+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2009src0114 started at 17:41:05 on 09-Feb-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2009src0114 in P-1 CELL 0.71073 8.8363 10.2749 11.6567 86.643 86.468 86.435 ZERR 2.00 0.0004 0.0003 0.0005 0.003 0.002 0.002 LATT 1 SFAC C H N O P CL PD UNIT 44 50 10 2 2 2 2 V = 1052.69 F(000) = 556.0 Mu = 1.11 mm-1 Cell Wt = 1096.58 Rho = 1.730 MERG 2 OMIT -3.00 55.00 SHEL 7 0.77 FMAP 2 PLAN 10 SIZE 0.01 0.04 0.08 ACTA BOND $H WGHT 0.00000 5.47260 L.S. 4 TEMP -153.00 FVAR 0.48483 C2 1 0.265401 0.932044 0.480069 11.00000 0.02713 0.01780 = 0.01669 -0.00251 0.00161 0.00912 AFIX 23 H2A 2 0.273709 0.996496 0.413783 11.00000 -1.20000 H2B 2 0.271714 0.978322 0.551608 11.00000 -1.20000 AFIX 0 C3 1 0.116020 0.867972 0.481700 11.00000 0.02325 0.02173 = 0.03138 0.01078 0.00647 0.00887 C5 1 0.174967 0.833485 0.275480 11.00000 0.01937 0.01630 = 0.03087 -0.00553 -0.00114 -0.00388 C6 1 0.100185 0.864182 0.174229 11.00000 0.02941 0.02358 = 0.04388 -0.00859 -0.01845 0.00192 AFIX 43 H6 2 -0.007688 0.870910 0.177416 11.00000 -1.20000 AFIX 0 C7 1 0.179417 0.884830 0.070185 11.00000 0.04429 0.02700 = 0.03317 -0.00810 -0.02399 0.01014 AFIX 43 H7 2 0.126537 0.903577 0.002069 11.00000 -1.20000 AFIX 0 C8 1 0.337195 0.878151 0.065119 11.00000 0.05582 0.01971 = 0.01809 -0.00447 -0.00317 0.00943 AFIX 43 H8 2 0.392404 0.896153 -0.005978 11.00000 -1.20000 AFIX 0 C9 1 0.414519 0.845011 0.164442 11.00000 0.02893 0.02303 = 0.01721 -0.00479 -0.00642 0.00820 AFIX 43 H9 2 0.522417 0.839569 0.160353 11.00000 -1.20000 AFIX 0 C10 1 0.334687 0.819677 0.270138 11.00000 0.02182 0.01478 = 0.01237 -0.00112 -0.00557 0.00219 C11 1 0.420270 0.780026 0.372954 11.00000 0.01501 0.01408 = 0.01650 -0.00324 -0.00033 -0.00266 C12 1 0.541387 0.674328 0.373562 11.00000 0.01773 0.01450 = 0.01792 0.00045 0.00215 -0.00443 C13 1 0.585465 0.600753 0.278797 11.00000 0.02465 0.02087 = 0.01642 0.00029 -0.00249 -0.00161 AFIX 43 H13 2 0.542760 0.623058 0.206926 11.00000 -1.20000 AFIX 0 C14 1 0.689670 0.496719 0.288383 11.00000 0.01942 0.02059 = 0.01864 -0.00649 0.00282 0.00035 AFIX 43 H14 2 0.720771 0.448945 0.222783 11.00000 -1.20000 AFIX 0 C15 1 0.749750 0.461043 0.393400 11.00000 0.01845 0.01699 = 0.02565 -0.00009 -0.00033 0.00027 AFIX 43 H15 2 0.820168 0.387698 0.400393 11.00000 -1.20000 AFIX 0 C16 1 0.706477 0.533129 0.488571 11.00000 0.02206 0.01867 = 0.01851 -0.00132 -0.00117 0.00219 AFIX 43 H16 2 0.747483 0.507099 0.560375 11.00000 -1.20000 AFIX 0 C17 1 0.604687 0.642561 0.482044 11.00000 0.01570 0.02065 = 0.01357 -0.00356 0.00143 -0.00693 C18 1 -0.060136 0.756344 0.376503 11.00000 0.02644 0.05099 = 0.10847 -0.01403 0.00839 -0.01990 AFIX 137 H18A 2 -0.086773 0.713611 0.451778 11.00000 -1.50000 H18B 2 -0.054695 0.691894 0.317429 11.00000 -1.50000 H18C 2 -0.137732 0.825575 0.358369 11.00000 -1.50000 AFIX 0 C20 1 0.828254 0.562868 0.753674 11.00000 0.02541 0.02175 = 0.02520 -0.00552 -0.00541 0.00586 AFIX 23 H20A 2 0.786900 0.476808 0.745190 11.00000 -1.20000 H20B 2 0.903699 0.578823 0.688802 11.00000 -1.20000 AFIX 0 C22 1 0.796097 0.533751 0.961734 11.00000 0.03788 0.02697 = 0.02349 0.00251 -0.01086 -0.00202 AFIX 23 H22A 2 0.746840 0.452193 0.949292 11.00000 -1.20000 H22B 2 0.853837 0.518244 1.031868 11.00000 -1.20000 AFIX 0 C24 1 0.572071 0.647286 0.888243 11.00000 0.02275 0.02329 = 0.01547 0.00009 -0.00224 -0.00022 AFIX 23 H24A 2 0.489639 0.714187 0.905649 11.00000 -1.20000 H24B 2 0.525531 0.562757 0.883263 11.00000 -1.20000 AFIX 0 C25 1 0.777608 0.828471 0.791875 11.00000 0.02413 0.02255 = 0.01684 -0.00363 0.00017 0.00141 AFIX 23 H25A 2 0.851511 0.853745 0.728419 11.00000 -1.20000 H25B 2 0.705988 0.904793 0.805218 11.00000 -1.20000 AFIX 0 C27 1 0.971279 0.685901 0.878003 11.00000 0.02299 0.02657 = 0.03274 -0.00800 -0.00814 -0.00118 AFIX 23 H27A 2 1.036395 0.675364 0.944452 11.00000 -1.20000 H27B 2 1.037169 0.707639 0.808614 11.00000 -1.20000 AFIX 0 C28 1 0.753065 0.759153 0.993278 11.00000 0.02973 0.03538 = 0.01192 -0.00586 -0.00625 0.00024 AFIX 23 H28A 2 0.673745 0.830887 1.001791 11.00000 -1.20000 H28B 2 0.808957 0.751205 1.064634 11.00000 -1.20000 AFIX 0 N1 3 0.388660 0.830500 0.470719 11.00000 0.02120 0.01513 = 0.01300 0.00085 0.00216 0.00191 N4 3 0.088212 0.813336 0.379407 11.00000 0.01487 0.02438 = 0.04457 -0.00021 0.00296 -0.00432 N21 3 0.903769 0.560668 0.863401 11.00000 0.02398 0.02623 = 0.02470 -0.00149 -0.00702 0.00313 N23 3 0.678026 0.636400 0.982364 11.00000 0.02755 0.02490 = 0.01502 -0.00123 -0.00488 -0.00141 N26 3 0.859155 0.795196 0.896559 11.00000 0.02170 0.02634 = 0.02219 -0.00546 -0.00489 -0.00064 O3 4 0.029796 0.860573 0.565666 11.00000 0.03166 0.04583 = 0.03896 0.01594 0.01677 0.01167 P19 5 0.671131 0.692618 0.747950 11.00000 0.01912 0.01906 = 0.01264 -0.00163 -0.00156 0.00255 CL1 6 0.391214 0.900023 0.742304 11.00000 0.03541 0.03288 = 0.01632 -0.00698 -0.00388 0.01380 PD1 7 0.517517 0.756461 0.606099 11.00000 0.02036 0.01824 = 0.01223 -0.00136 -0.00095 0.00304 HKLF 4 Covalent radii and connectivity table for 2009src0114 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 P 1.100 CL 0.990 PD 1.380 C2 - N1 C3 C3 - O3 N4 C2 C5 - C6 N4 C10 C6 - C7 C5 C7 - C6 C8 C8 - C7 C9 C9 - C8 C10 C10 - C9 C5 C11 C11 - N1 C12 C10 C12 - C13 C17 C11 C13 - C14 C12 C14 - C13 C15 C15 - C14 C16 C16 - C15 C17 C17 - C16 C12 Pd1 C18 - N4 C20 - N21 P19 C22 - N23 N21 C24 - N23 P19 C25 - N26 P19 C27 - N26 N21 C28 - N26 N23 N1 - C11 C2 Pd1 N4 - C3 C5 C18 N21 - C22 C27 C20 N23 - C22 C28 C24 N26 - C28 C27 C25 O3 - C3 P19 - C25 C24 C20 Pd1 Cl1 - Pd1 Pd1 - C17 N1 P19 Cl1 16135 Reflections read, of which 23 rejected -11 =< h =< 11, -13 =< k =< 12, -15 =< l =< 15, Max. 2-theta = 54.96 0 Systematic absence violations 0 Inconsistent equivalents 4783 Unique reflections, of which 0 suppressed R(int) = 0.0534 R(sigma) = 0.0591 Friedel opposites merged Maximum memory for data reduction = 2870 / 47937 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 = 3673 / 353426 wR2 = 0.1097 before cycle 1 for 4783 data and 281 / 281 parameters GooF = S = 1.124; Restrained GooF = 1.124 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 5.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.48483 0.00074 0.001 OSF Mean shift/su = 0.001 Maximum = 0.020 for U33 Pd1 Max. shift = 0.000 A for H18A Max. dU = 0.000 for C22 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3673 / 353426 wR2 = 0.1097 before cycle 2 for 4783 data and 281 / 281 parameters GooF = S = 1.124; Restrained GooF = 1.124 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 5.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.48483 0.00074 0.000 OSF Mean shift/su = 0.000 Maximum = 0.007 for U33 Pd1 Max. shift = 0.000 A for H18A Max. dU = 0.000 for C22 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3673 / 353426 wR2 = 0.1097 before cycle 3 for 4783 data and 281 / 281 parameters GooF = S = 1.124; Restrained GooF = 1.124 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 5.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.48483 0.00074 0.000 OSF Mean shift/su = 0.000 Maximum = 0.001 for z Pd1 Max. shift = 0.000 A for C13 Max. dU = 0.000 for C8 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3673 / 353426 wR2 = 0.1097 before cycle 4 for 4783 data and 281 / 281 parameters GooF = S = 1.124; Restrained GooF = 1.124 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 5.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.48483 0.00074 0.000 OSF Mean shift/su = 0.000 Maximum = 0.001 for z Pd1 Max. shift = 0.000 A for H28A Max. dU = 0.000 for C16 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2A 0.2737 0.9965 0.4138 23 0.990 0.000 C2 N1 C3 H2B 0.2717 0.9783 0.5516 23 0.990 0.000 C2 N1 C3 H6 -0.0077 0.8709 0.1774 43 0.950 0.000 C6 C7 C5 H7 0.1265 0.9036 0.0021 43 0.950 0.000 C7 C6 C8 H8 0.3924 0.8962 -0.0060 43 0.950 0.000 C8 C7 C9 H9 0.5224 0.8396 0.1604 43 0.950 0.000 C9 C8 C10 H13 0.5428 0.6231 0.2069 43 0.950 0.000 C13 C14 C12 H14 0.7208 0.4489 0.2228 43 0.950 0.000 C14 C13 C15 H15 0.8202 0.3877 0.4004 43 0.950 0.000 C15 C14 C16 H16 0.7475 0.5071 0.5604 43 0.950 0.000 C16 C15 C17 H18A -0.0868 0.7136 0.4518 137 0.980 0.000 C18 N4 H18A H18B -0.0547 0.6919 0.3174 137 0.980 0.000 C18 N4 H18A H18C -0.1377 0.8256 0.3584 137 0.980 0.000 C18 N4 H18A H20A 0.7869 0.4768 0.7452 23 0.990 0.000 C20 N21 P19 H20B 0.9037 0.5788 0.6888 23 0.990 0.000 C20 N21 P19 H22A 0.7468 0.4522 0.9493 23 0.990 0.000 C22 N23 N21 H22B 0.8538 0.5182 1.0319 23 0.990 0.000 C22 N23 N21 H24A 0.4896 0.7142 0.9056 23 0.990 0.000 C24 N23 P19 H24B 0.5255 0.5628 0.8833 23 0.990 0.000 C24 N23 P19 H25A 0.8515 0.8537 0.7284 23 0.990 0.000 C25 N26 P19 H25B 0.7060 0.9048 0.8052 23 0.990 0.000 C25 N26 P19 H27A 1.0364 0.6754 0.9445 23 0.990 0.000 C27 N26 N21 H27B 1.0372 0.7076 0.8086 23 0.990 0.000 C27 N26 N21 H28A 0.6737 0.8309 1.0018 23 0.990 0.000 C28 N26 N23 H28B 0.8090 0.7512 1.0646 23 0.990 0.000 C28 N26 N23 2009src0114 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C2 0.26540 0.93204 0.48007 1.00000 0.02713 0.01780 0.01669 -0.00251 0.00161 0.00912 0.02104 0.00794 0.00054 0.00044 0.00040 0.00000 0.00260 0.00227 0.00224 0.00173 0.00186 0.00185 0.00098 H2A 0.27371 0.99650 0.41378 1.00000 0.02524 0.00000 0.00000 H2B 0.27171 0.97832 0.55161 1.00000 0.02524 0.00000 0.00000 C3 0.11602 0.86797 0.48170 1.00000 0.02325 0.02173 0.03137 0.01078 0.00647 0.00887 0.02669 0.00930 0.00057 0.00047 0.00045 0.00000 0.00260 0.00246 0.00279 0.00201 0.00211 0.00193 0.00111 C5 0.17497 0.83348 0.27548 1.00000 0.01937 0.01630 0.03087 -0.00553 -0.00114 -0.00387 0.02191 0.00746 0.00053 0.00044 0.00043 0.00000 0.00239 0.00227 0.00266 0.00187 0.00195 0.00177 0.00098 C6 0.10019 0.86418 0.17423 1.00000 0.02941 0.02358 0.04388 -0.00860 -0.01845 0.00192 0.03149 0.00806 0.00063 0.00049 0.00049 0.00000 0.00287 0.00265 0.00332 0.00226 0.00246 0.00210 0.00123 H6 -0.00769 0.87091 0.17742 1.00000 0.03779 0.00000 0.00000 C7 0.17942 0.88483 0.07019 1.00000 0.04429 0.02699 0.03317 -0.00810 -0.02399 0.01013 0.03418 0.00846 0.00067 0.00051 0.00048 0.00000 0.00346 0.00280 0.00302 0.00222 0.00261 0.00236 0.00133 H7 0.12654 0.90358 0.00207 1.00000 0.04101 0.00000 0.00000 C8 0.33719 0.87815 0.06512 1.00000 0.05582 0.01971 0.01809 -0.00447 -0.00317 0.00943 0.03152 0.00889 0.00069 0.00048 0.00043 0.00000 0.00373 0.00251 0.00248 0.00190 0.00234 0.00234 0.00125 H8 0.39240 0.89615 -0.00598 1.00000 0.03782 0.00000 0.00000 C9 0.41452 0.84501 0.16444 1.00000 0.02893 0.02303 0.01721 -0.00478 -0.00642 0.00821 0.02311 0.00781 0.00058 0.00045 0.00039 0.00000 0.00269 0.00246 0.00232 0.00181 0.00195 0.00195 0.00102 H9 0.52242 0.83957 0.16035 1.00000 0.02773 0.00000 0.00000 C10 0.33469 0.81968 0.27014 1.00000 0.02182 0.01478 0.01238 -0.00112 -0.00557 0.00219 0.01626 0.00702 0.00051 0.00041 0.00036 0.00000 0.00235 0.00212 0.00205 0.00159 0.00171 0.00169 0.00088 C11 0.42027 0.78003 0.37295 1.00000 0.01501 0.01408 0.01650 -0.00324 -0.00033 -0.00267 0.01505 0.00681 0.00048 0.00041 0.00037 0.00000 0.00218 0.00208 0.00214 0.00161 0.00167 0.00163 0.00086 C12 0.54139 0.67433 0.37356 1.00000 0.01773 0.01450 0.01792 0.00045 0.00215 -0.00443 0.01676 0.00716 0.00050 0.00041 0.00038 0.00000 0.00226 0.00212 0.00220 0.00165 0.00173 0.00167 0.00088 C13 0.58546 0.60075 0.27880 1.00000 0.02465 0.02087 0.01642 0.00029 -0.00249 -0.00160 0.02063 0.00755 0.00054 0.00044 0.00039 0.00000 0.00251 0.00237 0.00223 0.00176 0.00184 0.00186 0.00096 H13 0.54276 0.62306 0.20693 1.00000 0.02476 0.00000 0.00000 C14 0.68967 0.49672 0.28838 1.00000 0.01942 0.02059 0.01864 -0.00649 0.00282 0.00035 0.01956 0.00741 0.00051 0.00044 0.00039 0.00000 0.00235 0.00232 0.00229 0.00177 0.00180 0.00179 0.00094 H14 0.72077 0.44895 0.22278 1.00000 0.02348 0.00000 0.00000 C15 0.74975 0.46104 0.39340 1.00000 0.01845 0.01699 0.02565 -0.00009 -0.00033 0.00028 0.02050 0.00753 0.00052 0.00044 0.00040 0.00000 0.00234 0.00224 0.00249 0.00180 0.00186 0.00174 0.00095 H15 0.82017 0.38770 0.40039 1.00000 0.02460 0.00000 0.00000 C16 0.70648 0.53313 0.48857 1.00000 0.02206 0.01867 0.01851 -0.00132 -0.00117 0.00219 0.01987 0.00756 0.00052 0.00043 0.00040 0.00000 0.00244 0.00229 0.00228 0.00173 0.00182 0.00180 0.00095 H16 0.74748 0.50710 0.56037 1.00000 0.02385 0.00000 0.00000 C17 0.60469 0.64256 0.48204 1.00000 0.01569 0.02065 0.01356 -0.00356 0.00144 -0.00693 0.01638 0.00687 0.00049 0.00043 0.00037 0.00000 0.00219 0.00227 0.00209 0.00166 0.00167 0.00170 0.00088 C18 -0.06014 0.75634 0.37650 1.00000 0.02644 0.05099 0.10847 -0.01403 0.00839 -0.01990 0.06136 0.01136 0.00070 0.00070 0.00076 0.00000 0.00338 0.00424 0.00659 0.00407 0.00368 0.00298 0.00214 H18A -0.08677 0.71361 0.45178 1.00000 0.09204 0.00000 0.00000 H18B -0.05469 0.69189 0.31743 1.00000 0.09204 0.00000 0.00000 H18C -0.13773 0.82557 0.35837 1.00000 0.09204 0.00000 0.00000 C20 0.82825 0.56287 0.75367 1.00000 0.02540 0.02175 0.02520 -0.00552 -0.00541 0.00586 0.02409 0.00790 0.00056 0.00047 0.00042 0.00000 0.00262 0.00245 0.00257 0.00192 0.00202 0.00194 0.00104 H20A 0.78690 0.47681 0.74519 1.00000 0.02891 0.00000 0.00000 H20B 0.90370 0.57882 0.68880 1.00000 0.02891 0.00000 0.00000 C22 0.79610 0.53375 0.96173 1.00000 0.03788 0.02697 0.02348 0.00251 -0.01086 -0.00202 0.02922 0.00855 0.00062 0.00050 0.00043 0.00000 0.00314 0.00269 0.00261 0.00202 0.00225 0.00221 0.00115 H22A 0.74684 0.45219 0.94929 1.00000 0.03506 0.00000 0.00000 H22B 0.85384 0.51824 1.03187 1.00000 0.03506 0.00000 0.00000 C24 0.57207 0.64729 0.88824 1.00000 0.02275 0.02329 0.01547 0.00009 -0.00224 -0.00022 0.02055 0.00754 0.00053 0.00046 0.00038 0.00000 0.00248 0.00242 0.00222 0.00176 0.00182 0.00186 0.00096 H24A 0.48964 0.71419 0.90565 1.00000 0.02466 0.00000 0.00000 H24B 0.52553 0.56276 0.88326 1.00000 0.02466 0.00000 0.00000 C25 0.77761 0.82847 0.79187 1.00000 0.02413 0.02255 0.01684 -0.00363 0.00017 0.00141 0.02124 0.00748 0.00054 0.00045 0.00039 0.00000 0.00252 0.00241 0.00226 0.00178 0.00185 0.00187 0.00097 H25A 0.85151 0.85374 0.72842 1.00000 0.02549 0.00000 0.00000 H25B 0.70599 0.90479 0.80522 1.00000 0.02549 0.00000 0.00000 C27 0.97128 0.68590 0.87800 1.00000 0.02299 0.02657 0.03274 -0.00800 -0.00814 -0.00118 0.02692 0.00778 0.00057 0.00048 0.00046 0.00000 0.00261 0.00264 0.00284 0.00210 0.00212 0.00199 0.00109 H27A 1.03639 0.67536 0.94445 1.00000 0.03231 0.00000 0.00000 H27B 1.03717 0.70764 0.80862 1.00000 0.03231 0.00000 0.00000 C28 0.75306 0.75915 0.99328 1.00000 0.02973 0.03537 0.01192 -0.00586 -0.00625 0.00024 0.02538 0.00769 0.00058 0.00050 0.00039 0.00000 0.00276 0.00284 0.00219 0.00192 0.00193 0.00214 0.00107 H28A 0.67374 0.83089 1.00179 1.00000 0.03045 0.00000 0.00000 H28B 0.80896 0.75121 1.06463 1.00000 0.03045 0.00000 0.00000 N1 0.38866 0.83050 0.47072 1.00000 0.02119 0.01512 0.01300 0.00085 0.00216 0.00191 0.01676 0.00612 0.00043 0.00035 0.00031 0.00000 0.00200 0.00183 0.00179 0.00139 0.00147 0.00147 0.00077 N4 0.08821 0.81334 0.37941 1.00000 0.01487 0.02438 0.04457 -0.00021 0.00296 -0.00432 0.02807 0.00708 0.00045 0.00040 0.00040 0.00000 0.00207 0.00222 0.00274 0.00189 0.00184 0.00163 0.00096 N21 0.90377 0.56067 0.86340 1.00000 0.02398 0.02623 0.02470 -0.00149 -0.00702 0.00313 0.02493 0.00664 0.00047 0.00040 0.00035 0.00000 0.00221 0.00221 0.00219 0.00167 0.00172 0.00168 0.00089 N23 0.67803 0.63640 0.98236 1.00000 0.02755 0.02490 0.01502 -0.00123 -0.00488 -0.00140 0.02234 0.00633 0.00047 0.00039 0.00033 0.00000 0.00227 0.00213 0.00192 0.00154 0.00163 0.00167 0.00085 N26 0.85916 0.79520 0.89656 1.00000 0.02170 0.02634 0.02218 -0.00546 -0.00489 -0.00064 0.02313 0.00631 0.00045 0.00039 0.00034 0.00000 0.00215 0.00219 0.00209 0.00163 0.00166 0.00165 0.00087 O3 0.02980 0.86057 0.56567 1.00000 0.03166 0.04584 0.03896 0.01594 0.01677 0.01167 0.04090 0.00761 0.00044 0.00039 0.00034 0.00000 0.00221 0.00240 0.00231 0.00183 0.00179 0.00177 0.00102 P19 0.67113 0.69262 0.74795 1.00000 0.01912 0.01906 0.01264 -0.00163 -0.00156 0.00254 0.01704 0.00190 0.00013 0.00011 0.00010 0.00000 0.00060 0.00058 0.00054 0.00043 0.00044 0.00045 0.00025 Cl1 0.39121 0.90002 0.74230 1.00000 0.03541 0.03288 0.01632 -0.00698 -0.00388 0.01381 0.02854 0.00209 0.00015 0.00012 0.00010 0.00000 0.00071 0.00067 0.00056 0.00046 0.00049 0.00053 0.00029 Pd1 0.51752 0.75646 0.60610 1.00000 0.02036 0.01824 0.01223 -0.00136 -0.00095 0.00304 0.01710 0.00058 0.00004 0.00003 0.00003 0.00000 0.00019 0.00018 0.00017 0.00012 0.00012 0.00013 0.00011 Final Structure Factor Calculation for 2009src0114 in P-1 Total number of l.s. parameters = 281 Maximum vector length = 511 Memory required = 3392 / 26061 wR2 = 0.1097 before cycle 5 for 4783 data and 0 / 281 parameters GooF = S = 1.124; Restrained GooF = 1.124 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 5.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0532 for 4043 Fo > 4sig(Fo) and 0.0686 for all 4783 data wR2 = 0.1097, GooF = S = 1.124, Restrained GooF = 1.124 for all data Occupancy sum of asymmetric unit = 31.00 for non-hydrogen and 25.00 for hydrogen atoms Principal mean square atomic displacements U 0.0350 0.0177 0.0104 C2 0.0490 0.0192 0.0118 C3 0.0319 0.0205 0.0133 C5 0.0553 0.0221 0.0171 C6 0.0648 0.0229 0.0148 C7 0.0600 0.0201 0.0144 C8 0.0380 0.0164 0.0149 C9 0.0245 0.0141 0.0101 C10 0.0185 0.0150 0.0117 C11 0.0214 0.0177 0.0111 C12 0.0248 0.0212 0.0159 C13 0.0252 0.0213 0.0121 C14 0.0261 0.0191 0.0163 C15 0.0244 0.0185 0.0167 C16 0.0252 0.0125 0.0114 C17 0.1128 0.0552 0.0161 C18 0.0343 0.0216 0.0164 C20 0.0419 0.0280 0.0177 C22 0.0243 0.0222 0.0151 C24 0.0264 0.0220 0.0153 C25 0.0384 0.0248 0.0176 C27 0.0373 0.0295 0.0093 C28 0.0242 0.0141 0.0119 N1 0.0458 0.0252 0.0133 N4 0.0318 0.0255 0.0174 N21 0.0283 0.0249 0.0138 N23 0.0295 0.0228 0.0170 N26 0.0779 0.0277 0.0171 O3 0.0230 0.0156 0.0125 P19 0.0514 0.0203 0.0140 Cl1 0.0239 0.0153 0.0121 Pd1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.022 0.043 0.064 0.082 0.103 0.126 0.148 0.181 0.240 1.000 Number in group 487. 471. 495. 463. 483. 483. 468. 487. 468. 478. GooF 1.165 1.216 1.225 1.136 1.193 1.179 1.119 1.076 0.980 0.898 K 2.544 1.173 1.096 1.004 1.002 0.996 1.002 1.013 1.008 1.009 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.15 1.32 1.66 inf Number in group 497. 467. 489. 460. 484. 480. 469. 479. 478. 480. GooF 1.218 1.196 1.187 1.193 1.169 1.091 1.030 0.992 0.933 1.185 K 1.030 1.033 1.027 1.025 1.023 1.003 1.014 1.007 1.001 1.005 R1 0.145 0.129 0.119 0.097 0.082 0.062 0.051 0.043 0.030 0.028 Recommended weighting scheme: WGHT 0.0000 5.4742 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) -4 2 10 395.65 1003.61 6.05 0.158 0.99 -1 2 0 2929.92 2144.95 5.43 0.231 4.32 -9 -8 1 281.80 676.53 3.70 0.130 0.79 3 11 6 531.65 251.92 3.67 0.079 0.84 -8 -5 6 202.83 31.83 3.60 0.028 0.86 6 -8 3 124.17 329.87 3.58 0.091 0.91 -3 2 0 1128.38 822.50 3.58 0.143 2.48 -3 -10 7 348.66 634.96 3.50 0.126 0.82 -2 9 11 244.19 485.53 3.49 0.110 0.77 1 2 1 1004.01 735.00 3.45 0.135 4.35 -8 -6 2 -23.04 54.24 3.40 0.037 0.93 -8 -2 9 -33.27 80.56 3.34 0.045 0.81 -9 3 7 229.43 71.24 3.31 0.042 0.80 8 -2 3 655.55 395.51 3.31 0.099 1.04 8 9 3 387.76 147.87 3.28 0.061 0.81 -4 5 12 372.84 700.45 3.24 0.132 0.81 -6 1 6 91.97 8.96 3.23 0.015 1.13 -2 -1 4 53.03 1.39 3.20 0.006 2.29 -9 3 3 1182.12 820.09 3.18 0.143 0.89 0 12 3 252.79 479.69 3.14 0.109 0.84 9 0 2 253.44 97.81 3.10 0.049 0.97 1 -12 5 498.08 182.59 3.08 0.067 0.78 -3 8 11 544.94 295.37 3.04 0.086 0.79 -7 2 11 86.40 272.15 3.03 0.082 0.78 3 -1 5 803.72 1069.31 3.02 0.163 1.82 0 -4 12 115.00 11.96 3.02 0.017 0.89 -5 2 1 1951.31 2352.96 2.98 0.242 1.61 8 2 6 250.91 488.38 2.95 0.110 0.98 8 5 7 120.62 281.36 2.93 0.084 0.88 -6 -9 2 210.50 3.70 2.92 0.010 0.90 -1 3 0 6387.49 5666.03 2.90 0.375 3.12 2 1 6 857.34 1110.51 2.89 0.166 1.81 3 -5 6 78.64 176.75 2.86 0.066 1.24 0 -3 1 105.75 40.98 2.85 0.032 3.23 4 -3 11 233.51 408.84 2.84 0.101 0.92 3 9 5 290.22 81.29 2.83 0.045 1.01 5 0 11 186.46 37.61 2.82 0.031 0.93 5 11 6 1129.07 648.35 2.77 0.127 0.80 -8 5 8 495.65 740.09 2.76 0.136 0.78 6 3 10 1596.55 2065.76 2.75 0.227 0.92 -8 -6 7 1572.63 1164.94 2.75 0.170 0.80 0 3 2 1074.23 1339.79 2.75 0.183 3.02 -5 3 12 102.25 276.96 2.74 0.083 0.81 -4 9 8 1123.32 778.23 2.73 0.139 0.82 -7 7 4 415.35 636.57 2.73 0.126 0.88 7 -6 2 330.22 162.58 2.73 0.064 0.97 0 2 2 2056.61 1707.79 2.73 0.206 3.95 -2 7 10 -26.02 60.80 2.71 0.039 0.90 6 2 0 847.39 1094.66 2.71 0.165 1.43 2 -1 7 401.57 574.94 2.71 0.120 1.55 Bond lengths and angles C2 - Distance Angles N1 1.4643 (0.0054) C3 1.5098 (0.0071) 108.42 (0.37) H2A 0.9900 110.01 110.01 H2B 0.9900 110.01 110.01 108.37 C2 - N1 C3 H2A C3 - Distance Angles O3 1.2045 (0.0059) N4 1.3889 (0.0070) 122.35 (0.51) C2 1.5098 (0.0071) 123.11 (0.51) 114.49 (0.41) C3 - O3 N4 C5 - Distance Angles C6 1.3985 (0.0069) N4 1.4050 (0.0064) 118.98 (0.45) C10 1.4075 (0.0064) 119.25 (0.46) 121.74 (0.43) C5 - C6 N4 C6 - Distance Angles C7 1.3747 (0.0083) C5 1.3985 (0.0069) 121.42 (0.50) H6 0.9500 119.29 119.29 C6 - C7 C5 C7 - Distance Angles C6 1.3747 (0.0083) C8 1.3894 (0.0081) 119.69 (0.47) H7 0.9500 120.16 120.16 C7 - C6 C8 C8 - Distance Angles C7 1.3894 (0.0081) C9 1.3948 (0.0066) 119.99 (0.51) H8 0.9500 120.01 120.01 C8 - C7 C9 C9 - Distance Angles C8 1.3948 (0.0066) C10 1.4005 (0.0064) 120.66 (0.48) H9 0.9500 119.67 119.67 C9 - C8 C10 C10 - Distance Angles C9 1.4005 (0.0065) C5 1.4075 (0.0064) 118.86 (0.41) C11 1.4800 (0.0058) 119.24 (0.40) 121.90 (0.41) C10 - C9 C5 C11 - Distance Angles N1 1.2875 (0.0055) C12 1.4766 (0.0059) 114.82 (0.39) C10 1.4800 (0.0058) 122.24 (0.39) 122.84 (0.38) C11 - N1 C12 C12 - Distance Angles C13 1.3970 (0.0063) C17 1.4264 (0.0060) 120.42 (0.41) C11 1.4766 (0.0059) 123.91 (0.40) 115.47 (0.39) C12 - C13 C17 C13 - Distance Angles C14 1.3709 (0.0063) C12 1.3970 (0.0063) 120.72 (0.42) H13 0.9500 119.64 119.64 C13 - C14 C12 C14 - Distance Angles C13 1.3709 (0.0063) C15 1.3849 (0.0064) 120.21 (0.42) H14 0.9500 119.90 119.90 C14 - C13 C15 C15 - Distance Angles C14 1.3849 (0.0064) C16 1.3908 (0.0064) 119.67 (0.42) H15 0.9500 120.17 120.17 C15 - C14 C16 C16 - Distance Angles C15 1.3908 (0.0064) C17 1.3970 (0.0061) 122.16 (0.42) H16 0.9500 118.92 118.92 C16 - C15 C17 C17 - Distance Angles C16 1.3970 (0.0062) C12 1.4264 (0.0060) 116.75 (0.40) Pd1 2.0007 (0.0043) 129.90 (0.33) 113.13 (0.32) C17 - C16 C12 C18 - Distance Angles N4 1.4716 (0.0068) H18A 0.9800 109.47 H18B 0.9800 109.47 109.47 H18C 0.9800 109.47 109.47 109.47 C18 - N4 H18A H18B C20 - Distance Angles N21 1.4770 (0.0059) P19 1.8655 (0.0046) 111.21 (0.32) H20A 0.9900 109.39 109.39 H20B 0.9900 109.39 109.39 108.01 C20 - N21 P19 H20A C22 - Distance Angles N23 1.4563 (0.0064) N21 1.4686 (0.0067) 115.22 (0.40) H22A 0.9900 108.47 108.47 H22B 0.9900 108.47 108.47 107.49 C22 - N23 N21 H22A C24 - Distance Angles N23 1.4805 (0.0056) P19 1.8554 (0.0047) 111.35 (0.32) H24A 0.9900 109.36 109.36 H24B 0.9900 109.36 109.36 107.99 C24 - N23 P19 H24A C25 - Distance Angles N26 1.4677 (0.0057) P19 1.8445 (0.0048) 112.85 (0.32) H25A 0.9900 109.02 109.02 H25B 0.9900 109.02 109.02 107.80 C25 - N26 P19 H25A C27 - Distance Angles N26 1.4674 (0.0061) N21 1.4745 (0.0064) 113.95 (0.40) H27A 0.9900 108.76 108.76 H27B 0.9900 108.76 108.76 107.66 C27 - N26 N21 H27A C28 - Distance Angles N26 1.4667 (0.0063) N23 1.4764 (0.0063) 114.99 (0.38) H28A 0.9900 108.52 108.52 H28B 0.9900 108.52 108.52 107.52 C28 - N26 N23 H28A N1 - Distance Angles C11 1.2875 (0.0055) C2 1.4643 (0.0054) 118.89 (0.37) Pd1 2.0829 (0.0036) 116.24 (0.30) 124.86 (0.28) N1 - C11 C2 N4 - Distance Angles C3 1.3889 (0.0070) C5 1.4050 (0.0064) 124.22 (0.41) C18 1.4716 (0.0068) 115.65 (0.49) 118.69 (0.50) N4 - C3 C5 N21 - Distance Angles C22 1.4686 (0.0067) C27 1.4745 (0.0064) 108.83 (0.40) C20 1.4770 (0.0059) 111.00 (0.39) 111.25 (0.39) N21 - C22 C27 N23 - Distance Angles C22 1.4563 (0.0064) C28 1.4764 (0.0064) 107.82 (0.39) C24 1.4805 (0.0056) 110.43 (0.37) 112.05 (0.36) N23 - C22 C28 N26 - Distance Angles C28 1.4667 (0.0063) C27 1.4674 (0.0061) 109.04 (0.39) C25 1.4677 (0.0057) 110.70 (0.37) 110.42 (0.37) N26 - C28 C27 O3 - Distance Angles C3 1.2045 (0.0059) O3 - P19 - Distance Angles C25 1.8445 (0.0048) C24 1.8554 (0.0047) 99.29 (0.21) C20 1.8655 (0.0047) 97.76 (0.22) 97.40 (0.22) Pd1 2.2463 (0.0012) 111.84 (0.15) 114.94 (0.15) 130.39 (0.16) P19 - C25 C24 C20 Cl1 - Distance Angles Pd1 2.4070 (0.0012) Cl1 - Pd1 - Distance Angles C17 2.0007 (0.0043) N1 2.0829 (0.0036) 80.27 (0.16) P19 2.2463 (0.0012) 100.36 (0.13) 174.46 (0.11) Cl1 2.4070 (0.0012) 173.96 (0.13) 93.87 (0.10) 85.61 (0.04) Pd1 - C17 N1 P19 FMAP and GRID set by program FMAP 2 1 22 GRID -2.632 -2 -2 2.632 2 2 R1 = 0.0676 for 4783 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.64 at 0.2718 0.8765 0.7388 [ 1.10 A from CL1 ] Deepest hole -0.63 at 0.4214 0.2213 0.3683 [ 0.69 A from PD1 ] Mean = 0.00, Rms deviation from mean = 0.14 e/A^3, Highest memory used = 3323 / 22543 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.2718 0.8765 0.7388 1.00000 0.05 0.64 1.10 CL1 2.36 H2B 2.84 H27B 2.85 PD1 Q2 1 0.8171 0.6302 0.8934 1.00000 0.05 0.60 1.07 N21 1.25 C22 1.51 C27 1.56 N23 Q3 1 0.1535 0.8975 0.0225 1.00000 0.05 0.55 0.35 H7 0.62 C7 1.72 C8 1.82 C6 Q4 1 0.6014 0.6000 1.0240 1.00000 0.05 0.54 0.90 N23 1.66 C24 1.88 H24B 1.93 C22 Q5 1 0.2865 0.8502 0.1253 1.00000 0.05 0.54 0.85 C8 1.20 C7 1.24 C9 1.71 C6 Q6 1 0.4279 0.9345 0.2877 1.00000 0.05 0.54 1.51 C10 1.76 C9 1.83 C11 1.94 H9 Q7 1 0.4256 0.7188 0.6014 1.00000 0.05 0.54 0.93 PD1 1.89 N1 2.18 C17 2.48 C15 Q8 1 0.6079 0.7164 0.8314 1.00000 0.05 0.53 1.00 C24 1.12 P19 1.32 H24A 1.83 H24B Q9 1 0.2554 0.9030 0.0687 1.00000 0.05 0.52 0.71 C7 0.75 C8 1.42 H7 1.45 H8 Q10 1 0.3318 0.8812 0.4650 1.00000 0.05 0.52 0.70 N1 0.78 C2 1.38 H2A 1.51 H2B Shortest distances between peaks (including symmetry equivalents) 5 9 0.88 3 9 1.08 3 5 1.76 2 8 2.15 6 10 2.24 7 10 2.38 2 4 2.39 4 8 2.48 5 6 2.55 1 7 2.61 4 4 2.91 Time profile in seconds ----------------------- 0.00: 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. 0.72: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 1.02: Structure factors and derivatives 2.44: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.03: Apply other restraints 0.23: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.13: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.05: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2009src0114 finished at 17:41:10 Total CPU time: 4.7 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++