ࡱ>  R bjbjVV2<<   ^^^^^rrr8r%<$a^^^^4```^^````ztrpv`0%`ada`a^`00L"`ndJ%a  $: Date: Oct, 26, 2010 Name: Jie Hong Tsai Advisor: Gan-Ong Phone: 886-2-789-8648 E-mail: tgong@chem.sinica.edu.tw Sample : i12741 Condition of recrystalization : Ether solution and crystallized under -20 Reaction scheme and proposes structure:  EMBED ChemDraw.Document.6.0  Method of collection: The data was collected under N2 streme at 100K Crystal morphology and size: Size: 0.25 0.28 0.30 mm Shape: prism Color : colorless        (9Wp{     + I K Èumi\TmuFh BB*CJKHaJphjhZ}UjyqqP hZ}UVo(h%}jh%}U$h B5B*CJKH\aJo(ph!h B5B*CJKH\aJph)h Bh BB*CJKHaJmH phsH )h Bh BB*CJKHaJmH phsH h BB*CJKHaJo(phhZ}B*CJKHaJphhZ}B*CJKHaJo(phh BB*CJKHaJph(9Op + Z w gdZ}gd B $7$8$H$a$gd%} 7$8$H$gd BK Z w h57jh57UhOvh BB*CJKHaJo(ph!h B5B*CJKH\aJphh BB*CJKHaJph gd B01h2P. 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CS ChemDraw DrawingChemDraw Interchange FormatChemDraw.Document.6.09q Oh+'0<x   $,4Date: Oct, 27, 2009heptNormal@aCONTENTSy1Table*aSummaryInformation( lDocumentSummaryInformation8 VjCD0100ChemDraw 8.09Microsoft Word - C:\Users\@a\Desktop\JHT\i11889.docP@9s    :;<   `  ffx# $$$$2Arialx6&6&g{6&dd'`${S&Bǚ33 $$pP_q1, ~rX;l! +?l_8l_"@%# `NsHm( 7tEF6 7uAF88 +,<b5_4b5|<<# `Nv1OE w9i 7xl9Q y 3^ 7z|$d_ 7{PS 7|R[#=|F }G Q b9 +M 7i +|!i&i&"Y# `NMM  79  79 7" (+|!"K"h&#`Zr`D) +F%,z %;5,# `Nw, 7v ,7 7yNDD 7O] 7]PF 7Yl)~P= 7 qr  rs  st  tu  uq  uv  rw  vx  xy  yz  z{  {|  |v  x}  |  w              q        }  }     }d{7 *+< 7.7^o 7.7կ 7* =կ 7=^o 7*]o +7z.]&].# `N* +z.)&).\# `C*)< +7z.)&).\# `N*  .7 in C2/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq Zr 0.36861 0.33973 0.23190 1.00000 0.01404 0.01917 0.01462 0.00044 0.00435 0.00052 0.01585 0.00040 0.00001 0.00002 0.00001 0.00000 0.00011 0.00013 0.00012 0.00009 0.00008 0.00008 0.00008 O1 0.46291 0.28794 0.32199 1.00000 0.01821 0.02160 0.01815 0.00324 0.00419 0.00460 0.01946 0.00294 0.00008 0.00012 0.00009 0.00000 0.00076 0.00087 0.00079 0.00065 0.00061 0.00065 0.00034 N1 0.50216 0.14136 0.39564 1.00000 0.01671 0.02007 0.02003 0.00436 0.00640 0.00208 0.01865 0.00365 0.00010 0.00014 0.00011 0.00000 0.00091 0.00104 0.00096 0.00076 0.00074 0.00074 0.00041 N2 0.58145 0.21586 0.33814 1.00000 0.01826 0.02079 0.02042 0.00370 0.00760 0.00320 0.01936 0.00366 0.00010 0.00015 0.00011 0.00000 0.00092 0.00105 0.00097 0.00079 0.00075 0.00077 0.00040 N3 0.26767 0.27094 0.18887 1.00000 0.01750 0.02542 0.02301 0.00126 0.00476 -0.00133 0.02211 0.00365 0.00010 0.00015 0.00011 0.00000 0.00093 0.00109 0.00102 0.00083 0.00077 0.00080 0.00042 N4 0.34509 0.42785 0.32106 1.00000 0.02003 0.02848 0.02049 -0.00187 0.00634 0.00498 0.02283 0.00378 0.00010 0.00016 0.00011 0.00000 0.00097 0.00115 0.00100 0.00084 0.00078 0.00083 0.00043 N5 0.38027 0.45029 0.15286 1.00000 0.02219 0.02303 0.01723 0.00267 0.00571 0.00100 0.02074 0.00365 0.00010 0.00015 0.00011 0.00000 0.00098 0.00107 0.00096 0.00079 0.00076 0.00080 0.00041 C1 0.38291 0.05569 0.38327 1.00000 0.02944 0.03303 0.02411 0.01074 0.00153 -0.00677 0.02996 0.00492 0.00014 0.00021 0.00015 0.00000 0.00133 0.00149 0.00129 0.00110 0.00103 0.00110 0.00058 C2 0.31760 0.04763 0.40982 1.00000 0.02285 0.04473 0.03843 0.02071 -0.00576 -0.01236 0.03805 0.00537 0.00014 0.00022 0.00017 0.00000 0.00130 0.00177 0.00161 0.00137 0.00112 0.00120 0.00072 H2A 0.28040 0.00193 0.38483 1.00000 0.04565 0.00000 0.00000 C3 0.30839 0.10598 0.47163 1.00000 0.02330 0.05253 0.04326 0.02182 0.01180 0.00575 0.03915 0.00609 0.00015 0.00024 0.00018 0.00000 0.00135 0.00193 0.00171 0.00148 0.00119 0.00128 0.00071 H3A 0.26498 0.09917 0.48816 1.00000 0.04697 0.00000 0.00000 C4 0.36171 0.17435 0.50986 1.00000 0.03012 0.03942 0.04104 0.01133 0.01955 0.00998 0.03493 0.00595 0.00015 0.00022 0.00018 0.00000 0.00140 0.00167 0.00159 0.00129 0.00121 0.00121 0.00064 H4A 0.35420 0.21325 0.55190 1.00000 0.04192 0.00000 0.00000 C5 0.42714 0.18594 0.48609 1.00000 0.02376 0.03065 0.03006 0.00811 0.01163 0.00624 0.02731 0.00518 0.00014 0.00020 0.00015 0.00000 0.00122 0.00142 0.00134 0.00109 0.00102 0.00104 0.00055 C6 0.43613 0.12644 0.42249 1.00000 0.01693 0.02599 0.02432 0.01089 0.00440 0.00091 0.02263 0.00465 0.00012 0.00019 0.00014 0.00000 0.00110 0.00128 0.00124 0.00100 0.00092 0.00094 0.00051 C7 0.39513 -0.00686 0.31613 1.00000 0.05846 0.04447 0.03281 -0.00184 0.00611 -0.02069 0.04644 0.00551 0.00018 0.00024 0.00017 0.00000 0.00197 0.00187 0.00158 0.00136 0.00138 0.00156 0.00079 H7A 0.39989 0.03704 0.27344 1.00000 0.06966 0.00000 0.00000 H7B 0.35340 -0.05173 0.29674 1.00000 0.06966 0.00000 0.00000 H7C 0.43996 -0.04620 0.33493 1.00000 0.06966 0.00000 0.00000 C8 0.48633 0.25958 0.52819 1.00000 0.04658 0.03447 0.03796 -0.00759 0.02089 -0.00482 0.03783 0.00535 0.00016 0.00022 0.00017 0.00000 0.00168 0.00160 0.00158 0.00127 0.00130 0.00131 0.00066 H8A 0.47259 0.28909 0.57294 1.00000 0.05674 0.00000 0.00000 H8B 0.49123 0.31234 0.49159 1.00000 0.05674 0.00000 0.00000 H8C 0.53308 0.22446 0.54701 1.00000 0.05674 0.00000 0.00000 C9 0.51245 0.21945 0.34858 1.00000 0.01797 0.01967 0.01346 -0.00044 0.00400 0.00106 0.01708 0.00411 0.00012 0.00017 0.00012 0.00000 0.00104 0.00117 0.00103 0.00087 0.00082 0.00088 0.00045 C10 0.56804 0.08518 0.41704 1.00000 0.02364 0.02240 0.02525 0.00810 0.00577 0.00622 0.02392 0.00469 0.00013 0.00019 0.00014 0.00000 0.00120 0.00126 0.00126 0.00099 0.00097 0.00097 0.00051 H10A 0.57746 0.02747 0.44929 1.00000 0.02870 0.00000 0.00000 C11 0.61506 0.13124 0.38169 1.00000 0.01875 0.02538 0.02655 0.00379 0.00657 0.00705 0.02346 0.00469 0.00013 0.00018 0.00014 0.00000 0.00113 0.00130 0.00128 0.00100 0.00095 0.00094 0.00052 H11A 0.66358 0.10969 0.38566 1.00000 0.02816 0.00000 0.00000 C12 0.24070 0.20564 0.24294 1.00000 0.03693 0.02942 0.04105 0.00245 0.01598 -0.00424 0.03474 0.00551 0.00016 0.00021 0.00017 0.00000 0.00150 0.00149 0.00160 0.00124 0.00122 0.00120 0.00062 H12A 0.19178 0.22746 0.24440 1.00000 0.05211 0.00000 0.00000 H12B 0.27417 0.20975 0.29584 1.00000 0.05211 0.00000 0.00000 H12C 0.23834 0.13663 0.22426 1.00000 0.05211 0.00000 0.00000 C13 0.21825 0.26919 0.10846 1.00000 0.02418 0.03979 0.03329 -0.00254 -0.00116 -0.00434 0.03414 0.00480 0.00014 0.00022 0.00016 0.00000 0.00129 0.00163 0.00147 0.00124 0.00108 0.00116 0.00062 H13A 0.17036 0.29598 0.10912 1.00000 0.05121 0.00000 0.00000 H13B 0.21251 0.20043 0.08906 1.00000 0.05121 0.00000 0.00000 H13C 0.23908 0.31001 0.07383 1.00000 0.05121 0.00000 0.00000 C14 0.28362 0.42344 0.35773 1.00000 0.03403 0.03284 0.02869 0.00213 0.01585 0.01053 0.03042 0.00536 0.00014 0.00021 0.00015 0.00000 0.00140 0.00149 0.00137 0.00112 0.00112 0.00115 0.00059 H14A 0.26823 0.49127 0.36632 1.00000 0.04563 0.00000 0.00000 H14B 0.29943 0.38859 0.40823 1.00000 0.04563 0.00000 0.00000 H14C 0.24249 0.38754 0.32294 1.00000 0.04563 0.00000 0.00000 C15 0.40660 0.48519 0.37230 1.00000 0.02938 0.03711 0.02698 -0.01022 0.00229 0.00828 0.03218 0.00478 0.00014 0.00021 0.00015 0.00000 0.00133 0.00156 0.00134 0.00116 0.00103 0.00115 0.00060 H15A 0.39102 0.55407 0.37679 1.00000 0.04826 0.00000 0.00000 H15B 0.44823 0.48476 0.34935 1.00000 0.04826 0.00000 0.00000 H15C 0.42116 0.45460 0.42458 1.00000 0.04826 0.00000 0.00000 C16 0.39158 0.55843 0.17014 1.00000 0.02496 0.02428 0.03172 0.00442 0.00767 0.00072 0.02698 0.00482 0.00014 0.00018 0.00015 0.00000 0.00123 0.00132 0.00137 0.00107 0.00102 0.00101 0.00054 H16A 0.35267 0.59651 0.13397 1.00000 0.04046 0.00000 0.00000 H16B 0.43917 0.57872 0.16346 1.00000 0.04046 0.00000 0.00000 H16C 0.39036 0.57135 0.22437 1.00000 0.04046 0.00000 0.00000 C17 0.37983 0.43044 0.06980 1.00000 0.02854 0.03587 0.02052 0.00771 0.00666 0.00338 0.02830 0.00501 0.00014 0.00021 0.00014 0.00000 0.00129 0.00151 0.00122 0.00108 0.00099 0.00111 0.00056 H17A 0.34033 0.46859 0.03455 1.00000 0.04245 0.00000 0.00000 H17B 0.37200 0.35914 0.05863 1.00000 0.04245 0.00000 0.00000 H17C 0.42688 0.45052 0.06156 1.00000 0.04245 0.00000 0.00000 Final Structure Factor Calculation for i11618 in C2/c Total number of l.s. parameters = 225 Maximum vector length = 511 Memory required = 3363 / 24017 wR2 = 0.0790 before cycle 11 for 4463 data and 0 / 225 parameters GooF = S = 1.006; Restrained GooF = 1.006 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0357 * P )^2 + 5.62 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0309 for 3639 Fo > 4sig(Fo) and 0.0425 for all 4463 data wR2 = 0.0790, GooF = S = 1.006, Restrained GooF = 1.006 for all data Occupancy sum of asymmetric unit = 24.00 for non-hydrogen and 29.00 for hydrogen atoms Principal mean square atomic displacements U 0.0193 0.0147 0.0136 Zr 0.0251 0.0191 0.0142 O1 0.0246 0.0157 0.0156 N1 0.0255 0.0169 0.0157 N2 0.0265 0.0225 0.0173 N3 0.0314 0.0209 0.0162 N4 0.0243 0.0219 0.0160 N5 0.0483 0.0248 0.0168 C1 0.0763 0.0207 0.0171 C2 0.0702 0.0256 0.0216 C3 0.0557 0.0289 0.0202 C4 0.0401 0.0223 0.0195 C5 0.0366 0.0171 0.0142 C6 0.0760 0.0349 0.0284 C7 0.0535 0.0340 0.0260 C8 0.0203 0.0175 0.0134 C9 0.0325 0.0252 0.0141 C10 0.0311 0.0250 0.0143 C11 0.0437 0.0360 0.0246 C12 0.0422 0.0407 0.0196 C13 0.0451 0.0283 0.0179 C14 0.0516 0.0248 0.0201 C15 0.0339 0.0248 0.0222 C16 0.0393 0.0283 0.0173 C17 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.021 0.041 0.063 0.088 0.115 0.147 0.181 0.226 0.301 1.000 Number in group 464. 430. 455. 440. 443. 459. 433. 444. 448. 447. GooF 0.761 1.054 1.131 1.138 1.018 1.078 1.026 0.954 0.976 0.872 K 1.169 0.821 0.874 0.962 0.978 0.986 1.005 1.009 1.015 1.010 Resolution(A) 0.78 0.81 0.84 0.88 0.93 0.99 1.06 1.17 1.34 1.67 inf Number in group 450. 461. 432. 443. 455. 441. 443. 448. 440. 450. GooF 0.959 0.938 0.955 0.937 0.982 0.909 0.829 0.886 0.927 1.548 K 1.005 1.007 1.005 1.010 1.013 1.009 1.006 0.999 1.005 1.007 R1 0.091 0.077 0.069 0.051 0.048 0.039 0.030 0.028 0.021 0.026 Recommended weighting scheme: WGHT 0.0285 6.3121 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) -8 0 4 1101.21 1930.71 6.41 0.120 2.24 3 3 4 3155.06 4231.03 5.24 0.177 2.50 4 4 3 1386.83 2011.18 4.93 0.122 2.26 -10 0 4 18206.08 15058.96 4.40 0.334 1.83 7 3 1 4428.17 3480.62 4.24 0.161 2.13 -7 3 1 1094.58 744.37 4.03 0.074 2.26 -4 4 6 4028.93 5024.47 4.01 0.193 2.09 -2 8 15 8463.16 6817.34 3.98 0.225 0.94 -11 1 4 72.19 271.19 3.97 0.045 1.66 -5 3 5 1184.65 805.19 3.91 0.077 2.39 0 0 6 1680.91 2241.65 3.86 0.129 2.78 -7 1 4 -21.83 82.69 3.79 0.025 2.46 -8 2 7 2044.76 2673.74 3.72 0.141 1.83 3 5 1 7663.83 9108.76 3.72 0.260 2.35 -2 4 4 50.89 165.53 3.65 0.035 2.60 0 6 1 201.62 73.08 3.64 0.023 2.17 -22 0 10 308.63 755.90 3.54 0.075 0.82 -7 5 6 1253.65 869.10 3.54 0.080 1.69 -14 8 2 -10.74 183.67 3.53 0.037 1.03 20 2 3 343.21 735.02 3.51 0.074 0.84 -7 11 10 102.93 444.46 3.49 0.057 0.96 -20 6 1 122.28 422.82 3.49 0.056 0.84 6 12 10 12568.98 9579.51 3.33 0.267 0.84 -12 12 4 7400.52 5894.91 3.30 0.209 0.89 -6 2 6 2141.47 2685.75 3.27 0.141 2.23 -19 5 6 124.32 450.87 3.24 0.058 0.91 -8 6 11 264.47 521.46 3.24 0.062 1.21 -2 2 8 3564.42 2941.85 3.23 0.148 2.05 -19 7 9 659.74 1253.23 3.23 0.096 0.85 -19 3 12 328.81 621.81 3.21 0.068 0.88 3 1 7 8917.27 10317.64 3.20 0.277 2.01 -10 2 3 562.93 347.49 3.16 0.051 1.79 1 3 7 4484.36 3784.09 3.11 0.168 2.02 3 5 2 1773.90 1417.31 3.04 0.103 2.25 -17 3 1 772.51 1217.37 3.03 0.095 1.04 6 2 4 137.29 268.05 3.02 0.045 2.06 1 1 7 5277.08 4511.13 3.01 0.183 2.25 -8 8 17 12.17 241.97 3.00 0.042 0.86 -5 1 4 2609.99 3152.94 3.00 0.153 3.08 -3 7 2 410.77 612.28 2.95 0.067 1.78 4 2 2 237.98 131.23 ^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.06686 0.00009 0.046 OSF 165 0.10509 0.02891 3.635 tors H8A Mean shift/esd = 0.043 Maximum = 3.635 for tors H8A Max. shift = 0.106 A for H8A Max. dU = 0.000 for C8 Least-squares cycle 10 Maximum vector length = 511 Memory required = 5762 / 543952 wR2 = 0.1153 before cycle 10 for 7633 data and 421 / 421 parameters GooF = S = 1.099; Restrained GooF = 1.099 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0561 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.06687 0.00009 0.062 OSF 165 0.11969 0.02876 4.162 tors H8A Mean shift/esd = 0.049 Maximum = 4.162 for tors H8A Max. shift = 0.121 A for H8A Max. dU = 0.000 for C8 Least-squares cycle 11 Maximum vector length = 511 Memory required = 5762 / 543952 wR2 = 0.1150 before cycle 11 for 7633 data and 421 / 421 parameters GooF = S = 1.096; Restrained GooF = 1.096 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0561 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.06687 0.00009 0.057 OSF 165 0.11274 0.02839 3.971 tors H8A Mean shift/esd = 0.048 Maximum = 3.971 for tors H8A Max. shift = 0.114 A for H8A Max. dU = 0.000 for C27 Least-squares cycle 12 Maximum vector length = 511 Memory required = 5762 / 543952 wR2 = 0.1148 before cycle 12 for 7633 data and 421 / 421 parameters GooF = S = 1.094; Restrained GooF = 1.094 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0561 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.06687 0.00009 0.032 OSF Mean shift/esd = 0.038 Maximum = 2.955 for tors H8A Max. shift = 0.083 A for H8A Max. dU = 0.000 for C27 Least-squares cycle 13 Maximum vector length = 511 Memory required = 5762 / 543952 wR2 = 0.1146 before cycle 13 for 7633 data and 421 / 421 parameters GooF = S = 1.093; Restrained GooF = 1.093 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0561 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.06687 0.00009 0.014 OSF Mean shift/esd = 0.025 Maximum = 1.886 for tors H8A Max. shift = 0.052 A for H8C Max. dU = 0.000 for C22 Least-squares cycle 14 Maximum vector length = 511 Memory required = 5762 / 543952 wR2 = 0.1146 before cycle 14 for 7633 data and 421 / 421 parameters GooF = S = 1.093; Restrained GooF = 1.093 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0561 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.06687 0.00009 0.002 OSF Mean shift/esd = 0.014 Maximum = 1.127 for tors H8A Max. shift = 0.031 A for H8C Max. dU = 0.000 for C22 Least-squares cycle 15 Maximum vector length = 511 Memory required = 5762 / 543952 wR2 = 0.1146 before cycle 15 for 7633 data and 421 / 421 parameters GooF = S = 1.093; Restrained GooF = 1.093 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0561 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.06687 0.00009 0.002 OSF Mean shift/esd = 0.008 Maximum = 0.659 for tors H8A Max. shift = 0.018 A for H8C Max. dU = 0.000 for C22 Least-squares cycle 16 Maximum vector length = 511 Memory required = 5762 / 543952 wR2 = 0.1146 before cycle 16 for 7633 data and 421 / 421 parameters GooF = S = 1.092; Restrained GooF = 1.092 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0561 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.06687 0.00009 -0.001 OSF Mean shift/esd = 0.005 Maximum = 0.383 for tors H8A Max. shift = 0.011 A for H8C Max. dU = 0.000 for C22 Least-squares cycle 17 Maximum vector length = 511 Memory required = 5762 / 543952 wR2 = 0.1146 before cycle 17 for 7633 data and 421 / 421 parameters GooF = S = 1.092; Restrained GooF = 1.092 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0561 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.06687 0.00009 0.001 OSF Mean shift/esd = 0.003 Maximum = 0.222 for tors H8A Max. shift = 0.006 A for H8C Max. dU = 0.000 for C22 Least-squares cycle 18 Maximum vector length = 511 Memory required = 5762 / 543952 wR2 = 0.1146 before cycle 18 for 7633 data and 421 / 421 parameters GooF = S = 1.092; Restrained GooF = 1.092 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0561 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.06687 0.00009 0.000 OSF Mean shift/esd = 0.002 Maximum = 0.129 for tors H8A Max. shift = 0.004 A for H8C Max. dU = 0.000 for C22 Least-squares cycle 19 Maximum vector length = 511 Memory required = 5762 / 543952 wR2 = 0.1146 before cycle 19 for 7633 data and 421 / 421 parameters GooF = S = 1.092; Restrained GooF = 1.092 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0561 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.06687 0.00009 -0.001 OSF Mean shift/esd = 0.001 Maximum = 0.075 for tors H8A Max. shift = 0.002 A for H8C Max. dU = 0.000 for C22 Least-squares cycle 20 Maximum vector length = 511 Memory required = 5762 / 543952 wR2 = 0.1146 before cycle 20 for 7633 data and 421 / 421 parameters GooF = S = 1.092; Restrained GooF = 1.092 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0561 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.06687 0.00009 0.002 OSF Mean shift/esd = 0.001 Maximum = 0.044 for tors H8A Max. shift = 0.001 A for H8C Max. dU = 0.000 for C22 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 21 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2A 0.9926 -0.0551 0.1494 43 0.950 0.000 C2 C1 C3 H4A 0.6915 -0.0194 0.2663 43 0.950 0.000 C4 C5 C3 H7A 1.0593 0.0436 0.0773 137 0.980 0.000 C7 C1 H7A H7B 1.0033 0.1317 0.0851 137 0.980 0.000 C7 C1 H7A H7C 0.9238 0.0709 0.0365 137 0.980 0.000 C7 C1 H7A H8A 0.9772 -0.1291 0.2590 137 0.980 0.000 C8 C3 H8A H8B 0.8594 -0.1711 0.2142 137 0.980 0.000 C8 C3 H8A H8C 0.8275 -0.1340 0.2826 137 0.980 0.000 C8 C3 H8A H9A 0.5521 0.0921 0.2575 137 0.980 0.000 C9 C5 H9A H9B 0.5285 0.1249 0.1849 137 0.980 0.000 C9 C5 H9A H9C 0.6267 0.1712 0.2370 137 0.980 0.000 C9 C5 H9A H11A 0.8580 0.2518 0.1854 43 0.950 0.000 C11 C12 N1 H12A 0.7855 0.3505 0.1001 43 0.950 0.000 C12 C11 N2 H13A 0.6179 0.3453 -0.0038 23 0.990 0.000 C13 N2 C16 H13B 0.5588 0.2607 -0.0268 23 0.990 0.000 C13 N2 C16 H14A 0.8607 0.1697 -0.1691 43 0.950 0.000 C14 N3 C15 H15A 0.7065 0.1715 -0.0916 43 0.950 0.000 C15 C14 C16 H17A 0.8109 0.3990 -0.0539 43 0.950 0.000 C17 C16 C18 H18A 0.9626 0.3896 -0.1332 43 0.950 0.000 C18 N3 C17 H20A 0.4359 0.5856 0.1762 43 0.950 0.000 C20 C19 C21 H22A 0.1637 0.4852 0.2846 43 0.950 0.000 C22 C23 C21 H25A 0.5187 0.5216 0.0853 137 0.980 0.000 C25 C19 H25A H25B 0.4058 0.4684 0.0468 137 0.980 0.000 C25 C19 H25A H25C 0.5248 0.4271 0.0912 137 0.980 0.000 C25 C19 H25A H26A 0.2737 0.6048 0.3224 137 0.980 0.000 C26 C21 H26A H26B 0.2391 0.6588 0.2597 137 0.980 0.000 C26 C21 H26A H26C 0.3932 0.6414 0.2841 137 0.980 0.000 C26 C21 H26A H27A 0.0943 0.3512 0.2677 137 0.980 0.000 C27 C23 H27A H27B 0.1628 0.2986 0.2148 137 0.980 0.000 C27 C23 H27A H27C 0.0364 0.3541 0.1933 137 0.980 0.000 C27 C23 H27A H29A 0.4536 0.2754 0.1586 43 0.950 0.000 C29 C30 N4 H30A 0.3819 0.1777 0.0734 43 0.950 0.000 C30 C29 N5 H31A 0.0760 0.2487 -0.0237 23 0.990 0.000 C31 N5 C34 H31B 0.1454 0.1658 -0.0033 23 0.990 0.000 C31 N5 C34 H32A 0.3489 0.3504 -0.1764 43 0.950 0.000 C32 N6 C33 H33A 0.2175 0.3450 -0.0885 43 0.950 0.000 C33 C34 C32 H35A 0.3183 0.1145 -0.0671 43 0.950 0.000 C35 C34 C36 H36A 0.4499 0.1272 -0.1539 43 0.950 0.000 C36 N6 C35 i11488 in P2(1)/n ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq Ag1 0.61559 0.08038 0.00896 1.00000 0.02957 0.01576 0.02813 -0.00201 -0.00448 -0.00139 0.02483 0.00050 0.00003 0.00002 0.00001 0.00000 0.00017 0.00016 0.00018 0.00012 0.00013 0.00011 0.00010 Ag2 0.04703 0.41423 0.04536 1.00000 0.02246 0.01941 0.02966 -0.00152 0.00000 0.00471 0.02394 0.00051 0.00003 0.00002 0.00001 0.00000 0.00016 0.00016 0.00018 0.00012 0.00013 0.00011 0.00010 Cl1 0.60378 -0.01719 -0.07417 1.00000 0.03933 0.02004 0.03073 -0.00679 0.01619 -0.00643 0.02934 0.00177 0.00010 0.00005 0.00005 0.00000 0.00055 0.00047 0.00055 0.00041 0.00045 0.00041 0.00023 Cl2 -0.14618 0.49550 0.05973 1.00000 0.02499 0.01550 0.03233 0.00169 0.01109 0.00203 0.02381 0.00172 0.00009 0.00005 0.00005 0.00000 0.00045 0.00042 0.00054 0.00039 0.00040 0.00035 0.00021 N1 0.76124 0.16911 0.12185 1.00000 0.02157 0.01553 0.01872 0.00021 0.00849 -0.00144 0.01825 0.00528 0.00029 0.00017 0.00014 0.00000 0.00152 0.00150 0.00160 0.00128 0.00129 0.00124 0.00064 N2 0.69786 0.25422 0.04982 1.00000 0.02216 0.01605 0.01860 0.00264 0.00686 -0.00014 0.01866 0.00537 0.00029 0.00017 0.00015 0.00000 0.00151 0.00149 0.00159 0.00129 0.00129 0.00126 0.00064 N3 0.92667 0.27893 -0.15904 1.00000 0.02455 0.03625 0.02283 0.00405 0.00572 0.00163 0.02768 0.00610 0.00032 0.00020 0.00016 0.00000 0.00170 0.00195 0.00182 0.00155 0.00145 0.00150 0.00076 N4 0.29230 0.34386 0.11838 1.00000 0.02267 0.01534 0.01740 -0.00117 0.00692 0.00244 0.01819 0.00532 0.00029 0.00017 0.00014 0.00000 0.00155 0.00148 0.00157 0.00125 0.00129 0.00122 0.00064 N5 0.22975 0.25919 0.04557 1.00000 0.02160 0.02031 0.01598 -0.00443 0.00859 0.00078 0.01893 0.00530 0.00029 0.00017 0.00014 0.00000 0.00154 0.00158 0.00157 0.00129 0.00129 0.00126 0.00065 N6 0.41090 0.23970 -0.17397 1.00000 0.02239 0.03552 0.02016 -0.00166 0.00691 0.00034 0.02575 0.00574 0.00031 0.00020 0.00015 0.00000 0.00161 0.00194 0.00173 0.00151 0.00139 0.00145 0.00074 C1 0.89494 0.04845 0.13255 1.00000 0.01781 0.02559 0.02066 0.00054 0.00379 -0.00275 0.02123 0.00660 0.00036 0.00023 0.00018 0.00000 0.00177 0.00199 0.00198 0.00164 0.00153 0.00155 0.00080 C2 0.92117 -0.02308 0.16287 1.00000 0.02158 0.02227 0.02731 -0.00175 -0.00057 0.00213 0.02384 0.00659 0.00037 0.00022 0.00019 0.00000 0.00186 0.00197 0.00217 0.00169 0.00164 0.00157 0.00084 H2A 0.99257 -0.05514 0.14942 1.00000 0.02861 0.00000 0.00000 C3 0.84666 -0.04957 0.21226 1.00000 0.02593 0.01799 0.02478 0.00174 -0.00725 0.00003 0.02337 0.00662 0.00038 0.00022 0.00019 0.00000 0.00199 0.00185 0.00211 0.00164 0.00167 0.00158 0.00084 C4 0.74264 -0.00183 0.23202 1.00000 0.02645 0.02535 0.01692 0.00438 0.00030 -0.00990 0.02297 0.00632 0.00037 0.00022 0.00018 0.00000 0.00195 0.00199 0.00192 0.00163 0.00160 0.00163 0.00083 H4A 0.69155 -0.01942 0.26629 1.00000 0.02757 0.00000 0.00000 C5 0.71199 0.07044 0.20301 1.00000 0.01610 0.02215 0.01665 -0.00268 0.00220 -0.00285 0.01825 0.00620 0.00035 0.00021 0.00018 0.00000 0.00172 0.00187 0.00185 0.00152 0.00146 0.00143 0.00076 C6 0.78958 0.09419 0.15366 1.00000 0.02064 0.01299 0.01618 0.00259 0.00127 -0.00255 0.01661 0.00618 0.00036 0.00020 0.00017 0.00000 0.00177 0.00169 0.00180 0.00140 0.00145 0.00137 0.00074 C7 0.97767 0.07612 0.07804 1.00000 0.02519 0.03434 0.02785 0.00381 0.01005 0.00562 0.02872 0.00759 0.00039 0.00023 0.00020 0.00000 0.00204 0.00231 0.00223 0.00185 0.00176 0.00174 0.00092 H7A 1.05933 0.04359 0.07735 1.00000 0.04307 0.00000 0.00000 H7B 1.00327 0.13170 0.08508 1.00000 0.04307 0.00000 0.00000 H7C 0.92381 0.07094 0.03652 1.00000 0.04307 0.00000 0.00000 C8 0.88068 -0.12781 0.24490 1.00000 0.03890 0.02565 0.03693 0.01149 -0.00658 -0.00260 0.03431 0.00770 0.00044 0.00024 0.00022 0.00000 0.00244 0.00219 0.00258 0.00195 0.00203 0.00186 0.00103 H8A 0.97718 -0.12913 0.25905 1.00000 0.05147 0.00000 0.00000 H8B 0.85943 -0.17110 0.21422 1.00000 0.05147 0.00000 0.00000 H8C 0.82752 -0.13400 0.28261 1.00000 0.05147 0.00000 0.00000 C9 0.59460 0.11888 0.22230 1.00000 0.02362 0.02781 0.02648 -0.00212 0.01056 -0.00081 0.02553 0.00710 0.00037 0.00023 J#0.!))!9Z1 2>>!!O5.B#7 0.!019?>&95'00"? 37 >67>#"-1 1.66'&0 2+!$ 0.$7$01&/61 X!.0 > " '^7A?75 C10 29>**B'1 A?(*<)3 *"3*#9%.06$?0010:%3 02/#("< #.05 0.!%.860.46 C3 1!;? 6C8 1.5*.T' 1>8 0H&A3Q190.0!">) .1Z.R-30.4&52 !>;".," 843/3<)! 0>>5)$.=!?44 1.!>3*&YG2 " 76A< 2.47 P<$7 2.54 Y4 F20 2 1 0.7."&.6!.31540# (0>*!8 1>> 3.&.X,C 0>>!& 0>8%"'T#& 0>? +&W1760?<4/0Y17A 4137&$K!5 Sxrqweo~distancv}6retween `kpyj (incluugvr symmhgry ta{y~q|unts; 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251.140 L 158.040 250.180 L 157.600 249.380 L 156.960 248.760 L S 157.840 257.000 M 157.580 256.660 L 156.640 255.960 L 155.200 254.980 L 153.480 253.920 L 151.720 252.900 L 150.200 252.100 L 149.160 251.640 L 148.740 251.560 L S 156.360 248.380 M 155.780 248.240 L 155.100 248.360 L 154.340 248.680 L 153.560 249.220 L 152.760 249.980 L 151.980 250.880 L 151.260 251.920 L 150.600 253.040 L 150.060 254.220 L 149.640 255.400 L 149.360 256.540 L 149.220 257.580 L 149.260 258.520 L 149.440 259.280 L 149.760 259.840 L 150.240 260.200 L S 180.600 323.620 M 200.760 320.240 L S 200.740 319.900 M 180.120 323.420 L S 179.940 323.180 M 200.720 319.560 L S 200.740 319.200 M 179.860 322.900 L S 180.060 322.600 M 200.760 318.860 L S 180.060 322.600 M 179.860 322.900 L 179.940 323.180 L 180.120 323.420 L 180.600 323.620 L S 175.140 329.360 M 173.960 329.040 L 172.840 328.520 L 171.860 327.820 L 171.040 326.980 L 170.420 326.000 L 170.020 324.940 L 169.860 323.840 L 169.920 322.740 L 170.240 321.680 L 170.760 320.720 L 171.520 319.860 L 172.420 319.160 L 173.500 318.640 L 174.660 318.320 L 175.880 318.200 L 177.100 318.320 L 178.280 318.640 L 179.400 319.160 L 180.380 319.860 L 181.200 320.700 L 181.640 321.400 L S 182.380 323.980 M 182.320 324.940 L 182.000 326.000 L 181.480 326.960 L 180.740 327.820 L 179.820 328.520 L 178.760 329.040 L 177.600 329.360 L 176.380 329.480 L 175.140 329.360 L S 170.640 320.900 M 171.040 320.540 L 171.620 320.300 L 172.400 320.200 L 173.300 320.240 L 174.300 320.420 L 175.400 320.740 L 176.500 321.160 L 177.600 321.700 L 178.640 322.320 L 179.560 322.980 L S 180.220 323.540 M 180.400 323.700 L 181.040 324.400 L 181.500 325.100 L 181.740 325.740 L 181.780 326.300 L 181.600 326.780 L S 182.380 323.980 M 182.320 324.700 L 182.020 325.600 L 181.500 326.440 L 180.760 327.200 L 179.860 327.800 L 178.800 328.260 L 177.640 328.560 L 176.420 328.680 L 175.200 328.600 L 174.000 328.340 L 172.900 327.920 L 171.900 327.320 L 171.080 326.600 L 170.440 325.780 L 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324.220 L S 433.100 347.220 M 459.120 346.240 L S 459.140 345.920 M 432.640 346.960 L S 432.480 346.700 M 459.160 345.580 L S 459.220 345.240 M 432.460 346.420 L S 432.740 346.140 M 459.300 344.900 L S 432.740 346.140 M 432.460 346.420 L 432.480 346.700 L 432.640 346.960 L 433.100 347.220 L S 423.260 343.760 M 396.660 329.500 L S 396.540 329.800 M 423.200 344.060 L S 423.000 344.280 M 396.400 330.080 L S 396.240 330.360 M 422.780 344.500 L S 422.440 344.640 M 396.060 330.620 L S 422.440 344.640 M 422.780 344.500 L 423.000 344.280 L 423.200 344.060 L 423.260 343.760 L S 427.760 341.340 M 429.140 341.420 L 430.480 341.700 L 431.700 342.180 L 432.780 342.860 L 433.680 343.680 L 434.360 344.620 L 434.600 345.200 L S 434.840 347.780 M 434.840 347.820 L 434.460 348.860 L 433.820 349.840 L 432.980 350.700 L 431.920 351.420 L 430.700 351.960 L 429.400 352.300 L 428.020 352.440 L 426.640 352.360 L 425.300 352.080 L 424.080 351.600 L 422.980 350.940 L 422.100 350.120 L 421.420 349.160 L 421.000 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385.400 327.400 M 356.760 329.540 L S 356.940 329.240 M 385.380 327.060 L S 356.940 329.240 M 356.760 329.540 L 356.780 329.820 L 356.880 330.080 L 357.200 330.340 L S 346.540 328.460 M 347.020 327.100 L 347.720 325.860 L 348.620 324.760 L 349.700 323.880 L 350.920 323.240 L 352.220 322.860 L 353.560 322.760 L 354.880 322.920 L 356.120 323.380 L 357.260 324.080 L 358.240 325.020 L 359.020 326.160 L 359.500 327.280 L S 359.740 331.500 M 359.720 331.680 L 359.240 333.040 L 358.540 334.300 L 357.640 335.380 L 356.560 336.260 L 355.340 336.920 L 354.040 337.300 L 352.700 337.400 L 351.380 337.220 L 350.140 336.780 L 349.000 336.060 L 348.020 335.120 L 347.240 334.000 L 346.680 332.700 L 346.380 331.320 L 346.340 329.900 L 346.540 328.460 L S 350.460 323.440 M 349.380 324.140 L 348.440 325.060 L 347.700 326.180 L 347.140 327.440 L 346.820 328.800 L 346.740 330.220 L 346.920 331.640 L 347.320 332.980 L 347.960 334.220 L 348.780 335.300 L 349.780 336.180 L 350.900 336.820 L 352.120 337.200 L 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