+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 06skc0065p21n started at 09:53:32 on 18-Jan-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 06skc0065p21n in P2(1)/n CELL 0.71073 17.3078 9.0088 18.9320 90.000 105.305 90.000 ZERR 6.00 0.0022 0.0014 0.0026 0.000 0.007 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N O UNIT 96 192 12 48 V = 2847.23 F(000) = 1236.0 Mu = 0.11 mm-1 Cell Wt = 2282.62 Rho = 1.331 MERG 2 OMIT -3.00 55.00 OMIT -3 2 7 SHEL 7 0.77 HTAB N42 O51A HTAB N42 O51B EQIV_$1 -x+1/2, y-1/2, -z+1/2 HTAB O5B O51A_$1 HTAB N22 O1B_$1 HTAB N22 O1A_$1 EQIV_$2 -x+1, -y+1, -z HTAB O35A O1B_$2 EQIV_$3 -x+3/2, y-1/2, -z+1/2 HTAB N45 O31A_$3 HTAB N45 O31B_$3 EQIV_$4 x-1/2, -y+3/2, z-1/2 HTAB O55A O31B_$4 MPLA C51 O51A O51B MPLA C55 O55A O55B FMAP 2 PLAN 10 SIZE 0.07 0.11 0.18 ACTA BOND $H WGHT 0.20000 L.S. 4 TEMP -153.00 FVAR 0.27712 MOLE 1 C1 1 0.175442 0.041143 0.158271 11.00000 0.04850 0.04343 = 0.03352 -0.00857 0.00268 0.01548 C2 1 0.251122 -0.034163 0.196148 11.00000 0.04679 0.06611 = 0.05411 -0.01811 0.00343 0.02047 AFIX 23 H2A 2 0.265138 -0.103490 0.160885 11.00000 -1.20000 H2B 2 0.293792 0.042048 0.208361 11.00000 -1.20000 AFIX 0 C3 1 0.253333 -0.115886 0.261863 11.00000 0.10576 0.04936 = 0.07065 0.01638 0.03885 0.02183 AFIX 23 H3A 2 0.303799 -0.173430 0.276147 11.00000 -1.20000 H3B 2 0.208305 -0.187385 0.251661 11.00000 -1.20000 AFIX 0 C4 1 0.247822 -0.016302 0.326100 11.00000 0.07382 0.07016 = 0.03743 0.00929 0.01422 0.02190 AFIX 23 H4A 2 0.203263 0.054541 0.307983 11.00000 -1.20000 H4B 2 0.233195 -0.079644 0.363309 11.00000 -1.20000 AFIX 0 C5 1 0.319798 0.069774 0.363014 11.00000 0.06088 0.08452 = 0.04885 0.03178 0.03542 0.02830 O1A 4 0.111543 0.022391 0.176421 11.00000 0.03639 0.05956 = 0.04641 0.00310 0.00995 0.00376 O1B 4 0.178153 0.130272 0.105600 11.00000 0.05468 0.06747 = 0.05497 -0.00854 0.02614 -0.00832 O5A 4 0.383746 0.059250 0.347940 11.00000 0.05249 0.09162 = 0.08666 0.03559 0.03424 0.01541 O5B 4 0.314263 0.163825 0.418959 11.00000 0.03536 0.10206 = 0.04630 0.00312 0.00745 -0.00604 AFIX 83 H5 2 0.267803 0.159537 0.424663 11.00000 -1.50000 AFIX 0 MOLE 2 C21 1 0.462916 -0.221039 0.526073 11.00000 0.06124 0.05474 = 0.09626 0.00846 0.05190 0.00498 AFIX 137 H21A 2 0.440421 -0.288068 0.556264 11.00000 -1.50000 H21B 2 0.425172 -0.139918 0.507922 11.00000 -1.50000 H21C 2 0.513650 -0.180099 0.555597 11.00000 -1.50000 AFIX 0 C23 1 0.524593 -0.443313 0.486333 11.00000 0.02750 0.04500 = 0.04095 0.01063 0.01016 0.00873 AFIX 23 H23A 2 0.573208 -0.419398 0.525765 11.00000 -1.20000 H23B 2 0.541805 -0.485057 0.444557 11.00000 -1.20000 AFIX 0 C24 1 0.518255 -0.208510 0.418330 11.00000 0.04145 0.04537 = 0.05022 0.01246 0.00208 -0.01277 AFIX 137 H24A 2 0.529220 -0.267069 0.378437 11.00000 -1.50000 H24B 2 0.568757 -0.170907 0.449914 11.00000 -1.50000 H24C 2 0.483335 -0.124835 0.397819 11.00000 -1.50000 AFIX 0 N22 3 0.477415 -0.304993 0.462664 11.00000 0.03171 0.05306 = 0.05289 0.00176 0.00424 -0.00276 AFIX 13 H22 2 0.427842 -0.332542 0.432524 11.00000 0.08783 AFIX 0 MOLE 3 C31 1 0.832157 1.000561 0.168501 11.00000 0.04614 0.08834 = 0.02694 -0.00242 0.00901 0.02035 C32 1 0.775737 1.121512 0.129602 11.00000 0.05330 0.05912 = 0.05053 -0.00862 -0.00469 0.02123 AFIX 23 H32A 2 0.756079 1.178715 0.166006 11.00000 -1.20000 H32B 2 0.805219 1.190549 0.105421 11.00000 -1.20000 AFIX 0 C33 1 0.705983 1.057998 0.073631 11.00000 0.05703 0.07146 = 0.03665 -0.00284 -0.00001 0.02529 AFIX 23 H33A 2 0.665823 1.136989 0.055718 11.00000 -1.20000 H33B 2 0.680544 0.979841 0.096615 11.00000 -1.20000 AFIX 0 C34 1 0.731292 0.992086 0.009177 11.00000 0.04139 0.06508 = 0.03137 -0.00833 0.00482 0.00899 AFIX 23 H34A 2 0.746786 1.073405 -0.019495 11.00000 -1.20000 H34B 2 0.778829 0.928175 0.027892 11.00000 -1.20000 AFIX 0 C35 1 0.664990 0.900923 -0.040766 11.00000 0.04762 0.08202 = 0.03463 0.00751 0.00670 0.02024 O31A 4 0.901235 1.001279 0.159838 11.00000 0.05029 0.08078 = 0.07409 0.01321 0.02217 0.02077 O31B 4 0.812868 0.908093 0.210326 11.00000 0.05339 0.08308 = 0.03751 -0.00248 0.00733 0.00911 O35A 4 0.684664 0.822720 -0.091041 11.00000 0.04705 0.10324 = 0.04624 -0.01211 0.02052 -0.02166 AFIX 147 H35 2 0.733283 0.836490 -0.088677 11.00000 -1.50000 AFIX 0 O35B 4 0.597053 0.904693 -0.034544 11.00000 0.03365 0.09990 = 0.05849 0.01537 0.01827 0.00593 MOLE 4 C41 1 0.515441 0.788496 0.078673 11.00000 0.04142 0.06238 = 0.03870 0.00404 0.01610 -0.01061 AFIX 137 H41A 2 0.568457 0.819065 0.108274 11.00000 -1.50000 H41B 2 0.483438 0.876722 0.059967 11.00000 -1.50000 H41C 2 0.521354 0.727722 0.037485 11.00000 -1.50000 AFIX 0 C43 1 0.520625 0.560933 0.150905 11.00000 0.03415 0.04606 = 0.03535 0.00300 0.01264 -0.00005 AFIX 23 H43A 2 0.537178 0.514663 0.109771 11.00000 -1.20000 H43B 2 0.569711 0.586134 0.189531 11.00000 -1.20000 AFIX 0 C44 1 0.472077 0.452004 0.180782 11.00000 0.03699 0.05015 = 0.04814 -0.00033 0.01588 -0.00038 AFIX 23 H44A 2 0.450308 0.501369 0.218123 11.00000 -1.20000 H44B 2 0.426367 0.417363 0.140801 11.00000 -1.20000 AFIX 0 C46 1 0.476346 0.229377 0.253500 11.00000 0.04704 0.06167 = 0.05992 0.00501 0.02089 0.00196 AFIX 137 H46A 2 0.510229 0.146274 0.276612 11.00000 -1.50000 H46B 2 0.427993 0.190926 0.218878 11.00000 -1.50000 H46C 2 0.461174 0.288431 0.291201 11.00000 -1.50000 AFIX 0 C47 1 0.462280 0.789677 0.187233 11.00000 0.03917 0.05779 = 0.05883 -0.00505 0.01841 0.00081 AFIX 137 H47A 2 0.514348 0.819910 0.218892 11.00000 -1.50000 H47B 2 0.433874 0.729397 0.215440 11.00000 -1.50000 H47C 2 0.430487 0.878115 0.168488 11.00000 -1.50000 AFIX 0 C48 1 0.553815 0.236734 0.163534 11.00000 0.04916 0.05820 = 0.06155 0.01743 0.02532 0.02207 AFIX 137 H48A 2 0.509859 0.198610 0.123804 11.00000 -1.50000 H48B 2 0.584907 0.153424 0.189912 11.00000 -1.50000 H48C 2 0.588648 0.299801 0.143034 11.00000 -1.50000 AFIX 0 N42 3 0.474677 0.700652 0.124537 11.00000 0.02633 0.04571 = 0.04529 0.00606 0.01451 -0.00193 AFIX 13 H42 2 0.424543 0.673487 0.095359 11.00000 0.11609 AFIX 0 N45 3 0.521081 0.323702 0.213970 11.00000 0.02687 0.05539 = 0.03168 -0.00771 0.00489 -0.00585 AFIX 13 H45 2 0.564699 0.361698 0.249130 11.00000 0.04762 AFIX 0 MOLE 5 C51 1 0.326035 0.549096 0.002330 11.00000 0.03588 0.05975 = 0.05236 0.00649 0.01329 -0.00044 C52 1 0.245295 0.470012 -0.034990 11.00000 0.05371 0.05888 = 0.05296 -0.00060 0.02308 0.00005 AFIX 23 H52A 2 0.228434 0.411582 0.002659 11.00000 -1.20000 H52B 2 0.204005 0.546972 -0.053181 11.00000 -1.20000 AFIX 0 C53 1 0.247089 0.372150 -0.095307 11.00000 0.04229 0.05970 = 0.06278 -0.00443 0.00702 -0.00887 AFIX 23 H53A 2 0.198389 0.309468 -0.106201 11.00000 -1.20000 H53B 2 0.293922 0.305410 -0.079475 11.00000 -1.20000 AFIX 0 C54 1 0.251536 0.449083 -0.164916 11.00000 0.04341 0.06783 = 0.03942 0.01330 0.01486 -0.00758 AFIX 23 H54A 2 0.262975 0.374255 -0.199100 11.00000 -1.20000 H54B 2 0.296679 0.520330 -0.153315 11.00000 -1.20000 AFIX 0 C55 1 0.174424 0.532637 -0.203253 11.00000 0.03974 0.07949 = 0.02515 -0.00003 0.00577 -0.00191 O51A 4 0.321150 0.641131 0.053317 11.00000 0.04082 0.06592 = 0.03630 -0.00047 0.01521 0.01022 O51B 4 0.384979 0.530780 -0.017935 11.00000 0.03723 0.08048 = 0.04842 -0.01199 0.01711 -0.00774 O55A 4 0.176675 0.602412 -0.264322 11.00000 0.05419 0.09562 = 0.03964 0.00840 0.00676 0.01096 AFIX 147 H55 2 0.222004 0.590913 -0.271852 11.00000 -1.5000 AFIX 0 O55B 4 0.115345 0.530348 -0.182753 11.00000 0.03418 0.10486 = 0.04961 -0.01441 0.01115 -0.01055 HKLF 4 Covalent radii and connectivity table for 06skc0065p21n in P2(1)/n C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1A O1B C2 C2 - C3 C1 C3 - C2 C4 C4 - C5 C3 C5 - O5A O5B C4 O1A - C1 O1B - C1 O5A - C5 O5B - C5 C21 - N22 C23 - N22 C23_$5 C24 - N22 N22 - C23 C21 C24 C31 - O31A O31B C32 C32 - C33 C31 C33 - C32 C34 C34 - C35 C33 C35 - O35B O35A C34 O31A - C31 O31B - C31 O35A - C35 O35B - C35 C41 - N42 C43 - C44 N42 C44 - N45 C43 C46 - N45 C47 - N42 C48 - N45 N42 - C41 C47 C43 N45 - C48 C44 C46 C51 - O51B O51A C52 C52 - C53 C51 C53 - C52 C54 C54 - C53 C55 C55 - O55B O55A C54 O51A - C51 O51B - C51 O55A - C55 O55B - C55 Operators for generating equivalent atoms: $1 -x+1/2, y-1/2, -z+1/2 $2 -x+1, -y+1, -z $3 -x+3/2, y-1/2, -z+1/2 $4 x-1/2, -y+3/2, z-1/2 $5 -x+1, -y-1, -z+1 h k l Fo^2 Sigma Why rejected 0 0 5 19.70 4.84 observed but should be systematically absent 53588 Reflections read, of which 2400 rejected -22 =< h =< 22, -11 =< k =< 11, -24 =< l =< 23, Max. 2-theta = 54.97 1 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 11 1 0 7.38 2.15 18 12.34 14 5 0 76.41 11.90 7 72.00 -12 9 2 -0.38 4.09 3 26.68 10 7 3 12.94 4.19 10 27.40 -13 5 5 -0.14 0.13 10 4.34 9 7 5 42.96 11.66 4 76.81 -11 9 6 16.03 5.76 2 34.91 -16 3 10 77.97 17.79 2 323.67 11 2 11 90.41 27.88 2 477.45 9 4 11 81.56 24.57 3 246.83 -11 5 11 0.45 0.42 7 2.92 -16 7 11 -1.28 4.15 5 24.76 -8 5 13 -0.32 0.14 9 3.67 -4 1 14 -0.14 0.39 12 2.13 -2 9 14 1.86 2.66 4 14.98 2 4 16 11.00 4.79 11 47.22 1 3 17 103.35 37.08 2 575.27 5 3 17 133.39 34.51 2 481.73 -11 5 18 -2.85 2.07 2 30.16 19 Inconsistent equivalents 6444 Unique reflections, of which 0 suppressed R(int) = 0.3562 R(sigma) = 0.3075 Friedel opposites merged Maximum memory for data reduction = 4408 / 64332 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 = 5524 / 460773 wR2 = 0.4538 before cycle 1 for 6444 data and 363 / 363 parameters GooF = S = 1.014; Restrained GooF = 1.014 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.27713 0.00203 0.004 OSF Mean shift/esd = 0.001 Maximum = 0.021 for U11 O55A Max. shift = 0.000 A for H35 Max. dU = 0.000 for H42 Least-squares cycle 2 Maximum vector length = 511 Memory required = 5524 / 460773 wR2 = 0.4538 before cycle 2 for 6444 data and 363 / 363 parameters GooF = S = 1.014; Restrained GooF = 1.014 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.27713 0.00203 0.000 OSF Mean shift/esd = 0.001 Maximum = 0.010 for U11 O55A Max. shift = 0.000 A for H35 Max. dU = 0.000 for H42 Least-squares cycle 3 Maximum vector length = 511 Memory required = 5524 / 460773 wR2 = 0.4538 before cycle 3 for 6444 data and 363 / 363 parameters GooF = S = 1.014; Restrained GooF = 1.014 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.27713 0.00203 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.002 for U11 O55A Max. shift = 0.000 A for H35 Max. dU = 0.000 for H22 Least-squares cycle 4 Maximum vector length = 511 Memory required = 5524 / 460773 wR2 = 0.4538 before cycle 4 for 6444 data and 363 / 363 parameters GooF = S = 1.014; Restrained GooF = 1.014 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.27713 0.00203 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for U11 O55A Max. shift = 0.000 A for H55 Max. dU = 0.000 for H22 Largest correlation matrix elements 0.598 U13 C21 / U11 C21 0.533 U13 C5 / U11 C5 0.525 z C21 / x C21 0.590 U13 C21 / U33 C21 0.532 U13 C5 / U33 C5 0.502 U13 N42 / U11 N42 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2A 0.2651 -0.1035 0.1609 23 0.990 0.000 C2 C3 C1 H2B 0.2938 0.0421 0.2084 23 0.990 0.000 C2 C3 C1 H3A 0.3038 -0.1734 0.2761 23 0.990 0.000 C3 C2 C4 H3B 0.2083 -0.1874 0.2517 23 0.990 0.000 C3 C2 C4 H4A 0.2033 0.0545 0.3080 23 0.990 0.000 C4 C5 C3 H4B 0.2332 -0.0796 0.3633 23 0.990 0.000 C4 C5 C3 H5 0.2678 0.1595 0.4247 83 0.840 0.000 O5B C5 H5 H21A 0.4404 -0.2881 0.5563 137 0.980 0.000 C21 N22 H21A H21B 0.4252 -0.1399 0.5079 137 0.980 0.000 C21 N22 H21A H21C 0.5137 -0.1801 0.5556 137 0.980 0.000 C21 N22 H21A H23A 0.5732 -0.4194 0.5258 23 0.990 0.000 C23 N22 C23_$5 H23B 0.5418 -0.4851 0.4446 23 0.990 0.000 C23 N22 C23_$5 H24A 0.5292 -0.2671 0.3784 137 0.980 0.000 C24 N22 H24A H24B 0.5688 -0.1709 0.4499 137 0.980 0.000 C24 N22 H24A H24C 0.4833 -0.1248 0.3978 137 0.980 0.000 C24 N22 H24A H22 0.4278 -0.3325 0.4325 13 0.930 0.000 N22 C23 C21 C24 H32A 0.7561 1.1787 0.1660 23 0.990 0.000 C32 C33 C31 H32B 0.8052 1.1905 0.1054 23 0.990 0.000 C32 C33 C31 H33A 0.6658 1.1370 0.0557 23 0.990 0.000 C33 C32 C34 H33B 0.6805 0.9798 0.0966 23 0.990 0.000 C33 C32 C34 H34A 0.7468 1.0734 -0.0195 23 0.990 0.000 C34 C35 C33 H34B 0.7788 0.9282 0.0279 23 0.990 0.000 C34 C35 C33 H35 0.7333 0.8365 -0.0887 147 0.840 0.000 O35A C35 H35 H41A 0.5685 0.8191 0.1083 137 0.980 0.000 C41 N42 H41A H41B 0.4834 0.8767 0.0600 137 0.980 0.000 C41 N42 H41A H41C 0.5214 0.7277 0.0375 137 0.980 0.000 C41 N42 H41A H43A 0.5372 0.5147 0.1098 23 0.990 0.000 C43 C44 N42 H43B 0.5697 0.5861 0.1895 23 0.990 0.000 C43 C44 N42 H44A 0.4503 0.5014 0.2181 23 0.990 0.000 C44 N45 C43 H44B 0.4264 0.4174 0.1408 23 0.990 0.000 C44 N45 C43 H46A 0.5102 0.1463 0.2766 137 0.980 0.000 C46 N45 H46A H46B 0.4280 0.1909 0.2189 137 0.980 0.000 C46 N45 H46A H46C 0.4612 0.2884 0.2912 137 0.980 0.000 C46 N45 H46A H47A 0.5143 0.8199 0.2189 137 0.980 0.000 C47 N42 H47A H47B 0.4339 0.7294 0.2154 137 0.980 0.000 C47 N42 H47A H47C 0.4305 0.8781 0.1685 137 0.980 0.000 C47 N42 H47A H48A 0.5099 0.1986 0.1238 137 0.980 0.000 C48 N45 H48A H48B 0.5849 0.1534 0.1899 137 0.980 0.000 C48 N45 H48A H48C 0.5886 0.2998 0.1430 137 0.980 0.000 C48 N45 H48A H42 0.4245 0.6735 0.0954 13 0.930 0.000 N42 C41 C47 C43 H45 0.5647 0.3617 0.2491 13 0.930 0.000 N45 C48 C44 C46 H52A 0.2284 0.4116 0.0027 23 0.990 0.000 C52 C53 C51 H52B 0.2040 0.5470 -0.0532 23 0.990 0.000 C52 C53 C51 H53A 0.1984 0.3095 -0.1062 23 0.990 0.000 C53 C52 C54 H53B 0.2939 0.3054 -0.0795 23 0.990 0.000 C53 C52 C54 H54A 0.2630 0.3743 -0.1991 23 0.990 0.000 C54 C53 C55 H54B 0.2967 0.5203 -0.1533 23 0.990 0.000 C54 C53 C55 H55 0.2220 0.5909 -0.2719 147 0.840 0.000 O55A C55 H55 06skc0065p21n in P2(1)/n ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.17544 0.04114 0.15827 1.00000 0.04852 0.04342 0.03352 -0.00857 0.00269 0.01547 0.04336 0.01500 0.00048 0.00090 0.00044 0.00000 0.00537 0.00509 0.00503 0.00425 0.00418 0.00437 0.00208 C2 0.25112 -0.03416 0.19615 1.00000 0.04680 0.06611 0.05411 -0.01811 0.00343 0.02047 0.05754 0.01652 0.00046 0.00101 0.00047 0.00000 0.00520 0.00603 0.00615 0.00516 0.00454 0.00465 0.00250 H2A 0.26514 -0.10349 0.16089 1.00000 0.06905 0.00000 0.00000 H2B 0.29379 0.04205 0.20836 1.00000 0.06905 0.00000 0.00000 C3 0.25334 -0.11588 0.26186 1.00000 0.10577 0.04937 0.07064 0.01638 0.03886 0.02185 0.07232 0.02098 0.00063 0.00102 0.00052 0.00000 0.00837 0.00623 0.00751 0.00542 0.00638 0.00537 0.00304 H3A 0.30380 -0.17343 0.27615 1.00000 0.08678 0.00000 0.00000 H3B 0.20831 -0.18739 0.25166 1.00000 0.08678 0.00000 0.00000 C4 0.24782 -0.01630 0.32610 1.00000 0.07382 0.07016 0.03742 0.00928 0.01421 0.02189 0.06055 0.01839 0.00055 0.00103 0.00046 0.00000 0.00668 0.00642 0.00548 0.00476 0.00501 0.00556 0.00255 H4A 0.20326 0.05454 0.30798 1.00000 0.07266 0.00000 0.00000 H4B 0.23320 -0.07965 0.36331 1.00000 0.07266 0.00000 0.00000 C5 0.31980 0.06977 0.36301 1.00000 0.06090 0.08450 0.04884 0.03178 0.03542 0.02830 0.06079 0.02199 0.00056 0.00113 0.00051 0.00000 0.00652 0.00728 0.00633 0.00552 0.00540 0.00572 0.00278 O1A 0.11154 0.02239 0.17642 1.00000 0.03640 0.05956 0.04641 0.00310 0.00995 0.00376 0.04764 0.00991 0.00029 0.00058 0.00028 0.00000 0.00304 0.00368 0.00357 0.00283 0.00271 0.00276 0.00148 O1B 0.17815 0.13027 0.10560 1.00000 0.05469 0.06748 0.05496 -0.00854 0.02615 -0.00831 0.05683 0.01055 0.00032 0.00064 0.00032 0.00000 0.00369 0.00419 0.00411 0.00347 0.00312 0.00307 0.00166 O5A 0.38375 0.05925 0.34794 1.00000 0.05251 0.09163 0.08667 0.03560 0.03425 0.01542 0.07393 0.01345 0.00034 0.00073 0.00036 0.00000 0.00376 0.00481 0.00508 0.00402 0.00369 0.00358 0.00204 O5B 0.31426 0.16383 0.41896 1.00000 0.03537 0.10206 0.04630 0.00313 0.00745 -0.00605 0.06187 0.01096 0.00030 0.00072 0.00030 0.00000 0.00319 0.00489 0.00373 0.00364 0.00279 0.00319 0.00175 H5 0.26781 0.15954 0.42466 1.00000 0.09281 0.00000 0.00000 C21 0.46292 -0.22104 0.52607 1.00000 0.06125 0.05474 0.09627 0.00846 0.05192 0.00499 0.06487 0.01917 0.00053 0.00094 0.00054 0.00000 0.00597 0.00584 0.00792 0.00555 0.00584 0.00468 0.00281 H21A 0.44042 -0.28807 0.55627 1.00000 0.09730 0.00000 0.00000 H21B 0.42517 -0.13992 0.50792 1.00000 0.09730 0.00000 0.00000 H21C 0.51365 -0.18010 0.55560 1.00000 0.09730 0.00000 0.00000 C23 0.52459 -0.44331 0.48633 1.00000 0.02751 0.04501 0.04095 0.01063 0.01016 0.00872 0.03761 0.01463 0.00039 0.00079 0.00041 0.00000 0.00402 0.00486 0.00479 0.00389 0.00346 0.00353 0.00191 H23A 0.57321 -0.41940 0.52576 1.00000 0.04513 0.00000 0.00000 H23B 0.54180 -0.48506 0.44456 1.00000 0.04513 0.00000 0.00000 C24 0.51825 -0.20851 0.41833 1.00000 0.04147 0.04536 0.05022 0.01246 0.00208 -0.01277 0.04758 0.01487 0.00044 0.00084 0.00042 0.00000 0.00469 0.00515 0.00544 0.00426 0.00404 0.00395 0.00220 H24A 0.52923 -0.26707 0.37844 1.00000 0.07137 0.00000 0.00000 H24B 0.56875 -0.17089 0.44992 1.00000 0.07137 0.00000 0.00000 H24C 0.48333 -0.12484 0.39781 1.00000 0.07137 0.00000 0.00000 N22 0.47741 -0.30499 0.46266 1.00000 0.03172 0.05305 0.05289 0.00177 0.00424 -0.00277 0.04720 0.01308 0.00037 0.00071 0.00036 0.00000 0.00382 0.00450 0.00450 0.00378 0.00348 0.00345 0.00178 H22 0.42784 -0.33254 0.43252 1.00000 0.08777 0.00000 0.03328 C31 0.83216 1.00056 0.16850 1.00000 0.04615 0.08834 0.02695 -0.00242 0.00902 0.02033 0.05393 0.01722 0.00050 0.00113 0.00045 0.00000 0.00550 0.00730 0.00500 0.00486 0.00433 0.00521 0.00246 C32 0.77574 1.12151 0.12960 1.00000 0.05331 0.05912 0.05052 -0.00863 -0.00469 0.02122 0.05780 0.01626 0.00049 0.00095 0.00047 0.00000 0.00549 0.00586 0.00570 0.00472 0.00465 0.00466 0.00251 H32A 0.75608 1.17872 0.16601 1.00000 0.06936 0.00000 0.00000 H32B 0.80522 1.19055 0.10542 1.00000 0.06936 0.00000 0.00000 C33 0.70598 1.05800 0.07363 1.00000 0.05704 0.07146 0.03666 -0.00284 0.00001 0.02528 0.05739 0.01646 0.00049 0.00102 0.00043 0.00000 0.00568 0.00627 0.00515 0.00466 0.00441 0.00494 0.00251 H33A 0.66582 1.13698 0.05572 1.00000 0.06887 0.00000 0.00000 H33B 0.68055 0.97984 0.09662 1.00000 0.06887 0.00000 0.00000 C34 0.73129 0.99209 0.00918 1.00000 0.04139 0.06508 0.03136 -0.00834 0.00481 0.00898 0.04685 0.01479 0.00044 0.00093 0.00042 0.00000 0.00466 0.00583 0.00473 0.00425 0.00389 0.00427 0.00218 H34A 0.74679 1.07341 -0.01950 1.00000 0.05622 0.00000 0.00000 H34B 0.77883 0.92818 0.02789 1.00000 0.05622 0.00000 0.00000 C35 0.66499 0.90093 -0.04077 1.00000 0.04764 0.08201 0.03463 0.00751 0.00672 0.02025 0.05554 0.01784 0.00052 0.00104 0.00046 0.00000 0.00563 0.00687 0.00538 0.00490 0.00447 0.00521 0.00244 O31A 0.90123 1.00128 0.15984 1.00000 0.05030 0.08077 0.07410 0.01322 0.02217 0.02077 0.06730 0.01245 0.00033 0.00068 0.00034 0.00000 0.00361 0.00455 0.00459 0.00361 0.00336 0.00336 0.00184 O31B 0.81287 0.90809 0.21032 1.00000 0.05338 0.08308 0.03752 -0.00249 0.00733 0.00911 0.05888 0.01097 0.00033 0.00071 0.00032 0.00000 0.00367 0.00451 0.00364 0.00339 0.00296 0.00325 0.00168 O35A 0.68466 0.82272 -0.09104 1.00000 0.04704 0.10325 0.04625 -0.01210 0.02052 -0.02166 0.06396 0.01071 0.00032 0.00076 0.00031 0.00000 0.00363 0.00495 0.00372 0.00370 0.00314 0.00356 0.00181 H35 0.73329 0.83646 -0.08866 1.00000 0.09594 0.00000 0.00000 O35B 0.59705 0.90470 -0.03454 1.00000 0.03364 0.09990 0.05849 0.01537 0.01827 0.00593 0.06285 0.01151 0.00032 0.00070 0.00031 0.00000 0.00326 0.00498 0.00413 0.00347 0.00300 0.00318 0.00185 C41 0.51544 0.78850 0.07867 1.00000 0.04142 0.06238 0.03871 0.00403 0.01610 -0.01061 0.04646 0.01496 0.00044 0.00090 0.00041 0.00000 0.00468 0.00571 0.00493 0.00426 0.00391 0.00407 0.00216 H41A 0.56846 0.81907 0.10827 1.00000 0.06969 0.00000 0.00000 H41B 0.48343 0.87672 0.05996 1.00000 0.06969 0.00000 0.00000 H41C 0.52136 0.72772 0.03749 1.00000 0.06969 0.00000 0.00000 C43 0.52063 0.56093 0.15091 1.00000 0.03415 0.04606 0.03535 0.00299 0.01264 -0.00005 0.03786 0.01431 0.00041 0.00081 0.00040 0.00000 0.00417 0.00477 0.00464 0.00394 0.00364 0.00386 0.00191 H43A 0.53718 0.51466 0.10977 1.00000 0.04544 0.00000 0.00000 H43B 0.56971 0.58613 0.18953 1.00000 0.04544 0.00000 0.00000 C44 0.47208 0.45200 0.18078 1.00000 0.03698 0.05014 0.04815 -0.00033 0.01588 -0.00037 0.04421 0.01536 0.00043 0.00087 0.00044 0.00000 0.00436 0.00516 0.00531 0.00428 0.00402 0.00417 0.00207 H44A 0.45031 0.50136 0.21812 1.00000 0.05306 0.00000 0.00000 H44B 0.42637 0.41736 0.14080 1.00000 0.05306 0.00000 0.00000 C46 0.47635 0.22938 0.25350 1.00000 0.04704 0.06167 0.05993 0.00501 0.02090 0.00195 0.05493 0.01709 0.00048 0.00093 0.00047 0.00000 0.00510 0.00576 0.00599 0.00476 0.00455 0.00447 0.00236 H46A 0.51023 0.14627 0.27661 1.00000 0.08240 0.00000 0.00000 H46B 0.42799 0.19092 0.21888 1.00000 0.08240 0.00000 0.00000 H46C 0.46117 0.28843 0.29120 1.00000 0.08240 0.00000 0.00000 C47 0.46228 0.78968 0.18723 1.00000 0.03916 0.05780 0.05884 -0.00505 0.01840 0.00081 0.05090 0.01574 0.00046 0.00091 0.00045 0.00000 0.00481 0.00575 0.00588 0.00474 0.00437 0.00413 0.00229 H47A 0.51435 0.81991 0.21889 1.00000 0.07635 0.00000 0.00000 H47B 0.43387 0.72940 0.21544 1.00000 0.07635 0.00000 0.00000 H47C 0.43048 0.87811 0.16849 1.00000 0.07635 0.00000 0.00000 C48 0.55381 0.23673 0.16353 1.00000 0.04916 0.05819 0.06155 0.01743 0.02532 0.02206 0.05428 0.01797 0.00048 0.00092 0.00047 0.00000 0.00518 0.00561 0.00597 0.00477 0.00469 0.00445 0.00243 H48A 0.50986 0.19861 0.12380 1.00000 0.08142 0.00000 0.00000 H48B 0.58491 0.15342 0.18991 1.00000 0.08142 0.00000 0.00000 H48C 0.58865 0.29980 0.14303 1.00000 0.08142 0.00000 0.00000 N42 0.47468 0.70065 0.12454 1.00000 0.02634 0.04571 0.04530 0.00606 0.01452 -0.00193 0.03816 0.01228 0.00034 0.00066 0.00033 0.00000 0.00361 0.00416 0.00417 0.00333 0.00324 0.00303 0.00165 H42 0.42454 0.67349 0.09536 1.00000 0.11621 0.00000 0.04099 N45 0.52108 0.32370 0.21397 1.00000 0.02687 0.05540 0.03168 -0.00772 0.00489 -0.00585 0.03852 0.01168 0.00034 0.00070 0.00032 0.00000 0.00345 0.00421 0.00363 0.00342 0.00308 0.00332 0.00161 H45 0.56470 0.36170 0.24913 1.00000 0.04763 0.00000 0.02298 C51 0.32604 0.54909 0.00233 1.00000 0.03587 0.05976 0.05234 0.00649 0.01329 -0.00045 0.04901 0.01669 0.00046 0.00097 0.00048 0.00000 0.00494 0.00581 0.00598 0.00492 0.00448 0.00446 0.00224 C52 0.24530 0.47001 -0.03499 1.00000 0.05370 0.05889 0.05297 -0.00060 0.02308 0.00005 0.05348 0.01615 0.00047 0.00096 0.00046 0.00000 0.00544 0.00569 0.00601 0.00479 0.00459 0.00459 0.00235 H52A 0.22843 0.41158 0.00266 1.00000 0.06418 0.00000 0.00000 H52B 0.20401 0.54697 -0.05318 1.00000 0.06418 0.00000 0.00000 C53 0.24709 0.37215 -0.09531 1.00000 0.04230 0.05970 0.06279 -0.00443 0.00703 -0.00887 0.05622 0.01602 0.00047 0.00098 0.00047 0.00000 0.00526 0.00609 0.00639 0.00506 0.00465 0.00431 0.00248 H53A 0.19839 0.30947 -0.10620 1.00000 0.06747 0.00000 0.00000 H53B 0.29392 0.30541 -0.07948 1.00000 0.06747 0.00000 0.00000 C54 0.25154 0.44908 -0.16491 1.00000 0.04340 0.06784 0.03943 0.01330 0.01487 -0.00759 0.04948 0.01613 0.00044 0.00097 0.00043 0.00000 0.00482 0.00581 0.00519 0.00442 0.00404 0.00438 0.00223 H54A 0.26298 0.37426 -0.19910 1.00000 0.05937 0.00000 0.00000 H54B 0.29668 0.52033 -0.15331 1.00000 0.05937 0.00000 0.00000 C55 0.17442 0.53264 -0.20325 1.00000 0.03972 0.07948 0.02518 -0.00005 0.00577 -0.00191 0.04866 0.01549 0.00047 0.00101 0.00043 0.00000 0.00509 0.00653 0.00496 0.00452 0.00405 0.00470 0.00226 O51A 0.32115 0.64113 0.05332 1.00000 0.04082 0.06593 0.03630 -0.00047 0.01521 0.01022 0.04673 0.01043 0.00028 0.00062 0.00028 0.00000 0.00322 0.00382 0.00334 0.00294 0.00262 0.00273 0.00148 O51B 0.38498 0.53078 -0.01793 1.00000 0.03723 0.08049 0.04842 -0.01199 0.01711 -0.00775 0.05428 0.01003 0.00030 0.00064 0.00029 0.00000 0.00309 0.00430 0.00368 0.00314 0.00278 0.00302 0.00162 O55A 0.17668 0.60241 -0.26433 1.00000 0.05431 0.09552 0.03958 0.00840 0.00671 0.01093 0.06421 0.01218 0.00033 0.00074 0.00031 0.00000 0.00374 0.00491 0.00371 0.00346 0.00301 0.00361 0.00180 H55 0.22202 0.59091 -0.27185 1.00000 0.09632 0.00000 0.00000 O55B 0.11535 0.53035 -0.18275 1.00000 0.03417 0.10486 0.04962 -0.01441 0.01114 -0.01054 0.06287 0.01053 0.00031 0.00072 0.00031 0.00000 0.00312 0.00502 0.00389 0.00349 0.00287 0.00333 0.00182 Final Structure Factor Calculation for 06skc0065p21n in P2(1)/n Total number of l.s. parameters = 363 Maximum vector length = 511 Memory required = 5161 / 22995 wR2 = 0.4538 before cycle 5 for 6444 data and 0 / 363 parameters GooF = S = 1.014; Restrained GooF = 1.014 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.1472 for 1866 Fo > 4sig(Fo) and 0.3760 for all 6444 data wR2 = 0.4538, GooF = S = 1.014, Restrained GooF = 1.014 for all data Occupancy sum of asymmetric unit = 39.00 for non-hydrogen and 48.00 for hydrogen atoms Principal mean square atomic displacements U 0.0702 0.0328 0.0271 C1 0.0969 0.0439 0.0319 C2 0.1170 0.0604 0.0396 C3 0.0940 0.0527 0.0349 C4 0.1164 0.0424 0.0236 C5 0.0605 0.0466 0.0358 O1A 0.0765 0.0550 0.0390 O1B 0.1267 0.0549 0.0402 O5A 0.1031 0.0479 0.0347 O5B 0.1094 0.0533 0.0318 C21 0.0545 0.0344 0.0239 C23 0.0747 0.0385 0.0295 C24 0.0591 0.0517 0.0308 N22 0.0976 0.0379 0.0262 C31 0.0948 0.0455 0.0332 C32 0.0963 0.0441 0.0318 C33 0.0722 0.0390 0.0293 C34 0.0914 0.0441 0.0311 C35 0.0964 0.0665 0.0391 O31A 0.0867 0.0528 0.0371 O31B 0.1118 0.0458 0.0343 O35A 0.1051 0.0536 0.0299 O35B 0.0675 0.0436 0.0283 C41 0.0468 0.0371 0.0296 C43 0.0503 0.0488 0.0336 C44 0.0666 0.0566 0.0416 C46 0.0634 0.0540 0.0353 C47 0.0861 0.0458 0.0309 C48 0.0516 0.0406 0.0223 N42 0.0580 0.0334 0.0242 N45 0.0637 0.0486 0.0347 C51 0.0605 0.0588 0.0411 C52 0.0675 0.0634 0.0378 C53 0.0756 0.0450 0.0279 C54 0.0796 0.0413 0.0251 C55 0.0696 0.0410 0.0295 O51A 0.0852 0.0451 0.0326 O51B 0.0985 0.0572 0.0370 O55A 0.1089 0.0471 0.0326 O55B Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.003 0.005 0.008 0.010 0.014 0.018 0.024 0.032 0.052 1.000 Number in group 877. 550. 725. 459. 768. 575. 630. 568. 656. 636. GooF 0.966 0.942 0.973 1.035 0.975 1.007 1.029 1.073 1.146 1.009 K 38.744 23.830 6.407 7.181 1.679 1.411 1.357 1.103 0.950 1.054 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.15 1.32 1.66 inf Number in group 644. 648. 642. 658. 642. 630. 643. 646. 646. 645. GooF 0.861 0.861 0.899 1.020 1.034 1.080 1.077 1.062 1.066 1.138 K 0.157 1.152 1.636 2.280 2.643 1.269 1.084 1.107 1.123 1.034 R1 0.697 0.686 0.639 0.598 0.544 0.405 0.282 0.204 0.155 0.091 Recommended weighting scheme: WGHT 0.2000 0.0000 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) -10 6 3 720.64 253.60 4.57 0.042 1.13 14 6 9 2.10 202.16 4.43 0.037 0.79 -2 2 1 158.28 26.32 3.79 0.013 3.98 14 1 9 12931.08 10.68 3.73 0.009 0.92 3 2 1 89.97 0.15 3.66 0.001 3.34 4 5 1 100.22 9.76 3.66 0.008 1.63 -7 2 3 219.77 90.55 3.62 0.025 2.15 1 7 15 521.61 79.21 3.61 0.023 0.87 -1 8 3 1096.89 448.33 3.56 0.056 1.11 3 1 1 62.04 1.15 3.52 0.003 4.35 1 1 1 85.26 12.12 3.49 0.009 6.96 10 4 2 146.87 17.78 3.47 0.011 1.29 2 1 2 129.45 41.90 3.43 0.017 4.68 -1 3 8 125.17 2.55 3.38 0.004 1.85 13 4 8 428.10 9.94 3.37 0.008 0.92 5 3 13 395.96 140.07 3.37 0.031 1.10 -3 1 18 192.76 0.03 3.33 0.000 1.04 17 2 6 -49.28 394.94 3.33 0.052 0.85 -15 4 5 176.23 9.60 3.31 0.008 1.03 -2 1 4 195.95 78.79 3.27 0.023 4.06 -15 4 9 1462.09 666.55 3.25 0.068 0.99 7 1 9 121.95 18.61 3.20 0.011 1.36 13 2 10 15004.99 3.11 3.18 0.005 0.92 0 7 10 200.65 33.35 3.18 0.015 1.05 -10 3 13 114.83 5.69 3.14 0.006 1.15 8 5 0 1288.70 704.17 3.13 0.070 1.36 -15 2 1 116.63 0.00 3.13 0.000 1.10 -2 1 20 12457.00 11.58 3.11 0.009 0.93 4 0 20 484.32 96.86 3.10 0.026 0.85 6 8 3 -26.29 138.73 3.09 0.031 1.01 5 7 7 -40.89 76.42 3.08 0.023 1.05 2 1 1 59.11 10.64 3.03 0.009 5.49 4 1 1 102.70 31.97 3.02 0.015 3.54 -14 2 10 102.47 0.05 3.01 0.001 1.11 -8 4 7 2.40 108.21 3.01 0.027 1.45 -3 7 7 120.94 8.62 2.99 0.008 1.16 4 0 8 339.04 123.08 2.95 0.029 1.81 -9 1 11 100.73 24.31 2.95 0.013 1.42 -13 5 15 -99.50 132.01 2.94 0.030 0.89 4 2 17 614.85 296.36 2.91 0.045 0.96 -4 1 6 178.29 75.92 2.90 0.023 2.71 -11 1 20 279.39 40.18 2.90 0.017 0.89 -4 1 10 85.15 3.43 2.89 0.005 1.82 -17 1 6 386.99 179.64 2.89 0.035 1.01 9 5 13 277.14 5.30 2.87 0.006 0.87 -5 1 1 72.27 11.17 2.87 0.009 3.22 -3 5 8 97.48 4.47 2.86 0.006 1.43 -6 7 3 139.73 311.54 2.83 0.046 1.17 11 3 5 136.63 0.10 2.82 0.001 1.18 11 1 12 329.03 49.24 2.81 0.018 0.95 Bond lengths and angles C1 - Distance Angles O1A 1.2531 (0.0086) O1B 1.2907 (0.0090) 120.69 (0.70) C2 1.4813 (0.0104) 122.49 (0.81) 116.81 (0.77) C1 - O1A O1B C2 - Distance Angles C3 1.4374 (0.0115) C1 1.4813 (0.0104) 118.14 (0.80) H2A 0.9900 107.77 107.77 H2B 0.9900 107.77 107.77 107.13 C2 - C3 C1 H2A C3 - Distance Angles C2 1.4374 (0.0115) C4 1.5343 (0.0117) 113.17 (0.74) H3A 0.9900 108.94 108.94 H3B 0.9900 108.94 108.94 107.75 C3 - C2 C4 H3A C4 - Distance Angles C5 1.4771 (0.0126) C3 1.5343 (0.0117) 117.44 (0.79) H4A 0.9900 107.94 107.94 H4B 0.9900 107.94 107.94 107.22 C4 - C5 C3 H4A C5 - Distance Angles O5A 1.2175 (0.0086) O5B 1.3793 (0.0107) 118.65 (0.97) C4 1.4771 (0.0126) 123.61 (0.95) 117.71 (0.68) C5 - O5A O5B O1A - Distance Angles C1 1.2531 (0.0086) O1A - O1B - Distance Angles C1 1.2907 (0.0090) O1B - O5A - Distance Angles C5 1.2175 (0.0086) O5A - O5B - Distance Angles C5 1.3793 (0.0107) H5 0.8400 109.47 O5B - C5 C21 - Distance Angles N22 1.4950 (0.0100) H21A 0.9800 109.47 H21B 0.9800 109.47 109.47 H21C 0.9800 109.47 109.47 109.47 C21 - N22 H21A H21B C23 - Distance Angles N22 1.4924 (0.0087) C23_$5 1.5061 (0.0130) 110.81 (0.66) H23A 0.9900 109.48 109.48 H23B 0.9900 109.48 109.48 108.06 C23 - N22 C23_$5 H23A C24 - Distance Angles N22 1.5076 (0.0087) H24A 0.9800 109.47 H24B 0.9800 109.47 109.47 H24C 0.9800 109.47 109.47 109.47 C24 - N22 H24A H24B N22 - Distance Angles C23 1.4924 (0.0087) C21 1.4950 (0.0100) 112.07 (0.62) C24 1.5076 (0.0087) 110.41 (0.54) 110.98 (0.62) H22 0.9300 107.73 107.73 107.73 N22 - C23 C21 C24 C31 - Distance Angles O31A 1.2489 (0.0089) O31B 1.2538 (0.0096) 120.67 (0.81) C32 1.5177 (0.0117) 116.63 (0.87) 122.61 (0.75) C31 - O31A O31B C32 - Distance Angles C33 1.4941 (0.0113) C31 1.5177 (0.0117) 111.41 (0.72) H32A 0.9900 109.34 109.34 H32B 0.9900 109.34 109.34 107.98 C32 - C33 C31 H32A C33 - Distance Angles C32 1.4941 (0.0114) C34 1.5217 (0.0100) 111.62 (0.68) H33A 0.9900 109.30 109.30 H33B 0.9900 109.30 109.30 107.96 C33 - C32 C34 H33A C34 - Distance Angles C35 1.5207 (0.0113) C33 1.5217 (0.0099) 112.31 (0.65) H34A 0.9900 109.14 109.14 H34B 0.9900 109.14 109.14 107.87 C34 - C35 C33 H34A C35 - Distance Angles O35B 1.2127 (0.0088) O35A 1.2998 (0.0092) 122.31 (0.84) C34 1.5207 (0.0113) 121.09 (0.78) 116.58 (0.70) C35 - O35B O35A O31A - Distance Angles C31 1.2489 (0.0089) O31A - O31B - Distance Angles C31 1.2538 (0.0096) O31B - O35A - Distance Angles C35 1.2998 (0.0092) H35 0.8400 109.47 O35A - C35 O35B - Distance Angles C35 1.2127 (0.0088) O35B - C41 - Distance Angles N42 1.4837 (0.0082) H41A 0.9800 109.47 H41B 0.9800 109.47 109.47 H41C 0.9800 109.47 109.47 109.47 C41 - N42 H41A H41B C43 - Distance Angles C44 1.4966 (0.0100) N42 1.5021 (0.0088) 111.98 (0.56) H43A 0.9900 109.22 109.22 H43B 0.9900 109.22 109.22 107.91 C43 - C44 N42 H43A C44 - Distance Angles N45 1.4727 (0.0091) C43 1.4966 (0.0101) 111.00 (0.58) H44A 0.9900 109.44 109.44 H44B 0.9900 109.44 109.44 108.04 C44 - N45 C43 H44A C46 - Distance Angles N45 1.4790 (0.0088) H46A 0.9800 109.47 H46B 0.9800 109.47 109.47 H46C 0.9800 109.47 109.47 109.47 C46 - N45 H46A H46B C47 - Distance Angles N42 1.4942 (0.0089) H47A 0.9800 109.47 H47B 0.9800 109.47 109.47 H47C 0.9800 109.47 109.47 109.47 C47 - N42 H47A H47B C48 - Distance Angles N45 1.4602 (0.0088) H48A 0.9800 109.47 H48B 0.9800 109.47 109.47 H48C 0.9800 109.47 109.47 109.47 C48 - N45 H48A H48B N42 - Distance Angles C41 1.4837 (0.0083) C47 1.4942 (0.0089) 111.64 (0.59) C43 1.5021 (0.0088) 110.46 (0.52) 111.11 (0.56) H42 0.9300 107.82 107.82 107.82 N42 - C41 C47 C43 N45 - Distance Angles C48 1.4602 (0.0088) C44 1.4727 (0.0091) 114.92 (0.59) C46 1.4790 (0.0088) 111.59 (0.62) 110.32 (0.55) H45 0.9300 106.49 106.49 106.49 N45 - C48 C44 C46 C51 - Distance Angles O51B 1.1924 (0.0082) O51A 1.2921 (0.0093) 124.02 (0.77) C52 1.5615 (0.0110) 122.06 (0.81) 113.80 (0.67) C51 - O51B O51A C52 - Distance Angles C53 1.4495 (0.0109) C51 1.5615 (0.0110) 115.55 (0.68) H52A 0.9900 108.39 108.39 H52B 0.9900 108.39 108.39 107.45 C52 - C53 C51 H52A C53 - Distance Angles C52 1.4495 (0.0109) C54 1.5088 (0.0105) 115.17 (0.76) H53A 0.9900 108.48 108.48 H53B 0.9900 108.48 108.48 107.50 C53 - C52 C54 H53A C54 - Distance Angles C53 1.5088 (0.0105) C55 1.5373 (0.0108) 113.53 (0.63) H54A 0.9900 108.86 108.86 H54B 0.9900 108.86 108.86 107.71 C54 - C53 C55 H54A C55 - Distance Angles O55B 1.1858 (0.0080) O55A 1.3257 (0.0089) 121.35 (0.78) C54 1.5373 (0.0108) 123.58 (0.76) 114.97 (0.64) C55 - O55B O55A O51A - Distance Angles C51 1.2921 (0.0093) O51A - O51B - Distance Angles C51 1.1924 (0.0081) O51B - O55A - Distance Angles C55 1.3257 (0.0089) H55 0.8400 109.47 O55A - C55 O55B - Distance Angles C55 1.1858 (0.0080) O55B - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.93 1.78 2.697(8) 168.2 N42-H42...O51A 0.93 2.44 3.133(8) 131.5 N42-H42...O51B 0.84 1.71 2.542(7) 172.8 O5B-H5...O51A_$1 0.93 1.82 2.725(9) 164.7 N22-H22...O1B_$1 0.93 2.38 3.095(8) 133.1 N22-H22...O1A_$1 0.84 1.67 2.498(7) 166.2 O35A-H35...O1B_$2 0.93 2.09 2.895(8) 144.2 N45-H45...O31A_$3 0.93 2.10 2.953(8) 152.4 N45-H45...O31B_$3 0.84 1.69 2.528(8) 172.4 O55A-H55...O31B_$4 Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane) - 2.0765 (0.2033) x + 6.4799 (0.0734) y - 11.8957 (0.0771) z = 2.8534 (0.1121) * 0.0000 (0.0000) C51 * 0.0000 (0.0000) O51A * 0.0000 (0.0000) O51B Rms deviation of fitted atoms = 0.0000 2.7374 (0.2047) x + 7.5539 (0.0658) y + 8.7316 (0.1111) z = 2.7262 (0.0374) Angle to previous plane (with approximate esd) = 76.86 ( 0.60 ) * 0.0000 (0.0000) C55 * 0.0000 (0.0000) O55A * 0.0000 (0.0000) O55B Rms deviation of fitted atoms = 0.0000 FMAP and GRID set by program FMAP 2 3 25 GRID -1.136 -2 -2 1.136 2 2 R1 = 0.3759 for 6444 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.58 at 0.7411 0.0164 0.1334 [ 1.13 A from C32 ] Deepest hole -0.39 at 0.7592 0.4490 0.0723 [ 0.81 A from H52B ] Mean = 0.00, Rms deviation from mean = 0.08 e/A^3, Highest memory used = 4957 / 29388 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.7411 1.0164 0.1334 1.00000 0.05 0.58 1.13 C32 1.14 H33B 1.19 C33 1.55 C31 Q2 1 0.7517 1.1367 0.0713 1.00000 0.05 0.54 1.07 C33 1.08 C32 1.09 H32B 1.44 H33A Q3 1 0.6617 0.9308 -0.1126 1.00000 0.05 0.53 1.09 O35A 1.37 C35 1.47 H35 2.09 O35B Q4 1 0.4185 0.1196 0.3905 1.00000 0.05 0.51 1.03 O5A 1.44 H21C 1.71 C5 2.05 O5B Q5 1 0.3011 -0.0393 0.2644 1.00000 0.05 0.45 1.07 C3 1.23 H3A 1.27 H2B 1.35 C2 Q6 1 0.1994 0.6918 -0.2442 1.00000 0.05 0.42 0.93 O55A 1.17 H55 1.74 C55 1.88 H32A Q7 1 0.8233 0.8420 0.2333 1.00000 0.05 0.41 0.73 O31B 1.83 H55 1.89 H45 1.91 C31 Q8 1 0.8775 0.9574 0.1386 1.00000 0.05 0.39 0.63 O31A 1.15 C31 2.02 O31B 2.27 H45 Q9 1 0.4244 -0.2502 0.4818 1.00000 0.05 0.39 0.96 C21 1.11 H21B 1.18 N22 1.21 H22 Q10 1 0.2292 -0.1379 0.2107 1.00000 0.05 0.38 0.97 C3 1.04 H3B 1.07 C2 1.30 H2A Shortest distances between peaks (including symmetry equivalents) 5 10 1.64 1 2 1.64 6 7 2.31 1 8 2.40 7 8 2.46 1 7 2.58 2 8 2.74 Time profile in seconds ----------------------- 0.11: Read and process instructions 0.00: Fit rigid groups 0.02: 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 0.02: Analyse other restraints etc. 2.48: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 2.77: Structure factors and derivatives 5.31: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.42: Solve l.s. equations 0.00: Generate HTAB table 0.05: Other dependent quantities, CIF, tables 0.14: Analysis of variance 0.05: Merge reflections for Fourier and .fcf 0.06: Fourier summations 0.03: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 06skc0065p21n finished at 09:53:44 Total CPU time: 11.5 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++