+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + shelxl started at 22:55:35 on 12-Nov-2010 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008lsh011 in P2(1) CELL 0.71073 9.7285 13.3392 12.9849 90.000 103.791 90.000 ZERR 8.00 0.0005 0.0007 0.0005 0.000 0.003 0.000 LATT -1 SYMM - X, 1/2 + Y, - Z SFAC C H N O UNIT 64 64 16 24 V = 1636.48 F(000) = 752.0 Mu = 0.11 mm-1 Cell Wt = 1441.31 Rho = 1.463 MERG 2 OMIT -33.00 55.00 OMIT 0 1 4 OMIT 0 -1 4 OMIT 1 -1 3 OMIT -2 1 2 OMIT 1 1 3 OMIT 0 -1 2 DFIX 0.88 0.02 N1 H1N DFIX 0.88 0.02 N11 H11N DFIX 0.88 0.02 N21 H21N DFIX 0.88 0.02 N31 H31N FMAP 2 PLAN 5 SIZE 0.3 0.2 0.2 EQIV $1 x-1, y, z HTAB N1 O11 HTAB N11 O1_$1 HTAB N21 O31 HTAB N31 O21_$1 HTAB ACTA BOND $H L.S. 8 TEMP -153.00 WGHT 0.0626 0.5071 FVAR 0.95629 MOLE 1 C1 1 0.213157 0.346833 0.616884 11.00000 0.02143 0.01632 = 0.02158 0.00198 0.00586 0.00174 C2 1 0.340780 0.395614 0.616141 11.00000 0.02009 0.02245 = 0.02194 0.00080 0.00549 0.00178 AFIX 43 H2 2 0.419077 0.359600 0.602954 11.00000 -1.20000 AFIX 0 C3 1 0.348957 0.496752 0.635016 11.00000 0.02268 0.01758 = 0.02085 0.00299 0.00529 -0.00310 C4 1 0.239965 0.554703 0.655534 11.00000 0.03277 0.01460 = 0.02803 0.00305 0.00780 0.00190 AFIX 43 H4 2 0.249933 0.624894 0.667354 11.00000 -1.20000 AFIX 0 C5 1 0.114836 0.504313 0.657875 11.00000 0.02680 0.02165 = 0.03344 0.00192 0.01218 0.00631 AFIX 43 H5 2 0.037603 0.540438 0.672673 11.00000 -1.20000 AFIX 0 C6 1 0.102485 0.402888 0.638949 11.00000 0.02296 0.01896 = 0.03432 0.00192 0.01029 0.00189 AFIX 43 H6 2 0.016435 0.370154 0.640947 11.00000 -1.20000 AFIX 0 C7 1 0.279908 0.172397 0.579497 11.00000 0.02162 0.02122 = 0.02556 -0.00069 0.00896 -0.00018 C8 1 0.214499 0.071114 0.552007 11.00000 0.02546 0.02108 = 0.03950 -0.00707 0.00988 -0.00121 AFIX 137 H8A 2 0.251393 0.041378 0.495018 11.00000 -1.50000 H8B 2 0.111489 0.078074 0.528391 11.00000 -1.50000 H8C 2 0.237873 0.027709 0.614651 11.00000 -1.50000 AFIX 0 N1 3 0.186832 0.244990 0.592419 11.00000 0.01975 0.01674 = 0.03102 -0.00088 0.00740 -0.00090 N2 3 0.482815 0.548854 0.632392 11.00000 0.02642 0.02169 = 0.02630 0.00223 0.00450 -0.00540 O1 4 0.406975 0.188642 0.589866 11.00000 0.01855 0.02053 = 0.04384 -0.00017 0.00881 0.00142 O2 4 0.579227 0.498698 0.614350 11.00000 0.02801 0.03083 = 0.04093 -0.00157 0.01205 -0.00692 O3 4 0.489806 0.639021 0.649148 11.00000 0.03891 0.01812 = 0.05546 0.00105 0.00698 -0.00849 H1N 2 0.100760 0.227254 0.590233 11.00000 0.05655 MOLE 2 C11 1 -0.284493 0.015391 0.630138 11.00000 0.02346 0.01574 = 0.02024 -0.00052 0.00230 -0.00054 C12 1 -0.156733 -0.034093 0.633849 11.00000 0.02174 0.01607 = 0.02177 -0.00102 0.00418 -0.00109 AFIX 43 H12 2 -0.075824 0.001555 0.624936 11.00000 -1.20000 AFIX 0 C13 1 -0.151671 -0.136884 0.650949 11.00000 0.02400 0.01772 = 0.01958 -0.00073 0.00393 0.00137 C14 1 -0.265719 -0.193139 0.664249 11.00000 0.03369 0.01868 = 0.02387 0.00100 0.00722 -0.00404 AFIX 43 H14 2 -0.258621 -0.263687 0.674101 11.00000 -1.20000 AFIX 0 C15 1 -0.390972 -0.142483 0.662638 11.00000 0.02700 0.02661 = 0.02937 0.00264 0.00816 -0.00456 AFIX 43 H15 2 -0.471042 -0.178517 0.672589 11.00000 -1.20000 AFIX 0 C16 1 -0.399874 -0.040269 0.646697 11.00000 0.02002 0.02268 = 0.02746 -0.00118 0.00673 -0.00026 AFIX 43 H16 2 -0.485960 -0.006746 0.646918 11.00000 -1.20000 AFIX 0 C17 1 -0.214485 0.186809 0.589195 11.00000 0.02139 0.01868 = 0.02590 -0.00034 0.00726 0.00020 C18 1 -0.276160 0.289557 0.558609 11.00000 0.02417 0.01988 = 0.04219 0.00216 0.01113 0.00156 AFIX 137 H18A 2 -0.250670 0.334474 0.619932 11.00000 -1.50000 H18B 2 -0.379442 0.284593 0.535414 11.00000 -1.50000 H18C 2 -0.238373 0.316250 0.500641 11.00000 -1.50000 AFIX 0 N11 3 -0.308239 0.117596 0.606724 11.00000 0.01618 0.01600 = 0.03175 0.00148 0.00689 0.00287 N12 3 -0.018383 -0.188848 0.652107 11.00000 0.02859 0.01794 = 0.02804 -0.00133 0.00571 0.00613 O11 4 -0.088164 0.168833 0.596571 11.00000 0.01988 0.02201 = 0.04249 0.00050 0.00978 -0.00102 O12 4 0.079616 -0.140238 0.631382 11.00000 0.02518 0.03023 = 0.04936 0.00029 0.01269 0.00463 O13 4 -0.009010 -0.278529 0.674385 11.00000 0.04616 0.01911 = 0.05288 0.00560 0.01579 0.00867 H11N 2 -0.393037 0.138798 0.601728 11.00000 0.04149 MOLE 3 C21 1 0.249211 -0.066663 0.868864 11.00000 0.02485 0.01924 = 0.02290 -0.00002 0.00472 0.00072 C22 1 0.133848 -0.004487 0.864518 11.00000 0.02124 0.02019 = 0.02209 -0.00064 0.00560 -0.00072 AFIX 43 H22 2 0.046656 -0.031080 0.873060 11.00000 -1.20000 AFIX 0 C23 1 0.147790 0.096328 0.847634 11.00000 0.02137 0.02265 = 0.02312 -0.00271 0.00455 0.00130 C24 1 0.272241 0.140642 0.835639 11.00000 0.03087 0.02029 = 0.02677 0.00094 0.00822 -0.00431 AFIX 43 H24 2 0.279716 0.210970 0.826805 11.00000 -1.20000 AFIX 0 C25 1 0.385668 0.076152 0.837283 11.00000 0.02619 0.03460 = 0.02965 0.00026 0.00815 -0.00264 AFIX 43 H25 2 0.472053 0.102916 0.827297 11.00000 -1.20000 AFIX 0 C26 1 0.375183 -0.026685 0.853244 11.00000 0.02459 0.02921 = 0.02869 0.00152 0.00548 0.00385 AFIX 43 H26 2 0.453481 -0.069316 0.853478 11.00000 -1.20000 AFIX 0 C27 1 0.324964 -0.245071 0.902783 11.00000 0.02281 0.02632 = 0.03408 -0.00487 0.00414 0.00259 C28 1 0.275195 -0.343258 0.936514 11.00000 0.02985 0.02777 = 0.03724 0.00331 0.00796 0.00395 AFIX 137 H28A 2 0.237905 -0.384815 0.873842 11.00000 -1.50000 H28B 2 0.200475 -0.331326 0.974061 11.00000 -1.50000 H28C 2 0.354636 -0.377884 0.983711 11.00000 -1.50000 AFIX 0 N21 3 0.231232 -0.169591 0.892109 11.00000 0.02667 0.02359 = 0.03030 -0.00026 0.00763 0.00138 N22 3 0.024259 0.161321 0.843739 11.00000 0.03220 0.02481 = 0.02680 -0.00115 0.00433 0.00767 O21 4 0.444795 -0.235069 0.886907 11.00000 0.02624 0.03129 = 0.06736 0.00397 0.02021 0.00157 O22 4 -0.085296 0.123696 0.855776 11.00000 0.02861 0.03202 = 0.04969 -0.00009 0.01285 0.00484 O23 4 0.037896 0.252417 0.828514 11.00000 0.04508 0.02073 = 0.04811 0.00306 0.01283 0.01035 H21N 2 0.140749 -0.189850 0.905172 11.00000 0.02860 MOLE 4 C31 1 -0.245470 -0.389357 0.883083 11.00000 0.02436 0.02110 = 0.02336 0.00207 0.00493 0.00143 C32 1 -0.359637 -0.452116 0.884725 11.00000 0.02148 0.02504 = 0.02276 0.00442 0.00540 0.00165 AFIX 43 H32 2 -0.444820 -0.426044 0.897683 11.00000 -1.20000 AFIX 0 C33 1 -0.345222 -0.553617 0.866904 11.00000 0.02777 0.01633 = 0.02394 0.00367 0.00358 -0.00184 C34 1 -0.223468 -0.596234 0.849396 11.00000 0.03377 0.02143 = 0.02660 0.00131 0.00690 0.00209 AFIX 43 H34 2 -0.216255 -0.666470 0.839764 11.00000 -1.20000 AFIX 0 C35 1 -0.113324 -0.532901 0.846489 11.00000 0.02646 0.02891 = 0.03687 0.00118 0.01057 0.00741 AFIX 43 H35 2 -0.028728 -0.560042 0.833554 11.00000 -1.20000 AFIX 0 C36 1 -0.121848 -0.430722 0.861837 11.00000 0.02240 0.03073 = 0.03171 0.00267 0.00885 0.00021 AFIX 43 H36 2 -0.044541 -0.388520 0.858066 11.00000 -1.20000 AFIX 0 C37 1 -0.166782 -0.212579 0.919525 11.00000 0.02125 0.03250 = 0.02914 0.00295 0.00767 0.00011 C38 1 -0.221073 -0.111080 0.941811 11.00000 0.02466 0.02025 = 0.03785 -0.00229 0.00720 -0.00091 AFIX 137 H38A 2 -0.150917 -0.078191 0.998486 11.00000 -1.50000 H38B 2 -0.309955 -0.119044 0.963972 11.00000 -1.50000 H38C 2 -0.237671 -0.069966 0.877476 11.00000 -1.50000 AFIX 0 N31 3 -0.263989 -0.287644 0.903889 11.00000 0.02600 0.01859 = 0.03089 0.00159 0.00998 0.00088 N32 3 -0.466220 -0.619041 0.868220 11.00000 0.02693 0.03021 = 0.03010 0.00349 0.00409 -0.00444 O31 4 -0.042465 -0.226328 0.916804 11.00000 0.02320 0.03008 = 0.05118 0.00092 0.01002 -0.00033 O32 4 -0.573939 -0.582075 0.885663 11.00000 0.03100 0.04267 = 0.04347 -0.00069 0.01350 -0.00905 O33 4 -0.454751 -0.709718 0.851170 11.00000 0.04649 0.02435 = 0.06262 -0.00015 0.00763 -0.00796 H31N 2 -0.350921 -0.255023 0.905432 11.00000 0.05707 HKLF 4 Covalent radii and connectivity table for 2008lsh011 in P2(1) C 0.770 H 0.320 N 0.700 O 0.660 C1 - C6 C2 N1 C2 - C3 C1 C3 - C2 C4 N2 C4 - C3 C5 C5 - C6 C4 C6 - C5 C1 C7 - O1 N1 C8 C8 - C7 N1 - C7 C1 N2 - O2 O3 C3 O1 - C7 O2 - N2 O3 - N2 C11 - C12 N11 C16 C12 - C13 C11 C13 - C14 C12 N12 C14 - C13 C15 C15 - C16 C14 C16 - C15 C11 C17 - O11 N11 C18 C18 - C17 N11 - C17 C11 N12 - O13 O12 C13 O11 - C17 O12 - N12 O13 - N12 C21 - C22 C26 N21 C22 - C23 C21 C23 - C22 C24 N22 C24 - C23 C25 C25 - C26 C24 C26 - C25 C21 C27 - O21 N21 C28 C28 - C27 N21 - C27 C21 N22 - O22 O23 C23 O21 - C27 O22 - N22 O23 - N22 C31 - C32 N31 C36 C32 - C33 C31 C33 - C34 C32 N32 C34 - C35 C33 C35 - C34 C36 C36 - C35 C31 C37 - O31 N31 C38 C38 - C37 N31 - C37 C31 N32 - O32 O33 C33 O31 - C37 O32 - N32 O33 - N32 Operators for generating equivalent atoms: $1 x-1, y, z Floating origin restraints generated h k l Fo^2 Sigma Why rejected 0 9 0 21.49 5.36 observed but should be systematically absent 24487 Reflections read, of which 40 rejected -12 =< h =< 12, -17 =< k =< 17, -16 =< l =< 16, Max. 2-theta = 55.00 1 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) -5 -4 14 17.37 1.56 3 8.38 -1 -2 15 17.41 2.08 2 11.36 2 Inconsistent equivalents 7352 Unique reflections, of which 0 suppressed R(int) = 0.0426 R(sigma) = 0.0490 Friedel opposites not merged Maximum memory for data reduction = 4136 / 73298 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 = 5423 / 643536 wR2 = 0.1274 before cycle 1 for 7352 data and 489 / 489 parameters Disagreeable restraints before cycle 1 Observed Target Error Sigma Restraint 0.9736 0.8800 0.0936 0.0200 DFIX N21 H21N 0.9555 0.8800 0.0755 0.0200 DFIX N31 H31N Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.061 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.072; Restrained GooF = 1.074 for 5 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0626 * P )^2 + 0.51 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.95585 0.00162 -0.273 OSF Mean shift/esd = 0.037 Maximum = -0.273 for OSF Max. shift = 0.006 A for H21N Max. dU = 0.000 for H21N Least-squares cycle 2 Maximum vector length = 511 Memory required = 5423 / 643536 wR2 = 0.1273 before cycle 2 for 7352 data and 489 / 489 parameters Disagreeable restraints before cycle 2 Observed Target Error Sigma Restraint 0.9755 0.8800 0.0955 0.0200 DFIX N21 H21N 0.9572 0.8800 0.0772 0.0200 DFIX N31 H31N Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.063 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.071; Restrained GooF = 1.074 for 5 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0626 * P )^2 + 0.51 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.95565 0.00162 -0.120 OSF Mean shift/esd = 0.014 Maximum = -0.120 for OSF Max. shift = 0.001 A for H21N Max. dU = 0.000 for H31N Least-squares cycle 3 Maximum vector length = 511 Memory required = 5423 / 643536 wR2 = 0.1273 before cycle 3 for 7352 data and 489 / 489 parameters Disagreeable restraints before cycle 3 Observed Target Error Sigma Restraint 0.9767 0.8800 0.0967 0.0200 DFIX N21 H21N 0.9579 0.8800 0.0779 0.0200 DFIX N31 H31N Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.063 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.071; Restrained GooF = 1.074 for 5 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0626 * P )^2 + 0.51 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.95565 0.00162 0.000 OSF Mean shift/esd = 0.002 Maximum = -0.021 for tors H8A Max. shift = 0.001 A for H21N Max. dU = 0.000 for H21N Least-squares cycle 4 Maximum vector length = 511 Memory required = 5423 / 643536 wR2 = 0.1273 before cycle 4 for 7352 data and 489 / 489 parameters Disagreeable restraints before cycle 4 Observed Target Error Sigma Restraint 0.9772 0.8800 0.0972 0.0200 DFIX N21 H21N 0.9582 0.8800 0.0782 0.0200 DFIX N31 H31N Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.064 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.071; Restrained GooF = 1.074 for 5 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0626 * P )^2 + 0.51 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.95566 0.00162 0.005 OSF Mean shift/esd = 0.001 Maximum = -0.012 for x H21N Max. shift = 0.000 A for H21N Max. dU = 0.000 for H1N Least-squares cycle 5 Maximum vector length = 511 Memory required = 5423 / 643536 wR2 = 0.1273 before cycle 5 for 7352 data and 489 / 489 parameters Disagreeable restraints before cycle 5 Observed Target Error Sigma Restraint 0.9775 0.8800 0.0975 0.0200 DFIX N21 H21N 0.9583 0.8800 0.0783 0.0200 DFIX N31 H31N Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.064 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.071; Restrained GooF = 1.074 for 5 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0626 * P )^2 + 0.51 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.95566 0.00162 -0.001 OSF Mean shift/esd = 0.000 Maximum = -0.004 for x H21N Max. shift = 0.000 A for H21N Max. dU = 0.000 for H1N Least-squares cycle 6 Maximum vector length = 511 Memory required = 5423 / 643536 wR2 = 0.1273 before cycle 6 for 7352 data and 489 / 489 parameters Disagreeable restraints before cycle 6 Observed Target Error Sigma Restraint 0.9775 0.8800 0.0975 0.0200 DFIX N21 H21N 0.9583 0.8800 0.0783 0.0200 DFIX N31 H31N Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.064 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.071; Restrained GooF = 1.074 for 5 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0626 * P )^2 + 0.51 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.95566 0.00162 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.002 for tors H8A Max. shift = 0.000 A for H21N Max. dU = 0.000 for H1N Least-squares cycle 7 Maximum vector length = 511 Memory required = 5423 / 643536 wR2 = 0.1273 before cycle 7 for 7352 data and 489 / 489 parameters Disagreeable restraints before cycle 7 Observed Target Error Sigma Restraint 0.9776 0.8800 0.0976 0.0200 DFIX N21 H21N 0.9583 0.8800 0.0783 0.0200 DFIX N31 H31N Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.064 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.071; Restrained GooF = 1.074 for 5 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0626 * P )^2 + 0.51 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.95566 0.00162 0.001 OSF Mean shift/esd = 0.000 Maximum = -0.001 for x H21N Max. shift = 0.000 A for H21N Max. dU = 0.000 for H1N Least-squares cycle 8 Maximum vector length = 511 Memory required = 5423 / 643536 wR2 = 0.1273 before cycle 8 for 7352 data and 489 / 489 parameters Disagreeable restraints before cycle 8 Observed Target Error Sigma Restraint 0.9776 0.8800 0.0976 0.0200 DFIX N21 H21N 0.9583 0.8800 0.0783 0.0200 DFIX N31 H31N Summary of restraints applied in cycle 8 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.064 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.071; Restrained GooF = 1.074 for 5 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0626 * P )^2 + 0.51 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.95566 0.00162 -0.001 OSF Mean shift/esd = 0.000 Maximum = -0.001 for OSF Max. shift = 0.000 A for H21N Max. dU = 0.000 for H1N No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 9 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.4191 0.3596 0.6030 43 0.950 0.000 C2 C3 C1 H4 0.2499 0.6249 0.6673 43 0.950 0.000 C4 C3 C5 H5 0.0376 0.5404 0.6727 43 0.950 0.000 C5 C6 C4 H6 0.0164 0.3701 0.6409 43 0.950 0.000 C6 C5 C1 H8A 0.2512 0.0415 0.4949 137 0.980 0.000 C8 C7 H8A H8B 0.1115 0.0780 0.5286 137 0.980 0.000 C8 C7 H8A H8C 0.2381 0.0276 0.6146 137 0.980 0.000 C8 C7 H8A H12 -0.0758 0.0016 0.6249 43 0.950 0.000 C12 C13 C11 H14 -0.2586 -0.2637 0.6741 43 0.950 0.000 C14 C13 C15 H15 -0.4710 -0.1785 0.6725 43 0.950 0.000 C15 C16 C14 H16 -0.4860 -0.0067 0.6469 43 0.950 0.000 C16 C15 C11 H18A -0.2507 0.3345 0.6200 137 0.980 0.000 C18 C17 H18A H18B -0.3794 0.2846 0.5354 137 0.980 0.000 C18 C17 H18A H18C -0.2384 0.3163 0.5007 137 0.980 0.000 C18 C17 H18A H22 0.0467 -0.0311 0.8731 43 0.950 0.000 C22 C23 C21 H24 0.2797 0.2110 0.8268 43 0.950 0.000 C24 C23 C25 H25 0.4721 0.1029 0.8273 43 0.950 0.000 C25 C26 C24 H26 0.4535 -0.0693 0.8535 43 0.950 0.000 C26 C25 C21 H28A 0.2379 -0.3848 0.8739 137 0.980 0.000 C28 C27 H28A H28B 0.2005 -0.3313 0.9741 137 0.980 0.000 C28 C27 H28A H28C 0.3546 -0.3779 0.9837 137 0.980 0.000 C28 C27 H28A H32 -0.4448 -0.4260 0.8977 43 0.950 0.000 C32 C33 C31 H34 -0.2163 -0.6665 0.8397 43 0.950 0.000 C34 C35 C33 H35 -0.0287 -0.5601 0.8336 43 0.950 0.000 C35 C34 C36 H36 -0.0446 -0.3885 0.8580 43 0.950 0.000 C36 C35 C31 H38A -0.1508 -0.0781 0.9984 137 0.980 0.000 C38 C37 H38A H38B -0.3098 -0.1190 0.9641 137 0.980 0.000 C38 C37 H38A H38C -0.2379 -0.0700 0.8774 137 0.980 0.000 C38 C37 H38A 2008lsh011 in P2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.21317 0.34685 0.61688 1.00000 0.02137 0.01637 0.02140 0.00201 0.00592 0.00175 0.01958 0.00457 0.00025 0.00018 0.00018 0.00000 0.00125 0.00119 0.00116 0.00088 0.00089 0.00093 0.00049 C2 0.34077 0.39563 0.61614 1.00000 0.02001 0.02236 0.02181 0.00080 0.00549 0.00170 0.02131 0.00460 0.00025 0.00019 0.00018 0.00000 0.00120 0.00137 0.00120 0.00092 0.00090 0.00100 0.00052 H2 0.41907 0.35963 0.60296 1.00000 0.02557 0.00000 0.00000 C3 0.34893 0.49676 0.63501 1.00000 0.02257 0.01757 0.02074 0.00301 0.00525 -0.00317 0.02028 0.00458 0.00025 0.00019 0.00018 0.00000 0.00126 0.00127 0.00114 0.00088 0.00089 0.00093 0.00051 C4 0.23997 0.55468 0.65552 1.00000 0.03268 0.01457 0.02785 0.00303 0.00775 0.00182 0.02494 0.00492 0.00027 0.00020 0.00019 0.00000 0.00142 0.00121 0.00129 0.00097 0.00101 0.00107 0.00055 H4 0.24994 0.62487 0.66733 1.00000 0.02993 0.00000 0.00000 C5 0.11485 0.50431 0.65787 1.00000 0.02682 0.02156 0.03342 0.00189 0.01222 0.00635 0.02642 0.00515 0.00028 0.00020 0.00020 0.00000 0.00137 0.00138 0.00136 0.00103 0.00101 0.00104 0.00056 H5 0.03762 0.54044 0.67267 1.00000 0.03170 0.00000 0.00000 C6 0.10248 0.40288 0.63894 1.00000 0.02291 0.01889 0.03418 0.00188 0.01032 0.00185 0.02474 0.00505 0.00027 0.00019 0.00021 0.00000 0.00128 0.00135 0.00135 0.00098 0.00101 0.00102 0.00055 H6 0.01643 0.37014 0.64093 1.00000 0.02968 0.00000 0.00000 C7 0.27991 0.17240 0.57949 1.00000 0.02169 0.02128 0.02542 -0.00067 0.00895 -0.00007 0.02223 0.00458 0.00025 0.00019 0.00018 0.00000 0.00124 0.00130 0.00118 0.00096 0.00091 0.00101 0.00050 C8 0.21451 0.07111 0.55202 1.00000 0.02549 0.02089 0.03931 -0.00698 0.00993 -0.00114 0.02819 0.00484 0.00027 0.00020 0.00021 0.00000 0.00132 0.00139 0.00143 0.00107 0.00105 0.00105 0.00056 H8A 0.25119 0.04145 0.49489 1.00000 0.04228 0.00000 0.00000 H8B 0.11147 0.07804 0.52860 1.00000 0.04228 0.00000 0.00000 H8C 0.23812 0.02765 0.61461 1.00000 0.04228 0.00000 0.00000 N1 0.18683 0.24499 0.59242 1.00000 0.01974 0.01664 0.03091 -0.00092 0.00741 -0.00093 0.02220 0.00389 0.00022 0.00016 0.00016 0.00000 0.00110 0.00108 0.00107 0.00079 0.00085 0.00086 0.00044 N2 0.48280 0.54886 0.63240 1.00000 0.02638 0.02158 0.02614 0.00219 0.00445 -0.00546 0.02501 0.00400 0.00023 0.00017 0.00016 0.00000 0.00116 0.00118 0.00108 0.00083 0.00083 0.00089 0.00047 O1 0.40698 0.18865 0.58985 1.00000 0.01851 0.02051 0.04368 -0.00013 0.00878 0.00138 0.02734 0.00332 0.00017 0.00013 0.00014 0.00000 0.00090 0.00092 0.00103 0.00077 0.00071 0.00073 0.00039 O2 0.57924 0.49870 0.61435 1.00000 0.02795 0.03079 0.04090 -0.00158 0.01203 -0.00685 0.03257 0.00361 0.00020 0.00014 0.00015 0.00000 0.00100 0.00111 0.00106 0.00085 0.00080 0.00084 0.00045 O3 0.48980 0.63904 0.64916 1.00000 0.03882 0.01803 0.05533 0.00102 0.00692 -0.00841 0.03812 0.00379 0.00022 0.00015 0.00017 0.00000 0.00117 0.00104 0.00126 0.00086 0.00093 0.00083 0.00049 H1N 0.10087 0.22691 0.59009 1.00000 0.05670 0.05514 0.00227 0.00290 0.00267 0.00000 0.01109 C11 -0.28449 0.01539 0.63013 1.00000 0.02340 0.01563 0.02013 -0.00054 0.00224 -0.00049 0.02022 0.00439 0.00025 0.00019 0.00017 0.00000 0.00125 0.00114 0.00114 0.00089 0.00088 0.00098 0.00049 C12 -0.15673 -0.03409 0.63384 1.00000 0.02166 0.01609 0.02164 -0.00099 0.00412 -0.00111 0.01997 0.00443 0.00025 0.00018 0.00018 0.00000 0.00122 0.00124 0.00114 0.00087 0.00089 0.00094 0.00049 H12 -0.07582 0.00156 0.62493 1.00000 0.02396 0.00000 0.00000 C13 -0.15166 -0.13688 0.65094 1.00000 0.02387 0.01755 0.01952 -0.00079 0.00393 0.00139 0.02052 0.00452 0.00026 0.00019 0.00018 0.00000 0.00131 0.00128 0.00114 0.00088 0.00092 0.00095 0.00052 C14 -0.26575 -0.19314 0.66426 1.00000 0.03360 0.01868 0.02378 0.00101 0.00722 -0.00405 0.02529 0.00484 0.00027 0.00021 0.00019 0.00000 0.00146 0.00123 0.00125 0.00098 0.00100 0.00109 0.00054 H14 -0.25864 -0.26368 0.67415 1.00000 0.03035 0.00000 0.00000 C15 -0.39097 -0.14250 0.66262 1.00000 0.02683 0.02644 0.02928 0.00256 0.00818 -0.00451 0.02727 0.00506 0.00029 0.00021 0.00020 0.00000 0.00142 0.00145 0.00133 0.00107 0.00103 0.00108 0.00057 H15 -0.47105 -0.17853 0.67255 1.00000 0.03272 0.00000 0.00000 C16 -0.39987 -0.04027 0.64667 1.00000 0.01996 0.02260 0.02736 -0.00115 0.00672 -0.00026 0.02312 0.00467 0.00026 0.00019 0.00019 0.00000 0.00123 0.00135 0.00127 0.00094 0.00094 0.00099 0.00052 H16 -0.48596 -0.00675 0.64687 1.00000 0.02775 0.00000 0.00000 C17 -0.21447 0.18680 0.58920 1.00000 0.02137 0.01869 0.02579 -0.00033 0.00731 0.00019 0.02167 0.00463 0.00025 0.00019 0.00018 0.00000 0.00124 0.00124 0.00117 0.00094 0.00090 0.00100 0.00049 C18 -0.27616 0.28957 0.55863 1.00000 0.02416 0.01988 0.04208 0.00224 0.01116 0.00151 0.02816 0.00520 0.00028 0.00019 0.00022 0.00000 0.00136 0.00141 0.00153 0.00106 0.00110 0.00102 0.00058 H18A -0.25069 0.33447 0.61997 1.00000 0.04223 0.00000 0.00000 H18B -0.37944 0.28460 0.53542 1.00000 0.04223 0.00000 0.00000 H18C -0.23836 0.31628 0.50068 1.00000 0.04223 0.00000 0.00000 N11 -0.30823 0.11759 0.60673 1.00000 0.01622 0.01590 0.03156 0.00151 0.00688 0.00281 0.02103 0.00393 0.00021 0.00015 0.00016 0.00000 0.00104 0.00108 0.00107 0.00078 0.00081 0.00082 0.00043 N12 -0.01838 -0.18884 0.65210 1.00000 0.02856 0.01804 0.02794 -0.00131 0.00574 0.00620 0.02501 0.00409 0.00022 0.00016 0.00016 0.00000 0.00120 0.00112 0.00110 0.00086 0.00086 0.00092 0.00047 O11 -0.08817 0.16883 0.59658 1.00000 0.01984 0.02195 0.04241 0.00055 0.00976 -0.00104 0.02767 0.00335 0.00018 0.00014 0.00014 0.00000 0.00091 0.00096 0.00102 0.00077 0.00072 0.00077 0.00040 O12 0.07962 -0.14023 0.63139 1.00000 0.02507 0.03018 0.04935 0.00034 0.01276 0.00462 0.03421 0.00394 0.00021 0.00015 0.00016 0.00000 0.00103 0.00111 0.00115 0.00087 0.00083 0.00083 0.00046 O13 -0.00903 -0.27852 0.67438 1.00000 0.04613 0.01902 0.05281 0.00558 0.01571 0.00867 0.03866 0.00400 0.00022 0.00015 0.00016 0.00000 0.00127 0.00101 0.00126 0.00085 0.00097 0.00088 0.00050 H11N -0.39317 0.13868 0.60175 1.00000 0.04193 0.05971 0.00220 0.00265 0.00239 0.00000 0.00951 C21 0.24921 -0.06665 0.86885 1.00000 0.02476 0.01921 0.02277 -0.00009 0.00472 0.00078 0.02241 0.00469 0.00026 0.00020 0.00018 0.00000 0.00128 0.00126 0.00119 0.00095 0.00095 0.00103 0.00052 C22 0.13386 -0.00450 0.86452 1.00000 0.02112 0.02008 0.02208 -0.00058 0.00556 -0.00070 0.02102 0.00457 0.00026 0.00019 0.00018 0.00000 0.00117 0.00125 0.00114 0.00088 0.00088 0.00094 0.00048 H22 0.04668 -0.03110 0.87308 1.00000 0.02523 0.00000 0.00000 C23 0.14782 0.09633 0.84762 1.00000 0.02131 0.02255 0.02302 -0.00265 0.00453 0.00134 0.02242 0.00458 0.00026 0.00020 0.00018 0.00000 0.00120 0.00127 0.00121 0.00092 0.00090 0.00099 0.00051 C24 0.27222 0.14064 0.83563 1.00000 0.03081 0.02019 0.02663 0.00090 0.00819 -0.00428 0.02565 0.00487 0.00027 0.00020 0.00019 0.00000 0.00139 0.00131 0.00129 0.00096 0.00102 0.00105 0.00055 H24 0.27967 0.21097 0.82679 1.00000 0.03078 0.00000 0.00000 C25 0.38568 0.07616 0.83728 1.00000 0.02607 0.03457 0.02959 0.00027 0.00814 -0.00269 0.02983 0.00514 0.00028 0.00023 0.00019 0.00000 0.00135 0.00161 0.00135 0.00111 0.00102 0.00115 0.00059 H25 0.47206 0.10293 0.82729 1.00000 0.03579 0.00000 0.00000 C26 0.37521 -0.02668 0.85325 1.00000 0.02464 0.02913 0.02852 0.00153 0.00547 0.00392 0.02758 0.00501 0.00027 0.00021 0.00020 0.00000 0.00131 0.00149 0.00136 0.00104 0.00101 0.00112 0.00057 H26 0.45352 -0.06931 0.85352 1.00000 0.03309 0.00000 0.00000 C27 0.32495 -0.24509 0.90277 1.00000 0.02284 0.02646 0.03395 -0.00481 0.00415 0.00253 0.02819 0.00489 0.00027 0.00021 0.00020 0.00000 0.00130 0.00144 0.00133 0.00105 0.00102 0.00113 0.00056 C28 0.27519 -0.34327 0.93652 1.00000 0.02983 0.02756 0.03724 0.00333 0.00790 0.00396 0.03156 0.00547 0.00030 0.00021 0.00022 0.00000 0.00141 0.00153 0.00147 0.00110 0.00111 0.00118 0.00061 H28A 0.23789 -0.38483 0.87386 1.00000 0.04734 0.00000 0.00000 H28B 0.20048 -0.33133 0.97408 1.00000 0.04734 0.00000 0.00000 H28C 0.35464 -0.37789 0.98372 1.00000 0.04734 0.00000 0.00000 N21 0.23121 -0.16961 0.89211 1.00000 0.02664 0.02364 0.03024 -0.00026 0.00759 0.00147 0.02670 0.00418 0.00024 0.00016 0.00017 0.00000 0.00120 0.00121 0.00115 0.00083 0.00089 0.00095 0.00048 N22 0.02426 0.16130 0.84375 1.00000 0.03211 0.02481 0.02670 -0.00123 0.00427 0.00771 0.02833 0.00416 0.00024 0.00017 0.00016 0.00000 0.00125 0.00121 0.00113 0.00086 0.00090 0.00097 0.00050 O21 0.44481 -0.23506 0.88691 1.00000 0.02621 0.03134 0.06717 0.00387 0.02018 0.00156 0.04005 0.00412 0.00020 0.00016 0.00017 0.00000 0.00101 0.00113 0.00132 0.00100 0.00094 0.00089 0.00049 O22 -0.08528 0.12367 0.85580 1.00000 0.02858 0.03201 0.04958 -0.00008 0.01284 0.00477 0.03613 0.00393 0.00020 0.00016 0.00016 0.00000 0.00105 0.00111 0.00120 0.00087 0.00087 0.00088 0.00047 O23 0.03787 0.25241 0.82850 1.00000 0.04508 0.02064 0.04808 0.00307 0.01284 0.01032 0.03764 0.00397 0.00022 0.00014 0.00016 0.00000 0.00122 0.00104 0.00115 0.00081 0.00092 0.00087 0.00048 H21N 0.14039 -0.19026 0.90507 1.00000 0.02772 0.04904 0.00215 0.00236 0.00207 0.00000 0.00742 C31 -0.24547 -0.38936 0.88309 1.00000 0.02432 0.02095 0.02334 0.00204 0.00490 0.00148 0.02300 0.00469 0.00027 0.00018 0.00019 0.00000 0.00128 0.00139 0.00120 0.00090 0.00094 0.00102 0.00053 C32 -0.35961 -0.45211 0.88472 1.00000 0.02139 0.02503 0.02268 0.00446 0.00536 0.00167 0.02302 0.00471 0.00026 0.00020 0.00018 0.00000 0.00125 0.00133 0.00118 0.00096 0.00092 0.00101 0.00052 H32 -0.44479 -0.42602 0.89767 1.00000 0.02762 0.00000 0.00000 C33 -0.34525 -0.55361 0.86691 1.00000 0.02760 0.01630 0.02382 0.00367 0.00354 -0.00183 0.02301 0.00476 0.00027 0.00018 0.00019 0.00000 0.00134 0.00127 0.00122 0.00090 0.00098 0.00099 0.00053 C34 -0.22347 -0.59622 0.84939 1.00000 0.03357 0.02135 0.02658 0.00133 0.00690 0.00219 0.02721 0.00502 0.00028 0.00021 0.00020 0.00000 0.00146 0.00141 0.00133 0.00097 0.00104 0.00109 0.00058 H34 -0.21628 -0.66645 0.83972 1.00000 0.03265 0.00000 0.00000 C35 -0.11330 -0.53293 0.84651 1.00000 0.02636 0.02878 0.03668 0.00118 0.01054 0.00737 0.03010 0.00539 0.00028 0.00021 0.00021 0.00000 0.00137 0.00153 0.00152 0.00109 0.00110 0.00113 0.00060 H35 -0.02869 -0.56008 0.83362 1.00000 0.03611 0.00000 0.00000 C36 -0.12186 -0.43073 0.86184 1.00000 0.02234 0.03067 0.03165 0.00275 0.00882 0.00026 0.02781 0.00526 0.00028 0.00022 0.00020 0.00000 0.00126 0.00156 0.00133 0.00107 0.00100 0.00108 0.00056 H36 -0.04457 -0.38852 0.85804 1.00000 0.03338 0.00000 0.00000 C37 -0.16679 -0.21258 0.91953 1.00000 0.02121 0.03270 0.02907 0.00301 0.00764 0.00008 0.02738 0.00494 0.00026 0.00020 0.00020 0.00000 0.00128 0.00156 0.00126 0.00105 0.00098 0.00108 0.00057 C38 -0.22106 -0.11107 0.94181 1.00000 0.02460 0.02023 0.03781 -0.00227 0.00718 -0.00094 0.02759 0.00485 0.00026 0.00019 0.00021 0.00000 0.00128 0.00131 0.00145 0.00101 0.00103 0.00107 0.00055 H38A -0.15081 -0.07812 0.99837 1.00000 0.04139 0.00000 0.00000 H38B -0.30984 -0.11903 0.96412 1.00000 0.04139 0.00000 0.00000 H38C -0.23786 -0.07001 0.87743 1.00000 0.04139 0.00000 0.00000 N31 -0.26400 -0.28765 0.90389 1.00000 0.02602 0.01853 0.03082 0.00157 0.01000 0.00085 0.02458 0.00411 0.00023 0.00016 0.00016 0.00000 0.00114 0.00114 0.00109 0.00083 0.00086 0.00091 0.00046 N32 -0.46619 -0.61906 0.86823 1.00000 0.02687 0.03036 0.03001 0.00355 0.00408 -0.00439 0.02953 0.00427 0.00023 0.00019 0.00017 0.00000 0.00121 0.00129 0.00118 0.00092 0.00090 0.00099 0.00051 O31 -0.04245 -0.22634 0.91681 1.00000 0.02319 0.03016 0.05120 0.00083 0.01003 -0.00032 0.03465 0.00365 0.00019 0.00015 0.00015 0.00000 0.00099 0.00108 0.00114 0.00087 0.00082 0.00082 0.00045 O32 -0.57395 -0.58204 0.88566 1.00000 0.03087 0.04267 0.04336 -0.00072 0.01347 -0.00898 0.03819 0.00387 0.00020 0.00017 0.00016 0.00000 0.00109 0.00124 0.00117 0.00092 0.00088 0.00094 0.00049 O33 -0.45476 -0.70970 0.85116 1.00000 0.04647 0.02430 0.06250 -0.00018 0.00760 -0.00798 0.04533 0.00406 0.00024 0.00016 0.00018 0.00000 0.00134 0.00120 0.00140 0.00092 0.00105 0.00093 0.00054 H31N -0.35118 -0.25493 0.90544 1.00000 0.05644 0.06786 0.00258 0.00269 0.00271 0.00000 0.01065 Final Structure Factor Calculation for 2008lsh011 in P2(1) Total number of l.s. parameters = 489 Maximum vector length = 511 Memory required = 4936 / 25046 wR2 = 0.1273 before cycle 9 for 7352 data and 2 / 489 parameters Disagreeable restraints before cycle 9 Observed Target Error Sigma Restraint 0.9776 0.8800 0.0976 0.0200 DFIX N21 H21N 0.9583 0.8800 0.0783 0.0200 DFIX N31 H31N Summary of restraints applied in cycle 9 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.064 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.071; Restrained GooF = 1.074 for 5 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0626 * P )^2 + 0.51 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0499 for 6174 Fo > 4sig(Fo) and 0.0647 for all 7352 data wR2 = 0.1273, GooF = S = 1.071, Restrained GooF = 1.074 for all data Flack x parameter = -0.3367 with esd 0.9472 Expected values are 0 (within 3 esd's) for correct and +1 for inverted absolute structure. Note that this rough estimate ignores correlation with other parameters; if the above value differs significantly from zero, it is ESSENTIAL to test the inverted structure or refine x as a full-matrix parameter using TWIN and BASF Absolute structure cannot be determined reliably Occupancy sum of asymmetric unit = 52.00 for non-hydrogen and 32.00 for hydrogen atoms Principal mean square atomic displacements U 0.0229 0.0203 0.0155 C1 0.0235 0.0214 0.0190 C2 0.0251 0.0215 0.0141 C3 0.0329 0.0281 0.0139 C4 0.0364 0.0263 0.0166 C5 0.0348 0.0212 0.0182 C6 0.0268 0.0213 0.0186 C7 0.0417 0.0244 0.0185 C8 0.0310 0.0193 0.0164 N1 0.0324 0.0250 0.0176 N2 0.0438 0.0211 0.0171 O1 0.0420 0.0344 0.0213 O2 0.0583 0.0411 0.0150 O3 0.0261 0.0191 0.0155 C11 0.0230 0.0212 0.0157 C12 0.0250 0.0195 0.0170 C13 0.0348 0.0239 0.0172 C14 0.0320 0.0296 0.0202 C15 0.0276 0.0223 0.0194 C16 0.0261 0.0203 0.0186 C17 0.0424 0.0227 0.0194 C18 0.0317 0.0183 0.0131 N11 0.0327 0.0276 0.0148 N12 0.0424 0.0223 0.0183 O11 0.0494 0.0325 0.0208 O12 0.0556 0.0440 0.0164 O13 0.0255 0.0226 0.0191 C21 0.0224 0.0210 0.0197 C22 0.0264 0.0213 0.0196 C23 0.0323 0.0265 0.0181 C24 0.0354 0.0298 0.0243 C25 0.0314 0.0290 0.0223 C26 0.0383 0.0249 0.0213 C27 0.0383 0.0320 0.0244 C28 0.0303 0.0270 0.0229 N21 0.0390 0.0262 0.0198 N22 0.0680 0.0309 0.0212 O21 0.0496 0.0350 0.0238 O22 0.0504 0.0456 0.0169 O23 0.0250 0.0245 0.0195 C31 0.0285 0.0214 0.0192 C32 0.0308 0.0236 0.0146 C33 0.0341 0.0268 0.0208 C34 0.0379 0.0332 0.0192 C35 0.0340 0.0285 0.0209 C36 0.0344 0.0275 0.0202 C37 0.0383 0.0246 0.0199 C38 0.0320 0.0234 0.0183 N31 0.0377 0.0271 0.0238 N32 0.0514 0.0302 0.0224 O31 0.0481 0.0427 0.0238 O32 0.0661 0.0481 0.0217 O33 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.025 0.039 0.052 0.063 0.077 0.095 0.117 0.151 0.217 1.000 Number in group 750. 732. 773. 699. 755. 703. 740. 731. 731. 738. GooF 1.128 1.081 1.065 1.071 1.074 1.082 1.038 0.928 1.022 1.204 K 1.595 1.090 0.984 0.989 0.996 0.985 1.001 1.009 1.013 1.000 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.15 1.32 1.64 inf Number in group 736. 756. 720. 726. 751. 737. 717. 738. 732. 739. GooF 0.952 0.936 1.009 0.990 1.026 1.005 1.007 0.972 1.150 1.534 K 1.014 1.032 1.003 0.999 1.007 1.015 1.035 1.027 1.034 0.971 R1 0.151 0.134 0.116 0.091 0.065 0.053 0.041 0.037 0.039 0.043 Recommended weighting scheme: WGHT 0.0616 0.5236 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) -4 1 2 225.24 123.00 6.70 0.107 2.37 -10 -2 13 13.97 55.45 6.67 0.072 0.77 1 6 0 58.52 20.07 6.39 0.043 2.16 -4 -1 2 217.73 123.27 6.17 0.107 2.37 9 -4 8 2.98 56.03 5.69 0.072 0.77 1 -6 0 54.16 20.17 5.68 0.043 2.16 -10 0 2 70.57 24.70 5.66 0.048 0.97 4 0 2 23.49 2.41 5.57 0.015 2.06 -4 0 4 78.56 41.26 5.21 0.062 2.15 2 6 1 174.20 105.10 5.16 0.098 1.96 -6 -9 6 20.91 0.85 5.12 0.009 1.03 -2 -5 1 470.18 317.54 4.95 0.171 2.33 -2 5 1 468.84 317.59 4.88 0.171 2.33 2 -6 1 171.77 105.33 4.85 0.099 1.96 1 0 1 -6.92 3.97 4.65 0.019 6.82 0 -11 2 41.26 15.27 4.62 0.038 1.19 3 -6 4 25.22 7.06 4.58 0.026 1.49 2 -5 1 750.99 544.25 4.43 0.224 2.24 0 -2 0 163.32 264.16 4.36 0.156 6.67 2 5 1 746.02 544.09 4.27 0.224 2.24 -1 1 8 7.80 0.64 4.08 0.008 1.61 -2 6 3 48.92 25.05 4.08 0.048 1.89 -1 -1 8 7.15 0.64 3.99 0.008 1.61 2 1 0 499.98 680.42 3.92 0.251 4.45 -8 4 6 20.82 5.09 3.90 0.022 1.09 2 -1 0 498.47 681.26 3.80 0.251 4.45 4 0 4 139.84 95.77 3.79 0.094 1.71 -5 -3 2 366.10 267.91 3.78 0.157 1.78 3 6 4 34.56 7.10 3.66 0.026 1.49 0 2 0 176.49 265.40 3.66 0.156 6.67 -8 -7 3 123.31 186.87 3.65 0.131 1.02 2 6 5 110.11 73.85 3.63 0.083 1.50 -2 11 2 143.90 96.73 3.60 0.094 1.17 10 0 2 69.30 39.49 3.60 0.060 0.90 -6 8 12 25.02 45.59 3.59 0.065 0.85 -2 -6 3 45.56 25.24 3.58 0.048 1.89 -10 -5 2 53.80 90.61 3.51 0.091 0.91 0 0 5 -0.87 4.81 3.50 0.021 2.52 -7 9 4 22.48 46.93 3.46 0.066 1.00 -1 7 4 402.03 306.52 3.45 0.168 1.64 -6 -10 1 113.61 168.99 3.40 0.125 1.03 -5 3 2 355.96 267.93 3.39 0.157 1.78 -1 -7 4 399.02 306.92 3.37 0.168 1.64 -8 -7 7 15.47 35.05 3.36 0.057 0.96 4 -5 0 125.04 174.62 3.36 0.127 1.77 -6 0 2 18.31 4.57 3.32 0.021 1.62 -6 5 1 26.15 10.84 3.32 0.032 1.38 -5 13 9 33.27 8.88 3.31 0.029 0.80 -2 -7 3 66.97 44.25 3.25 0.064 1.68 4 -1 0 317.83 237.72 3.23 0.148 2.33 Bond lengths and angles C1 - Distance Angles C6 1.3955 (0.0033) C2 1.4036 (0.0034) 118.69 (0.22) N1 1.4049 (0.0031) 117.15 (0.22) 124.11 (0.21) C1 - C6 C2 C2 - Distance Angles C3 1.3699 (0.0036) C1 1.4036 (0.0034) 117.97 (0.23) H2 0.9500 121.02 121.02 C2 - C3 C1 C3 - Distance Angles C2 1.3699 (0.0036) C4 1.3878 (0.0035) 124.62 (0.23) N2 1.4837 (0.0031) 118.09 (0.22) 117.28 (0.22) C3 - C2 C4 C4 - Distance Angles C3 1.3878 (0.0035) C5 1.3971 (0.0037) 116.47 (0.23) H4 0.9500 121.76 121.76 C4 - C3 C5 C5 - Distance Angles C6 1.3753 (0.0038) C4 1.3971 (0.0037) 120.58 (0.25) H5 0.9500 119.71 119.71 C5 - C6 C4 C6 - Distance Angles C5 1.3753 (0.0038) C1 1.3955 (0.0033) 121.65 (0.25) H6 0.9500 119.18 119.18 C6 - C5 C1 C7 - Distance Angles O1 1.2304 (0.0029) N1 1.3631 (0.0032) 122.75 (0.24) C8 1.4999 (0.0035) 122.88 (0.22) 114.37 (0.20) C7 - O1 N1 C8 - Distance Angles C7 1.4999 (0.0035) H8A 0.9800 109.47 H8B 0.9800 109.47 109.47 H8C 0.9800 109.47 109.47 109.47 C8 - C7 H8A H8B N1 - Distance Angles C7 1.3631 (0.0032) C1 1.4049 (0.0031) 128.61 (0.22) H1N 0.8639 (0.0182) 117.60 (2.68) 113.63 (2.65) N1 - C7 C1 N2 - Distance Angles O2 1.2198 (0.0029) O3 1.2215 (0.0029) 124.17 (0.23) C3 1.4837 (0.0031) 117.84 (0.20) 117.98 (0.22) N2 - O2 O3 O1 - Distance Angles C7 1.2304 (0.0029) O1 - O2 - Distance Angles N2 1.2198 (0.0029) O2 - O3 - Distance Angles N2 1.2215 (0.0029) O3 - C11 - Distance Angles C12 1.3980 (0.0034) N11 1.4038 (0.0031) 124.41 (0.23) C16 1.4044 (0.0034) 118.79 (0.23) 116.76 (0.22) C11 - C12 N11 C12 - Distance Angles C13 1.3880 (0.0034) C11 1.3980 (0.0034) 117.99 (0.23) H12 0.9500 121.01 121.01 C12 - C13 C11 C13 - Distance Angles C14 1.3844 (0.0036) C12 1.3880 (0.0034) 123.82 (0.24) N12 1.4672 (0.0032) 118.39 (0.22) 117.77 (0.22) C13 - C14 C12 C14 - Distance Angles C13 1.3844 (0.0036) C15 1.3887 (0.0039) 117.44 (0.24) H14 0.9500 121.28 121.28 C14 - C13 C15 C15 - Distance Angles C16 1.3789 (0.0038) C14 1.3887 (0.0039) 120.45 (0.25) H15 0.9500 119.77 119.77 C15 - C16 C14 C16 - Distance Angles C15 1.3789 (0.0038) C11 1.4044 (0.0034) 121.47 (0.24) H16 0.9500 119.27 119.27 C16 - C15 C11 C17 - Distance Angles O11 1.2330 (0.0029) N11 1.3547 (0.0032) 123.57 (0.23) C18 1.5111 (0.0036) 121.53 (0.23) 114.91 (0.21) C17 - O11 N11 C18 - Distance Angles C17 1.5111 (0.0036) H18A 0.9800 109.47 H18B 0.9800 109.47 109.47 H18C 0.9800 109.47 109.47 109.47 C18 - C17 H18A H18B N11 - Distance Angles C17 1.3547 (0.0032) C11 1.4038 (0.0031) 127.99 (0.21) H11N 0.8606 (0.0178) 115.95 (2.47) 116.05 (2.47) N11 - C17 C11 N12 - Distance Angles O13 1.2290 (0.0029) O12 1.2346 (0.0029) 123.02 (0.22) C13 1.4672 (0.0031) 118.55 (0.22) 118.43 (0.21) N12 - O13 O12 O11 - Distance Angles C17 1.2330 (0.0029) O11 - O12 - Distance Angles N12 1.2346 (0.0029) O12 - O13 - Distance Angles N12 1.2290 (0.0029) O13 - C21 - Distance Angles C22 1.3855 (0.0035) C26 1.3950 (0.0035) 119.78 (0.24) N21 1.4260 (0.0033) 116.46 (0.23) 123.74 (0.23) C21 - C22 C26 C22 - Distance Angles C23 1.3748 (0.0036) C21 1.3855 (0.0035) 118.81 (0.23) H22 0.9500 120.59 120.59 C22 - C23 C21 C23 - Distance Angles C22 1.3748 (0.0036) C24 1.3885 (0.0035) 123.80 (0.24) N22 1.4729 (0.0032) 118.05 (0.22) 118.15 (0.23) C23 - C22 C24 C24 - Distance Angles C23 1.3885 (0.0035) C25 1.3955 (0.0039) 116.31 (0.24) H24 0.9500 121.84 121.84 C24 - C23 C25 C25 - Distance Angles C26 1.3947 (0.0040) C24 1.3955 (0.0039) 121.53 (0.26) H25 0.9500 119.23 119.23 C25 - C26 C24 C26 - Distance Angles C25 1.3947 (0.0040) C21 1.3950 (0.0035) 119.69 (0.24) H26 0.9500 120.15 120.15 C26 - C25 C21 C27 - Distance Angles O21 1.2387 (0.0032) N21 1.3432 (0.0034) 123.01 (0.27) C28 1.4976 (0.0039) 121.73 (0.25) 115.26 (0.23) C27 - O21 N21 C28 - Distance Angles C27 1.4976 (0.0039) H28A 0.9800 109.47 H28B 0.9800 109.47 109.47 H28C 0.9800 109.47 109.47 109.47 C28 - C27 H28A H28B N21 - Distance Angles C27 1.3432 (0.0034) C21 1.4260 (0.0033) 128.98 (0.23) H21N 0.9776 (0.0171) 112.98 (1.92) 118.00 (1.91) N21 - C27 C21 N22 - Distance Angles O22 1.2213 (0.0030) O23 1.2435 (0.0030) 123.46 (0.23) C23 1.4729 (0.0032) 118.93 (0.22) 117.61 (0.23) N22 - O22 O23 O21 - Distance Angles C27 1.2387 (0.0032) O21 - O22 - Distance Angles N22 1.2213 (0.0030) O22 - O23 - Distance Angles N22 1.2435 (0.0030) O23 - C31 - Distance Angles C32 1.3947 (0.0035) N31 1.4034 (0.0032) 115.97 (0.23) C36 1.4089 (0.0035) 119.20 (0.24) 124.83 (0.24) C31 - C32 N31 C32 - Distance Angles C33 1.3863 (0.0035) C31 1.3947 (0.0035) 118.12 (0.24) H32 0.9500 120.94 120.94 C32 - C33 C31 C33 - Distance Angles C34 1.3809 (0.0036) C32 1.3863 (0.0035) 123.65 (0.24) N32 1.4685 (0.0033) 118.59 (0.23) 117.76 (0.23) C33 - C34 C32 C34 - Distance Angles C35 1.3719 (0.0038) C33 1.3809 (0.0036) 117.24 (0.25) H34 0.9500 121.38 121.38 C34 - C35 C33 C35 - Distance Angles C34 1.3719 (0.0038) C36 1.3831 (0.0040) 121.90 (0.25) H35 0.9500 119.05 119.05 C35 - C34 C36 C36 - Distance Angles C35 1.3831 (0.0040) C31 1.4089 (0.0035) 119.85 (0.25) H36 0.9500 120.08 120.08 C36 - C35 C31 C37 - Distance Angles O31 1.2323 (0.0031) N31 1.3589 (0.0034) 122.61 (0.25) C38 1.5063 (0.0037) 122.06 (0.24) 115.32 (0.21) C37 - O31 N31 C38 - Distance Angles C37 1.5063 (0.0037) H38A 0.9800 109.47 H38B 0.9800 109.47 109.47 H38C 0.9800 109.47 109.47 109.47 C38 - C37 H38A H38B N31 - Distance Angles C37 1.3589 (0.0034) C31 1.4034 (0.0032) 128.64 (0.23) H31N 0.9583 (0.0181) 104.43 (2.35) 126.82 (2.35) N31 - C37 C31 N32 - Distance Angles O32 1.2277 (0.0029) O33 1.2391 (0.0032) 122.85 (0.24) C33 1.4685 (0.0033) 119.00 (0.23) 118.15 (0.22) N32 - O32 O33 O31 - Distance Angles C37 1.2323 (0.0031) O31 - O32 - Distance Angles N32 1.2277 (0.0029) O32 - O33 - Distance Angles N32 1.2391 (0.0032) O33 - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.864(18) 2.016(19) 2.874(3) 172(4) N1-H1N...O11 0.861(18) 2.026(18) 2.887(3) 180(4) N11-H11N...O1_$1 0.978(17) 1.884(18) 2.858(3) 175(2) N21-H21N...O31 0.958(18) 1.96(2) 2.875(3) 159(3) N31-H31N...O21_$1 Hydrogen bonds with H..A < r(A) + 2.000 Angstroms and 110 deg. D-H d(D-H) d(H..A)