++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XL - CRYSTAL STRUCTURE REFINEMENT - SHELXTL Ver. 6.12 W95/98/NT/2000/ME + + Copyright(c) 2001 Bruker Analytical X-ray Solutions All Rights Reserved + + bas07 started at 15:46:22 on 23-Jan-2007 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL bas07 in P-1 CELL 0.71073 11.1642 11.9757 15.3867 108.556 104.156 93.044 ZERR 2.00 0.0116 0.0126 0.0159 0.021 0.021 0.024 LATT 1 SFAC C H N CL CR O UNIT 76 108 6 4 2 4 V = 1871.74 F(000) = 754.0 Mu = 0.48 mm-1 Cell Wt = 1415.48 Rho = 1.256 TEMP -50 ACTA 45 CONF SIZE 0.15 0.25 0.25 L.S. 20 BOND $H FMAP 2 PLAN 10 wpdb WGHT 0.0799 0.4239 FVAR 0.17247 CR1 5 0.788726 0.337214 0.111142 11.00000 0.04043 0.02668 = 0.02627 0.00995 0.00473 -0.00251 CL1 4 0.915425 0.499916 0.226164 11.00000 0.05748 0.03514 = 0.03666 0.00578 0.00311 -0.01082 CL2 4 0.740953 0.430476 -0.000166 11.00000 0.06966 0.03719 = 0.03757 0.01971 0.00165 -0.00764 O1 6 0.634518 0.389817 0.150633 11.00000 0.04738 0.03073 = 0.03870 0.01073 0.00982 0.00595 O2 6 0.937824 0.281311 0.061970 11.00000 0.04660 0.03066 = 0.04132 0.01203 0.01685 -0.00386 N1 3 0.821481 0.247242 0.211075 11.00000 0.03490 0.02862 = 0.02351 0.00926 0.00464 0.00105 N2 3 0.690761 0.172168 0.024342 11.00000 0.03380 0.02519 = 0.02531 0.00792 0.00558 0.00078 N3 3 0.522924 0.091998 -0.226476 11.00000 0.04513 0.03278 = 0.03074 0.01376 0.00353 -0.00248 C1 1 0.884103 0.287155 0.313502 11.00000 0.04669 0.02336 = 0.02346 0.00775 0.00162 -0.00433 C2 1 0.814017 0.317619 0.378701 11.00000 0.05390 0.03067 = 0.03094 0.01139 0.00746 0.00243 C3 1 0.875773 0.346796 0.475751 11.00000 0.06890 0.05155 = 0.03228 0.01539 0.01403 0.00999 AFIX 43 H3A 2 0.829833 0.367548 0.520823 11.00000 -1.20000 AFIX 0 C4 1 1.001680 0.345729 0.506364 11.00000 0.07562 0.06165 = 0.02761 0.01297 -0.00941 -0.00148 AFIX 43 H4A 2 1.041296 0.363715 0.571557 11.00000 -1.20000 AFIX 0 C5 1 1.068948 0.318219 0.441016 11.00000 0.05100 0.06307 = 0.03762 0.01781 -0.00550 -0.00351 AFIX 43 H5A 2 1.155522 0.319262 0.462562 11.00000 -1.20000 AFIX 0 C6 1 1.013330 0.288538 0.343089 11.00000 0.04353 0.04665 = 0.03740 0.01702 0.00085 0.00009 C7 1 1.090808 0.256019 0.273644 11.00000 0.04314 0.08477 = 0.04409 0.02679 0.00465 0.00672 AFIX 13 H7A 2 1.038938 0.254340 0.210925 11.00000 -1.20000 AFIX 0 C8 1 1.128375 0.132866 0.261419 11.00000 0.07882 0.09201 = 0.07720 0.02146 0.02672 0.02447 AFIX 137 H8A 2 1.054230 0.075073 0.242220 11.00000 -1.50000 H8B 2 1.182129 0.132824 0.321382 11.00000 -1.50000 H8C 2 1.172721 0.112173 0.212859 11.00000 -1.50000 AFIX 0 C9 1 1.205830 0.348109 0.303074 11.00000 0.05215 0.13231 = 0.07400 0.04565 0.00642 -0.01365 AFIX 137 H9A 2 1.180467 0.425988 0.310014 11.00000 -1.50000 H9B 2 1.250322 0.327503 0.254604 11.00000 -1.50000 H9C 2 1.259991 0.349510 0.363355 11.00000 -1.50000 AFIX 0 C10 1 0.672849 0.317700 0.348887 11.00000 0.05640 0.04703 = 0.03438 0.01486 0.01554 0.00760 AFIX 13 H10A 2 0.650460 0.321269 0.283566 11.00000 -1.20000 AFIX 0 C11 1 0.633085 0.426980 0.412961 11.00000 0.07564 0.06544 = 0.06244 0.01446 0.02498 0.02226 AFIX 137 H11A 2 0.680211 0.498496 0.414770 11.00000 -1.50000 H11B 2 0.649114 0.423842 0.476950 11.00000 -1.50000 H11C 2 0.544695 0.427951 0.387825 11.00000 -1.50000 AFIX 0 C12 1 0.600815 0.207125 0.345181 11.00000 0.06475 0.05042 = 0.05682 0.01546 0.01759 -0.00247 AFIX 137 H12A 2 0.627272 0.138269 0.304944 11.00000 -1.50000 H12B 2 0.512477 0.207350 0.319133 11.00000 -1.50000 H12C 2 0.615798 0.203768 0.409053 11.00000 -1.50000 AFIX 0 C13 1 0.776480 0.137028 0.170936 11.00000 0.03764 0.02983 = 0.02929 0.01403 0.00685 0.00275 AFIX 43 H13A 2 0.787176 0.085708 0.206604 11.00000 -1.20000 AFIX 0 C14 1 0.709845 0.091587 0.071807 11.00000 0.03417 0.02997 = 0.02846 0.01336 0.00863 -0.00031 C15 1 0.661610 -0.022857 0.010227 11.00000 0.04234 0.02632 = 0.03590 0.01318 0.00763 -0.00367 AFIX 43 H15A 2 0.662929 -0.092829 0.025567 11.00000 -1.20000 AFIX 0 C16 1 0.610528 -0.013866 -0.079308 11.00000 0.04589 0.02866 = 0.02818 0.00522 0.00651 -0.00311 AFIX 43 H16A 2 0.571280 -0.077000 -0.136058 11.00000 -1.20000 AFIX 0 C17 1 0.628513 0.105051 -0.068779 11.00000 0.03605 0.02653 = 0.02672 0.00847 0.00647 -0.00066 C18 1 0.586028 0.157749 -0.142494 11.00000 0.03956 0.02744 = 0.02900 0.00880 0.00804 0.00003 AFIX 43 H18A 2 0.605120 0.240132 -0.128154 11.00000 -1.20000 AFIX 0 C19 1 0.486746 0.146314 -0.297246 11.00000 0.04759 0.02016 = 0.02419 0.00585 0.00521 -0.00038 C20 1 0.358660 0.149029 -0.332642 11.00000 0.05022 0.03189 = 0.03471 0.01181 0.01134 0.00484 C21 1 0.320781 0.199148 -0.403060 11.00000 0.05085 0.05520 = 0.04707 0.02777 0.00691 0.00896 AFIX 43 H21A 2 0.235650 0.203053 -0.426555 11.00000 -1.20000 AFIX 0 C22 1 0.406667 0.242876 -0.438434 11.00000 0.06254 0.05410 = 0.04462 0.02944 0.01040 0.01038 AFIX 43 H22A 2 0.380619 0.278532 -0.484890 11.00000 -1.20000 AFIX 0 C23 1 0.530678 0.234761 -0.406217 11.00000 0.05785 0.05274 = 0.03956 0.02368 0.01809 0.00516 AFIX 43 H23A 2 0.588040 0.262275 -0.433096 11.00000 -1.20000 AFIX 0 C24 1 0.574108 0.186827 -0.334681 11.00000 0.04851 0.03416 = 0.03351 0.01245 0.01197 0.00196 C25 1 0.265258 0.098903 -0.294301 11.00000 0.05382 0.03845 = 0.05506 0.02339 0.01571 0.00278 AFIX 13 H25A 2 0.304241 0.039066 -0.269137 11.00000 -1.20000 AFIX 0 C26 1 0.237654 0.191302 -0.211669 11.00000 0.10143 0.06838 = 0.09340 0.03371 0.06506 0.01460 AFIX 137 H26A 2 0.315260 0.230831 -0.163691 11.00000 -1.50000 H26B 2 0.185522 0.153171 -0.184197 11.00000 -1.50000 H26C 2 0.194401 0.249413 -0.233900 11.00000 -1.50000 AFIX 0 C27 1 0.144469 0.033348 -0.370738 11.00000 0.05619 0.11161 = 0.08029 0.04179 0.00622 -0.01950 AFIX 137 H27A 2 0.164259 -0.026714 -0.422607 11.00000 -1.50000 H27B 2 0.100371 0.089666 -0.394907 11.00000 -1.50000 H27C 2 0.092219 -0.004456 -0.343146 11.00000 -1.50000 AFIX 0 C28 1 0.712139 0.174213 -0.305836 11.00000 0.04789 0.08401 = 0.05642 0.04310 0.01835 0.00859 AFIX 13 H28A 2 0.725059 0.135018 -0.257163 11.00000 -1.20000 AFIX 0 C29 1 0.793898 0.292840 -0.263169 11.00000 0.06092 0.10782 = 0.10490 0.02528 0.01371 -0.02131 AFIX 137 H29A 2 0.880588 0.281067 -0.245406 11.00000 -1.50000 H29B 2 0.771862 0.340836 -0.206991 11.00000 -1.50000 H29C 2 0.782021 0.333193 -0.309568 11.00000 -1.50000 AFIX 0 C30 1 0.750391 0.095735 -0.391388 11.00000 0.09119 0.10928 = 0.10003 0.02709 0.03851 0.05725 AFIX 137 H30A 2 0.838042 0.087904 -0.371727 11.00000 -1.50000 H30B 2 0.736716 0.131720 -0.440615 11.00000 -1.50000 H30C 2 0.700729 0.017697 -0.416204 11.00000 -1.50000 AFIX 0 C31 1 0.511662 0.331627 0.092991 11.00000 0.04108 0.05150 = 0.07101 0.00756 0.01294 0.00105 AFIX 23 H31A 2 0.501294 0.247360 0.086608 11.00000 -1.20000 H31B 2 0.494841 0.338036 0.029318 11.00000 -1.20000 AFIX 0 C32 1 0.427748 0.398315 0.147472 11.00000 0.05726 0.09660 = 0.08265 0.03136 0.02257 0.03046 AFIX 23 H32A 2 0.345600 0.394660 0.104540 11.00000 -1.20000 H32B 2 0.416947 0.365375 0.196225 11.00000 -1.20000 AFIX 0 C33 1 0.492563 0.521922 0.191832 11.00000 0.08283 0.07998 = 0.10182 -0.01273 -0.02132 0.04652 AFIX 23 H33A 2 0.481001 0.558370 0.255419 11.00000 -1.20000 H33B 2 0.459900 0.569773 0.152602 11.00000 -1.20000 AFIX 0 C34 1 0.626097 0.514724 0.198404 11.00000 0.08482 0.03290 = 0.06872 0.00755 0.02048 0.01803 AFIX 23 H34A 2 0.657202 0.564817 0.166915 11.00000 -1.20000 H34B 2 0.675599 0.541462 0.265291 11.00000 -1.20000 AFIX 0 C35 1 1.032566 0.365071 0.054391 11.00000 0.05159 0.04798 = 0.06426 0.01955 0.02226 -0.00937 AFIX 23 H35A 2 0.996055 0.433306 0.042597 11.00000 -1.20000 H35B 2 1.101432 0.394134 0.113120 11.00000 -1.20000 AFIX 0 C36 1 1.076511 0.296936 -0.026256 11.00000 0.08810 0.07283 = 0.08284 0.00601 0.04552 -0.02411 AFIX 23 H36A 2 1.029762 0.307273 -0.085331 11.00000 -1.20000 H36B 2 1.165496 0.322286 -0.015182 11.00000 -1.20000 AFIX 0 C37 1 1.054408 0.173116 -0.031804 11.00000 0.12900 0.06233 = 0.17357 0.02583 0.11583 0.01041 AFIX 23 H37A 2 1.037581 0.119240 -0.097836 11.00000 -1.20000 H37B 2 1.127153 0.152637 0.007475 11.00000 -1.20000 AFIX 0 C38 1 0.947088 0.164482 0.003615 11.00000 0.07397 0.04075 = 0.08495 0.01084 0.04732 0.00290 AFIX 23 H38A 2 0.871338 0.132609 -0.049664 11.00000 -1.20000 H38B 2 0.957129 0.111232 0.041032 11.00000 -1.20000 HKLF 4 Covalent radii and connectivity table for bas07 in P-1 C 0.770 H 0.320 N 0.700 CL 0.990 CR 1.240 O 0.660 Cr1 - O1 O2 N2 N1 Cl1 Cl2 Cl1 - Cr1 Cl2 - Cr1 O1 - C31 C34 Cr1 O2 - C38 C35 Cr1 N1 - C13 C1 Cr1 N2 - C17 C14 Cr1 N3 - C18 C19 C1 - C2 C6 N1 C2 - C1 C3 C10 C3 - C4 C2 C4 - C5 C3 C5 - C4 C6 C6 - C5 C1 C7 C7 - C6 C8 C9 C8 - C7 C9 - C7 C10 - C12 C11 C2 C11 - C10 C12 - C10 C13 - N1 C14 C14 - N2 C15 C13 C15 - C14 C16 C16 - C17 C15 C17 - C16 N2 C18 C18 - N3 C17 C19 - C24 C20 N3 C20 - C21 C19 C25 C21 - C22 C20 C22 - C21 C23 C23 - C22 C24 C24 - C19 C23 C28 C25 - C20 C26 C27 C26 - C25 C27 - C25 C28 - C29 C24 C30 C29 - C28 C30 - C28 C31 - O1 C32 C32 - C33 C31 C33 - C32 C34 C34 - O1 C33 C35 - C36 O2 C36 - C37 C35 C37 - C38 C36 C38 - O2 C37 10040 Reflections read, of which 0 rejected -14 =< h =< 13, -10 =< k =< 15, -19 =< l =< 18, Max. 2-theta = 56.85 0 Systematic absence violations 0 Inconsistent equivalents 6959 Unique reflections, of which 0 suppressed R(int) = 0.0369 R(sigma) = 0.0728 Friedel opposites merged Maximum memory for data reduction = 5573 / 72071 Default effective X-H distances for T = -50.0 C AFIX m = 1 2 3 4 4[N] 3[N] 15[B] 8[O] 9 9[N] 16 d(X-H) = 0.99 0.98 0.97 0.94 0.87 0.90 1.11 0.83 0.94 0.87 0.94 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 = 6872 / 547867 wR2 = 0.1667 before cycle 1 for 6959 data and 423 / 423 parameters GooF = S = 1.023; Restrained GooF = 1.023 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0799 * P )^2 + 0.42 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.17275 0.00036 0.777 OSF 185 -0.11534 0.02879 -4.007 tors H12A Mean shift/esd = 0.164 Maximum = -4.007 for tors H12A Max. shift = 0.117 A for H12B Max. dU =-0.001 for C37 Least-squares cycle 2 Maximum vector length = 511 Memory required = 6872 / 547867 wR2 = 0.1660 before cycle 2 for 6959 data and 423 / 423 parameters GooF = S = 1.017; Restrained GooF = 1.017 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0799 * P )^2 + 0.42 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.17287 0.00036 0.354 OSF Mean shift/esd = 0.077 Maximum = -2.083 for tors H12A Max. shift = 0.074 A for H30A Max. dU =-0.001 for C37 Least-squares cycle 3 Maximum vector length = 511 Memory required = 6872 / 547867 wR2 = 0.1658 before cycle 3 for 6959 data and 423 / 423 parameters GooF = S = 1.016; Restrained GooF = 1.016 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0799 * P )^2 + 0.42 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.17288 0.00036 0.015 OSF Mean shift/esd = 0.019 Maximum = 0.850 for tors H30A Max. shift = 0.037 A for H30A Max. dU = 0.000 for C37 Least-squares cycle 4 Maximum vector length = 511 Memory required = 6872 / 547867 wR2 = 0.1658 before cycle 4 for 6959 data and 423 / 423 parameters GooF = S = 1.016; Restrained GooF = 1.016 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0799 * P )^2 + 0.42 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.17288 0.00036 0.007 OSF Mean shift/esd = 0.008 Maximum = 0.403 for tors H30A Max. shift = 0.018 A for H30C Max. dU = 0.000 for C37 Least-squares cycle 5 Maximum vector length = 511 Memory required = 6872 / 547867 wR2 = 0.1658 before cycle 5 for 6959 data and 423 / 423 parameters GooF = S = 1.016; Restrained GooF = 1.016 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0799 * P )^2 + 0.42 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.17288 0.00036 0.001 OSF Mean shift/esd = 0.003 Maximum = 0.188 for tors H30A Max. shift = 0.008 A for H30C Max. dU = 0.000 for C37 Least-squares cycle 6 Maximum vector length = 511 Memory required = 6872 / 547867 wR2 = 0.1658 before cycle 6 for 6959 data and 423 / 423 parameters GooF = S = 1.016; Restrained GooF = 1.016 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0799 * P )^2 + 0.42 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.17288 0.00036 0.001 OSF Mean shift/esd = 0.002 Maximum = 0.086 for tors H30A Max. shift = 0.004 A for H30C Max. dU = 0.000 for C37 Least-squares cycle 7 Maximum vector length = 511 Memory required = 6872 / 547867 wR2 = 0.1658 before cycle 7 for 6959 data and 423 / 423 parameters GooF = S = 1.016; Restrained GooF = 1.016 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0799 * P )^2 + 0.42 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.17288 0.00036 0.001 OSF Mean shift/esd = 0.001 Maximum = 0.040 for tors H30A Max. shift = 0.002 A for H30C Max. dU = 0.000 for C37 Least-squares cycle 8 Maximum vector length = 511 Memory required = 6872 / 547867 wR2 = 0.1658 before cycle 8 for 6959 data and 423 / 423 parameters GooF = S = 1.016; Restrained GooF = 1.016 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0799 * P )^2 + 0.42 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.17288 0.00036 0.002 OSF Mean shift/esd = 0.000 Maximum = 0.018 for tors H30A Max. shift = 0.001 A for H30C Max. dU = 0.000 for C37 Least-squares cycle 9 Maximum vector length = 511 Memory required = 6872 / 547867 wR2 = 0.1658 before cycle 9 for 6959 data and 423 / 423 parameters GooF = S = 1.016; Restrained GooF = 1.016 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0799 * P )^2 + 0.42 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.17288 0.00036 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.008 for tors H30A Max. shift = 0.000 A for H30C Max. dU = 0.000 for C37 Least-squares cycle 10 Maximum vector length = 511 Memory required = 6872 / 547867 wR2 = 0.1658 before cycle 10 for 6959 data and 423 / 423 parameters GooF = S = 1.016; Restrained GooF = 1.016 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0799 * P )^2 + 0.42 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.17288 0.00036 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.004 for tors H30A Max. shift = 0.000 A for H30C Max. dU = 0.000 for C38 Least-squares cycle 11 Maximum vector length = 511 Memory required = 6872 / 547867 wR2 = 0.1658 before cycle 11 for 6959 data and 423 / 423 parameters GooF = S = 1.016; Restrained GooF = 1.016 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0799 * P )^2 + 0.42 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.17288 0.00036 -0.001 OSF Mean shift/esd = 0.000 Maximum = 0.002 for tors H30A Max. shift = 0.000 A for H30C Max. dU = 0.000 for C37 Least-squares cycle 12 Maximum vector length = 511 Memory required = 6872 / 547867 wR2 = 0.1658 before cycle 12 for 6959 data and 423 / 423 parameters GooF = S = 1.016; Restrained GooF = 1.016 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0799 * P )^2 + 0.42 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.17288 0.00036 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for tors H30A Max. shift = 0.000 A for H30C Max. dU = 0.000 for C26 Least-squares cycle 13 Maximum vector length = 511 Memory required = 6872 / 547867 wR2 = 0.1658 before cycle 13 for 6959 data and 423 / 423 parameters GooF = S = 1.016; Restrained GooF = 1.016 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0799 * P )^2 + 0.42 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.17288 0.00036 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x Cr1 Max. shift = 0.000 A for H30C Max. dU = 0.000 for C37 Least-squares cycle 14 Maximum vector length = 511 Memory required = 6872 / 547867 wR2 = 0.1658 before cycle 14 for 6959 data and 423 / 423 parameters GooF = S = 1.016; Restrained GooF = 1.016 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0799 * P )^2 + 0.42 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.17288 0.00036 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x Cr1 Max. shift = 0.000 A for H30C Max. dU = 0.000 for C26 Least-squares cycle 15 Maximum vector length = 511 Memory required = 6872 / 547867 wR2 = 0.1658 before cycle 15 for 6959 data and 423 / 423 parameters GooF = S = 1.016; Restrained GooF = 1.016 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0799 * P )^2 + 0.42 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.17288 0.00036 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x Cr1 Max. shift = 0.000 A for H30A Max. dU = 0.000 for C36 Least-squares cycle 16 Maximum vector length = 511 Memory required = 6872 / 547867 wR2 = 0.1658 before cycle 16 for 6959 data and 423 / 423 parameters GooF = S = 1.016; Restrained GooF = 1.016 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0799 * P )^2 + 0.42 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.17288 0.00036 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H9C Max. dU = 0.000 for C8 Least-squares cycle 17 Maximum vector length = 511 Memory required = 6872 / 547867 wR2 = 0.1658 before cycle 17 for 6959 data and 423 / 423 parameters GooF = S = 1.016; Restrained GooF = 1.016 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0799 * P )^2 + 0.42 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.17288 0.00036 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x Cr1 Max. shift = 0.000 A for H30C Max. dU = 0.000 for C33 Least-squares cycle 18 Maximum vector length = 511 Memory required = 6872 / 547867 wR2 = 0.1658 before cycle 18 for 6959 data and 423 / 423 parameters GooF = S = 1.016; Restrained GooF = 1.016 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0799 * P )^2 + 0.42 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.17288 0.00036 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x Cr1 Max. shift = 0.000 A for H30A Max. dU = 0.000 for C37 Least-squares cycle 19 Maximum vector length = 511 Memory required = 6872 / 547867 wR2 = 0.1658 before cycle 19 for 6959 data and 423 / 423 parameters GooF = S = 1.016; Restrained GooF = 1.016 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0799 * P )^2 + 0.42 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.17288 0.00036 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x Cr1 Max. shift = 0.000 A for H26C Max. dU = 0.000 for C33 Least-squares cycle 20 Maximum vector length = 511 Memory required = 6872 / 547867 wR2 = 0.1658 before cycle 20 for 6959 data and 423 / 423 parameters GooF = S = 1.016; Restrained GooF = 1.016 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0799 * P )^2 + 0.42 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.17288 0.00036 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x Cl1 Max. shift = 0.000 A for H26A Max. dU = 0.000 for C26 Largest correlation matrix elements 0.663 U13 C37 / U33 C37 0.569 U23 C21 / U22 C21 0.544 U23 Cl2 / U33 Cl2 0.661 U13 C37 / U11 C37 0.567 U12 C37 / U23 C37 0.542 U13 C26 / U11 C26 0.627 U23 C28 / U22 C28 0.562 U23 C23 / U22 C23 0.539 U12 C33 / U22 C33 0.622 U23 C28 / U33 C28 0.559 U23 C21 / U33 C21 0.539 U23 Cr1 / U22 Cr1 0.611 z C37 / x C37 0.556 U23 C23 / U33 C23 0.537 U23 C9 / U33 C9 0.600 U23 C22 / U22 C22 0.555 U23 C13 / U22 C13 0.535 U23 C14 / U22 C14 0.585 U23 C22 / U33 C22 0.552 U23 C25 / U22 C25 0.533 U23 C26 / U22 C26 0.573 U23 Cl2 / U22 Cl2 0.545 U23 C25 / U33 C25 0.526 U23 C27 / U33 C27 Idealized hydrogen atom generation before cycle 21 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H3A 0.8299 0.3677 0.5209 43 0.940 0.000 C3 C4 C2 H4A 1.0411 0.3638 0.5716 43 0.940 0.000 C4 C5 C3 H5A 1.1555 0.3192 0.4626 43 0.940 0.000 C5 C4 C6 H7A 1.0390 0.2544 0.2109 13 0.990 0.000 C7 C6 C8 C9 H8A 1.0538 0.0742 0.2370 137 0.970 0.000 C8 C7 H8A H8B 1.1760 0.1307 0.3225 137 0.970 0.000 C8 C7 H8A H8C 1.1786 0.1148 0.2168 137 0.970 0.000 C8 C7 H8A H9A 1.1805 0.4253 0.3077 137 0.970 0.000 C9 C7 H9A H9B 1.2520 0.3256 0.2557 137 0.970 0.000 C9 C7 H9A H9C 1.2586 0.3513 0.3644 137 0.970 0.000 C9 C7 H9A H10A 0.6505 0.3213 0.2835 13 0.990 0.000 C10 C12 C11 C2 H11A 0.6820 0.4985 0.4163 137 0.970 0.000 C11 C10 H11A H11B 0.6465 0.4227 0.4764 137 0.970 0.000 C11 C10 H11A H11C 0.5452 0.4293 0.3866 137 0.970 0.000 C11 C10 H11A H12A 0.6148 0.1395 0.2956 137 0.970 0.000 C12 C10 H12A H12B 0.5127 0.2141 0.3317 137 0.970 0.000 C12 C10 H12A H12C 0.6286 0.1955 0.4063 137 0.970 0.000 C12 C10 H12A H13A 0.7870 0.0857 0.2066 43 0.940 0.000 C13 N1 C14 H15A 0.6630 -0.0927 0.0256 43 0.940 0.000 C15 C14 C16 H16A 0.5712 -0.0772 -0.1360 43 0.940 0.000 C16 C17 C15 H18A 0.6048 0.2399 -0.1282 43 0.940 0.000 C18 N3 C17 H21A 0.2357 0.2028 -0.4265 43 0.940 0.000 C21 C22 C20 H22A 0.3806 0.2786 -0.4848 43 0.940 0.000 C22 C21 C23 H23A 0.5881 0.2622 -0.4331 43 0.940 0.000 C23 C22 C24 H25A 0.3042 0.0390 -0.2692 13 0.990 0.000 C25 C20 C26 C27 H26A 0.3156 0.2320 -0.1643 137 0.970 0.000 C26 C25 H26A H26B 0.1872 0.1531 -0.1832 137 0.970 0.000 C26 C25 H26A H26C 0.1930 0.2485 -0.2340 137 0.970 0.000 C26 C25 H26A H27A 0.1647 -0.0244 -0.4240 137 0.970 0.000 C27 C25 H27A H27B 0.0985 0.0899 -0.3931 137 0.970 0.000 C27 C25 H27A H27C 0.0939 -0.0078 -0.3442 137 0.970 0.000 C27 C25 H27A H28A 0.7250 0.1351 -0.2572 13 0.990 0.000 C28 C29 C24 C30 H29A 0.8802 0.2812 -0.2427 137 0.970 0.000 C29 C28 H29A H29B 0.7692 0.3423 -0.2091 137 0.970 0.000 C29 C28 H29A H29C 0.7851 0.3313 -0.3108 137 0.970 0.000 C29 C28 H29A H30A 0.8304 0.0718 -0.3691 137 0.970 0.000 C30 C28 H30A H30B 0.7563 0.1399 -0.4333 137 0.970 0.000 C30 C28 H30A H30C 0.6881 0.0257 -0.4253 137 0.970 0.000 C30 C28 H30A H31A 0.5012 0.2475 0.0866 23 0.980 0.000 C31 O1 C32 H31B 0.4948 0.3383 0.0294 23 0.980 0.000 C31 O1 C32 H32A 0.3458 0.3949 0.1047 23 0.980 0.000 C32 C33 C31 H32B 0.4172 0.3655 0.1963 23 0.980 0.000 C32 C33 C31 H33A 0.4809 0.5579 0.2555 23 0.980 0.000 C33 C32 C34 H33B 0.4597 0.5696 0.1528 23 0.980 0.000 C33 C32 C34 H34A 0.6570 0.5648 0.1669 23 0.980 0.000 C34 O1 C33 H34B 0.6756 0.5414 0.2653 23 0.980 0.000 C34 O1 C33 H35A 0.9959 0.4332 0.0425 23 0.980 0.000 C35 C36 O2 H35B 1.1013 0.3943 0.1132 23 0.980 0.000 C35 C36 O2 H36A 1.0298 0.3067 -0.0855 23 0.980 0.000 C36 C37 C35 H36B 1.1656 0.3219 -0.0153 23 0.980 0.000 C36 C37 C35 H37A 1.0381 0.1189 -0.0976 23 0.980 0.000 C37 C38 C36 H37B 1.1272 0.1527 0.0080 23 0.980 0.000 C37 C38 C36 H38A 0.8712 0.1329 -0.0500 23 0.980 0.000 C38 O2 C37 H38B 0.9564 0.1109 0.0407 23 0.980 0.000 C38 O2 C37 bas07 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq Cr1 0.78871 0.33721 0.11114 1.00000 0.04075 0.02698 0.02640 0.01006 0.00485 -0.00241 0.03225 0.00110 0.00005 0.00005 0.00003 0.00000 0.00029 0.00040 0.00027 0.00025 0.00020 0.00023 0.00018 Cl1 0.91543 0.49990 0.22619 1.00000 0.05790 0.03528 0.03682 0.00580 0.00321 -0.01086 0.04749 0.00182 0.00008 0.00009 0.00006 0.00000 0.00053 0.00069 0.00047 0.00044 0.00037 0.00043 0.00028 Cl2 0.74096 0.43047 -0.00016 1.00000 0.07002 0.03744 0.03777 0.01992 0.00178 -0.00754 0.04970 0.00200 0.00009 0.00009 0.00006 0.00000 0.00059 0.00069 0.00047 0.00046 0.00040 0.00047 0.00029 O1 0.63441 0.38971 0.15055 1.00000 0.04767 0.03173 0.03871 0.01136 0.00968 0.00611 0.03994 0.00525 0.00021 0.00023 0.00016 0.00000 0.00130 0.00176 0.00134 0.00123 0.00099 0.00113 0.00062 O2 0.93792 0.28140 0.06205 1.00000 0.04658 0.03159 0.04152 0.01247 0.01704 -0.00361 0.03936 0.00531 0.00021 0.00024 0.00017 0.00000 0.00129 0.00182 0.00137 0.00128 0.00101 0.00112 0.00063 N1 0.82142 0.24734 0.21107 1.00000 0.03538 0.02815 0.02337 0.00897 0.00492 0.00099 0.02966 0.00569 0.00022 0.00027 0.00017 0.00000 0.00131 0.00198 0.00130 0.00128 0.00099 0.00119 0.00066 N2 0.69075 0.17227 0.02434 1.00000 0.03384 0.02523 0.02560 0.00798 0.00569 0.00052 0.02901 0.00547 0.00022 0.00025 0.00017 0.00000 0.00127 0.00187 0.00133 0.00127 0.00098 0.00113 0.00065 N3 0.52301 0.09216 -0.22639 1.00000 0.04518 0.03302 0.03101 0.01393 0.00370 -0.00265 0.03726 0.00600 0.00025 0.00028 0.00019 0.00000 0.00151 0.00209 0.00146 0.00143 0.00113 0.00130 0.00075 C1 0.88418 0.28721 0.31347 1.00000 0.04669 0.02431 0.02364 0.00814 0.00211 -0.00372 0.03332 0.00678 0.00029 0.00032 0.00022 0.00000 0.00177 0.00227 0.00155 0.00151 0.00128 0.00149 0.00083 C2 0.81390 0.31762 0.37871 1.00000 0.05484 0.03067 0.03100 0.01146 0.00766 0.00302 0.03951 0.00759 0.00032 0.00034 0.00024 0.00000 0.00201 0.00254 0.00179 0.00173 0.00145 0.00167 0.00090 C3 0.87575 0.34688 0.47581 1.00000 0.07049 0.05085 0.03183 0.01491 0.01446 0.01028 0.05074 0.00868 0.00037 0.00039 0.00026 0.00000 0.00253 0.00309 0.00192 0.00200 0.00167 0.00208 0.00108 H3A 0.82985 0.36769 0.52091 1.00000 0.06089 0.00000 0.00000 C4 1.00152 0.34580 0.50635 1.00000 0.07589 0.06175 0.02781 0.01340 -0.00908 -0.00098 0.06041 0.00843 0.00040 0.00041 0.00027 0.00000 0.00274 0.00338 0.00192 0.00208 0.00182 0.00229 0.00129 H4A 1.04113 0.36384 0.57155 1.00000 0.07249 0.00000 0.00000 C5 1.06893 0.31817 0.44097 1.00000 0.05115 0.06364 0.03829 0.01843 -0.00513 -0.00352 0.05450 0.00826 0.00036 0.00041 0.00027 0.00000 0.00213 0.00338 0.00212 0.00219 0.00165 0.00200 0.00119 H5A 1.15549 0.31917 0.46256 1.00000 0.06540 0.00000 0.00000 C6 1.01345 0.28847 0.34305 1.00000 0.04385 0.04595 0.03795 0.01704 0.00112 -0.00025 0.04407 0.00777 0.00031 0.00037 0.00025 0.00000 0.00184 0.00282 0.00196 0.00191 0.00145 0.00170 0.00099 C7 1.09083 0.25605 0.27364 1.00000 0.04313 0.08368 0.04414 0.02612 0.00457 0.00631 0.05743 0.00929 0.00034 0.00046 0.00028 0.00000 0.00199 0.00389 0.00223 0.00242 0.00159 0.00212 0.00125 H7A 1.03895 0.25444 0.21094 1.00000 0.06891 0.00000 0.00000 C8 1.12821 0.13274 0.26137 1.00000 0.07831 0.09497 0.07760 0.02212 0.02753 0.02480 0.08385 0.01248 0.00047 0.00053 0.00039 0.00000 0.00326 0.00501 0.00361 0.00343 0.00261 0.00314 0.00168 H8A 1.05382 0.07416 0.23696 1.00000 0.12578 0.00000 0.00000 H8B 1.17601 0.13075 0.32252 1.00000 0.12578 0.00000 0.00000 H8C 1.17861 0.11475 0.21680 1.00000 0.12578 0.00000 0.00000 C9 1.20589 0.34786 0.30300 1.00000 0.05315 0.13157 0.07477 0.04545 0.00784 -0.01344 0.08685 0.01097 0.00040 0.00056 0.00036 0.00000 0.00254 0.00560 0.00329 0.00359 0.00220 0.00282 0.00186 H9A 1.18052 0.42530 0.30767 1.00000 0.13028 0.00000 0.00000 H9B 1.25199 0.32555 0.25566 1.00000 0.13028 0.00000 0.00000 H9C 1.25856 0.35127 0.36439 1.00000 0.13028 0.00000 0.00000 C10 0.67287 0.31786 0.34891 1.00000 0.05637 0.04745 0.03427 0.01494 0.01562 0.00793 0.04520 0.00849 0.00033 0.00038 0.00026 0.00000 0.00212 0.00297 0.00190 0.00196 0.00153 0.00191 0.00099 H10A 0.65046 0.32131 0.28355 1.00000 0.05423 0.00000 0.00000 C11 0.63301 0.42705 0.41287 1.00000 0.07547 0.06410 0.06248 0.01317 0.02432 0.02132 0.06803 0.01069 0.00042 0.00045 0.00033 0.00000 0.00291 0.00381 0.00295 0.00270 0.00226 0.00254 0.00135 H11A 0.68198 0.49848 0.41630 1.00000 0.10204 0.00000 0.00000 H11B 0.64653 0.42268 0.47635 1.00000 0.10204 0.00000 0.00000 H11C 0.54523 0.42933 0.38657 1.00000 0.10204 0.00000 0.00000 C12 0.60092 0.20702 0.34534 1.00000 0.06395 0.05213 0.05731 0.01555 0.01717 -0.00315 0.05895 0.00949 0.00038 0.00042 0.00031 0.00000 0.00251 0.00343 0.00261 0.00237 0.00195 0.00217 0.00121 H12A 0.61477 0.13946 0.29562 1.00000 0.08843 0.00000 0.00000 H12B 0.51268 0.21413 0.33174 1.00000 0.08843 0.00000 0.00000 H12C 0.62858 0.19546 0.40634 1.00000 0.08843 0.00000 0.00000 C13 0.77635 0.13703 0.17089 1.00000 0.03754 0.03048 0.02986 0.01471 0.00720 0.00305 0.03200 0.00722 0.00027 0.00034 0.00022 0.00000 0.00159 0.00247 0.00164 0.00164 0.00124 0.00148 0.00081 H13A 0.78703 0.08571 0.20656 1.00000 0.03841 0.00000 0.00000 C14 0.70977 0.09161 0.07185 1.00000 0.03444 0.03029 0.02849 0.01330 0.00883 0.00023 0.03041 0.00703 0.00027 0.00033 0.00022 0.00000 0.00152 0.00237 0.00161 0.00161 0.00119 0.00141 0.00079 C15 0.66160 -0.02272 0.01022 1.00000 0.04250 0.02586 0.03613 0.01319 0.00770 -0.00361 0.03511 0.00718 0.00028 0.00034 0.00023 0.00000 0.00173 0.00240 0.00178 0.00168 0.00133 0.00149 0.00084 H15A 0.66299 -0.09268 0.02558 1.00000 0.04214 0.00000 0.00000 C16 0.61050 -0.01398 -0.07929 1.00000 0.04594 0.02859 0.02860 0.00527 0.00636 -0.00336 0.03657 0.00740 0.00030 0.00034 0.00023 0.00000 0.00180 0.00254 0.00169 0.00159 0.00132 0.00156 0.00087 H16A 0.57123 -0.07718 -0.13600 1.00000 0.04389 0.00000 0.00000 C17 0.62853 0.10514 -0.06879 1.00000 0.03623 0.02689 0.02685 0.00852 0.00687 -0.00050 0.03070 0.00694 0.00027 0.00033 0.00021 0.00000 0.00156 0.00240 0.00161 0.00157 0.00119 0.00141 0.00080 C18 0.58584 0.15751 -0.14255 1.00000 0.03983 0.02757 0.03001 0.00951 0.00822 -0.00018 0.03302 0.00730 0.00028 0.00034 0.00022 0.00000 0.00164 0.00237 0.00165 0.00161 0.00125 0.00145 0.00082 H18A 0.60477 0.23992 -0.12817 1.00000 0.03962 0.00000 0.00000 C19 0.48685 0.14633 -0.29721 1.00000 0.04797 0.02125 0.02456 0.00628 0.00533 -0.00026 0.03272 0.00689 0.00030 0.00032 0.00022 0.00000 0.00178 0.00223 0.00156 0.00151 0.00127 0.00147 0.00080 C20 0.35866 0.14910 -0.33267 1.00000 0.04998 0.03202 0.03494 0.01170 0.01111 0.00457 0.03909 0.00779 0.00031 0.00035 0.00024 0.00000 0.00193 0.00252 0.00183 0.00174 0.00143 0.00164 0.00089 C21 0.32085 0.19903 -0.40300 1.00000 0.05012 0.05597 0.04705 0.02766 0.00688 0.00886 0.04973 0.00885 0.00035 0.00039 0.00027 0.00000 0.00206 0.00314 0.00222 0.00221 0.00162 0.00192 0.00108 H21A 0.23570 0.20282 -0.42654 1.00000 0.05967 0.00000 0.00000 C22 0.40665 0.24285 -0.43841 1.00000 0.06269 0.05377 0.04501 0.02928 0.01058 0.01061 0.05146 0.00896 0.00036 0.00039 0.00027 0.00000 0.00235 0.00317 0.00218 0.00223 0.00174 0.00207 0.00110 H22A 0.38056 0.27856 -0.48483 1.00000 0.06175 0.00000 0.00000 C23 0.53073 0.23470 -0.40621 1.00000 0.05810 0.05352 0.03996 0.02411 0.01845 0.00539 0.04770 0.00861 0.00035 0.00038 0.00025 0.00000 0.00220 0.00306 0.00202 0.00208 0.00161 0.00195 0.00102 H23A 0.58808 0.26215 -0.43313 1.00000 0.05724 0.00000 0.00000 C24 0.57414 0.18684 -0.33471 1.00000 0.04793 0.03442 0.03388 0.01245 0.01196 0.00174 0.03859 0.00772 0.00031 0.00035 0.00024 0.00000 0.00187 0.00261 0.00181 0.00178 0.00140 0.00163 0.00089 C25 0.26515 0.09884 -0.29432 1.00000 0.05367 0.03951 0.05487 0.02352 0.01604 0.00352 0.04745 0.00882 0.00034 0.00039 0.00028 0.00000 0.00212 0.00288 0.00240 0.00218 0.00172 0.00184 0.00102 H25A 0.30418 0.03902 -0.26917 1.00000 0.05694 0.00000 0.00000 C26 0.23779 0.19134 -0.21158 1.00000 0.10130 0.06898 0.09500 0.03483 0.06486 0.01328 0.07966 0.01289 0.00049 0.00049 0.00039 0.00000 0.00377 0.00432 0.00401 0.00346 0.00315 0.00301 0.00160 H26A 0.31557 0.23197 -0.16431 1.00000 0.11949 0.00000 0.00000 H26B 0.18721 0.15306 -0.18317 1.00000 0.11949 0.00000 0.00000 H26C 0.19297 0.24853 -0.23400 1.00000 0.11949 0.00000 0.00000 C27 0.14451 0.03312 -0.37093 1.00000 0.05720 0.11092 0.08190 0.04268 0.00726 -0.01902 0.08438 0.01051 0.00040 0.00054 0.00036 0.00000 0.00265 0.00520 0.00351 0.00352 0.00231 0.00274 0.00180 H27A 0.16467 -0.02437 -0.42404 1.00000 0.12656 0.00000 0.00000 H27B 0.09850 0.08988 -0.39309 1.00000 0.12656 0.00000 0.00000 H27C 0.09390 -0.00779 -0.34420 1.00000 0.12656 0.00000 0.00000 C28 0.71205 0.17418 -0.30590 1.00000 0.04786 0.08456 0.05687 0.04336 0.01852 0.00934 0.05759 0.01009 0.00035 0.00046 0.00030 0.00000 0.00209 0.00389 0.00252 0.00269 0.00175 0.00218 0.00125 H28A 0.72497 0.13510 -0.25715 1.00000 0.06910 0.00000 0.00000 C29 0.79387 0.29278 -0.26336 1.00000 0.06064 0.10877 0.10532 0.02747 0.01330 -0.02022 0.09691 0.01160 0.00044 0.00056 0.00043 0.00000 0.00292 0.00554 0.00441 0.00396 0.00276 0.00302 0.00204 H29A 0.88018 0.28125 -0.24273 1.00000 0.14537 0.00000 0.00000 H29B 0.76916 0.34232 -0.20905 1.00000 0.14537 0.00000 0.00000 H29C 0.78507 0.33134 -0.31083 1.00000 0.14537 0.00000 0.00000 C30 0.75017 0.09576 -0.39113 1.00000 0.09194 0.11115 0.10139 0.02823 0.03991 0.05811 0.09933 0.01422 0.00051 0.00058 0.00042 0.00000 0.00388 0.00547 0.00481 0.00418 0.00331 0.00372 0.00205 H30A 0.83043 0.07176 -0.36914 1.00000 0.14899 0.00000 0.00000 H30B 0.75634 0.13987 -0.43330 1.00000 0.14899 0.00000 0.00000 H30C 0.68806 0.02567 -0.42530 1.00000 0.14899 0.00000 0.00000 C31 0.51168 0.33183 0.09308 1.00000 0.04163 0.05136 0.07089 0.00766 0.01301 0.00119 0.05860 0.00900 0.00033 0.00042 0.00032 0.00000 0.00202 0.00331 0.00293 0.00240 0.00183 0.00189 0.00123 H31A 0.50119 0.24755 0.08663 1.00000 0.07032 0.00000 0.00000 H31B 0.49483 0.33832 0.02943 1.00000 0.07032 0.00000 0.00000 C32 0.42797 0.39853 0.14762 1.00000 0.05726 0.09742 0.08383 0.03153 0.02263 0.03070 0.07801 0.01224 0.00042 0.00053 0.00038 0.00000 0.00261 0.00487 0.00367 0.00351 0.00239 0.00286 0.00161 H32A 0.34580 0.39492 0.10472 1.00000 0.09362 0.00000 0.00000 H32B 0.41718 0.36552 0.19634 1.00000 0.09362 0.00000 0.00000 C33 0.49242 0.52165 0.19190 1.00000 0.08341 0.07872 0.10204 -0.01308 -0.02070 0.04622 0.10624 0.01159 0.00047 0.00053 0.00043 0.00000 0.00355 0.00488 0.00457 0.00345 0.00314 0.00333 0.00250 H33A 0.48090 0.55795 0.25552 1.00000 0.12749 0.00000 0.00000 H33B 0.45965 0.56957 0.15276 1.00000 0.12749 0.00000 0.00000 C34 0.62599 0.51462 0.19839 1.00000 0.08646 0.03408 0.06776 0.00728 0.02071 0.01975 0.06495 0.01058 0.00043 0.00042 0.00035 0.00000 0.00321 0.00324 0.00306 0.00242 0.00235 0.00239 0.00130 H34A 0.65697 0.56476 0.16688 1.00000 0.07795 0.00000 0.00000 H34B 0.67557 0.54135 0.26526 1.00000 0.07795 0.00000 0.00000 C35 1.03245 0.36510 0.05445 1.00000 0.05220 0.04845 0.06429 0.01973 0.02186 -0.00966 0.05446 0.00922 0.00035 0.00041 0.00031 0.00000 0.00219 0.00323 0.00271 0.00239 0.00186 0.00195 0.00115 H35A 0.99585 0.43321 0.04249 1.00000 0.06535 0.00000 0.00000 H35B 1.10127 0.39433 0.11320 1.00000 0.06535 0.00000 0.00000 C36 1.07658 0.29655 -0.02633 1.00000 0.08887 0.07398 0.08359 0.00566 0.04628 -0.02427 0.08465 0.01187 0.00049 0.00054 0.00039 0.00000 0.00355 0.00488 0.00376 0.00328 0.00286 0.00297 0.00179 H36A 1.02982 0.30668 -0.08549 1.00000 0.10158 0.00000 0.00000 H36B 1.16555 0.32192 -0.01527 1.00000 0.10158 0.00000 0.00000 C37 1.05460 0.17297 -0.03163 1.00000 0.12570 0.06305 0.16987 0.02565 0.11177 0.01001 0.10997 0.01691 0.00060 0.00058 0.00055 0.00000 0.00508 0.00524 0.00675 0.00455 0.00487 0.00366 0.00242 H37A 1.03815 0.11891 -0.09756 1.00000 0.13196 0.00000 0.00000 H37B 1.12722 0.15274 0.00796 1.00000 0.13196 0.00000 0.00000 C38 0.94687 0.16439 0.00346 1.00000 0.07436 0.04089 0.08618 0.01126 0.04775 0.00332 0.06516 0.01115 0.00042 0.00044 0.00037 0.00000 0.00287 0.00356 0.00349 0.00278 0.00248 0.00228 0.00131 H38A 0.87124 0.13287 -0.04997 1.00000 0.07820 0.00000 0.00000 H38B 0.95643 0.11093 0.04069 1.00000 0.07820 0.00000 0.00000 Final Structure Factor Calculation for bas07 in P-1 Total number of l.s. parameters = 423 Maximum vector length = 511 Memory required = 6449 / 25039 wR2 = 0.1658 before cycle 21 for 6959 data and 0 / 423 parameters GooF = S = 1.016; Restrained GooF = 1.016 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0799 * P )^2 + 0.42 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0591 for 4592 Fo > 4sig(Fo) and 0.0945 for all 6959 data wR2 = 0.1658, GooF = S = 1.016, Restrained GooF = 1.016 for all data Occupancy sum of asymmetric unit = 46.00 for non-hydrogen and 54.00 for hydrogen atoms Principal mean square atomic displacements U 0.0465 0.0260 0.0243 Cr1 0.0714 0.0449 0.0261 Cl1 0.0852 0.0377 0.0262 Cl2 0.0492 0.0391 0.0315 O1 0.0545 0.0388 0.0248 O2 0.0385 0.0275 0.0231 N1 0.0365 0.0264 0.0241 N2 0.0539 0.0307 0.0272 N3 0.0540 0.0239 0.0221 C1 0.0577 0.0314 0.0294 C2 0.0713 0.0507 0.0302 C3 0.0952 0.0632 0.0229 C4 0.0765 0.0573 0.0296 C5 0.0583 0.0418 0.0321 C6 0.0845 0.0521 0.0358 C7 0.1061 0.0819 0.0636 C8 0.1452 0.0673 0.0481 C9 0.0564 0.0475 0.0317 C10 0.0840 0.0720 0.0481 C11 0.0734 0.0571 0.0463 C12 0.0400 0.0326 0.0234 C13 0.0382 0.0306 0.0224 C14 0.0488 0.0356 0.0209 C15 0.0512 0.0343 0.0242 C16 0.0394 0.0273 0.0253 C17 0.0426 0.0302 0.0263 C18 0.0515 0.0260 0.0207 C19 0.0507 0.0348 0.0318 C20 0.0623 0.0533 0.0336 C21 0.0656 0.0592 0.0296 C22 0.0597 0.0550 0.0284 C23 0.0498 0.0347 0.0313 C24 0.0563 0.0548 0.0313 C25 0.1292 0.0696 0.0402 C26 0.1334 0.0737 0.0460 C27 0.0901 0.0486 0.0340 C28 0.1314 0.1112 0.0481 C29 0.1473 0.1051 0.0456 C30 0.0848 0.0511 0.0399 C31 0.1047 0.0836 0.0457 C32 0.2186 0.0597 0.0404 C33 may be split into 0.4882 0.5208 0.2036 and 0.4966 0.5225 0.1802 0.0912 0.0748 0.0288 C34 0.0731 0.0617 0.0286 C35 0.1472 0.0645 0.0423 C36 0.2213 0.0632 0.0454 C37 may be split into 1.0703 0.1762 -0.0212 and 1.0389 0.1697 -0.0420 0.1105 0.0443 0.0407 C38 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.008 0.016 0.024 0.035 0.046 0.059 0.077 0.106 0.160 1.000 Number in group 702. 722. 685. 738. 683. 660. 689. 686. 693. 701. GooF 0.850 0.899 1.015 1.044 1.041 1.091 1.121 1.099 1.025 0.953 K 3.270 1.428 1.215 1.115 1.072 1.062 1.030 1.009 0.988 1.041 Resolution(A) 0.75 0.79 0.83 0.88 0.93 1.00 1.09 1.21 1.40 1.78 inf Number in group 702. 700. 711. 674. 706. 685. 693. 692. 698. 698. GooF 1.056 0.888 0.937 0.963 0.934 0.906 0.892 0.943 1.085 1.435 K 1.230 1.095 1.060 1.029 0.993 0.996 0.983 0.988 1.007 1.061 R1 0.276 0.208 0.202 0.148 0.110 0.084 0.072 0.061 0.050 0.048 Recommended weighting scheme: WGHT 0.0763 0.5191 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) -1 2 2 41.54 9.71 5.51 0.018 3.89 -4 -4 7 291.81 180.44 5.00 0.077 1.74 -1 -1 2 176.84 105.17 4.88 0.059 6.55 -1 2 6 43.01 9.19 4.57 0.017 2.00 2 2 1 90.97 149.07 4.38 0.070 3.21 1 0 6 99.71 50.21 4.32 0.041 2.16 5 0 1 506.46 349.91 4.16 0.108 2.04 2 0 3 190.37 108.46 4.15 0.060 3.12 1 -2 17 295.40 180.88 4.11 0.077 0.84 3 -4 18 185.94 99.52 4.09 0.057 0.76 2 -4 12 375.42 243.08 4.07 0.090 1.15 1 -1 7 5963.69 4341.26 3.80 0.379 1.97 5 -2 1 1087.17 783.00 3.76 0.161 2.04 -5 -5 2 132.17 73.73 3.73 0.049 1.55 1 -1 1 151.22 101.59 3.67 0.058 7.32 -1 6 2 148.89 81.35 3.67 0.052 1.70 4 -1 5 39.60 69.09 3.56 0.048 1.78 -2 -2 3 722.58 517.83 3.56 0.131 3.68 -3 -1 2 34.73 12.51 3.54 0.020 3.47 3 -3 1 207.44 131.72 3.50 0.066 2.76 3 11 7 168.96 83.44 3.50 0.053 0.75 1 -2 6 725.75 529.91 3.50 0.133 2.30 5 0 0 57.01 93.42 3.43 0.056 2.14 -4 -3 6 26.41 1.09 3.42 0.006 1.98 1 7 11 58.89 1.54 3.41 0.007 0.84 2 -9 14 42.83 110.66 3.39 0.061 0.92 12 -3 5 79.54 34.94 3.35 0.034 0.81 4 0 2 106.70 154.86 3.33 0.072 2.30 1 3 4 -8.03 19.48 3.31 0.025 2.06 0 0 3 6464.54 4855.29 3.29 0.401 4.67 -4 -4 4 940.95 718.10 3.24 0.154 1.97 1 9 11 64.24 10.41 3.23 0.019 0.75 -4 -2 16 561.08 793.46 3.22 0.162 0.95 -1 -5 7 82.64 34.15 3.21 0.034 1.86 3 4 0 419.22 298.16 3.20 0.099 2.07 2 -3 6 131.11 86.58 3.19 0.054 2.04 1 -6 4 80.63 135.33 3.17 0.067 1.92 -3 -2 5 164.70 110.94 3.14 0.061 2.56 4 11 6 367.03 237.14 3.14 0.089 0.75 2 4 6 87.59 52.66 3.14 0.042 1.40 1 -3 6 32.52 61.93 3.13 0.045 2.24 2 -1 16 270.98 188.71 3.12 0.079 0.85 1 -2 1 74.94 42.69 3.11 0.038 5.29 2 3 5 64.33 39.13 3.10 0.036 1.69 -9 7 2 456.02 307.71 3.09 0.101 1.02 3 10 8 191.71 104.62 3.09 0.059 0.77 -5 3 8 44.16 0.53 3.09 0.004 1.37 0 -3 7 360.02 256.27 3.09 0.092 2.09 2 -1 2 685.26 499.27 3.08 0.129 3.94 -11 -9 2 49.85 6.98 3.08 0.015 0.75 Bond lengths and angles Cr1 - Distance Angles O1 2.0283 (0.0031) O2 2.0504 (0.0030) 176.20 (0.09) N2 2.0637 (0.0032) 90.87 (0.12) 86.94 (0.12) N1 2.1158 (0.0030) 89.87 (0.11) 92.86 (0.11) 80.93 (0.13) Cl1 2.2843 (0.0020) 92.50 (0.10) 90.24 (0.10) 168.66 (0.08) 88.25 (0.11) Cl2 2.3018 (0.0020) 87.71 (0.09) 89.46 (0.09) 96.78 (0.11) 176.64 (0.07) 94.17 (0.09) Cr1 - O1 O2 N2 N1 Cl1 Cl1 - Distance Angles Cr1 2.2843 (0.0020) Cl1 - Cl2 - Distance Angles Cr1 2.3018 (0.0020) Cl2 - O1 - Distance Angles C31 1.4339 (0.0042) C34 1.4617 (0.0051) 107.89 (0.31) Cr1 2.0283 (0.0031) 121.33 (0.25) 122.13 (0.24) O1 - C31 C34 O2 - Distance Angles C38 1.4287 (0.0052) C35 1.4679 (0.0045) 108.04 (0.31) Cr1 2.0504 (0.0030) 127.14 (0.22) 121.75 (0.26) O2 - C38 C35 N1 - Distance Angles C13 1.2798 (0.0044) C1 1.4652 (0.0038) 116.59 (0.27) Cr1 2.1158 (0.0030) 110.84 (0.21) 132.57 (0.23) N1 - C13 C1 N2 - Distance Angles C17 1.3795 (0.0039) C14 1.3812 (0.0042) 105.21 (0.29) Cr1 2.0637 (0.0032) 143.53 (0.23) 110.10 (0.20) N2 - C17 C14 N3 - Distance Angles C18 1.2749 (0.0041) C19 1.4262 (0.0042) 118.56 (0.32) N3 - C18 C1 - Distance Angles C2 1.3924 (0.0050) C6 1.4008 (0.0048) 121.59 (0.29) N1 1.4652 (0.0038) 119.59 (0.28) 118.76 (0.31) C1 - C2 C6 C2 - Distance Angles C1 1.3924 (0.0050) C3 1.4029 (0.0047) 118.06 (0.33) C10 1.5289 (0.0051) 122.93 (0.29) 118.99 (0.34) C2 - C1 C3 C3 - Distance Angles C4 1.3694 (0.0057) C2 1.4029 (0.0047) 121.46 (0.39) H3A 0.9400 119.27 119.27 C3 - C4 C2 C4 - Distance Angles C5 1.3685 (0.0059) C3 1.3694 (0.0057) 119.32 (0.33) H4A 0.9400 120.34 120.34 C4 - C5 C3 C5 - Distance Angles C4 1.3685 (0.0059) C6 1.3997 (0.0048) 122.28 (0.36) H5A 0.9400 118.86 118.86 C5 - C4 C6 C6 - Distance Angles C5 1.3997 (0.0048) C1 1.4008 (0.0048) 117.25 (0.36) C7 1.5035 (0.0056) 120.41 (0.33) 122.32 (0.30) C6 - C5 C1 C7 - Distance Angles C6 1.5035 (0.0056) C8 1.5221 (0.0071) 111.41 (0.39) C9 1.5209 (0.0061) 111.71 (0.40) 110.34 (0.41) H7A 0.9900 107.73 107.73 107.73 C7 - C6 C8 C9 C8 - Distance Angles C7 1.5221 (0.0071) H8A 0.9700 109.47 H8B 0.9700 109.47 109.47 H8C 0.9700 109.47 109.47 109.47 C8 - C7 H8A H8B C9 - Distance Angles C7 1.5209 (0.0061) H9A 0.9700 109.47 H9B 0.9700 109.47 109.47 H9C 0.9700 109.47 109.47 109.47 C9 - C7 H9A H9B C10 - Distance Angles C12 1.4929 (0.0057) C11 1.5276 (0.0060) 110.05 (0.37) C2 1.5289 (0.0051) 112.41 (0.34) 112.17 (0.33) H10A 0.9900 107.30 107.30 107.30 C10 - C12 C11 C2 C11 - Distance Angles C10 1.5276 (0.0060) H11A 0.9700 109.47 H11B 0.9700 109.47 109.47 H11C 0.9700 109.47 109.47 109.47 C11 - C10 H11A H11B C12 - Distance Angles C10 1.4929 (0.0057) H12A 0.9700 109.47 H12B 0.9700 109.47 109.47 H12C 0.9700 109.47 109.47 109.47 C12 - C10 H12A H12B C13 - Distance Angles N1 1.2798 (0.0044) C14 1.4304 (0.0042) 120.19 (0.30) H13A 0.9400 119.91 119.91 C13 - N1 C14 C14 - Distance Angles N2 1.3812 (0.0042) C15 1.3817 (0.0049) 110.73 (0.28) C13 1.4304 (0.0042) 117.37 (0.32) 131.86 (0.32) C14 - N2 C15 C15 - Distance Angles C14 1.3817 (0.0049) C16 1.3955 (0.0045) 106.55 (0.32) H15A 0.9400 126.73 126.73 C15 - C14 C16 C16 - Distance Angles C17 1.3815 (0.0052) C15 1.3955 (0.0045) 107.02 (0.30) H16A 0.9400 126.49 126.49 C16 - C17 C15 C17 - Distance Angles C16 1.3815 (0.0052) N2 1.3795 (0.0039) 110.49 (0.28) C18 1.4590 (0.0045) 126.62 (0.30) 122.85 (0.33) C17 - C16 N2 C18 - Distance Angles N3 1.2749 (0.0041) C17 1.4590 (0.0045) 120.38 (0.35) H18A 0.9400 119.81 119.81 C18 - N3 C17 C19 - Distance Angles C24 1.3859 (0.0049) C20 1.4076 (0.0047) 121.19 (0.30) N3 1.4262 (0.0042) 120.96 (0.29) 117.68 (0.30) C19 - C24 C20 C20 - Distance Angles C21 1.3864 (0.0050) C19 1.4076 (0.0047) 118.82 (0.34) C25 1.5036 (0.0052) 120.98 (0.32) 120.20 (0.31) C20 - C21 C19 C21 - Distance Angles C22 1.3688 (0.0055) C20 1.3864 (0.0050) 120.47 (0.34) H21A 0.9400 119.77 119.77 C21 - C22 C20 C22 - Distance Angles C21 1.3688 (0.0055) C23 1.3724 (0.0052) 120.06 (0.35) H22A 0.9400 119.97 119.97 C22 - C21 C23 C23 - Distance Angles C22 1.3724 (0.0052) C24 1.3943 (0.0049) 121.86 (0.35) H23A 0.9400 119.07 119.07 C23 - C22 C24 C24 - Distance Angles C19 1.3859 (0.0049) C23 1.3943 (0.0049) 117.50 (0.31) C28 1.5244 (0.0052) 123.13 (0.32) 119.25 (0.33) C24 - C19 C23 C25 - Distance Angles C20 1.5036 (0.0052) C26 1.5065 (0.0063) 112.31 (0.37) C27 1.5308 (0.0054) 113.37 (0.35) 111.07 (0.42) H25A 0.9900 106.52 106.52 106.52 C25 - C20 C26 C27 C26 - Distance Angles C25 1.5065 (0.0063) H26A 0.9700 109.47 H26B 0.9700 109.47 109.47 H26C 0.9700 109.47 109.47 109.47 C26 - C25 H26A H26B C27 - Distance Angles C25 1.5308 (0.0054) H27A 0.9700 109.47 H27B 0.9700 109.47 109.47 H27C 0.9700 109.47 109.47 109.47 C27 - C25 H27A H27B C28 - Distance Angles C29 1.5028 (0.0069) C24 1.5244 (0.0052) 112.00 (0.42) C30 1.5213 (0.0067) 109.87 (0.43) 110.53 (0.36) H28A 0.9900 108.11 108.11 108.11 C28 - C29 C24 C30 C29 - Distance Angles C28 1.5028 (0.0069) H29A 0.9700 109.47 H29B 0.9700 109.47 109.47 H29C 0.9700 109.47 109.47 109.47 C29 - C28 H29A H29B C30 - Distance Angles C28 1.5213 (0.0067) H30A 0.9700 109.47 H30B 0.9700 109.47 109.47 H30C 0.9700 109.47 109.47 109.47 C30 - C28 H30A H30B C31 - Distance Angles O1 1.4339 (0.0042) C32 1.5006 (0.0063) 103.37 (0.36) H31A 0.9800 111.09 111.09 H31B 0.9800 111.09 111.09 109.05 C31 - O1 C32 H31A C32 - Distance Angles C33 1.4711 (0.0075) C31 1.5006 (0.0063) 104.71 (0.44) H32A 0.9800 110.81 110.81 H32B 0.9800 110.81 110.81 108.87 C32 - C33 C31 H32A C33 - Distance Angles C32 1.4711 (0.0075) C34 1.4787 (0.0067) 106.26 (0.42) H33A 0.9800 110.48 110.48 H33B 0.9800 110.48 110.48 108.66 C33 - C32 C34 H33A C34 - Distance Angles O1 1.4617 (0.0051) C33 1.4787 (0.0067) 106.26 (0.38) H34A 0.9800 110.48 110.48 H34B 0.9800 110.48 110.48 108.66 C34 - O1 C33 H34A C35 - Distance Angles C36 1.4678 (0.0066) O2 1.4679 (0.0045) 105.15 (0.37) H35A 0.9800 110.72 110.72 H35B 0.9800 110.72 110.72 108.81 C35 - C36 O2 H35A C36 - Distance Angles C37 1.4601 (0.0078) C35 1.4678 (0.0065) 104.93 (0.45) H36A 0.9800 110.76 110.76 H36B 0.9800 110.76 110.76 108.84 C36 - C37 C35 H36A C37 - Distance Angles C38 1.4451 (0.0062) C36 1.4601 (0.0078) 105.59 (0.47) H37A 0.9800 110.62 110.62 H37B 0.9800 110.62 110.62 108.75 C37 - C38 C36 H37A C38 - Distance Angles O2 1.4287 (0.0052) C37 1.4451 (0.0062) 107.45 (0.40) H38A 0.9800 110.22 110.22 H38B 0.9800 110.22 110.22 108.50 C38 - O2 C37 H38A Selected torsion angles 33.44 ( 1.67) O2 - Cr1 - O1 - C31 -21.38 ( 0.30) N2 - Cr1 - O1 - C31 -102.30 ( 0.31) N1 - Cr1 - O1 - C31 169.46 ( 0.29) Cl1 - Cr1 - O1 - C31 75.38 ( 0.30) Cl2 - Cr1 - O1 - C31 -110.37 ( 1.54) O2 - Cr1 - O1 - C34 -165.18 ( 0.28) N2 - Cr1 - O1 - C34 113.90 ( 0.29) N1 - Cr1 - O1 - C34 25.65 ( 0.27) Cl1 - Cr1 - O1 - C34 -68.43 ( 0.28) Cl2 - Cr1 - O1 - C34 -62.62 ( 1.64) O1 - Cr1 - O2 - C38 -7.70 ( 0.32) N2 - Cr1 - O2 - C38 73.04 ( 0.34) N1 - Cr1 - O2 - C38 161.30 ( 0.32) Cl1 - Cr1 - O2 - C38 -104.53 ( 0.33) Cl2 - Cr1 - O2 - C38 95.11 ( 1.56) O1 - Cr1 - O2 - C35 150.03 ( 0.25) N2 - Cr1 - O2 - C35 -129.22 ( 0.25) N1 - Cr1 - O2 - C35 -40.96 ( 0.25) Cl1 - Cr1 - O2 - C35 53.21 ( 0.25) Cl2 - Cr1 - O2 - C35 95.96 ( 0.24) O1 - Cr1 - N1 - C13 -81.38 ( 0.24) O2 - Cr1 - N1 - C13 5.06 ( 0.23) N2 - Cr1 - N1 - C13 -171.54 ( 0.22) Cl1 - Cr1 - N1 - C13 52.22 ( 1.62) Cl2 - Cr1 - N1 - C13 -84.32 ( 0.30) O1 - Cr1 - N1 - C1 98.34 ( 0.30) O2 - Cr1 - N1 - C1 -175.22 ( 0.30) N2 - Cr1 - N1 - C1 8.19 ( 0.28) Cl1 - Cr1 - N1 - C1 -128.06 ( 1.41) Cl2 - Cr1 - N1 - C1 98.75 ( 0.37) O1 - Cr1 - N2 - C17 -78.14 ( 0.37) O2 - Cr1 - N2 - C17 -171.53 ( 0.38) N1 - Cr1 - N2 - C17 -153.96 ( 0.34) Cl1 - Cr1 - N2 - C17 10.95 ( 0.37) Cl2 - Cr1 - N2 - C17 -96.42 ( 0.22) O1 - Cr1 - N2 - C14 86.69 ( 0.22) O2 - Cr1 - N2 - C14 -6.69 ( 0.21) N1 - Cr1 - N2 - C14 10.88 ( 0.57) Cl1 - Cr1 - N2 - C14 175.79 ( 0.20) Cl2 - Cr1 - N2 - C14 -84.20 ( 0.41) C13 - N1 - C1 - C2 96.09 ( 0.36) Cr1 - N1 - C1 - C2 92.91 ( 0.40) C13 - N1 - C1 - C6 -86.80 ( 0.41) Cr1 - N1 - C1 - C6 -1.68 ( 0.56) C6 - C1 - C2 - C3 175.34 ( 0.35) N1 - C1 - C2 - C3 179.65 ( 0.36) C6 - C1 - C2 - C10 -3.33 ( 0.53) N1 - C1 - C2 - C10 -0.04 ( 0.62) C1 - C2 - C3 - C4 178.69 ( 0.39) C10 - C2 - C3 - C4 1.48 ( 0.68) C2 - C3 - C4 - C5 -1.27 ( 0.69) C3 - C4 - C5 - C6 -0.38 ( 0.64) C4 - C5 - C6 - C1 -178.61 ( 0.42) C4 - C5 - C6 - C7 1.87 ( 0.57) C2 - C1 - C6 - C5 -175.17 ( 0.35) N1 - C1 - C6 - C5 -179.93 ( 0.37) C2 - C1 - C6 - C7 3.03 ( 0.56) N1 - C1 - C6 - C7 73.44 ( 0.50) C5 - C6 - C7 - C8 -104.70 ( 0.45) C1 - C6 - C7 - C8 -50.48 ( 0.56) C5 - C6 - C7 - C9 131.38 ( 0.42) C1 - C6 - C7 - C9 98.49 ( 0.42) C1 - C2 - C10 - C12 -80.17 ( 0.47) C3 - C2 - C10 - C12 -136.86 ( 0.39) C1 - C2 - C10 - C11 44.48 ( 0.51) C3 - C2 - C10 - C11 177.79 ( 0.29) C1 - N1 - C13 - C14 -2.43 ( 0.38) Cr1 - N1 - C13 - C14 0.35 ( 0.35) C17 - N2 - C14 - C15 -170.37 ( 0.23) Cr1 - N2 - C14 - C15 178.38 ( 0.28) C17 - N2 - C14 - C13 7.66 ( 0.35) Cr1 - N2 - C14 - C13 -3.63 ( 0.47) N1 - C13 - C14 - N2 173.89 ( 0.35) N1 - C13 - C14 - C15 0.05 ( 0.38) N2 - C14 - C15 - C16 -177.60 ( 0.35) C13 - C14 - C15 - C16 -0.44 ( 0.39) C14 - C15 - C16 - C17 0.68 ( 0.39) C15 - C16 - C17 - N2 -177.27 ( 0.32) C15 - C16 - C17 - C18 -0.64 ( 0.36) C14 - N2 - C17 - C16 164.61 ( 0.28) Cr1 - N2 - C17 - C16 177.40 ( 0.29) C14 - N2 - C17 - C18 -17.35 ( 0.56) Cr1 - N2 - C17 - C18 -177.84 ( 0.31) C19 - N3 - C18 - C17 1.41 ( 0.54) C16 - C17 - C18 - N3 -176.30 ( 0.31) N2 - C17 - C18 - N3 71.10 ( 0.48) C18 - N3 - C19 - C24 -113.54 ( 0.38) C18 - N3 - C19 - C20 -3.32 ( 0.58) C24 - C19 - C20 - C21 -178.66 ( 0.36) N3 - C19 - C20 - C21 176.83 ( 0.38) C24 - C19 - C20 - C25 1.48 ( 0.54) N3 - C19 - C20 - C25 1.16 ( 0.64) C19 - C20 - C21 - C22 -178.99 ( 0.41) C25 - C20 - C21 - C22 1.76 ( 0.69) C20 - C21 - C22 - C23 -2.66 ( 0.68) C21 - C22 - C23 - C24 2.46 ( 0.58) C20 - C19 - C24 - C23 177.66 ( 0.34) N3 - C19 - C24 - C23 -173.58 ( 0.37) C20 - C19 - C24 - C28 1.61 ( 0.59) N3 - C19 - C24 - C28 0.53 ( 0.62) C22 - C23 - C24 - C19 176.73 ( 0.40) C22 - C23 - C24 - C28 -88.41 ( 0.49) C21 - C20 - C25 - C26 91.44 ( 0.48) C19 - C20 - C25 - C26 38.51 ( 0.61) C21 - C20 - C25 - C27 -141.64 ( 0.42) C19 - C20 - C25 - C27 -120.08 ( 0.46) C19 - C24 - C28 - C29 63.94 ( 0.54) C23 - C24 - C28 - C29 117.05 ( 0.48) C19 - C24 - C28 - C30 -58.93 ( 0.57) C23 - C24 - C28 - C30 -31.29 ( 0.46) C34 - O1 - C31 - C32 -179.58 ( 0.28) Cr1 - O1 - C31 - C32 33.70 ( 0.50) O1 - C31 - C32 - C33 -23.59 ( 0.60) C31 - C32 - C33 - C34 16.98 ( 0.51) C31 - O1 - C34 - C33 164.96 ( 0.34) Cr1 - O1 - C34 - C33 4.81 ( 0.60) C32 - C33 - C34 - O1 12.37 ( 0.47) C38 - O2 - C35 - C36 -149.11 ( 0.33) Cr1 - O2 - C35 - C36 -26.04 ( 0.56) O2 - C35 - C36 - C37 30.21 ( 0.69) C35 - C36 - C37 - C38 6.37 ( 0.55) C35 - O2 - C38 - C37 166.56 ( 0.38) Cr1 - O2 - C38 - C37 -22.77 ( 0.69) C36 - C37 - C38 - O2 FMAP and GRID set by program FMAP 2 3 40 GRID -1.351 -2 -2 1.351 2 2 R1 = 0.0925 for 6959 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.54 at 0.6985 0.3505 0.1195 [ 1.01 A from O1 ] Deepest hole -0.30 at 0.7994 0.2749 0.1314 [ 0.90 A from CR1 ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 6057 / 35927 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.6985 0.3505 0.1195 1.00000 0.05 0.54 1.01 O1 1.06 CR1 2.01 C31 2.15 N2 Q2 1 1.1338 0.2734 0.0255 1.00000 0.05 0.36 1.02 C36 1.08 H36B 1.35 C37 1.38 H37B Q3 1 0.5816 0.3830 0.1301 1.00000 0.05 0.36 0.58 O1 0.91 C31 1.52 H31B 1.56 C34 Q4 1 0.8896 0.3181 0.0936 1.00000 0.05 0.36 0.86 O2 1.24 CR1 1.95 C35 2.16 C38 Q5 1 0.6797 0.3664 -0.0038 1.00000 0.05 0.35 0.98 CL2 1.97 H18A 2.03 CR1 2.28 H31B Q6 1 0.8304 0.5043 0.2281 1.00000 0.05 0.34 0.96 CL1 1.98 H34B 2.16 CR1 2.20 H34A Q7 1 0.6521 0.1654 -0.0258 1.00000 0.05 0.34 0.76 N2 0.79 C17 1.74 C18 1.97 C14 Q8 1 0.7365 0.0556 -0.3332 1.00000 0.05 0.33 1.17 C30 1.29 H28A 1.31 H30C 1.33 H30A Q9 1 0.7330 0.1427 0.0571 1.00000 0.05 0.33 0.77 C14 0.79 N2 1.72 C13 1.90 C17 Q10 1 0.9781 0.1755 -0.0723 1.00000 0.05 0.33 0.94 C37 1.03 H37A 1.34 C38 1.43 H38A Shortest distances between peaks (including symmetry equivalents) 1 3 1.41 7 9 1.48 1 5 1.93 2 10 2.01 1 6 2.21 1 4 2.29 5 7 2.31 1 9 2.45 4 9 2.48 1 7 2.52 3 5 2.52 4 5 2.65 4 6 2.75 3 6 2.87 4 7 2.95 Time profile in seconds ----------------------- 0.02: Read and process instructions 0.00: Fit rigid groups 0.00: 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 0.00: Analyse other restraints etc. 0.05: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.02: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.02: Generate idealized H-atoms 1.91: Structure factors and derivatives 11.19: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 1.03: Solve l.s. equations 0.00: Generate HTAB table 0.05: Other dependent quantities, CIF, tables 0.03: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.03: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + bas07 finished at 15:46:37 Total CPU time: 14.4 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++