+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2005slh0404 started at 23:38:32 on 27-Apr-2005 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2005slh0404 in P2(1)/n CELL 0.71073 12.1056 17.5149 15.3373 90.000 99.041 90.000 ZERR 4.00 0.0006 0.0011 0.0012 0.000 0.006 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N O P S CD UNIT 112 128 8 16 8 16 4 V = 3211.54 F(000) = 1552.0 Mu = 1.08 mm-1 Cell Wt = 3052.54 Rho = 1.578 MERG 2 OMIT -3.00 55.00 OMIT 0 2 2 OMIT 1 2 1 EXTI 0.00103 FMAP 2 PLAN 5 SIZE 0.08 0.24 0.28 ACTA BOND $H WGHT 0.02370 2.59180 L.S. 6 TEMP -153.00 FVAR 0.26649 C1 1 -0.260654 0.845207 0.759072 11.00000 0.01514 0.04008 = 0.03299 0.01326 -0.00374 0.00273 AFIX 137 H1A 2 -0.252593 0.899381 0.774771 11.00000 -1.50000 H1B 2 -0.335862 0.827848 0.765652 11.00000 -1.50000 H1C 2 -0.249258 0.838214 0.697716 11.00000 -1.50000 AFIX 0 C2 1 0.011187 0.747446 0.893958 11.00000 0.01818 0.01574 = 0.01686 0.00085 0.00094 -0.00072 C3 1 0.105538 0.708010 0.878046 11.00000 0.02358 0.02379 = 0.01870 0.00273 0.00688 0.00255 AFIX 43 H3 2 0.138803 0.720793 0.827847 11.00000 -1.20000 AFIX 0 C4 1 0.152270 0.650171 0.934164 11.00000 0.02672 0.02496 = 0.02182 0.00298 0.00733 0.00944 AFIX 43 H4 2 0.217490 0.624224 0.922910 11.00000 -1.20000 AFIX 0 C5 1 0.102710 0.630729 1.006755 11.00000 0.02528 0.01861 = 0.01819 0.00172 -0.00114 0.00107 C6 1 0.008865 0.670387 1.024504 11.00000 0.02382 0.02971 = 0.02251 0.00819 0.00910 0.00221 AFIX 43 H6 2 -0.024674 0.657372 1.074495 11.00000 -1.20000 AFIX 0 C7 1 -0.035023 0.728626 0.969079 11.00000 0.01711 0.02680 = 0.02276 0.00487 0.00572 0.00445 AFIX 43 H7 2 -0.097760 0.756414 0.982228 11.00000 -1.20000 AFIX 0 C8 1 0.242378 0.537285 1.057634 11.00000 0.04435 0.03224 = 0.02220 0.00546 0.00549 0.02110 AFIX 137 H8A 2 0.233294 0.509259 1.001659 11.00000 -1.50000 H8B 2 0.262026 0.501507 1.106748 11.00000 -1.50000 H8C 2 0.302039 0.575234 1.058553 11.00000 -1.50000 AFIX 0 C9 1 0.396109 0.753327 0.717781 11.00000 0.03036 0.01735 = 0.03773 -0.00348 -0.00156 -0.00061 AFIX 137 H9A 2 0.376810 0.729826 0.771390 11.00000 -1.50000 H9B 2 0.445145 0.718936 0.691009 11.00000 -1.50000 H9C 2 0.327667 0.762733 0.675808 11.00000 -1.50000 AFIX 0 C10 1 0.489380 0.967535 0.789246 11.00000 0.01427 0.01586 = 0.01986 -0.00109 0.00359 0.00116 C11 1 0.537456 0.985070 0.874956 11.00000 0.02018 0.02258 = 0.01804 0.00319 0.00088 -0.00031 AFIX 43 H11 2 0.514023 0.958345 0.922761 11.00000 -1.20000 AFIX 0 C12 1 0.619664 1.041278 0.892294 11.00000 0.02324 0.02357 = 0.01690 -0.00030 -0.00110 -0.00427 AFIX 43 H12 2 0.652232 1.052620 0.951328 11.00000 -1.20000 AFIX 0 C13 1 0.653247 1.080366 0.822373 11.00000 0.01773 0.02076 = 0.02568 -0.00199 0.00443 -0.00340 C14 1 0.604294 1.063988 0.735461 11.00000 0.02414 0.02726 = 0.01847 0.00087 0.00601 -0.00635 AFIX 43 H14 2 0.626667 1.091399 0.687712 11.00000 -1.20000 AFIX 0 C15 1 0.523549 1.007993 0.719326 11.00000 0.02130 0.02473 = 0.01745 -0.00200 0.00272 -0.00050 AFIX 43 H15 2 0.490829 0.996765 0.660298 11.00000 -1.20000 AFIX 0 C16 1 0.779916 1.159188 0.917993 11.00000 0.05525 0.05881 = 0.03045 -0.00454 -0.00048 -0.04120 AFIX 137 H16A 2 0.720263 1.177426 0.949153 11.00000 -1.50000 H16B 2 0.834127 1.200291 0.915025 11.00000 -1.50000 H16C 2 0.817618 1.115527 0.949746 11.00000 -1.50000 AFIX 0 C17 1 0.286053 1.093374 0.815033 11.00000 0.02116 0.01630 = 0.01970 -0.00167 0.00511 -0.00009 AFIX 43 H17 2 0.294418 1.085419 0.755148 11.00000 -1.20000 AFIX 0 C18 1 0.355180 1.145931 0.864516 11.00000 0.02079 0.01479 = 0.02692 -0.00166 0.00552 -0.00144 AFIX 43 H18 2 0.410270 1.172604 0.838718 11.00000 -1.20000 AFIX 0 C19 1 0.343696 1.159450 0.951724 11.00000 0.01661 0.01341 = 0.02447 -0.00267 -0.00096 0.00246 C20 1 0.261013 1.118401 0.985503 11.00000 0.02461 0.01847 = 0.01823 -0.00371 0.00212 0.00052 AFIX 43 H20 2 0.249496 1.126140 1.044720 11.00000 -1.20000 AFIX 0 C21 1 0.196264 1.066647 0.932521 11.00000 0.02252 0.01872 = 0.02000 -0.00059 0.00491 -0.00462 AFIX 43 H21 2 0.140713 1.039047 0.956747 11.00000 -1.20000 AFIX 0 C22 1 0.413672 1.218083 1.007268 11.00000 0.01979 0.02005 = 0.02934 -0.00564 -0.00274 -0.00110 C23 1 -0.058579 1.077965 0.712886 11.00000 0.02020 0.01636 = 0.02135 0.00065 0.00390 -0.00114 AFIX 43 H23 2 -0.074634 1.067229 0.770306 11.00000 -1.20000 AFIX 0 C24 1 -0.117061 1.136310 0.664663 11.00000 0.01746 0.01525 = 0.02761 -0.00087 0.00388 0.00089 AFIX 43 H24 2 -0.171538 1.164840 0.689083 11.00000 -1.20000 AFIX 0 C25 1 -0.095298 1.152502 0.580821 11.00000 0.01668 0.01472 = 0.02689 0.00274 -0.00218 -0.00116 C26 1 -0.014227 1.109313 0.548441 11.00000 0.03094 0.02839 = 0.01929 0.00785 0.00470 0.00798 AFIX 43 H26 2 0.003231 1.118675 0.491132 11.00000 -1.20000 AFIX 0 C27 1 0.040594 1.052449 0.601151 11.00000 0.02787 0.02530 = 0.02052 0.00323 0.00712 0.00879 AFIX 43 H27 2 0.096162 1.023516 0.578567 11.00000 -1.20000 AFIX 0 C28 1 -0.158580 1.214469 0.525414 11.00000 0.01952 0.01819 = 0.03054 0.00777 -0.00373 0.00052 N1 3 0.207941 1.053356 0.848247 11.00000 0.01743 0.01536 = 0.01862 -0.00101 0.00107 -0.00096 N2 3 0.019636 1.036066 0.681945 11.00000 0.01691 0.01559 = 0.01852 0.00243 0.00056 0.00081 O1 4 -0.178369 0.801196 0.816748 11.00000 0.01295 0.02225 = 0.02195 0.00451 0.00107 -0.00153 O3 4 0.453372 0.825058 0.740176 11.00000 0.01633 0.01653 = 0.02572 -0.00251 0.00180 0.00250 O4 4 0.732896 1.136331 0.830616 11.00000 0.02955 0.03200 = 0.02382 -0.00189 0.00404 -0.01657 O9 4 0.139843 0.575038 1.066307 11.00000 0.03222 0.02609 = 0.02279 0.00912 0.00478 0.00918 P1 5 -0.048971 0.823529 0.823621 11.00000 0.01279 0.01435 = 0.01636 0.00210 0.00241 -0.00086 P2 5 0.381212 0.896291 0.766246 11.00000 0.01247 0.01607 = 0.01650 0.00000 0.00112 0.00113 S1 6 -0.021242 0.924901 0.884833 11.00000 0.01943 0.01657 = 0.01972 -0.00119 0.00671 -0.00203 S2 6 0.002404 0.822104 0.706352 11.00000 0.02050 0.01741 = 0.01633 0.00048 0.00430 -0.00089 S3 6 0.308253 0.870474 0.869652 11.00000 0.01688 0.02458 = 0.01689 0.00394 0.00252 -0.00070 S4 6 0.271563 0.928009 0.660191 11.00000 0.01447 0.02191 = 0.01482 0.00090 0.00089 0.00203 CD1 7 0.125214 0.944269 0.773089 11.00000 0.01281 0.01343 = 0.01566 0.00074 0.00233 -0.00019 H22A 2 0.476549 1.235281 0.976554 11.00000 0.04153 H22B 2 0.445125 1.197209 1.062319 11.00000 0.04326 H28A 2 -0.192739 1.192432 0.471311 11.00000 0.03683 H28B 2 -0.224895 1.230848 0.555313 11.00000 0.03803 HKLF 4 Covalent radii and connectivity table for 2005slh0404 in P2(1)/n C 0.770 H 0.320 N 0.700 O 0.660 P 1.100 S 1.030 CD 1.490 C1 - O1 C2 - C3 C7 P1 C3 - C2 C4 C4 - C5 C3 C5 - O9 C4 C6 C6 - C7 C5 C7 - C6 C2 C8 - O9 C9 - O3 C10 - C11 C15 P2 C11 - C10 C12 C12 - C13 C11 C13 - O4 C12 C14 C14 - C15 C13 C15 - C14 C10 C16 - O4 C17 - N1 C18 C18 - C19 C17 C19 - C18 C20 C22 C20 - C21 C19 C21 - N1 C20 C22 - C19 C28_$2 C23 - N2 C24 C24 - C25 C23 C25 - C24 C26 C28 C26 - C27 C25 C27 - N2 C26 C28 - C25 C22_$1 N1 - C17 C21 Cd1 N2 - C27 C23 Cd1 O1 - C1 P1 O3 - C9 P2 O4 - C13 C16 O9 - C5 C8 P1 - O1 C2 S2 S1 P2 - O3 C10 S3 S4 S1 - P1 Cd1 S2 - P1 Cd1 S3 - P2 Cd1 S4 - P2 Cd1 Cd1 - N2 N1 S1 S4 S2 S3 Operators for generating equivalent atoms: $1 x-1/2, -y+5/2, z-1/2 $2 x+1/2, -y+5/2, z+1/2 h k l Fo^2 Sigma Why rejected -5 0 2 18.85 3.92 observed but should be systematically absent -5 0 2 18.81 3.34 observed but should be systematically absent 38707 Reflections read, of which 740 rejected -15 =< h =< 15, -21 =< k =< 22, -19 =< l =< 19, Max. 2-theta = 54.95 2 Systematic absence violations 0 Inconsistent equivalents 7340 Unique reflections, of which 0 suppressed R(int) = 0.0371 R(sigma) = 0.0343 Friedel opposites merged Maximum memory for data reduction = 3662 / 72468 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 = 4731 / 503081 wR2 = 0.0647 before cycle 1 for 7340 data and 391 / 391 parameters GooF = S = 1.059; Restrained GooF = 1.059 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0237 * P )^2 + 2.59 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.26625 0.00026 -0.950 OSF 2 0.00100 0.00012 -0.217 EXTI Mean shift/esd = 0.100 Maximum = -1.317 for U22 Cd1 Max. shift = 0.003 A for H22A Max. dU =-0.001 for H22B Least-squares cycle 2 Maximum vector length = 511 Memory required = 4731 / 503081 wR2 = 0.0647 before cycle 2 for 7340 data and 391 / 391 parameters GooF = S = 1.059; Restrained GooF = 1.059 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0237 * P )^2 + 2.59 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.26614 0.00026 -0.417 OSF 2 0.00099 0.00012 -0.089 EXTI Mean shift/esd = 0.032 Maximum = -0.423 for U22 Cd1 Max. shift = 0.001 A for H22A Max. dU = 0.000 for H22B Least-squares cycle 3 Maximum vector length = 511 Memory required = 4731 / 503081 wR2 = 0.0647 before cycle 3 for 7340 data and 391 / 391 parameters GooF = S = 1.060; Restrained GooF = 1.060 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0237 * P )^2 + 2.59 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.26614 0.00026 -0.001 OSF 2 0.00099 0.00012 -0.007 EXTI Mean shift/esd = 0.001 Maximum = -0.007 for EXTI Max. shift = 0.000 A for H22B Max. dU = 0.000 for H22A Least-squares cycle 4 Maximum vector length = 511 Memory required = 4731 / 503081 wR2 = 0.0647 before cycle 4 for 7340 data and 391 / 391 parameters GooF = S = 1.060; Restrained GooF = 1.060 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0237 * P )^2 + 2.59 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.26614 0.00026 -0.001 OSF 2 0.00099 0.00012 -0.001 EXTI Mean shift/esd = 0.000 Maximum = 0.002 for z Cd1 Max. shift = 0.000 A for H28B Max. dU = 0.000 for H22B Least-squares cycle 5 Maximum vector length = 511 Memory required = 4731 / 503081 wR2 = 0.0647 before cycle 5 for 7340 data and 391 / 391 parameters GooF = S = 1.060; Restrained GooF = 1.060 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0237 * P )^2 + 2.59 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.26614 0.00026 -0.001 OSF 2 0.00099 0.00012 -0.001 EXTI Mean shift/esd = 0.000 Maximum = 0.002 for z Cd1 Max. shift = 0.000 A for H22B Max. dU = 0.000 for H28B Least-squares cycle 6 Maximum vector length = 511 Memory required = 4731 / 503081 wR2 = 0.0647 before cycle 6 for 7340 data and 391 / 391 parameters GooF = S = 1.060; Restrained GooF = 1.060 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0237 * P )^2 + 2.59 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.26614 0.00026 0.000 OSF 2 0.00099 0.00012 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.002 for z Cd1 Max. shift = 0.000 A for H22B Max. dU = 0.000 for H28B Largest correlation matrix elements 0.576 EXTI / OSF 0.566 U11 Cd1 / OSF 0.575 U22 Cd1 / OSF 0.531 U33 Cd1 / OSF Idealized hydrogen atom generation before cycle 7 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1A -0.2526 0.8994 0.7747 137 0.980 0.000 C1 O1 H1A H1B -0.3359 0.8279 0.7657 137 0.980 0.000 C1 O1 H1A H1C -0.2493 0.8382 0.6977 137 0.980 0.000 C1 O1 H1A H3 0.1388 0.7208 0.8278 43 0.950 0.000 C3 C2 C4 H4 0.2175 0.6242 0.9230 43 0.950 0.000 C4 C5 C3 H6 -0.0247 0.6573 1.0744 43 0.950 0.000 C6 C7 C5 H7 -0.0977 0.7564 0.9822 43 0.950 0.000 C7 C6 C2 H8A 0.2333 0.5093 1.0016 137 0.980 0.000 C8 O9 H8A H8B 0.2621 0.5015 1.1067 137 0.980 0.000 C8 O9 H8A H8C 0.3020 0.5753 1.0585 137 0.980 0.000 C8 O9 H8A H9A 0.3767 0.7299 0.7714 137 0.980 0.000 C9 O3 H9A H9B 0.4452 0.7189 0.6911 137 0.980 0.000 C9 O3 H9A H9C 0.3277 0.7627 0.6758 137 0.980 0.000 C9 O3 H9A H11 0.5141 0.9583 0.9227 43 0.950 0.000 C11 C10 C12 H12 0.6522 1.0526 0.9513 43 0.950 0.000 C12 C13 C11 H14 0.6266 1.0914 0.6878 43 0.950 0.000 C14 C15 C13 H15 0.4908 0.9968 0.6603 43 0.950 0.000 C15 C14 C10 H16A 0.7204 1.1773 0.9492 137 0.980 0.000 C16 O4 H16A H16B 0.8342 1.2002 0.9151 137 0.980 0.000 C16 O4 H16A H16C 0.8177 1.1155 0.9497 137 0.980 0.000 C16 O4 H16A H17 0.2944 1.0854 0.7552 43 0.950 0.000 C17 N1 C18 H18 0.4103 1.1725 0.8388 43 0.950 0.000 C18 C19 C17 H20 0.2495 1.1261 1.0447 43 0.950 0.000 C20 C21 C19 H21 0.1407 1.0391 0.9567 43 0.950 0.000 C21 N1 C20 H23 -0.0746 1.0673 0.7703 43 0.950 0.000 C23 N2 C24 H24 -0.1715 1.1648 0.6890 43 0.950 0.000 C24 C25 C23 H26 0.0032 1.1187 0.4912 43 0.950 0.000 C26 C27 C25 H27 0.0962 1.0236 0.5786 43 0.950 0.000 C27 N2 C26 2005slh0404 in P2(1)/n ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 -0.26066 0.84522 0.75905 1.00000 0.01504 0.03997 0.03283 0.01310 -0.00373 0.00279 0.03008 0.00466 0.00018 0.00015 0.00017 0.00000 0.00105 0.00144 0.00141 0.00114 0.00093 0.00100 0.00056 H1A -0.25255 0.89940 0.77471 1.00000 0.04512 0.00000 0.00000 H1B -0.33587 0.82789 0.76568 1.00000 0.04512 0.00000 0.00000 H1C -0.24932 0.83818 0.69769 1.00000 0.04512 0.00000 0.00000 C2 0.01119 0.74743 0.89397 1.00000 0.01789 0.01553 0.01668 0.00078 0.00092 -0.00085 0.01689 0.00371 0.00017 0.00012 0.00014 0.00000 0.00099 0.00101 0.00110 0.00083 0.00080 0.00081 0.00042 C3 0.10553 0.70799 0.87805 1.00000 0.02368 0.02344 0.01849 0.00267 0.00707 0.00251 0.02147 0.00410 0.00018 0.00013 0.00015 0.00000 0.00110 0.00115 0.00115 0.00091 0.00088 0.00090 0.00046 H3 0.13879 0.72076 0.82785 1.00000 0.02576 0.00000 0.00000 C4 0.15224 0.65018 0.93419 1.00000 0.02660 0.02469 0.02173 0.00277 0.00731 0.00959 0.02397 0.00435 0.00019 0.00013 0.00015 0.00000 0.00116 0.00118 0.00122 0.00096 0.00093 0.00095 0.00049 H4 0.21747 0.62423 0.92295 1.00000 0.02876 0.00000 0.00000 C5 0.10272 0.63076 1.00672 1.00000 0.02504 0.01834 0.01818 0.00166 -0.00115 0.00102 0.02101 0.00394 0.00018 0.00012 0.00015 0.00000 0.00112 0.00108 0.00115 0.00088 0.00088 0.00089 0.00046 C6 0.00886 0.67037 1.02447 1.00000 0.02359 0.02945 0.02247 0.00815 0.00912 0.00211 0.02458 0.00437 0.00019 0.00013 0.00015 0.00000 0.00112 0.00127 0.00123 0.00099 0.00093 0.00095 0.00050 H6 -0.02471 0.65732 1.07443 1.00000 0.02950 0.00000 0.00000 C7 -0.03498 0.72860 0.96908 1.00000 0.01687 0.02655 0.02276 0.00480 0.00559 0.00441 0.02179 0.00413 0.00017 0.00013 0.00015 0.00000 0.00101 0.00120 0.00121 0.00094 0.00086 0.00088 0.00047 H7 -0.09770 0.75640 0.98224 1.00000 0.02615 0.00000 0.00000 C8 0.24238 0.53730 1.05762 1.00000 0.04449 0.03217 0.02213 0.00559 0.00546 0.02121 0.03291 0.00518 0.00022 0.00015 0.00017 0.00000 0.00150 0.00135 0.00131 0.00106 0.00110 0.00117 0.00059 H8A 0.23329 0.50927 1.00164 1.00000 0.04936 0.00000 0.00000 H8B 0.26206 0.50152 1.10673 1.00000 0.04936 0.00000 0.00000 H8C 0.30202 0.57526 1.05853 1.00000 0.04936 0.00000 0.00000 C9 0.39610 0.75333 0.71778 1.00000 0.03016 0.01708 0.03796 -0.00357 -0.00162 -0.00072 0.02915 0.00419 0.00020 0.00013 0.00017 0.00000 0.00124 0.00116 0.00151 0.00102 0.00105 0.00095 0.00055 H9A 0.37674 0.72986 0.77139 1.00000 0.04372 0.00000 0.00000 H9B 0.44516 0.71892 0.69106 1.00000 0.04372 0.00000 0.00000 H9C 0.32769 0.76273 0.67577 1.00000 0.04372 0.00000 0.00000 C10 0.48938 0.96752 0.78926 1.00000 0.01409 0.01571 0.01974 -0.00096 0.00364 0.00133 0.01641 0.00378 0.00016 0.00012 0.00014 0.00000 0.00095 0.00100 0.00111 0.00085 0.00080 0.00080 0.00042 C11 0.53747 0.98507 0.87493 1.00000 0.02011 0.02222 0.01798 0.00328 0.00106 -0.00033 0.02031 0.00389 0.00017 0.00012 0.00015 0.00000 0.00105 0.00113 0.00113 0.00089 0.00084 0.00086 0.00045 H11 0.51406 0.95834 0.92274 1.00000 0.02437 0.00000 0.00000 C12 0.61965 1.04128 0.89228 1.00000 0.02303 0.02332 0.01676 -0.00031 -0.00107 -0.00418 0.02149 0.00396 0.00018 0.00013 0.00015 0.00000 0.00110 0.00114 0.00114 0.00090 0.00086 0.00090 0.00047 H12 0.65219 1.05265 0.95131 1.00000 0.02579 0.00000 0.00000 C13 0.65324 1.08035 0.82235 1.00000 0.01757 0.02040 0.02569 -0.00189 0.00442 -0.00338 0.02111 0.00399 0.00018 0.00013 0.00015 0.00000 0.00103 0.00110 0.00125 0.00093 0.00088 0.00086 0.00046 C14 0.60428 1.06398 0.73550 1.00000 0.02404 0.02694 0.01841 0.00100 0.00611 -0.00622 0.02283 0.00409 0.00018 0.00013 0.00015 0.00000 0.00113 0.00121 0.00118 0.00094 0.00090 0.00093 0.00048 H14 0.62665 1.09140 0.68776 1.00000 0.02740 0.00000 0.00000 C15 0.52355 1.00800 0.71932 1.00000 0.02110 0.02455 0.01722 -0.00204 0.00268 -0.00048 0.02099 0.00402 0.00018 0.00013 0.00015 0.00000 0.00105 0.00116 0.00113 0.00090 0.00084 0.00089 0.00046 H15 0.49083 0.99679 0.66029 1.00000 0.02519 0.00000 0.00000 C16 0.78000 1.15913 0.91802 1.00000 0.05525 0.05878 0.03048 -0.00458 -0.00048 -0.04140 0.04894 0.00455 0.00026 0.00018 0.00018 0.00000 0.00181 0.00195 0.00155 0.00138 0.00131 0.00158 0.00082 H16A 0.72037 1.17734 0.94923 1.00000 0.07341 0.00000 0.00000 H16B 0.83420 1.20024 0.91507 1.00000 0.07341 0.00000 0.00000 H16C 0.81772 1.11545 0.94971 1.00000 0.07341 0.00000 0.00000 C17 0.28604 1.09338 0.81506 1.00000 0.02108 0.01596 0.01949 -0.00168 0.00525 -0.00006 0.01862 0.00387 0.00017 0.00012 0.00015 0.00000 0.00106 0.00104 0.00114 0.00086 0.00086 0.00084 0.00044 H17 0.29441 1.08545 0.75517 1.00000 0.02235 0.00000 0.00000 C18 0.35514 1.14589 0.86456 1.00000 0.02053 0.01466 0.02669 -0.00146 0.00553 -0.00138 0.02043 0.00394 0.00018 0.00012 0.00015 0.00000 0.00105 0.00104 0.00125 0.00090 0.00089 0.00084 0.00046 H18 0.41026 1.17253 0.83876 1.00000 0.02452 0.00000 0.00000 C19 0.34369 1.15945 0.95171 1.00000 0.01645 0.01312 0.02436 -0.00258 -0.00095 0.00257 0.01842 0.00376 0.00017 0.00012 0.00015 0.00000 0.00098 0.00100 0.00119 0.00086 0.00084 0.00080 0.00044 C20 0.26101 1.11841 0.98548 1.00000 0.02463 0.01824 0.01804 -0.00366 0.00214 0.00065 0.02043 0.00391 0.00018 0.00012 0.00015 0.00000 0.00110 0.00108 0.00114 0.00087 0.00087 0.00087 0.00046 H20 0.24950 1.12614 1.04470 1.00000 0.02452 0.00000 0.00000 C21 0.19626 1.06667 0.93251 1.00000 0.02224 0.01855 0.01999 -0.00051 0.00484 -0.00453 0.02010 0.00393 0.00018 0.00012 0.00015 0.00000 0.00109 0.00107 0.00117 0.00088 0.00087 0.00086 0.00046 H21 0.14069 1.03909 0.95674 1.00000 0.02412 0.00000 0.00000 C22 0.41364 1.21806 1.00726 1.00000 0.01975 0.01996 0.02913 -0.00553 -0.00277 -0.00109 0.02365 0.00405 0.00019 0.00013 0.00017 0.00000 0.00110 0.00115 0.00136 0.00100 0.00097 0.00092 0.00049 C23 -0.05856 1.07798 0.71287 1.00000 0.02011 0.01627 0.02114 0.00063 0.00392 -0.00124 0.01910 0.00390 0.00017 0.00012 0.00015 0.00000 0.00105 0.00104 0.00117 0.00086 0.00086 0.00083 0.00045 H23 -0.07461 1.06728 0.77030 1.00000 0.02292 0.00000 0.00000 C24 -0.11703 1.13629 0.66464 1.00000 0.01724 0.01490 0.02759 -0.00088 0.00389 0.00081 0.01987 0.00389 0.00017 0.00012 0.00015 0.00000 0.00102 0.00103 0.00125 0.00090 0.00087 0.00082 0.00045 H24 -0.17154 1.16480 0.68904 1.00000 0.02384 0.00000 0.00000 C25 -0.09527 1.15252 0.58082 1.00000 0.01639 0.01443 0.02675 0.00260 -0.00213 -0.00130 0.01978 0.00385 0.00017 0.00012 0.00015 0.00000 0.00099 0.00102 0.00123 0.00090 0.00086 0.00082 0.00045 C26 -0.01423 1.10931 0.54847 1.00000 0.03088 0.02810 0.01907 0.00779 0.00476 0.00785 0.02593 0.00448 0.00019 0.00013 0.00016 0.00000 0.00124 0.00124 0.00120 0.00097 0.00095 0.00101 0.00051 H26 0.00322 1.11865 0.49115 1.00000 0.03111 0.00000 0.00000 C27 0.04059 1.05247 0.60116 1.00000 0.02755 0.02511 0.02050 0.00301 0.00708 0.00871 0.02403 0.00436 0.00019 0.00013 0.00015 0.00000 0.00119 0.00121 0.00121 0.00094 0.00095 0.00094 0.00050 H27 0.09619 1.02356 0.57859 1.00000 0.02884 0.00000 0.00000 C28 -0.15856 1.21445 0.52539 1.00000 0.01950 0.01817 0.03035 0.00779 -0.00384 0.00056 0.02351 0.00437 0.00019 0.00013 0.00017 0.00000 0.00109 0.00113 0.00137 0.00098 0.00098 0.00091 0.00050 N1 0.20792 1.05335 0.84824 1.00000 0.01731 0.01502 0.01849 -0.00107 0.00111 -0.00089 0.01712 0.00312 0.00014 0.00009 0.00012 0.00000 0.00086 0.00088 0.00096 0.00071 0.00071 0.00068 0.00037 N2 0.01962 1.03606 0.68196 1.00000 0.01671 0.01554 0.01837 0.00239 0.00060 0.00076 0.01711 0.00317 0.00014 0.00010 0.00012 0.00000 0.00084 0.00085 0.00095 0.00072 0.00069 0.00070 0.00037 O1 -0.17835 0.80119 0.81675 1.00000 0.01266 0.02204 0.02183 0.00450 0.00100 -0.00153 0.01903 0.00264 0.00011 0.00008 0.00010 0.00000 0.00067 0.00077 0.00082 0.00064 0.00058 0.00059 0.00032 O3 0.45337 0.82506 0.74017 1.00000 0.01612 0.01633 0.02552 -0.00261 0.00174 0.00244 0.01949 0.00262 0.00011 0.00008 0.00010 0.00000 0.00071 0.00075 0.00086 0.00063 0.00060 0.00058 0.00032 O4 0.73290 1.13634 0.83061 1.00000 0.02947 0.03178 0.02358 -0.00194 0.00409 -0.01661 0.02829 0.00280 0.00013 0.00009 0.00011 0.00000 0.00086 0.00092 0.00090 0.00072 0.00068 0.00072 0.00038 O9 0.13982 0.57503 1.06631 1.00000 0.03207 0.02600 0.02265 0.00914 0.00472 0.00928 0.02686 0.00312 0.00014 0.00009 0.00011 0.00000 0.00089 0.00085 0.00090 0.00069 0.00070 0.00070 0.00037 P1 -0.04897 0.82353 0.82362 1.00000 0.01264 0.01424 0.01633 0.00210 0.00243 -0.00087 0.01438 0.00095 0.00004 0.00003 0.00004 0.00000 0.00024 0.00026 0.00027 0.00021 0.00020 0.00019 0.00011 P2 0.38121 0.89629 0.76625 1.00000 0.01241 0.01594 0.01640 -0.00001 0.00113 0.00115 0.01504 0.00096 0.00004 0.00003 0.00004 0.00000 0.00024 0.00026 0.00028 0.00021 0.00020 0.00020 0.00012 S1 -0.02124 0.92490 0.88483 1.00000 0.01937 0.01641 0.01964 -0.00119 0.00675 -0.00204 0.01808 0.00097 0.00004 0.00003 0.00004 0.00000 0.00026 0.00026 0.00028 0.00021 0.00021 0.00020 0.00012 S2 0.00240 0.82210 0.70636 1.00000 0.02042 0.01721 0.01630 0.00049 0.00431 -0.00089 0.01783 0.00096 0.00004 0.00003 0.00004 0.00000 0.00025 0.00026 0.00027 0.00020 0.00020 0.00020 0.00011 S3 0.30825 0.87047 0.86965 1.00000 0.01680 0.02444 0.01683 0.00393 0.00253 -0.00067 0.01937 0.00098 0.00004 0.00003 0.00004 0.00000 0.00024 0.00028 0.00027 0.00022 0.00020 0.00021 0.00012 S4 0.27157 0.92801 0.66019 1.00000 0.01437 0.02176 0.01475 0.00092 0.00091 0.00204 0.01711 0.00095 0.00004 0.00003 0.00004 0.00000 0.00024 0.00027 0.00026 0.00021 0.00019 0.00020 0.00011 Cd1 0.12522 0.94427 0.77309 1.00000 0.01273 0.01328 0.01558 0.00073 0.00235 -0.00019 0.01385 0.00026 0.00001 0.00001 0.00001 0.00000 0.00008 0.00009 0.00009 0.00006 0.00006 0.00005 0.00006 H22A 0.47628 1.23529 0.97671 1.00000 0.04059 0.04999 0.00232 0.00156 0.00185 0.00000 0.00778 H22B 0.44491 1.19708 1.06227 1.00000 0.04162 0.05234 0.00231 0.00163 0.00198 0.00000 0.00804 H28A -0.19263 1.19257 0.47121 1.00000 0.03678 0.05244 0.00223 0.00153 0.00189 0.00000 0.00760 H28B -0.22480 1.23091 0.55512 1.00000 0.03816 0.04956 0.00228 0.00156 0.00183 0.00000 0.00750 Final Structure Factor Calculation for 2005slh0404 in P2(1)/n Total number of l.s. parameters = 391 Maximum vector length = 511 Memory required = 4340 / 26061 wR2 = 0.0647 before cycle 7 for 7340 data and 0 / 391 parameters GooF = S = 1.060; Restrained GooF = 1.060 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0237 * P )^2 + 2.59 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0281 for 6282 Fo > 4sig(Fo) and 0.0375 for all 7340 data wR2 = 0.0647, GooF = S = 1.060, Restrained GooF = 1.060 for all data Occupancy sum of asymmetric unit = 41.00 for non-hydrogen and 32.00 for hydrogen atoms Principal mean square atomic displacements U 0.0507 0.0279 0.0117 C1 0.0199 0.0157 0.0151 C2 0.0277 0.0211 0.0156 C3 0.0360 0.0202 0.0157 C4 0.0282 0.0195 0.0154 C5 0.0359 0.0234 0.0144 C6 0.0310 0.0195 0.0149 C7 0.0604 0.0232 0.0151 C8 0.0437 0.0275 0.0163 C9 0.0200 0.0164 0.0128 C10 0.0247 0.0204 0.0159 C11 0.0287 0.0210 0.0147 C12 0.0265 0.0215 0.0153 C13 0.0319 0.0215 0.0151 C14 0.0251 0.0212 0.0167 C15 0.0994 0.0335 0.0140 C16 0.0223 0.0185 0.0151 C17 0.0272 0.0198 0.0143 C18 0.0279 0.0158 0.0116 C19 0.0255 0.0213 0.0145 C20 0.0255 0.0195 0.0153 C21 0.0352 0.0209 0.0148 C22 0.0214 0.0202 0.0157 C23 0.0277 0.0174 0.0145 C24 0.0308 0.0148 0.0138 C25 0.0384 0.0250 0.0144 C26 0.0357 0.0190 0.0173 C27 0.0383 0.0195 0.0127 C28 0.0201 0.0171 0.0142 N1 0.0208 0.0170 0.0135 N2 0.0272 0.0174 0.0124 O1 0.0271 0.0178 0.0136 O3 0.0473 0.0236 0.0140 O4 0.0400 0.0267 0.0139 O9 0.0177 0.0137 0.0117 P1 0.0171 0.0161 0.0120 P2 0.0233 0.0162 0.0147 S1 0.0208 0.0174 0.0152 S2 0.0263 0.0168 0.0151 S3 0.0223 0.0161 0.0129 S4 0.0158 0.0132 0.0125 Cd1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.017 0.033 0.049 0.066 0.083 0.104 0.132 0.165 0.223 1.000 Number in group 776. 734. 725. 733. 699. 740. 743. 721. 729. 740. GooF 0.997 1.102 1.106 1.056 1.072 1.104 1.043 0.930 1.021 1.154 K 1.128 0.904 0.940 0.955 0.965 0.972 0.992 1.001 1.015 1.010 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.32 1.65 inf Number in group 751. 735. 721. 744. 732. 733. 721. 746. 718. 739. GooF 1.056 1.024 1.036 1.009 0.936 0.926 0.971 0.949 1.040 1.522 K 0.965 0.986 0.994 1.002 1.018 1.018 1.027 1.021 1.009 0.990 R1 0.087 0.071 0.060 0.049 0.036 0.030 0.027 0.021 0.019 0.022 Recommended weighting scheme: WGHT 0.0224 2.7230 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) 2 0 0 4515.92 7072.81 5.72 0.220 5.98 -1 2 2 1229.17 1871.86 5.71 0.113 5.42 -2 3 3 491.69 302.88 4.98 0.046 3.41 -5 2 9 105.30 3.53 4.87 0.005 1.47 4 0 0 2.21 63.79 4.81 0.021 2.99 -1 10 8 103.89 0.78 4.78 0.002 1.29 2 0 6 451.69 699.96 4.69 0.069 2.20 1 1 2 923.07 1401.49 4.60 0.098 5.66 2 5 0 1566.57 1967.68 4.59 0.116 3.02 -4 7 4 133.04 242.58 4.21 0.041 1.79 -11 11 8 -88.44 161.61 3.95 0.033 0.86 5 0 1 15338.83 17417.73 3.86 0.346 2.31 -4 0 2 13314.73 15146.54 3.84 0.323 2.94 1 6 5 2636.28 2221.41 3.81 0.124 2.03 2 7 3 4491.46 5163.95 3.74 0.188 2.05 -3 4 5 62.13 143.90 3.73 0.031 2.25 -6 3 3 1678.50 2005.09 3.61 0.117 1.86 -8 0 2 1084.88 1351.47 3.61 0.096 1.51 -1 1 8 4963.36 5707.79 3.58 0.198 1.91 0 4 3 1809.74 1521.34 3.46 0.102 3.31 -3 7 3 122.35 60.51 3.40 0.020 2.01 -1 8 8 150.38 57.23 3.35 0.020 1.44 2 1 9 88.14 179.42 3.35 0.035 1.55 -2 22 4 155.03 437.35 3.34 0.055 0.78 2 18 11 839.14 1242.60 3.34 0.092 0.78 4 2 2 3037.48 3472.68 3.29 0.154 2.53 -3 0 1 1973.46 2306.96 3.28 0.126 4.01 2 5 3 1529.18 1269.89 3.28 0.093 2.51 -4 5 2 340.74 239.33 3.28 0.041 2.25 3 5 5 1836.86 2159.83 3.28 0.122 1.89 -2 3 6 392.93 531.15 3.27 0.060 2.27 -3 5 6 1552.36 1842.77 3.27 0.113 1.92 -7 2 1 2794.41 3219.81 3.27 0.149 1.69 -6 9 2 1874.45 1519.34 3.26 0.102 1.40 -5 4 1 62.91 2.44 3.25 0.004 2.12 -5 18 7 1268.58 1643.38 3.24 0.106 0.85 -8 6 11 183.14 67.08 3.23 0.021 1.03 -1 20 4 1091.13 1425.85 3.22 0.099 0.85 11 13 5 5224.60 4284.60 3.16 0.172 0.79 8 11 0 269.88 385.43 3.12 0.051 1.09 3 6 6 1667.69 1395.01 3.12 0.098 1.65 4 0 4 14593.18 16232.47 3.12 0.334 2.19 4 12 6 125.88 219.22 3.11 0.039 1.13 12 8 1 -6.27 149.69 3.07 0.032 0.90 7 3 2 105.51 184.29 3.04 0.036 1.55 -6 6 3 34.57 1.35 3.03 0.003 1.63 5 21 1 892.98 1288.13 3.01 0.094 0.78 -6 17 10 752.06 1053.55 2.99 0.085 0.81 4 2 1 45.50 92.87 2.99 0.025 2.71 -6 2 1 510.26 396.39 2.96 0.052 1.97 Bond lengths and angles C1 - Distance Angles O1 1.4468 (0.0026) H1A 0.9800 109.47 H1B 0.9800 109.47 109.47 H1C 0.9800 109.47 109.47 109.47 C1 - O1 H1A H1B C2 - Distance Angles C3 1.3888 (0.0029) C7 1.3965 (0.0030) 118.31 (0.19) P1 1.7956 (0.0021) 122.05 (0.16) 119.59 (0.16) C2 - C3 C7 C3 - Distance Angles C2 1.3888 (0.0029) C4 1.3905 (0.0031) 121.27 (0.21) H3 0.9500 119.37 119.37 C3 - C2 C4 C4 - Distance Angles C5 1.3865 (0.0032) C3 1.3905 (0.0031) 119.37 (0.20) H4 0.9500 120.31 120.31 C4 - C5 C3 C5 - Distance Angles O9 1.3640 (0.0026) C4 1.3865 (0.0032) 125.09 (0.20) C6 1.3942 (0.0031) 114.70 (0.20) 120.19 (0.20) C5 - O9 C4 C6 - Distance Angles C7 1.3791 (0.0031) C5 1.3942 (0.0031) 119.63 (0.21) H6 0.9500 120.19 120.19 C6 - C7 C5 C7 - Distance Angles C6 1.3791 (0.0031) C2 1.3965 (0.0030) 121.17 (0.20) H7 0.9500 119.41 119.41 C7 - C6 C2 C8 - Distance Angles O9 1.4311 (0.0028) H8A 0.9800 109.47 H8B 0.9800 109.47 109.47 H8C 0.9800 109.47 109.47 109.47 C8 - O9 H8A H8B C9 - Distance Angles O3 1.4499 (0.0026) H9A 0.9800 109.47 H9B 0.9800 109.47 109.47 H9C 0.9800 109.47 109.47 109.47 C9 - O3 H9A H9B C10 - Distance Angles C11 1.3854 (0.0030) C15 1.4014 (0.0031) 118.89 (0.20) P2 1.8030 (0.0021) 121.55 (0.16) 119.53 (0.16) C10 - C11 C15 C11 - Distance Angles C10 1.3854 (0.0030) C12 1.3952 (0.0030) 121.21 (0.21) H11 0.9500 119.39 119.39 C11 - C10 C12 C12 - Distance Angles C13 1.3859 (0.0032) C11 1.3952 (0.0030) 119.20 (0.21) H12 0.9500 120.40 120.40 C12 - C13 C11 C13 - Distance Angles O4 1.3672 (0.0026) C12 1.3859 (0.0032) 124.81 (0.21) C14 1.3999 (0.0033) 114.97 (0.20) 120.22 (0.20) C13 - O4 C12 C14 - Distance Angles C15 1.3790 (0.0031) C13 1.3999 (0.0033) 119.93 (0.21) H14 0.9500 120.03 120.03 C14 - C15 C13 C15 - Distance Angles C14 1.3790 (0.0031) C10 1.4014 (0.0030) 120.53 (0.21) H15 0.9500 119.73 119.73 C15 - C14 C10 C16 - Distance Angles O4 1.4288 (0.0030) H16A 0.9800 109.47 H16B 0.9800 109.47 109.47 H16C 0.9800 109.47 109.47 109.47 C16 - O4 H16A H16B C17 - Distance Angles N1 1.3402 (0.0027) C18 1.3865 (0.0030) 122.68 (0.20) H17 0.9500 118.66 118.66 C17 - N1 C18 C18 - Distance Angles C19 1.3860 (0.0031) C17 1.3865 (0.0030) 119.91 (0.20) H18 0.9500 120.04 120.04 C18 - C19 C17 C19 - Distance Angles C18 1.3860 (0.0031) C20 1.3963 (0.0031) 117.10 (0.19) C22 1.5066 (0.0030) 121.99 (0.20) 120.87 (0.21) C19 - C18 C20 C20 - Distance Angles C21 1.3767 (0.0030) C19 1.3963 (0.0031) 119.66 (0.21) H20 0.9500 120.17 120.17 C20 - C21 C19 C21 - Distance Angles N1 1.3424 (0.0029) C20 1.3767 (0.0030) 123.11 (0.20) H21 0.9500 118.45 118.45 C21 - N1 C20 C22 - Distance Angles C19 1.5066 (0.0030) C28_$2 1.5215 (0.0032) 110.16 (0.18) H22A 0.9987 (0.0287) 109.95 (1.60) 110.57 (1.60) H22B 0.9433 (0.0296) 110.57 (1.77) 107.49 (1.74) 108.05 (2.30) C22 - C19 C28_$2 H22A C23 - Distance Angles N2 1.3419 (0.0028) C24 1.3880 (0.0030) 122.90 (0.21) H23 0.9500 118.55 118.55 C23 - N2 C24 C24 - Distance Angles C25 1.3817 (0.0032) C23 1.3880 (0.0030) 119.43 (0.20) H24 0.9500 120.28 120.28 C24 - C25 C23 C25 - Distance Angles C24 1.3817 (0.0032) C26 1.3909 (0.0032) 117.92 (0.20) C28 1.5105 (0.0029) 121.16 (0.20) 120.92 (0.21) C25 - C24 C26 C26 - Distance Angles C27 1.3843 (0.0031) C25 1.3909 (0.0031) 118.91 (0.22) H26 0.9500 120.55 120.55 C26 - C27 C25 C27 - Distance Angles N2 1.3346 (0.0029) C26 1.3843 (0.0031) 123.59 (0.21) H27 0.9500 118.21 118.21 C27 - N2 C26 C28 - Distance Angles C25 1.5105 (0.0029) C22_$1 1.5215 (0.0032) 113.93 (0.18) H28A 0.9486 (0.0284) 108.38 (1.63) 109.69 (1.66) H28B 1.0242 (0.0280) 108.35 (1.56) 112.03 (1.55) 103.93 (2.19) C28 - C25 C22_$1 H28A N1 - Distance Angles C17 1.3402 (0.0027) C21 1.3424 (0.0029) 117.52 (0.18) Cd1 2.3704 (0.0017) 120.42 (0.14) 120.53 (0.14) N1 - C17 C21 N2 - Distance Angles C27 1.3346 (0.0029) C23 1.3419 (0.0028) 117.25 (0.18) Cd1 2.3688 (0.0017) 122.02 (0.14) 120.53 (0.14) N2 - C27 C23 O1 - Distance Angles C1 1.4468 (0.0025) P1 1.6018 (0.0014) 118.84 (0.13) O1 - C1 O3 - Distance Angles C9 1.4499 (0.0026) P2 1.6091 (0.0015) 118.20 (0.13) O3 - C9 O4 - Distance Angles C13 1.3672 (0.0026) C16 1.4288 (0.0030) 117.32 (0.19) O4 - C13 O9 - Distance Angles C5 1.3640 (0.0026) C8 1.4311 (0.0028) 117.85 (0.18) O9 - C5 P1 - Distance Angles O1 1.6018 (0.0014) C2 1.7956 (0.0021) 99.11 (0.09) S2 1.9933 (0.0008) 112.21 (0.06) 112.23 (0.07) S1 2.0118 (0.0008) 109.63 (0.06) 110.64 (0.07) 112.29 (0.03) P1 - O1 C2 S2 P2 - Distance Angles O3 1.6091 (0.0015) C10 1.8030 (0.0021) 100.32 (0.09) S3 1.9849 (0.0008) 110.43 (0.06) 113.70 (0.07) S4 2.0094 (0.0007) 109.17 (0.06) 109.52 (0.07) 112.93 (0.03) P2 - O3 C10 S3 S1 - Distance Angles P1 2.0118 (0.0008) Cd1 2.6741 (0.0006) 83.78 (0.02) S1 - P1 S2 - Distance Angles P1 1.9933 (0.0008) Cd1 2.7126 (0.0006) 83.10 (0.02) S2 - P1 S3 - Distance Angles P2 1.9849 (0.0008) Cd1 2.7825 (0.0006) 83.46 (0.02) S3 - P2 S4 - Distance Angles P2 2.0094 (0.0007) Cd1 2.6800 (0.0006) 85.76 (0.02) S4 - P2 Cd1 - Distance Angles N2 2.3688 (0.0017) N1 2.3704 (0.0017) 83.53 (0.06) S1 2.6741 (0.0006) 96.53 (0.05) 93.58 (0.05) S4 2.6800 (0.0006) 92.36 (0.05) 97.37 (0.05) 166.61 (0.02) S2 2.7126 (0.0006) 95.73 (0.04) 169.69 (0.05) 76.26 (0.02) 92.93 (0.02) S3 2.7825 (0.0006) 160.07 (0.04) 82.84 (0.04) 98.78 (0.02) 75.08 (0.02) 100.24 (0.02) Cd1 - N2 N1 S1 S4 S2 FMAP and GRID set by program FMAP 2 2 22 GRID -1.316 -2 -2 1.316 2 2 R1 = 0.0368 for 7340 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.64 at 0.3793 0.0536 0.3185 [ 1.76 A from C15 ] Deepest hole -0.71 at 0.8828 0.0135 0.2050 [ 0.82 A from CD1 ] Mean = 0.00, Rms deviation from mean = 0.08 e/A^3, Highest memory used = 4295 / 29942 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.6207 0.9464 0.6815 1.00000 0.05 0.64 1.76 C15 1.79 H15 1.86 O9 2.09 H1A Q2 1 0.4599 0.9322 0.7826 1.00000 0.05 0.51 0.71 C10 1.14 P2 1.82 C11 1.88 C15 Q3 1 0.3749 0.6628 0.7248 1.00000 0.05 0.44 1.37 H9A 1.45 H9B 1.61 C9 1.95 H9C Q4 1 -0.1277 0.8962 0.7830 1.00000 0.05 0.42 1.50 H1A 1.65 P1 1.83 C1 1.87 O1 Q5 1 0.2906 0.8221 0.7290 1.00000 0.05 0.41 1.44 H9C 1.74 P2 1.78 C9 1.95 O3 Shortest distances between peaks (including symmetry equivalents) 1 2 2.68 2 5 2.84 3 5 2.97 Time profile in seconds ----------------------- 0.03: Read and process instructions 0.00: Fit rigid groups 0.01: Interpret restraints etc. 0.00: 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 0.01: Analyse other restraints etc. 1.91: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.01: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 5.12: Structure factors and derivatives 12.47: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.01: Apply other restraints 0.78: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.18: Analysis of variance 0.06: Merge reflections for Fourier and .fcf 0.07: Fourier summations 0.09: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2005slh0404 finished at 23:38:53 Total CPU time: 21.0 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++