229 0.01945 0.00489 0.00035 0.00022 0.00011 0.00000 0.00222 0.00235 0.00258 0.00198 0.00195 0.00183 0.00103 H32 0.13562 -0.09218 0.24388 1.00000 0.02334 0.00000 0.00000 N1 -0.10142 0.18359 0.07360 1.00000 0.01473 0.01681 0.01798 -0.00146 -0.00621 -0.00125 0.01696 0.00679 0.00042 0.00037 0.00016 0.00000 0.00191 0.00195 0.00199 0.00159 0.00158 0.00157 0.00084 O12A -0.09854 0.16366 0.18874 1.00000 0.01890 0.01873 0.01533 0.00182 -0.00386 -0.00113 0.01797 0.00580 0.00036 0.00031 0.00013 0.00000 0.00169 0.00174 0.00163 0.00134 0.00133 0.00137 0.00071 O12B -0.12331 -0.03548 0.17831 1.00000 0.03548 0.01788 0.03122 -0.00166 -0.00262 -0.00530 0.02852 0.00665 0.00043 0.00034 0.00015 0.00000 0.00221 0.00187 0.00210 0.00157 0.00173 0.00162 0.00088 P1 0.22519 0.11328 0.17633 1.00000 0.01446 0.01307 0.01352 0.00049 -0.00467 -0.00047 0.01403 0.00204 0.00013 0.00011 0.00005 0.00000 0.00055 0.00056 0.00055 0.00043 0.00044 0.00044 0.00025 S8 0.19581 0.12097 -0.04106 1.00000 0.02054 0.03167 0.01449 0.00005 -0.00189 0.00140 0.02243 0.00228 0.00014 0.00013 0.00005 0.00000 0.00060 0.00072 0.00056 0.00049 0.00047 0.00052 0.00028 Pd1 0.05120 0.14552 0.12525 1.00000 0.01302 0.01311 0.01280 -0.00052 -0.00370 0.00001 0.01326 0.00059 0.00004 0.00003 0.00001 0.00000 0.00018 0.00018 0.00018 0.00013 0.00013 0.00013 0.00012 C41 0.31469 0.44118 -0.00450 1.00000 0.14721 0.12231 0.13727 0.00340 0.01075 -0.00142 0.13570 0.02990 0.00138 0.00150 0.00058 0.00000 0.00699 0.00682 0.00690 0.00467 0.00473 0.00471 0.00562 H41A 0.29067 0.45323 -0.04147 1.00000 0.20355 0.00000 0.00000 H41B 0.34325 0.35685 0.00189 1.00000 0.20355 0.00000 0.00000 H41C 0.39287 0.49510 0.00740 1.00000 0.20355 0.00000 0.00000 C42 0.18293 0.47040 0.02524 1.00000 0.06230 0.04673 0.09432 0.01587 -0.00795 -0.00026 0.06865 0.01670 0.00090 0.00083 0.00039 0.00000 0.00395 0.00364 0.00456 0.00349 0.00358 0.00323 0.00242 H42A 0.16505 0.40371 0.04920 1.00000 0.08238 0.00000 0.00000 H42B 0.19850 0.54602 0.04534 1.00000 0.08238 0.00000 0.00000 C43 0.06551 0.48399 -0.01273 1.00000 0.06549 0.02156 0.04128 0.00069 -0.00617 -0.00457 0.04342 0.01172 0.00077 0.00059 0.00026 0.00000 0.00473 0.00303 0.00375 0.00267 0.00329 0.00305 0.00167 H43A 0.05003 0.40746 -0.03219 1.00000 0.05210 0.00000 0.00000 H43B 0.08630 0.54853 -0.03732 1.00000 0.05210 0.00000 0.00000 Final Structure Factor Calculation for 2009src0268p21c in P2(1)/c Total number of l.s. parameters = 321 Maximum vector length = 511 Memory required = 4098 / 27083 wR2 = 0.1427 before cycle 5 for 5891 data and 0 / 321 parameters Disagreeable restraints before cycle 5 Observed Target Error Sigma Restraint 0.1292 0.0200 SAME/SADI C41 C42 C42 C43 0.0219 0.0050 ISOR U22 C42 -0.0257 0.0050 ISOR U33 C42 -0.0159 0.0050 ISOR U23 C42 Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 1. 0. 0. 0. 0. 0. 12. 0. rms sigma 0.000 0.005 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.005 0.000 rms deviation 0.000 0.011 0.000 0.129 0.000 0.000 0.000 0.000 0.000 0.013 0.000 GooF = S = 1.041; Restrained GooF = 1.051 for 14 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0493 * P )^2 + 24.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0585 for 5109 Fo > 4sig(Fo) and 0.0681 for all 5891 data wR2 = 0.1427, GooF = S = 1.041, Restrained GooF = 1.051 for all data Occupancy sum of asymmetric unit = 38.00 for non-hydrogen and 31.00 for hydrogen atoms Principal mean square atomic displacements U 0.0254 0.0196 0.0176 C2 0.0351 0.0284 0.0124 C3 0.0405 0.0283 0.0116 C4 0.0336 0.0257 0.0107 C5 0.0241 0.0173 0.0128 C6 0.0233 0.0162 0.0122 C7 0.0318 0.0233 0.0147 C9 0.0301 0.0202 0.0122 C10 0.0198 0.0170 0.0106 C11 0.0269 0.0206 0.0061 C13 0.0344 0.0215 0.0207 C14 0.0213 0.0159 0.0114 C15 0.0310 0.0210 0.0111 C16 0.0372 0.0249 0.0174 C17 0.0339 0.0216 0.0139 C18 0.0312 0.0216 0.0186 C19 0.0323 0.0232 0.0134 C20 0.0258 0.0135 0.0108 C21 0.0296 0.0202 0.0104 C22 0.0373 0.0206 0.0150 C23 0.0364 0.0184 0.0155 C24 0.0281 0.0231 0.0150 C25 0.0246 0.0165 0.0127 C26 0.0295 0.0189 0.0074 C27 0.0289 0.0162 0.0155 C28 0.0348 0.0219 0.0183 C29 0.0342 0.0304 0.0205 C30 0.0377 0.0234 0.0135 C31 0.0317 0.0175 0.0091 C32 0.0249 0.0172 0.0088 N1 0.0241 0.0180 0.0118 O12A 0.0404 0.0292 0.0159 O12B 0.0205 0.0130 0.0085 P1 0.0319 0.0222 0.0132 S8 0.0182 0.0131 0.0084 Pd1 0.1479 0.1377 0.1215 C41 0.1055 0.0591 0.0414 C42 0.0711 0.0380 0.0211 C43 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.019 0.040 0.060 0.079 0.101 0.126 0.156 0.193 0.251 1.000 Number in group 597. 604. 592. 575. 592. 578. 600. 585. 575. 593. GooF 1.109 0.951 1.105 1.028 1.042 1.035 1.041 1.034 1.067 0.990 K 3.437 1.241 1.077 1.007 1.013 1.004 1.008 1.012 1.016 0.998 Resolution(A) 0.77 0.81 0.85 0.88 0.93 0.99 1.07 1.17 1.34 1.68 inf Number in group 603. 592. 573. 608. 569. 602. 575. 595. 580. 594. GooF 0.939 0.934 0.948 0.952 0.976 0.993 0.931 1.045 1.163 1.424 K 0.976 0.999 1.028 1.029 1.029 1.019 1.007 1.014 1.002 0.998 R1 0.107 0.099 0.084 0.078 0.073 0.067 0.059 0.056 0.051 0.050 Recommended weighting scheme: WGHT 0.0491 24.3713 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)/su Fc/Fc(max) Resolution(A) -2 1 7 5205.46 3331.20 4.85 0.193 2.94 1 0 4 795.25 272.75 4.68 0.055 5.15 3 0 0 2074.51 1104.79 4.63 0.111 3.15 2 4 11 1249.21 572.58 4.51 0.080 1.64 -3 3 2 704.24 242.71 4.43 0.052 2.38 -2 0 6 4321.09 6491.56 4.40 0.269 3.34 -2 2 6 1955.60 1139.28 4.00 0.113 2.86 1 0 12 3363.43 4986.92 3.99 0.236 2.07 5 1 7 2703.19 1704.63 3.96 0.138 1.61 0 2 10 1009.93 482.97 3.91 0.073 2.35 -1 2 12 1341.80 709.38 3.89 0.089 2.00 2 0 26 4454.43 2922.05 3.64 0.181 0.96 4 4 5 5063.96 3668.94 3.55 0.202 1.66 -1 2 15 204.32 28.91 3.53 0.018 1.65 7 0 22 326.62 848.10 3.41 0.097 0.85 1 1 4 649.01 294.90 3.38 0.057 4.66 2 6 14 823.82 406.12 3.36 0.067 1.24 1 2 16 120.57 3.72 3.31 0.006 1.52 5 0 8 347.95 107.95 3.30 0.035 1.57 2 4 17 1736.22 2621.37 3.27 0.171 1.26 2 1 2 4897.18 3635.50 3.26 0.201 4.02 0 2 5 876.02 1501.14 3.26 0.129 3.78 3 4 2 2563.33 3646.36 3.25 0.202 2.03 0 0 10 13985.39 11058.54 3.23 0.351 2.60 1 2 4 144.87 12.99 3.22 0.012 3.76 9 0 20 2841.11 1669.20 3.22 0.136 0.78 1 3 6 4197.15 3072.70 3.21 0.185 2.65 5 6 16 639.29 285.45 3.21 0.056 0.99 -2 4 5 952.87 519.18 3.21 0.076 2.20 2 2 12 3903.95 2857.39 3.17 0.179 1.80 2 1 28 362.40 73.74 3.13 0.029 0.89 4 2 22 65.10 319.46 3.07 0.060 1.00 4 5 6 998.21 1619.76 3.07 0.134 1.48 3 2 0 4782.81 3609.49 3.06 0.201 2.74 6 4 15 665.58 1190.29 3.04 0.115 1.04 7 7 12 316.68 81.49 3.04 0.030 0.90 -3 4 3 510.57 964.81 3.04 0.104 2.05 -3 0 30 2792.53 1830.82 3.04 0.143 0.85 5 6 18 2889.12 2033.14 3.04 0.151 0.95 -4 2 29 2235.94 1458.11 3.03 0.128 0.85 3 4 11 179.98 484.03 3.03 0.073 1.52 -2 6 14 6789.66 5249.03 3.01 0.242 1.28 -1 0 22 444.17 907.24 2.98 0.101 1.18 2 3 17 123.71 12.94 2.97 0.012 1.32 -3 3 10 4788.34 6223.19 2.97 0.263 1.82 -3 4 9 2241.83 1546.07 2.96 0.131 1.73 -3 4 15 2550.56 1759.63 2.95 0.140 1.37 3 6 4 5032.62 3844.59 2.95 0.207 1.53 -5 0 2 13248.93 16284.05 2.94 0.426 1.89 2 0 0 2304.18 1601.22 2.92 0.134 4.72 Bond lengths and angles C2 - Distance Angles C3 1.2710 (0.0069) N1 1.3903 (0.0067) 117.10 (0.51) H2 0.9500 121.45 121.45 C2 - C3 N1 C3 - Distance Angles C2 1.2710 (0.0069) C4 1.4547 (0.0081) 115.39 (0.51) H3 0.9500 122.31 122.31 C3 - C2 C4 C4 - Distance Angles C5 1.4390 (0.0081) C3 1.4547 (0.0081) 127.83 (0.45) H4 0.9500 116.09 116.09 C4 - C5 C3 C5 - Distance Angles C6 1.2809 (0.0066) C4 1.4390 (0.0081) 113.89 (0.50) H5 0.9500 123.05 123.05 C5 - C6 C4 C6 - Distance Angles C5 1.2809 (0.0066) N1 1.4289 (0.0066) 117.73 (0.49) C7 1.4780 (0.0070) 121.60 (0.49) 120.67 (0.40) C6 - C5 N1 C7 - Distance Angles C11 1.2737 (0.0065) C6 1.4780 (0.0070) 114.70 (0.46) S8 1.8710 (0.0052) 113.01 (0.40) 132.28 (0.35) C7 - C11 C6 C9 - Distance Angles C10 1.4190 (0.0075) S8 1.5945 (0.0050) 105.43 (0.38) H9 0.9500 127.28 127.28 C9 - C10 S8 C10 - Distance Angles C9 1.4190 (0.0075) C11 1.4945 (0.0070) 121.75 (0.42) H10 0.9500 119.13 119.13 C10 - C9 C11 C11 - Distance Angles C7 1.2737 (0.0065) C10 1.4945 (0.0070) 104.69 (0.44) Pd1 2.1696 (0.0049) 111.23 (0.38) 144.02 (0.34) C11 - C7 C10 C13 - Distance Angles O12B 1.2613 (0.0064) O12A 1.3073 (0.0060) 120.10 (0.46) C14 1.6393 (0.0073) 121.99 (0.45) 117.89 (0.44) C13 - O12B O12A C14 - Distance Angles C13 1.6393 (0.0073) H14A 0.9800 109.47 H14B 0.9800 109.47 109.47 H14C 0.9800 109.47 109.47 109.47 C14 - C13 H14A H14B C15 - Distance Angles C16 1.3900 C20 1.3900 120.00 P1 1.8364 (0.0025) 116.20 (0.17) 123.72 (0.17) C15 - C16 C20 C16 - Distance Angles C15 1.3900 C17 1.3900 120.00 H16 0.9500 120.00 120.00 C16 - C15 C17 C17 - Distance Angles C18 1.3900 C16 1.3900 120.00 H17 0.9500 120.00 120.00 C17 - C18 C16 C18 - Distance Angles C19 1.3900 C17 1.3900 120.00 H18 0.9500 120.00 120.00 C18 - C19 C17 C19 - Distance Angles C18 1.3900 C20 1.3900 120.00 H19 0.9500 120.00 120.00 C19 - C18 C20 C20 - Distance Angles C19 1.3900 C15 1.3900 120.00 H20 0.9500 120.00 120.00 C20 - C19 C15 C21 - Distance Angles C22 1.3689 (0.0067) C26 1.3998 (0.0069) 117.35 (0.46) P1 1.8684 (0.0050) 117.50 (0.39) 125.13 (0.37) C21 - C22 C26 C22 - Distance Angles C21 1.3689 (0.0067) C23 1.4131 (0.0075) 120.18 (0.48) H22 0.9500 119.91 119.91 C22 - C21 C23 C23 - Distance Angles C24 1.3856 (0.0078) C22 1.4131 (0.0075) 122.08 (0.49) H23 0.9500 118.96 118.96 C23 - C24 C22 C24 - Distance Angles C25 1.3602 (0.0075) C23 1.3856 (0.0078) 118.26 (0.50) H24 0.9500 120.87 120.87 C24 - C25 C23 C25 - Distance Angles C24 1.3602 (0.0075) C26 1.4134 (0.0071) 119.99 (0.49) H25 0.9500 120.01 120.01 C25 - C24 C26 C26 - Distance Angles C21 1.3998 (0.0069) C25 1.4134 (0.0071) 122.11 (0.46) H26 0.9500 118.94 118.94 C26 - C21 C25 C27 - Distance Angles C28 1.3900 C32 1.3900 120.00 P1 2.0182 (0.0026) 119.16 (0.17) 120.82 (0.17) C27 - C28 C32 C28 - Distance Angles C29 1.3900 C27 1.3900 120.00 H28 0.9500 120.00 120.00 C28 - C29 C27 C29 - Distance Angles C28 1.3900 C30 1.3900 120.00 H29 0.9500 120.00 120.00 C29 - C28 C30 C30 - Distance Angles C31 1.3900 C29 1.3900 120.00 H30 0.9500 120.00 120.00 C30 - C31 C29 C31 - Distance Angles C30 1.3900 C32 1.3900 120.00 H31 0.9500 120.00 120.00 C31 - C30 C32 C32 - Distance Angles C31 1.3900 C27 1.3900 120.00 H32 0.9500 120.00 120.00 C32 - C31 C27 N1 - Distance Angles C2 1.3903 (0.0067) C6 1.4289 (0.0066) 128.05 (0.40) Pd1 1.9351 (0.0038) 122.35 (0.34) 109.56 (0.31) N1 - C2 C6 O12A - Distance Angles C13 1.3073 (0.0060) Pd1 2.2824 (0.0036) 112.96 (0.31) O12A - C13 O12B - Distance Angles C13 1.2613 (0.0064) O12B - P1 - Distance Angles C15 1.8364 (0.0025) C21 1.8684 (0.0050) 105.22 (0.20) C27 2.0182 (0.0026) 111.20 (0.15) 109.19 (0.18) Pd1 2.0589 (0.0012) 109.02 (0.11) 113.99 (0.15) 108.24 (0.11) P1 - C15 C21 C27 S8 - Distance Angles C9 1.5945 (0.0050) C7 1.8710 (0.0052) 95.12 (0.25) S8 - C9 Pd1 - Distance Angles N1 1.9351 (0.0038) P1 2.0589 (0.0012) 174.97 (0.13) C11 2.1696 (0.0049) 83.55 (0.18) 92.43 (0.13) O12A 2.2824 (0.0036) 90.63 (0.15) 93.45 (0.09) 174.05 (0.14) Pd1 - N1 P1 C11 C41 - Distance Angles C42 1.5610 (0.0049) H41A 0.9800 109.48 H41B 0.9800 109.47 109.47 H41C 0.9800 109.47 109.47 109.47 C41 - C42 H41A H41B C42 - Distance Angles C43 1.4319 (0.0098) C41 1.5610 (0.0049) 106.62 (0.94) H42A 0.9900 110.40 110.40 H42B 0.9900 110.40 110.40 108.61 C42 - C43 C41 H42A C43 - Distance Angles C42 1.4319 (0.0098) C43_$1 1.5014 (0.0150) 110.03 (0.77) H43A 0.9900 109.66 109.65 H43B 0.9900 109.66 109.65 108.16 C43 - C42 C43_$1 H43A FMAP and GRID set by program FMAP 2 1 23 GRID -2.500 -2 -1 2.500 2 1 R1 = 0.0675 for 5891 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 2.15 at 0.4738 0.8390 0.2940 [ 0.36 A from C17 ] Deepest hole -2.05 at 0.4163 0.8393 0.2757 [ 0.33 A from C17 ] Mean = 0.00, Rms deviation from mean = 0.15 e/A^3, Highest memory used = 4462 / 42904 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.5262 0.3390 0.2060 1.00000 0.05 2.15 0.36 C17 1.25 C16 1.26 C18 1.31 H17 Q2 1 0.1698 0.4992 0.0556 1.00000 0.05 2.00 0.65 H42B 0.87 C42 1.07 H42A 1.97 C43 Q3 1 0.3587 0.3274 0.1497 1.00000 0.05 1.98 0.38 C20 1.16 C15 1.31 H20 1.35 C19 Q4 1 0.1808 0.0954 0.2362 1.00000 0.05 1.75 0.37 C27 1.59 C28 1.62 C32 1.66 P1 Q5 1 0.4203 0.4449 -0.0088 1.00000 0.05 1.56 0.76 H41C 1.02 C41 1.26 H41B 1.44 H41A Q6 1 0.0495 0.0596 0.3568 1.00000 0.05 1.46 0.37 C30 0.59 H30 1.59 C31 1.62 C29 Q7 1 0.4685 0.4330 0.1427 1.00000 0.05 1.39 0.32 C19 1.01 H19 1.12 C18 1.67 C20 Q8 1 0.5448 0.4333 0.1626 1.00000 0.05 1.36 0.37 C18 0.96 H18 1.15 C19 1.71 H19 Q9 1 0.4229 0.2387 0.2110 1.00000 0.05 1.29 0.33 C16 1.01 H16 1.13 C15 1.67 C17 Q10 1 0.0508 -0.0396 0.3224 1.00000 0.05 0.88 0.35 C31 0.82 H31 1.28 C30 1.72 C32 Shortest distances between peaks (including symmetry equivalents) 7 8 0.85 6 10 1.42 1 9 1.49 1 8 1.56 3 7 1.58 3 9 1.93 5 5 1.96 1 7 1.99 1 3 2.07 3 8 2.12 8 9 2.79 7 9 2.84 4 9 2.91 Time profile in seconds ----------------------- 0.02: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.02: Generate connectivity array 0.00: 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. 2.55: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 2.16: Structure factors and derivatives 3.92: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.31: Solve l.s. equations 0.00: Generate HTAB table 0.05: Other dependent quantities, CIF, tables 0.16: Analysis of variance 0.05: Merge reflections for Fourier and .fcf 0.09: Fourier summations 0.06: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + non-dis finished at 13:23:24 Total CPU time: 9.4 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++