+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 00skl038 started at 12:13:02 on 02-Sep-2000 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 00skl038 REM 00skl038 REM R1 = 0.3879 for 3471 Fo > 4sig(Fo) and 0.4794 for all 7647 data REM 118 parameters refined using 0 restraints REM Highest difference peak 15.906, deepest hole -2.891, 1-sigma level 1.077 REM 00skl038 REM R1 = 0.1533 for 3471 Fo > 4sig(Fo) and 0.2641 for all 7647 data REM 182 parameters refined using 0 restraints REM 00skl038 REM R1 = 0.0705 for 3471 Fo > 4sig(Fo) and 0.1866 for all 7647 data REM 280 parameters refined using 0 restraints REM Highest difference peak 1.442, deepest hole -0.799, 1-sigma level 0.201 REM 00skl038 REM R1 = 0.0619 for 3471 Fo > 4sig(Fo) and 0.1799 for all 7647 data REM 328 parameters refined using 0 restraints REM Highest difference peak 1.257, deepest hole -0.716, 1-sigma level 0.182 REM 00skl038 no abs corr REM R1 = 0.0577 for 3471 Fo > 4sig(Fo) and 0.1768 for all 7647 data REM 356 parameters refined using 0 restraints REM 00skl038 REM R1 = 0.0577 for 3471 Fo > 4sig(Fo) and 0.1768 for all 7647 data REM 356 parameters refined using 0 restraints REM Highest difference peak 1.318, deepest hole -0.709, 1-sigma level 0.184 REM 00skl038 REM R1 = 0.0562 for 3469 Fo > 4sig(Fo) and 0.1757 for all 7647 data REM 360 parameters refined using 0 restraints REM Highest difference peak 1.327, deepest hole -0.695, 1-sigma level 0.185 REM 00skl038 REM R1 = 0.0556 for 3469 Fo > 4sig(Fo) and 0.1752 for all 7647 data REM 352 parameters refined using 0 restraints REM 00skl038 REM R1 = 0.0556 for 3469 Fo > 4sig(Fo) and 0.1751 for all 7647 data REM 364 parameters refined using 0 restraints REM 00skl038 REM R1 = 0.0560 for 3471 Fo > 4sig(Fo) and 0.1755 for all 7647 data REM 364 parameters refined using 0 restraints REM Highest difference peak 1.341, deepest hole -0.710, 1-sigma level 0.187 CELL 0.71073 13.1826 12.8268 16.4122 90.000 105.964 90.000 ZERR 4.00 0.0002 0.0002 0.0003 0.000 0.001 0.001 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H BR CU N CL D UNIT 80 76 4 4 12 24 8 V = 2668.12 F(000) = 1312.0 Mu = 2.93 mm-1 Cell Wt = 2646.24 Rho = 1.647 MERG 2 MPLA N3 C9 C1 N2 C8 MPLA C10 C11 C15 C13 C12 C14 MPLA N3 C9 C1 N2 C8 MPLA C6 C4 C5 C3 N1 C2 FMAP 2 SIZE 0.05 0.05 0.05# PLAN -20 REM ACTA BOND $H CONF WPDB -1 WGHT 0.06880 L.S. 3 TEMP -123.00 FVAR 0.07589 BR1 3 0.164118 0.720748 0.390407 11.00000 0.03389 0.03362 = 0.04143 0.00369 0.00105 0.00170 CU1 4 -0.014802 0.741602 0.310898 11.00000 0.03104 0.02167 = 0.02720 -0.00012 0.00750 -0.00272 N3 5 -0.208998 0.671888 0.192594 11.00000 0.02360 0.01567 = 0.02861 0.00097 0.00677 -0.00317 C9 1 -0.260585 0.585698 0.147907 11.00000 0.02933 0.02551 = 0.03041 -0.00230 0.00628 -0.00583 C10 1 -0.254466 0.773447 0.194551 11.00000 0.02430 0.01981 = 0.02881 0.00045 0.00740 0.00328 C11 1 -0.235173 0.850361 0.142122 11.00000 0.02367 0.02529 = 0.02301 -0.00259 0.00537 -0.00046 C15 1 -0.316246 0.790499 0.249700 11.00000 0.02733 0.02736 = 0.03410 0.00216 0.01034 0.00462 C13 1 -0.338679 0.969697 0.200934 11.00000 0.02377 0.02829 = 0.03592 -0.00235 0.00359 0.00329 C12 1 -0.277924 0.948259 0.146324 11.00000 0.03264 0.02352 = 0.03502 0.01069 0.00625 -0.00053 C14 1 -0.357013 0.890015 0.251330 11.00000 0.03420 0.03791 = 0.03428 0.00062 0.01707 0.00918 C18 1 -0.382164 1.077074 0.205995 11.00000 0.05014 0.03350 = 0.06055 0.00482 0.02022 0.01235 C1 1 -0.108170 0.648694 0.234394 11.00000 0.03106 0.01774 = 0.02406 0.00275 0.01028 0.00353 C17 1 -0.335465 0.706090 0.306219 11.00000 0.05715 0.04417 = 0.05851 0.01469 0.03533 0.00307 CL5 6 0.466621 0.298095 0.485281 11.00000 0.04749 0.10056 = 0.05990 0.01982 0.00204 0.01557 CL3 6 0.218456 0.814297 0.189535 11.00000 0.11898 0.04238 = 0.05010 0.00478 0.01914 0.00507 CL1 6 0.337119 0.942407 0.102078 11.00000 0.07109 0.07404 = 0.11219 -0.02776 0.04158 -0.01442 CL2 6 0.118878 0.983178 0.084144 11.00000 0.08008 0.08043 = 0.06519 0.02915 0.03683 0.01751 CL6 6 0.548371 0.131578 0.598133 11.00000 0.12014 0.08598 = 0.16169 0.06407 0.09181 0.04998 CL4 6 0.588319 0.139717 0.434986 11.00000 0.08463 0.17027 = 0.12504 -0.09502 0.05200 -0.02979 N2 5 -0.098298 0.547305 0.214409 11.00000 0.02483 0.02094 = 0.02734 -0.00042 0.01021 0.00004 C6 1 0.051989 0.474766 0.172715 11.00000 0.02436 0.02010 = 0.03261 0.00172 0.00717 0.00491 C4 1 0.135624 0.547576 0.074940 11.00000 0.04347 0.04141 = 0.05633 0.02384 0.02065 0.00106 C7 1 0.000027 0.487124 0.242665 11.00000 0.03196 0.01868 = 0.02743 0.00233 0.00569 0.00426 C8 1 -0.191040 0.508272 0.161878 11.00000 0.03971 0.01832 = 0.03470 -0.00430 0.01411 -0.00426 C5 1 0.090297 0.559944 0.139363 11.00000 0.04594 0.02428 = 0.05107 0.00882 0.02129 -0.00178 C3 1 0.143555 0.448828 0.044356 11.00000 0.04779 0.05685 = 0.03982 0.01378 0.02638 0.01084 C20 1 0.569106 0.209643 0.519564 11.00000 0.02751 0.06748 = 0.05424 -0.01152 0.00695 -0.00746 C16 1 -0.171842 0.828205 0.079604 11.00000 0.04921 0.02923 = 0.04135 0.00831 0.02174 0.00531 C19 1 0.216085 0.886786 0.097861 11.00000 0.07215 0.04548 = 0.03816 -0.01202 0.02205 -0.01220 N1 5 0.058539 0.377707 0.143460 11.00000 0.02908 0.02477 = 0.02713 0.00286 0.00962 0.00240 C2 1 0.104517 0.367576 0.079754 11.00000 0.05187 0.03596 = 0.03548 0.00306 0.02407 0.01029 D2 7 0.633408 0.248225 0.539743 11.00000 0.01516 D1 7 0.198886 0.839624 0.057964 11.00000 0.03205 H16A 2 -0.168182 0.881167 0.058731 11.00000 0.05974 H16B 2 -0.210487 0.775719 0.037774 11.00000 0.06303 H16C 2 -0.105433 0.798051 0.106232 11.00000 0.04428 H18B 2 -0.443123 1.083799 0.166224 11.00000 0.06915 H12 2 -0.269557 0.997693 0.120054 11.00000 0.00568 H8 2 -0.193541 0.442481 0.143401 11.00000 0.02690 H17A 2 -0.377176 0.728387 0.340177 11.00000 0.06363 H9 2 -0.328811 0.593535 0.113244 11.00000 0.03616 H17C 2 -0.271346 0.684259 0.348543 11.00000 0.08982 H17B 2 -0.377073 0.657006 0.276757 11.00000 0.06276 H18A 2 -0.354714 1.123904 0.180365 11.00000 0.07288 H14 2 -0.388247 0.907163 0.293238 11.00000 0.06142 H2 2 0.101752 0.293906 0.056264 11.00000 0.02082 H7B 2 0.042766 0.520598 0.286590 11.00000 0.03162 H18C 2 -0.412130 1.087550 0.256346 11.00000 0.13876 H3 2 0.172366 0.435783 -0.002758 11.00000 0.05486 H4 2 0.160852 0.591084 0.054698 11.00000 0.05391 H7A 2 -0.017893 0.420687 0.264823 11.00000 0.02784 H5 2 0.082578 0.622168 0.159200 11.00000 0.02618 HKLF 4 Covalent radii and connectivity table for 00skl038 C 0.770 H 0.320 BR 1.140 CU 1.280 N 0.700 CL 0.990 D 0.320 Br1 - Cu1 Cu1 - C1 N1_$2 Br1 N3 - C1 C9 C10 C9 - H9 C8 N3 C10 - C11 C15 N3 C11 - C10 C12 C16 C15 - C14 C10 C17 C13 - C14 C12 C18 C12 - H12 C13 C11 C14 - H14 C13 C15 C18 - H18A H18B H18C C13 C1 - N3 N2 Cu1 C17 - H17B H17A H17C C15 Cl5 - C20 Cl3 - C19 Cl1 - C19 Cl2 - C19 Cl6 - C20 Cl4 - C20 N2 - C1 C8 C7 C6 - N1 C5 C7 C4 - H4 C5 C3 C7 - H7B H7A N2 C6 C8 - H8 C9 N2 C5 - H5 C4 C6 C3 - H3 C2 C4 C20 - Cl6 Cl4 Cl5 C16 - H16A H16C H16B C11 C19 - Cl1 Cl2 Cl3 N1 - C6 C2 Cu1_$1 C2 - H2 N1 C3 H16A - C16 H16B - C16 H16C - C16 H18B - C18 H12 - C12 H8 - C8 H17A - C17 H9 - C9 H17C - C17 H17B - C17 H18A - C18 H14 - C14 H2 - C2 H7B - C7 H18C - C18 H3 - C3 H4 - C4 H7A - C7 H5 - C5 Operators for generating equivalent atoms: $1 -x, y-1/2, -z+1/2 $2 -x, y+1/2, -z+1/2 27502 Reflections read, of which 785 rejected -18 =< h =< 17, -17 =< k =< 16, -16 =< l =< 23, Max. 2-theta = 61.02 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 1 0 0 1.24 0.07 4 3.57 1 1 0 7.96 0.06 10 2.25 1 5 0 10.66 0.09 8 1.28 1 6 0 10.40 0.17 8 1.32 -2 1 3 9.51 0.09 8 1.18 -1 2 3 33.39 0.10 8 9.56 -1 3 4 40.86 0.10 8 16.19 -1 5 5 10.70 0.10 7 1.60 -1 6 6 13.27 0.10 7 2.24 -4 4 7 19.20 0.35 6 2.21 -5 7 10 16.50 0.40 5 3.00 11 Inconsistent equivalents 7647 Unique reflections, of which 0 suppressed R(int) = 0.0926 R(sigma) = 0.1702 Friedel opposites merged Maximum memory for data reduction = 3665 / 76546 Least-squares cycle 1 Maximum vector length = 511 Memory required = 4527 / 465227 wR2 = 0.1531 before cycle 1 for 7647 data and 364 / 364 parameters GooF = S = 0.921; Restrained GooF = 0.921 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0688 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.07588 0.00014 -0.037 OSF Mean shift/esd = 0.002 Maximum = -0.037 for OSF Max. shift = 0.001 A for H18C Max. dU = 0.000 for H17C Least-squares cycle 2 Maximum vector length = 511 Memory required = 4527 / 465227 wR2 = 0.1531 before cycle 2 for 7647 data and 364 / 364 parameters GooF = S = 0.921; Restrained GooF = 0.921 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0688 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.07588 0.00014 0.000 OSF Mean shift/esd = 0.001 Maximum = 0.005 for U23 Br1 Max. shift = 0.000 A for H3 Max. dU = 0.000 for H17C Least-squares cycle 3 Maximum vector length = 511 Memory required = 4527 / 465227 wR2 = 0.1531 before cycle 3 for 7647 data and 364 / 364 parameters GooF = S = 0.921; Restrained GooF = 0.921 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0688 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.07588 0.00014 -0.001 OSF Mean shift/esd = 0.000 Maximum = 0.001 for y H16C Max. shift = 0.000 A for H16A Max. dU = 0.000 for H17B Largest correlation matrix elements 0.648 U13 Cl6 / U11 Cl6 0.543 U13 Cl4 / U11 Cl4 0.524 U13 Cl2 / U11 Cl2 0.631 U13 Cl6 / U33 Cl6 -0.539 U23 Cl4 / U33 Cl4 0.519 U13 Cl1 / U33 Cl1 -0.569 U23 Cl4 / U22 Cl4 0.536 U13 Cl2 / U33 Cl2 0.510 U13 Cl1 / U11 Cl1 0.561 z Cl6 / x Cl6 0.535 U13 Cl4 / U33 Cl4 0.509 U13 C3 / U11 C3 0.556 U12 Cl6 / U23 Cl6 0.534 z C17 / x C17 0.501 U13 C16 / U11 C16 0.555 U13 C17 / U11 C17 0.529 U13 C17 / U33 C17 00skl038 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq Br1 0.16412 0.72075 0.39041 1.00000 0.03389 0.03362 0.04143 0.00369 0.00105 0.00170 0.03816 0.00095 0.00004 0.00004 0.00003 0.00000 0.00031 0.00031 0.00031 0.00022 0.00023 0.00023 0.00017 Cu1 -0.01480 0.74160 0.31090 1.00000 0.03104 0.02167 0.02720 -0.00012 0.00750 -0.00272 0.02674 0.00103 0.00004 0.00004 0.00003 0.00000 0.00034 0.00031 0.00031 0.00022 0.00025 0.00024 0.00017 N3 -0.20900 0.67189 0.19259 1.00000 0.02361 0.01567 0.02861 0.00097 0.00677 -0.00317 0.02271 0.00649 0.00027 0.00025 0.00021 0.00000 0.00214 0.00187 0.00201 0.00149 0.00172 0.00160 0.00081 C9 -0.26059 0.58570 0.14791 1.00000 0.02933 0.02550 0.03043 -0.00230 0.00628 -0.00583 0.02881 0.00906 0.00040 0.00035 0.00029 0.00000 0.00292 0.00267 0.00272 0.00198 0.00237 0.00229 0.00109 C10 -0.25447 0.77345 0.19455 1.00000 0.02431 0.01982 0.02881 0.00045 0.00740 0.00328 0.02429 0.00825 0.00034 0.00031 0.00027 0.00000 0.00250 0.00237 0.00240 0.00185 0.00202 0.00197 0.00099 C11 -0.23517 0.85036 0.14212 1.00000 0.02368 0.02530 0.02301 -0.00259 0.00536 -0.00046 0.02421 0.00797 0.00034 0.00032 0.00026 0.00000 0.00254 0.00250 0.00232 0.00183 0.00198 0.00198 0.00100 C15 -0.31625 0.79050 0.24970 1.00000 0.02733 0.02737 0.03411 0.00217 0.01034 0.00462 0.02923 0.00882 0.00035 0.00034 0.00028 0.00000 0.00269 0.00260 0.00264 0.00201 0.00220 0.00214 0.00107 C13 -0.33868 0.96970 0.20093 1.00000 0.02377 0.02830 0.03594 -0.00235 0.00359 0.00328 0.03025 0.00854 0.00035 0.00034 0.00029 0.00000 0.00261 0.00271 0.00271 0.00207 0.00221 0.00207 0.00109 C12 -0.27792 0.94826 0.14632 1.00000 0.03263 0.02352 0.03503 0.01069 0.00625 -0.00053 0.03100 0.00920 0.00038 0.00038 0.00031 0.00000 0.00297 0.00272 0.00286 0.00230 0.00236 0.00230 0.00117 C14 -0.35701 0.89002 0.25133 1.00000 0.03421 0.03791 0.03427 0.00062 0.01707 0.00919 0.03395 0.00964 0.00038 0.00038 0.00031 0.00000 0.00299 0.00303 0.00281 0.00227 0.00246 0.00239 0.00117 C18 -0.38216 1.07707 0.20600 1.00000 0.05012 0.03350 0.06054 0.00482 0.02021 0.01235 0.04706 0.01428 0.00057 0.00046 0.00045 0.00000 0.00415 0.00339 0.00429 0.00288 0.00379 0.00296 0.00152 C1 -0.10817 0.64869 0.23439 1.00000 0.03106 0.01774 0.02408 0.00276 0.01028 0.00354 0.02376 0.00829 0.00035 0.00030 0.00025 0.00000 0.00276 0.00232 0.00231 0.00176 0.00209 0.00196 0.00099 C17 -0.33546 0.70609 0.30622 1.00000 0.05716 0.04417 0.05851 0.01468 0.03532 0.00306 0.04943 0.01651 0.00061 0.00052 0.00047 0.00000 0.00445 0.00378 0.00418 0.00324 0.00391 0.00353 0.00158 Cl5 0.46662 0.29809 0.48528 1.00000 0.04749 0.10056 0.05990 0.01982 0.00204 0.01557 0.07184 0.00339 0.00012 0.00014 0.00010 0.00000 0.00097 0.00129 0.00100 0.00090 0.00079 0.00090 0.00048 Cl3 0.21845 0.81430 0.18953 1.00000 0.11898 0.04238 0.05010 0.00478 0.01914 0.00506 0.07130 0.00327 0.00015 0.00011 0.00009 0.00000 0.00153 0.00084 0.00089 0.00067 0.00095 0.00092 0.00051 Cl1 0.33712 0.94241 0.10208 1.00000 0.07109 0.07404 0.11219 -0.02776 0.04158 -0.01442 0.08252 0.00336 0.00014 0.00014 0.00012 0.00000 0.00124 0.00119 0.00154 0.00101 0.00116 0.00096 0.00057 Cl2 0.11888 0.98318 0.08414 1.00000 0.08008 0.08044 0.06519 0.02915 0.03683 0.01751 0.07189 0.00366 0.00014 0.00013 0.00010 0.00000 0.00123 0.00118 0.00104 0.00085 0.00096 0.00094 0.00051 Cl6 0.54837 0.13158 0.59814 1.00000 0.12014 0.08599 0.16170 0.06407 0.09181 0.04998 0.11209 0.00534 0.00018 0.00016 0.00015 0.00000 0.00181 0.00140 0.00206 0.00135 0.00165 0.00128 0.00084 Cl4 0.58832 0.13972 0.43498 1.00000 0.08464 0.17028 0.12505 -0.09503 0.05200 -0.02979 0.12206 0.00370 0.00016 0.00020 0.00014 0.00000 0.00153 0.00232 0.00180 0.00168 0.00139 0.00145 0.00096 N2 -0.09830 0.54730 0.21441 1.00000 0.02483 0.02095 0.02735 -0.00042 0.01022 0.00003 0.02377 0.00670 0.00027 0.00026 0.00021 0.00000 0.00216 0.00200 0.00203 0.00153 0.00172 0.00165 0.00082 C6 0.05199 0.47477 0.17271 1.00000 0.02437 0.02010 0.03261 0.00171 0.00717 0.00490 0.02583 0.00840 0.00034 0.00032 0.00027 0.00000 0.00253 0.00251 0.00256 0.00190 0.00207 0.00197 0.00102 C4 0.13562 0.54758 0.07494 1.00000 0.04347 0.04142 0.05634 0.02385 0.02065 0.00106 0.04570 0.01203 0.00045 0.00047 0.00037 0.00000 0.00359 0.00365 0.00377 0.00299 0.00304 0.00285 0.00154 C7 0.00003 0.48712 0.24266 1.00000 0.03196 0.01868 0.02742 0.00233 0.00568 0.00426 0.02652 0.00998 0.00039 0.00037 0.00029 0.00000 0.00284 0.00255 0.00270 0.00207 0.00233 0.00217 0.00105 C8 -0.19104 0.50827 0.16188 1.00000 0.03972 0.01833 0.03469 -0.00431 0.01411 -0.00426 0.03015 0.00935 0.00039 0.00037 0.00029 0.00000 0.00317 0.00258 0.00270 0.00207 0.00235 0.00236 0.00112 C5 0.09030 0.55995 0.13936 1.00000 0.04593 0.02429 0.05107 0.00883 0.02130 -0.00178 0.03885 0.01076 0.00042 0.00041 0.00034 0.00000 0.00343 0.00297 0.00338 0.00249 0.00282 0.00253 0.00129 C3 0.14356 0.44883 0.04436 1.00000 0.04778 0.05686 0.03984 0.01378 0.02638 0.01083 0.04532 0.01143 0.00042 0.00045 0.00034 0.00000 0.00360 0.00395 0.00320 0.00273 0.00289 0.00291 0.00142 C20 0.56911 0.20964 0.51956 1.00000 0.02751 0.06748 0.05424 -0.01151 0.00695 -0.00744 0.05060 0.01098 0.00044 0.00046 0.00036 0.00000 0.00311 0.00404 0.00362 0.00295 0.00275 0.00294 0.00149 C16 -0.17184 0.82820 0.07960 1.00000 0.04921 0.02924 0.04134 0.00831 0.02174 0.00531 0.03809 0.01291 0.00052 0.00049 0.00037 0.00000 0.00395 0.00324 0.00329 0.00272 0.00298 0.00294 0.00134 C19 0.21608 0.88678 0.09786 1.00000 0.07215 0.04548 0.03815 -0.01202 0.02204 -0.01221 0.05057 0.01139 0.00049 0.00045 0.00035 0.00000 0.00442 0.00346 0.00321 0.00275 0.00308 0.00317 0.00155 N1 0.05854 0.37771 0.14346 1.00000 0.02908 0.02478 0.02714 0.00286 0.00962 0.00240 0.02663 0.00683 0.00028 0.00027 0.00021 0.00000 0.00224 0.00212 0.00201 0.00159 0.00177 0.00171 0.00086 C2 0.10452 0.36758 0.07975 1.00000 0.05188 0.03597 0.03549 0.00306 0.02409 0.01030 0.03872 0.01061 0.00042 0.00040 0.00030 0.00000 0.00355 0.00315 0.00286 0.00238 0.00267 0.00265 0.00126 D2 0.63340 0.24823 0.53974 1.00000 0.01519 0.07935 0.00322 0.00293 0.00242 0.00000 0.01032 D1 0.19886 0.83962 0.05796 1.00000 0.03206 0.08939 0.00353 0.00345 0.00281 0.00000 0.01317 H16A -0.16822 0.88115 0.05872 1.00000 0.05969 0.10701 0.00438 0.00452 0.00346 0.00000 0.02019 H16B -0.21049 0.77572 0.03777 1.00000 0.06304 0.11241 0.00437 0.00416 0.00348 0.00000 0.01797 H16C -0.10542 0.79809 0.10624 1.00000 0.04422 0.09653 0.00415 0.00385 0.00316 0.00000 0.01530 H18B -0.44312 1.08378 0.16625 1.00000 0.06918 0.11646 0.00486 0.00470 0.00383 0.00000 0.02154 H12 -0.26956 0.99769 0.12006 1.00000 0.00569 0.06992 0.00286 0.00299 0.00224 0.00000 0.01027 H8 -0.19354 0.44249 0.14340 1.00000 0.02692 0.08136 0.00321 0.00338 0.00250 0.00000 0.01221 H17A -0.37718 0.72840 0.34019 1.00000 0.06364 0.10868 0.00482 0.00418 0.00370 0.00000 0.01850 H9 -0.32881 0.59354 0.11324 1.00000 0.03619 0.08811 0.00363 0.00335 0.00276 0.00000 0.01361 H17C -0.27133 0.68427 0.34857 1.00000 0.08993 0.12613 0.00522 0.00499 0.00412 0.00000 0.02383 H17B -0.37704 0.65704 0.27679 1.00000 0.06272 0.11817 0.00457 0.00445 0.00365 0.00000 0.02100 H18A -0.35473 1.12388 0.18035 1.00000 0.07286 0.11796 0.00476 0.00478 0.00382 0.00000 0.02215 H14 -0.38825 0.90717 0.29325 1.00000 0.06145 0.10051 0.00409 0.00404 0.00336 0.00000 0.01710 H2 0.10176 0.29391 0.05626 1.00000 0.02082 0.07919 0.00313 0.00324 0.00244 0.00000 0.01072 H7B 0.04273 0.52058 0.28656 1.00000 0.03164 0.09213 0.00358 0.00338 0.00285 0.00000 0.01331 H18C -0.41213 1.08756 0.25639 1.00000 0.13875 0.14759 0.00618 0.00600 0.00496 0.00000 0.03083 H3 0.17235 0.43576 -0.00280 1.00000 0.05484 0.09629 0.00395 0.00377 0.00330 0.00000 0.01555 H4 0.16083 0.59107 0.05470 1.00000 0.05393 0.10121 0.00409 0.00424 0.00331 0.00000 0.01884 H7A -0.01790 0.42067 0.26482 1.00000 0.02789 0.07703 0.00312 0.00342 0.00248 0.00000 0.01171 H5 0.08258 0.62217 0.15920 1.00000 0.02616 0.08252 0.00334 0.00348 0.00257 0.00000 0.01280 Final Structure Factor Calculation for 00skl038 Total number of l.s. parameters = 364 Maximum vector length = 511 Memory required = 4163 / 26061 wR2 = 0.1531 before cycle 4 for 7647 data and 0 / 364 parameters GooF = S = 0.921; Restrained GooF = 0.921 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0688 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0560 for 3471 Fo > 4sig(Fo) and 0.1755 for all 7647 data wR2 = 0.1531, GooF = S = 0.921, Restrained GooF = 0.921 for all data Occupancy sum of asymmetric unit = 50.00 for non-hydrogen and 2.00 for hydrogen atoms Principal mean square atomic displacements U 0.0515 0.0350 0.0280 Br1 0.0321 0.0272 0.0209 Cu1 0.0291 0.0247 0.0143 N3 0.0341 0.0313 0.0210 C9 0.0289 0.0260 0.0180 C10 0.0272 0.0243 0.0212 C11 0.0354 0.0298 0.0225 C15 0.0406 0.0282 0.0220 C13 0.0439 0.0320 0.0170 C12 0.0463 0.0351 0.0204 C14 0.0638 0.0506 0.0268 C18 0.0324 0.0223 0.0165 C1 0.0772 0.0457 0.0255 C17 0.1090 0.0712 0.0354 Cl5 0.1221 0.0517 0.0401 Cl3 0.1293 0.0602 0.0580 Cl1 0.1125 0.0641 0.0390 Cl2 0.2243 0.0639 0.0481 Cl6 may be split into 0.5604 0.1388 0.6064 and 0.5364 0.1243 0.5899 0.2465 0.0753 0.0443 Cl4 may be split into 0.5818 0.1523 0.4274 and 0.5948 0.1272 0.4425 0.0287 0.0218 0.0208 N2 0.0331 0.0275 0.0169 C6 0.0739 0.0426 0.0206 C4 0.0346 0.0279 0.0171 C7 0.0421 0.0313 0.0171 C8 0.0563 0.0406 0.0197 C5 0.0714 0.0417 0.0228 C3 0.0741 0.0517 0.0260 C20 0.0558 0.0338 0.0247 C16 0.0776 0.0454 0.0287 C19 0.0314 0.0257 0.0229 N1 0.0597 0.0331 0.0233 C2 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.009 0.016 0.024 0.033 0.043 0.055 0.071 0.095 0.142 1.000 Number in group 823. 718. 781. 802. 759. 749. 742. 749. 757. 767. GooF 0.715 0.747 0.807 0.837 0.877 0.921 1.003 1.101 1.052 1.075 K 0.790 0.540 0.944 0.917 0.975 0.973 0.995 0.996 1.012 1.015 Resolution(A) 0.70 0.74 0.77 0.81 0.85 0.90 0.97 1.07 1.22 1.54 inf Number in group 765. 783. 746. 769. 762. 769. 768. 750. 767. 768. GooF 0.767 0.744 0.810 0.869 0.890 0.857 0.919 1.010 1.012 1.232 K 0.847 0.915 0.995 1.039 1.007 1.027 1.015 1.020 1.021 1.004 R1 0.539 0.441 0.382 0.306 0.252 0.152 0.101 0.072 0.048 0.032 Recommended weighting scheme: WGHT 0.0689 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) 1 0 0 214.56 22540.41 20.54 0.414 12.67 1 16 2 208.39 2182.98 5.11 0.129 0.79 4 3 6 412.15 682.12 4.84 0.072 1.66 -7 5 18 238.89 930.81 4.21 0.084 0.84 1 6 7 335.84 526.17 4.20 0.063 1.51 -8 4 12 -24.39 208.46 4.03 0.040 1.11 -2 7 4 845.39 1116.77 3.79 0.092 1.66 -1 4 6 119.98 51.86 3.66 0.020 2.08 -3 0 8 811.95 1092.92 3.62 0.091 2.01 -3 4 18 1964.37 1180.15 3.59 0.095 0.88 6 7 0 828.79 1113.17 3.52 0.092 1.38 3 3 2 2309.29 1835.28 3.50 0.118 2.64 7 5 7 1552.93 2122.09 3.44 0.127 1.13 2 6 19 -46.75 846.02 3.44 0.080 0.75 -1 10 13 104.30 543.99 3.44 0.064 0.89 2 5 10 2703.89 2083.15 3.42 0.126 1.26 1 1 3 2778.45 2239.58 3.40 0.130 4.20 10 1 6 980.57 547.64 3.36 0.065 1.03 -1 3 6 4011.01 3230.20 3.35 0.157 2.30 7 7 0 37.86 198.61 3.33 0.039 1.29 1 2 2 31.57 72.14 3.26 0.023 4.38 1 1 0 1382.41 2609.35 3.26 0.141 9.02 7 2 7 693.61 1023.26 3.22 0.088 1.23 -3 2 4 86.06 130.16 3.21 0.031 2.99 5 0 4 1487.67 2010.77 3.18 0.124 1.91 2 13 3 615.78 276.78 3.16 0.046 0.95 4 4 5 497.01 705.27 3.15 0.073 1.68 -8 2 8 445.64 609.32 3.15 0.068 1.41 11 9 3 705.27 1284.06 3.13 0.099 0.85 -12 4 10 551.93 928.21 3.09 0.084 0.97 4 3 7 387.97 222.70 3.09 0.041 1.53 9 6 4 1346.87 917.70 3.06 0.084 1.06 1 1 8 495.33 652.77 3.06 0.070 1.85 15 1 2 1904.26 1171.81 3.06 0.094 0.82 -2 1 11 159.27 261.69 3.05 0.045 1.48 0 14 1 2009.64 1368.83 3.05 0.102 0.91 -8 3 3 280.55 441.30 3.05 0.058 1.54 -2 2 14 241.35 84.29 3.03 0.025 1.15 -15 6 4 -122.43 536.30 3.01 0.064 0.81 1 7 6 1453.49 1846.69 3.01 0.118 1.47 7 5 6 2174.67 1670.03 3.00 0.113 1.18 0 3 14 805.07 1087.66 3.00 0.091 1.09 -1 5 1 746.30 935.63 3.00 0.084 2.50 -2 3 9 1155.90 917.98 3.00 0.084 1.68 -8 6 11 219.78 384.10 2.98 0.054 1.08 -16 4 8 7.89 460.92 2.98 0.059 0.79 7 8 4 1104.22 1469.19 2.96 0.106 1.09 3 2 9 648.84 858.96 2.96 0.081 1.44 4 1 12 905.92 570.49 2.95 0.066 1.11 3 4 7 1182.26 1491.19 2.94 0.106 1.57 Bond lengths and angles Br1 - Distance Angles Cu1 2.3758 (0.0007) Br1 - Cu1 - Distance Angles C1 1.9135 (0.0043) N1_$2 2.0442 (0.0035) 125.24 (0.16) Br1 2.3758 (0.0007) 130.73 (0.13) 103.43 (0.10) Cu1 - C1 N1_$2 N3 - Distance Angles C1 1.3506 (0.0052) C9 1.3958 (0.0054) 111.20 (0.36) C10 1.4380 (0.0052) 123.11 (0.34) 125.69 (0.37) N3 - C1 C9 C9 - Distance Angles H9 0.9281 (0.0445) C8 1.3281 (0.0065) 133.91 (2.78) N3 1.3958 (0.0054) 119.10 (2.78) 106.75 (0.43) C9 - H9 C8 C10 - Distance Angles C11 1.3780 (0.0057) C15 1.3913 (0.0060) 122.36 (0.38) N3 1.4380 (0.0052) 119.01 (0.36) 118.63 (0.37) C10 - C11 C15 C11 - Distance Angles C10 1.3780 (0.0057) C12 1.3858 (0.0061) 118.05 (0.40) C16 1.5172 (0.0066) 121.24 (0.41) 120.69 (0.43) C11 - C10 C12 C15 - Distance Angles C14 1.3881 (0.0063) C10 1.3913 (0.0060) 117.14 (0.41) C17 1.4920 (0.0070) 121.50 (0.46) 121.35 (0.44) C15 - C14 C10 C13 - Distance Angles C14 1.3773 (0.0064) C12 1.3839 (0.0064) 118.03 (0.43) C18 1.5029 (0.0070) 120.95 (0.46) 121.02 (0.48) C13 - C14 C12 C12 - Distance Angles H12 0.7912 (0.0367) C13 1.3839 (0.0064) 112.68 (2.70) C11 1.3858 (0.0061) 125.42 (2.72) 121.87 (0.45) C12 - H12 C13 C14 - Distance Angles H14 0.9204 (0.0530) C13 1.3773 (0.0064) 117.38 (3.33) C15 1.3881 (0.0063) 119.30 (3.31) 122.55 (0.44) C14 - H14 C13 C18 - Distance Angles H18A 0.8673 (0.0613) H18B 0.8890 (0.0599) 89.44 (4.97) H18C 1.0188 (0.0812) 127.53 (5.88) 96.25 (5.49) C13 1.5029 (0.0070) 113.04 (3.96) 109.25 (4.02) 113.88 (4.42) C18 - H18A H18B H18C C1 - Distance Angles N3 1.3506 (0.0052) N2 1.3562 (0.0049) 103.58 (0.36) Cu1 1.9135 (0.0043) 124.17 (0.29) 131.97 (0.33) C1 - N3 N2 C17 - Distance Angles H17B 0.8855 (0.0573) H17A 0.9293 (0.0624) 99.58 (5.09) H17C 0.9762 (0.0659) 118.01 (5.38) 101.58 (4.94) C15 1.4920 (0.0070) 111.22 (3.78) 112.29 (3.42) 112.88 (3.84) C17 - H17B H17A H17C Cl5 - Distance Angles C20 1.7352 (0.0059) Cl5 - Cl3 - Distance Angles C19 1.7616 (0.0055) Cl3 - Cl1 - Distance Angles C19 1.7317 (0.0061) Cl1 - Cl2 - Distance Angles C19 1.7501 (0.0063) Cl2 - Cl6 - Distance Angles C20 1.7129 (0.0061) Cl6 - Cl4 - Distance Angles C20 1.7288 (0.0057) Cl4 - N2 - Distance Angles C1 1.3562 (0.0049) C8 1.3816 (0.0056) 111.78 (0.37) C7 1.4698 (0.0053) 124.21 (0.37) 123.97 (0.37) N2 - C1 C8 C6 - Distance Angles N1 1.3456 (0.0052) C5 1.3786 (0.0063) 121.68 (0.42) C7 1.4983 (0.0063) 117.32 (0.37) 121.00 (0.42) C6 - N1 C5 C4 - Distance Angles H4 0.7699 (0.0517) C5 1.3593 (0.0075) 125.82 (4.19) C3 1.3770 (0.0077) 115.11 (4.16) 118.99 (0.53) C4 - H4 C5 C7 - Distance Angles H7B 0.8929 (0.0456) H7A 0.9808 (0.0429) 106.34 (3.68) N2 1.4698 (0.0053) 107.92 (2.85) 106.97 (2.41) C6 1.4983 (0.0063) 110.45 (2.87) 113.56 (2.33) 111.29 (0.35) C7 - H7B H7A N2 C8 - Distance Angles H8 0.8941 (0.0418) C9 1.3281 (0.0065) 133.46 (2.74) N2 1.3816 (0.0056) 119.82 (2.73) 106.68 (0.41) C8 - H8 C9 C5 - Distance Angles H5 0.8785 (0.0423) C4 1.3593 (0.0075) 120.99 (2.81) C6 1.3786 (0.0062) 118.72 (2.82) 120.25 (0.52) C5 - H5 C4 C3 - Distance Angles H3 0.9657 (0.0517) C2 1.3612 (0.0069) 119.15 (3.02) C4 1.3770 (0.0077) 122.53 (2.99) 118.24 (0.49) C3 - H3 C2 C20 - Distance Angles Cl6 1.7129 (0.0061) Cl4 1.7288 (0.0057) 112.96 (0.35) Cl5 1.7352 (0.0059) 110.80 (0.31) 110.60 (0.33) D2 0.9584 (0.0398) 110.53 (2.38) 103.56 (2.28) 108.07 (2.37) C20 - Cl6 Cl4 Cl5 C16 - Distance Angles H16A 0.7681 (0.0557) H16C 0.9468 (0.0529) 113.81 (5.28) H16B 0.9959 (0.0554) 111.89 (5.23) 105.97 (4.28) C11 1.5172 (0.0066) 104.45 (4.25) 112.04 (2.98) 108.70 (3.17) C16 - H16A H16C H16B C19 - Distance Angles Cl1 1.7317 (0.0061) Cl2 1.7501 (0.0063) 110.37 (0.32) Cl3 1.7616 (0.0055) 112.56 (0.35) 108.85 (0.30) D1 0.8744 (0.0436) 111.19 (3.01) 111.24 (3.08) 102.39 (2.93) C19 - Cl1 Cl2 Cl3 N1 - Distance Angles C6 1.3456 (0.0052) C2 1.3513 (0.0056) 116.84 (0.38) Cu1_$1 2.0442 (0.0035) 127.38 (0.28) 115.67 (0.30) N1 - C6 C2 C2 - Distance Angles H2 1.0174 (0.0403) N1 1.3513 (0.0056) 113.93 (2.21) C3 1.3612 (0.0069) 121.85 (2.20) 124.01 (0.47) C2 - H2 N1 H16A - Distance Angles C16 0.7681 (0.0556) H16A - H16B - Distance Angles C16 0.9959 (0.0555) H16B - H16C - Distance Angles C16 0.9468 (0.0527) H16C - H18B - Distance Angles C18 0.8890 (0.0599) H18B - H12 - Distance Angles C12 0.7912 (0.0366) H12 - H8 - Distance Angles C8 0.8941 (0.0418) H8 - H17A - Distance Angles C17 0.9293 (0.0624) H17A - H9 - Distance Angles C9 0.9281 (0.0445) H9 - H17C - Distance Angles C17 0.9762 (0.0656) H17C - H17B - Distance Angles C17 0.8855 (0.0573) H17B - H18A - Distance Angles C18 0.8673 (0.0610) H18A - H14 - Distance Angles C14 0.9204 (0.0530) H14 - H2 - Distance Angles C2 1.0174 (0.0404) H2 - H7B - Distance Angles C7 0.8929 (0.0454) H7B - H18C - Distance Angles C18 1.0188 (0.0811) H18C - H3 - Distance Angles C3 0.9657 (0.0516) H3 - H4 - Distance Angles C4 0.7699 (0.0516) H4 - H7A - Distance Angles C7 0.9808 (0.0429) H7A - H5 - Distance Angles C5 0.8785 (0.0423) H5 - Selected torsion angles -175.21 ( 3.07) C1 - N3 - C9 - H9 4.18 ( 3.15) C10 - N3 - C9 - H9 -0.18 ( 0.49) C1 - N3 - C9 - C8 179.20 ( 0.38) C10 - N3 - C9 - C8 80.98 ( 0.50) C1 - N3 - C10 - C11 -98.34 ( 0.51) C9 - N3 - C10 - C11 -98.83 ( 0.49) C1 - N3 - C10 - C15 81.86 ( 0.53) C9 - N3 - C10 - C15 1.14 ( 0.66) C15 - C10 - C11 - C12 -178.66 ( 0.39) N3 - C10 - C11 - C12 -177.05 ( 0.47) C15 - C10 - C11 - C16 3.16 ( 0.65) N3 - C10 - C11 - C16 -1.18 ( 0.67) C11 - C10 - C15 - C14 178.62 ( 0.40) N3 - C10 - C15 - C14 -179.64 ( 0.53) C11 - C10 - C15 - C17 0.16 ( 0.71) N3 - C10 - C15 - C17 -178.78 ( 2.96) C14 - C13 - C12 - H12 0.41 ( 3.06) C18 - C13 - C12 - H12 -0.65 ( 0.71) C14 - C13 - C12 - C11 178.53 ( 0.50) C18 - C13 - C12 - C11 177.69 ( 3.36) C10 - C11 - C12 - H12 -4.12 ( 3.47) C16 - C11 - C12 - H12 -0.19 ( 0.68) C10 - C11 - C12 - C13 178.00 ( 0.47) C16 - C11 - C12 - C13 170.49 ( 3.71) C12 - C13 - C14 - H14 -8.69 ( 3.81) C18 - C13 - C14 - H14 0.61 ( 0.73) C12 - C13 - C14 - C15 -178.58 ( 0.51) C18 - C13 - C14 - C15 -169.43 ( 3.80) C10 - C15 - C14 - H14 9.04 ( 3.89) C17 - C15 - C14 - H14 0.28 ( 0.72) C10 - C15 - C14 - C13 178.74 ( 0.55) C17 - C15 - C14 - C13 167.12 ( 4.53) C14 - C13 - C18 - H18A -12.04 ( 4.68) C12 - C13 - C18 - H18A -94.99 ( 4.27) C14 - C13 - C18 - H18B 85.85 ( 4.31) C12 - C13 - C18 - H18B 11.31 ( 4.91) C14 - C13 - C18 - H18C -167.85 ( 4.82) C12 - C13 - C18 - H18C 0.34 ( 0.44) C9 - N3 - C1 - N2 -179.06 ( 0.33) C10 - N3 - C1 - N2 -174.22 ( 0.29) C9 - N3 - C1 - Cu1 6.38 ( 0.53) C10 - N3 - C1 - Cu1 10.99 ( 0.42) N1_$2 - Cu1 - C1 - N3 -179.37 ( 0.24) Br1 - Cu1 - C1 - N3 -161.90 ( 0.34) N1_$2 - Cu1 - C1 - N2 7.74 ( 0.47) Br1 - Cu1 - C1 - N2 111.40 ( 4.06) C14 - C15 - C17 - H17B -70.20 ( 4.12) C10 - C15 - C17 - H17B 0.79 ( 4.08) C14 - C15 - C17 - H17A 179.19 ( 3.94) C10 - C15 - C17 - H17A -113.31 ( 4.15) C14 - C15 - C17 - H17C 65.09 ( 4.19) C10 - C15 - C17 - H17C -0.39 ( 0.44) N3 - C1 - N2 - C8 173.56 ( 0.32) Cu1 - C1 - N2 - C8 177.61 ( 0.34) N3 - C1 - N2 - C7 -8.44 ( 0.60) Cu1 - C1 - N2 - C7 18.06 ( 3.05) C1 - N2 - C7 - H7B -164.17 ( 2.94) C8 - N2 - C7 - H7B 132.14 ( 2.42) C1 - N2 - C7 - H7A -50.10 ( 2.45) C8 - N2 - C7 - H7A -103.28 ( 0.46) C1 - N2 - C7 - C6 74.48 ( 0.52) C8 - N2 - C7 - C6 125.57 ( 3.02) N1 - C6 - C7 - H7B -55.14 ( 3.05) C5 - C6 - C7 - H7B 6.21 ( 2.66) N1 - C6 - C7 - H7A -174.49 ( 2.60) C5 - C6 - C7 - H7A -114.57 ( 0.43) N1 - C6 - C7 - N2 64.73 ( 0.59) C5 - C6 - C7 - N2 -3.91 ( 5.28) H9 - C9 - C8 - H8 -177.88 ( 3.60) N3 - C9 - C8 - H8 173.90 ( 3.75) H9 - C9 - C8 - N2 -0.07 ( 0.48) N3 - C9 - C8 - N2 178.46 ( 2.99) C1 - N2 - C8 - H8 0.46 ( 3.06) C7 - N2 - C8 - H8 0.29 ( 0.49) C1 - N2 - C8 - C9 -177.71 ( 0.38) C7 - N2 - C8 - C9 5.33 ( 6.13) H4 - C4 - C5 - H5 -178.29 ( 3.32) C3 - C4 - C5 - H5 -177.06 ( 5.00) H4 - C4 - C5 - C6 -0.68 ( 0.84) C3 - C4 - C5 - C6 178.05 ( 3.24) N1 - C6 - C5 - H5 -1.22 ( 3.36) C7 - C6 - C5 - H5 0.38 ( 0.77) N1 - C6 - C5 - C4 -178.88 ( 0.48) C7 - C6 - C5 - C4 -5.84 ( 5.97) H4 - C4 - C3 - H3 177.40 ( 3.61) C5 - C4 - C3 - H3 177.35 ( 4.49) H4 - C4 - C3 - C2 0.59 ( 0.83) C5 - C4 - C3 - C2 -177.37 ( 4.40) C10 - C11 - C16 - H16A 4.50 ( 4.53) C12 - C11 - C16 - H16A -53.72 ( 3.30) C10 - C11 - C16 - H16C 128.14 ( 3.21) C12 - C11 - C16 - H16C 63.05 ( 3.35) C10 - C11 - C16 - H16B -115.08 ( 3.28) C12 - C11 - C16 - H16B 0.01 ( 0.66) C5 - C6 - N1 - C2 179.30 ( 0.41) C7 - C6 - N1 - C2 175.98 ( 0.35) C5 - C6 - N1 - Cu1_$1 -4.73 ( 0.57) C7 - C6 - N1 - Cu1_$1 -174.81 ( 2.51) C6 - N1 - C2 - H2 8.74 ( 2.59) Cu1_$1 - N1 - C2 - H2 -0.10 ( 0.73) C6 - N1 - C2 - C3 -176.54 ( 0.42) Cu1_$1 - N1 - C2 - C3 -2.82 ( 4.49) H3 - C3 - C2 - H2 174.11 ( 2.74) C4 - C3 - C2 - H2 -177.12 ( 3.45) H3 - C3 - C2 - N1 -0.20 ( 0.83) C4 - C3 - C2 - N1 Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane) - 7.0146 (0.0227) x - 3.6017 (0.0258) y + 15.0057 (0.0143) z = 1.9375 (0.0180) * -0.0015 (0.0025) N3 * 0.0003 (0.0026) C9 * 0.0021 (0.0023) C1 * -0.0019 (0.0024) N2 * 0.0010 (0.0026) C8 Rms deviation of fitted atoms = 0.0015 8.5545 (0.0186) x + 3.3902 (0.0234) y + 8.3288 (0.0267) z = 2.0586 (0.0229) Angle to previous plane (with approximate esd) = 81.35 ( 0.13 ) * 0.0072 (0.0031) C10 * -0.0037 (0.0031) C11 * -0.0042 (0.0032) C15 * 0.0053 (0.0033) C13 * -0.0025 (0.0033) C12 * -0.0020 (0.0034) C14 Rms deviation of fitted atoms = 0.0045 - 7.0146 (0.0227) x - 3.6017 (0.0258) y + 15.0057 (0.0143) z = 1.9375 (0.0180) Angle to previous plane (with approximate esd) = 81.35 ( 0.13 ) * -0.0015 (0.0025) N3 * 0.0003 (0.0026) C9 * 0.0021 (0.0023) C1 * -0.0019 (0.0024) N2 * 0.0010 (0.0026) C8 Rms deviation of fitted atoms = 0.0015 9.6974 (0.0181) x - 1.5057 (0.0268) y + 7.2065 (0.0306) z = 1.0342 (0.0130) Angle to previous plane (with approximate esd) = 79.96 ( 0.13 ) * -0.0002 (0.0032) C6 * -0.0034 (0.0039) C4 * 0.0027 (0.0037) C5 * 0.0018 (0.0038) C3 * -0.0014 (0.0030) N1 * 0.0006 (0.0036) C2 Rms deviation of fitted atoms = 0.0020 FMAP and GRID set by program FMAP 2 1 36 GRID -1.515 -2 -1 1.515 2 1 R1 = 0.1710 for 7647 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 1.34 at 0.4361 0.8556 0.3786 [ 0.41 A from CL6 ] Deepest hole -0.71 at 0.1412 0.7639 0.3567 [ 0.78 A from BR1 ] Mean = 0.00, Rms deviation from mean = 0.19 e/A^3, Highest memory used = 4522 / 54591 Molecule 1 scale 0.469 inches = 1.192 cm per Angstrom CL3 1 12C** 15 C20 3 4 2 CL4 CL4 2 4 3 CL5 7 CL511 CL6 10 1 16 18 CL2 1 C9 BR1 20 14 CL6 C18 C13 C12 C14 C11 C16 C8 C15 C10 17 C17 N3 3 BR1 CL3 4 N2 C2 CL4 8 C1 N1 CU*3 C6 C4 C7 C5 CL2 CU1 N1 CL3 BR1 CL4 Atom Peak x y z Sof Height Distances and Angles BR1 0.00 0.1641 0.7207 0.3904 1.000 2.4 0 CU1 2.376 0 H7B 3.249 61.9 20 D2 2.630 163.3 130.0 22 D1 2.771 116.4 102.9 74.9 24 H8 2.944 87.1 137.4 76.4 117.6 23 H12 3.206 116.8 54.9 75.8 81.3 140.4 25 H18A 3.288 126.0 80.2 55.1 108.1 98.4 42.2 6 CL3 3.758 83.2 88.7 85.3 160.1 57.3 92.7 57.5 15 CL4 4.114 144.2 153.0 27.7 63.1 65.8 98.8 82.7 99.6 CU1 0.19 -0.0148 0.7416 0.3109 1.000 2.4 0 BR1 2.376 0 C1 1.914 130.7 0 H16C 3.321 127.4 59.0 0 H7B 2.990 73.5 57.5 96.1 0 H5 3.457 80.6 63.3 58.0 47.6 19 N1 2.044 103.4 125.2 97.2 165.1 147.2 28 H7A 2.702 95.1 112.5 53.7 131.8 84.7 62.6 27 H2 2.809 99.0 109.4 128.5 120.2 167.5 45.2 107.7 10 CL2 4.140 94.2 63.1 121.8 54.7 100.1 111.9 170.1 67.4 6 CL3 4.202 62.6 104.5 65.1 84.3 44.9 107.5 50.5 145.4 138.1 N3 0.00 -0.2090 0.6719 0.1926 1.000 2.1 0 C9 1.396 0 C10 1.438 125.7 0 C1 1.351 111.2 123.1 0 H16B 2.864 91.1 72.4 108.6 0 H16C 2.749 115.8 75.4 80.4 32.0 0 H17C 2.900 107.0 73.1 92.4 145.4 136.4 0 H17B 2.922 82.7 70.9 120.9 129.0 146.2 31.8 C9 0.00 -0.2606 0.5857 0.1479 1.000 1.8 0 N3 1.396 0 C8 1.328 106.7 0 H9 0.928 119.1 133.9 C10 0.00 -0.2545 0.7734 0.1946 1.000 2.3 0 N3 1.438 0 C11 1.378 119.0 0 C15 1.391 118.6 122.4 C11 0.00 -0.2352 0.8504 0.1421 1.000 3.0 0 C10 1.378 0 C12 1.386 118.1 0 C16 1.517 121.2 120.7 0 14 1.939 95.8 24.7 140.8 C15 0.00 -0.3162 0.7905 0.2497 1.000 1.9 0 C10 1.391 0 C14 1.388 117.1 0 C17 1.492 121.3 121.5 0 20 1.910 161.8 67.2 57.9 0 18 1.921 81.8 50.7 139.3 89.5 C13 0.00 -0.3387 0.9697 0.2009 1.000 2.8 0 C12 1.384 0 C14 1.377 118.0 0 C18 1.503 121.0 120.9 0 17 0.564 76.2 79.8 113.1 0 14 0.693 33.7 108.1 120.9 105.7 0 18 1.489 79.8 62.8 128.7 117.5 51.3 C12 0.00 -0.2779 0.9483 0.1463 1.000 3.2 0 C11 1.386 0 C13 1.384 121.9 0 H12 0.791 125.4 112.7 0 14 0.894 114.9 25.5 115.0 0 17 1.364 111.4 23.7 118.1 47.5 0 18 1.844 84.7 52.6 134.6 32.1 67.2 C14 0.00 -0.3570 0.8900 0.2513 1.000 2.2 0 C15 1.388 0 C13 1.377 122.5 0 H14 0.920 119.3 117.4 0 17 1.393 111.4 23.5 119.8 0 18 1.497 83.4 62.2 135.5 77.9 0 14 1.724 103.6 22.5 137.0 35.7 42.5 0 20 1.877 69.8 158.5 57.4 176.4 105.6 147.8 C18 0.00 -0.3822 1.0771 0.2060 1.000 3.1 0 C13 1.503 0 H18B 0.889 109.2 0 H18A 0.867 113.0 89.4 0 H18C 1.019 113.9 96.2 127.5 0 17 1.801 16.7 125.9 107.9 110.1 0 14 1.952 17.7 96.6 101.4 129.3 30.7 C1 0.00 -0.1082 0.6487 0.2344 1.000 2.1 0 CU1 1.914 0 N3 1.351 124.2 0 N2 1.356 132.0 103.6 C17 0.00 -0.3355 0.7061 0.3062 1.000 1.2 0 C15 1.492 0 H17A 0.929 112.3 0 H17C 0.976 112.9 101.6 0 H17B 0.885 111.2 99.6 118.0 0 20 1.687 73.6 44.4 138.5 94.5 0 8 1.880 101.7 47.2 63.4 141.1 75.1 N2 0.00 -0.0983 0.5473 0.2144 1.000 1.8 0 C1 1.356 0 C7 1.470 124.2 0 C8 1.382 111.8 124.0 0 H5 2.935 84.3 63.2 125.5 10 CL2 3.489 87.7 82.5 102.7 130.6 C6 0.00 0.0520 0.4748 0.1727 1.000 2.2 0 C7 1.498 0 C5 1.379 121.0 0 N1 1.346 117.3 121.7 C4 0.00 0.1356 0.5476 0.0749 1.000 3.3 0 C5 1.359 0 C3 1.377 119.0 0 H4 0.770 125.8 115.1 C7 0.00 0.0000 0.4871 0.2427 1.000 1.7 0 N2 1.470 0 C6 1.498 111.3 0 H7B 0.893 107.9 110.5 0 H7A 0.981 107.0 113.6 106.3 C8 0.00 -0.1910 0.5083 0.1619 1.000 1.6 0 C9 1.328 0 N2 1.382 106.7 0 H8 0.894 133.5 119.8 C5 0.00 0.0903 0.5599 0.1394 1.000 2.8 0 C6 1.379 0 C4 1.359 120.2 0 H5 0.878 118.7 121.0 C3 0.00 0.1436 0.4488 0.0444 1.000 3.0 0 C4 1.377 0 C2 1.361 118.2 0 H3 0.966 122.5 119.2 C16 0.00 -0.1718 0.8282 0.0796 1.000 3.4 0 C11 1.517 0 H16A 0.768 104.4 0 H16B 0.996 108.7 111.9 0 H16C 0.947 112.0 113.8 106.0 N1 0.00 0.0585 0.3777 0.1435 1.000 2.0 0 C6 1.346 0 C2 1.351 116.8 0 H7A 2.528 55.8 172.5 3 CU1 2.044 127.4 115.7 71.6 1 BR1 3.476 117.3 111.1 75.5 41.7 C2 0.00 0.1045 0.3676 0.0798 1.000 2.4 0 C3 1.361 0 N1 1.351 124.0 0 H2 1.017 121.8 113.9 H16A 0.00 -0.1682 0.8812 0.0587 1.000 3.7 0 C16 0.768 9 CL2 3.129 151.3 H16B 0.00 -0.2105 0.7757 0.0378 1.000 3.3 0 N3 2.864 0 C16 0.996 79.9 4 CL5 3.305 84.2 109.4 H16C 0.00 -0.1054 0.7981 0.1062 1.000 3.3 0 CU1 3.321 0 N3 2.749 56.1 0 C16 0.947 125.9 87.2 H18B 0.00 -0.4431 1.0838 0.1662 1.000 3.1 0 C18 0.889 5 CL5 3.254 138.1 H12 0.00 -0.2696 0.9977 0.1201 1.000 3.6 0 C12 0.791 0 14 1.422 34.7 2 BR1 3.206 150.7 139.7 H8 0.00 -0.1935 0.4425 0.1434 1.000 1.4 0 C8 0.894 1 BR1 2.944 168.9 7 CL3 3.290 101.0 73.9 H17A 0.00 -0.3772 0.7284 0.3402 1.000 1.0 0 C17 0.929 0 20 1.212 103.2 0 8 1.422 104.2 111.4 11 CL6 3.256 158.7 55.7 83.3 H9 0.00 -0.3288 0.5935 0.1132 1.000 1.8 0 C9 0.928 13 CL6 3.286 109.0 H17C 0.00 -0.2713 0.6843 0.3486 1.000 1.1 0 N3 2.900 0 C17 0.976 77.7 10 CL2 3.270 87.6 143.0 H17B 0.00 -0.3770 0.6570 0.2768 1.000 1.1 0 N3 2.922 0 C17 0.885 77.0 H18A 0.00 -0.3547 1.1239 0.1803 1.000 3.5 0 C18 0.867 2 BR1 3.288 153.4 H14 0.00 -0.3882 0.9072 0.2933 1.000 1.9 0 C14 0.920 0 20 1.583 93.3 33 3 3.002 164.1 71.4 30 1 3.090 146.4 56.5 23.7 11 CL6 3.154 153.0 61.1 16.2 7.5 H2 0.00 0.1018 0.2939 0.0563 1.000 2.2 0 C2 1.017 3 CU1 2.809 84.7 H7B 0.00 0.0427 0.5206 0.2866 1.000 1.8 0 BR1 3.249 0 CU1 2.990 44.5 0 C7 0.893 156.0 115.9 H18C 0.00 -0.4121 1.0876 0.2564 1.000 2.8 0 C18 1.019 35 4 2.776 158.8 14 CL4 3.005 157.5 7.0 H3 0.00 0.1724 0.4358 -0.0028 1.000 3.3 0 C3 0.966 H4 0.00 0.1608 0.5911 0.0547 1.000 3.6 0 C4 0.770 H7A 0.00 -0.0179 0.4207 0.2648 1.000 1.3 0 C7 0.981 0 N1 2.528 73.0 3 CU1 2.702 118.9 45.9 10 CL2 3.221 105.2 177.9 135.9 7 CL3 3.241 138.3 128.1 89.5 52.5 H5 0.00 0.0826 0.6222 0.1592 1.000 3.0 0 CU1 3.457 0 N2 2.935 55.2 0 C5 0.878 140.7 90.2 6 CL3 3.006 80.8 135.6 133.0 1 1.34 -0.5639 0.6444 -0.1214 1.000 2.4 12 CL6 0.414 0 12 1.134 36.0 0 3 1.256 21.0 55.4 0 15 1.490 76.2 110.0 55.3 0 13 1.635 111.8 145.9 95.8 49.7 18 C20 1.887 59.3 54.4 75.5 114.2 104.5 21 D2 2.255 82.3 66.8 99.9 134.4 106.1 24.8 0 2 2.751 32.5 11.1 53.4 108.7 136.6 44.1 59.3 4 CL5 2.991 64.7 79.1 70.0 86.7 73.1 32.7 47.8 68.0 26 H14 3.090 95.2 125.0 74.2 22.1 48.0 135.3 150.9 126.8 105.0 16 CL4 3.163 42.0 26.8 62.6 115.2 127.7 27.6 43.2 16.9 55.0 136.3 0 4 3.464 41.8 31.2 61.7 112.6 122.6 23.5 41.5 20.6 49.9 134.2 31 2 3.482 39.6 57.1 30.0 58.8 108.3 98.6 120.0 61.8 99.8 68.3 8 CL3 3.640 156.5 121.6 161.9 120.7 91.5 118.6 93.8 127.5 128.0 99.1 2 1.12 -0.5752 0.5788 0.0355 1.000 1.3 16 CL4 0.960 0 4 1.315 11.6 0 12 1.652 113.0 118.9 18 C20 1.918 64.1 68.6 50.3 0 3 2.242 117.4 117.1 28.5 56.4 12 CL6 2.412 108.9 113.0 10.0 44.8 21.4 32 3 2.475 139.9 130.8 106.0 148.4 92.6 107.9 21 D2 2.512 58.1 66.3 55.6 19.7 70.8 54.0 161.6 0 1 2.751 106.7 111.9 7.6 43.3 26.7 5.3 111.2 50.5 13 CL6 3.174 132.5 122.3 110.0 144.3 92.1 110.0 11.0 162.7 114.1 4 CL5 3.216 59.3 58.1 67.2 26.8 59.0 58.5 133.9 43.6 59.6 125.0 31 2 3.263 153.6 144.0 66.8 105.4 49.3 66.0 43.3 119.6 70.2 44.0 29 1 3.482 127.8 117.6 114.4 145.5 95.4 114.0 14.7 164.9 118.2 4.8 3 1.11 -0.4917 0.6014 -0.0652 1.000 2.2 12 CL6 0.882 0 12 1.116 47.7 0 1 1.256 9.7 56.8 0 15 1.292 81.2 127.4 71.6 18 C20 1.987 59.3 50.2 66.8 118.8 0 2 2.242 90.2 45.0 99.9 171.0 53.5 31 2 2.475 136.6 108.5 135.4 100.7 140.4 87.4 21 D2 2.763 45.6 42.7 53.5 112.2 13.8 59.2 145.7 16 CL4 2.815 84.6 47.0 94.1 156.0 37.4 17.6 103.0 45.6 4 CL5 2.820 82.2 87.7 85.3 98.1 37.5 78.0 139.0 47.0 60.7 26 H14 3.002 91.7 133.2 82.0 16.2 135.0 170.1 84.5 127.7 172.1 111.9 0 4 3.073 88.0 53.0 97.3 152.9 36.5 22.4 104.3 46.5 6.5 55.6 17 CL4 3.268 129.3 110.0 126.5 91.7 149.3 95.8 10.9 151.2 112.2 148.2 32 3 3.414 121.9 76.4 128.9 141.5 99.7 46.4 41.0 105.2 62.4 114.2 34 4 3.480 123.4 107.5 120.3 89.0 151.1 98.1 16.6 149.9 115.0 154.3 4 0.88 -0.5747 0.6577 0.0868 1.000 1.4 16 CL4 0.422 0 2 1.315 27.2 18 C20 1.890 61.6 70.9 0 7 1.910 96.8 98.2 36.4 0 16 2.008 143.5 138.4 82.1 46.7 21 D2 2.319 63.5 82.5 23.6 48.1 85.1 4 CL5 2.757 98.1 98.0 38.4 3.2 45.5 51.2 0 3 3.073 49.2 40.5 38.7 57.9 99.8 59.7 57.5 12 CL6 3.167 42.4 44.5 27.0 56.1 102.1 44.9 56.7 16.2 0 1 3.464 42.2 47.5 23.5 55.1 101.6 40.1 56.1 21.1 5.0 32 3 3.480 56.8 32.6 99.6 115.7 132.7 114.7 113.9 62.4 72.8 76.8 7 0.61 -0.5073 0.7579 0.0332 1.000 2.3 0 10 0.700 4 CL5 0.858 77.3 18 C20 1.187 167.1 115.2 0 11 1.206 93.4 20.1 98.2 0 16 1.554 31.1 105.9 138.0 123.8 0 4 1.910 96.3 169.5 70.9 157.4 70.0 16 CL4 2.004 107.9 167.6 59.2 148.4 82.1 12.1 8 0.59 -0.3044 0.7743 0.4116 1.000 1.1 0 C17 1.880 0 H17A 1.422 28.6 10 0.54 -0.4740 0.7785 0.0706 1.000 2.3 0 7 0.700 4 CL5 0.981 58.5 0 16 1.020 128.2 159.6 0 11 1.430 57.3 10.3 169.2 18 C20 1.876 8.1 66.5 121.6 64.7 0 18 1.966 162.7 110.0 57.8 114.0 168.0 11 0.53 -0.4534 0.7897 -0.0101 1.000 2.8 4 CL5 0.497 0 7 1.206 36.3 0 10 1.430 20.7 29.3 18 C20 1.809 73.6 40.5 69.6 12 0.53 -0.5758 0.6032 -0.0635 1.000 1.9 12 CL6 0.836 0 3 1.116 51.3 0 1 1.134 16.9 67.8 18 C20 1.535 87.3 95.8 88.6 0 2 1.652 149.9 106.5 161.2 73.9 16 CL4 2.211 135.7 111.3 139.8 51.2 23.6 13 0.52 -0.4860 0.7186 -0.1584 1.000 3.2 0 15 1.320 0 1 1.635 59.4 12 CL6 1.830 51.7 12.1 14 0.52 -0.3375 0.9486 0.1623 1.000 2.9 0 C11 1.939 0 C13 0.693 127.0 0 C12 0.894 40.4 120.9 0 C14 1.724 97.8 49.4 126.5 0 C18 1.952 154.9 41.3 119.3 85.8 0 H12 1.422 69.1 116.6 30.3 150.2 95.7 0 17 1.005 95.7 32.7 91.6 53.9 66.3 99.5 0 18 1.186 86.0 101.5 124.3 58.5 116.4 141.7 112.0 15 0.52 -0.4550 0.6250 -0.1282 1.000 2.7 0 3 1.292 0 13 1.320 111.7 12 CL6 1.448 37.0 82.6 0 1 1.490 53.1 70.9 16.1 16 0.51 -0.4879 0.7854 0.1285 1.000 2.0 0 10 1.020 0 7 1.554 20.7 0 18 1.664 90.9 110.3 4 CL5 1.970 10.0 24.8 85.6 0 4 2.008 81.0 63.3 166.8 87.8 17 0.50 -0.2977 0.9642 0.2227 1.000 2.8 0 C13 0.564 0 C12 1.364 80.1 0 C14 1.393 76.7 118.3 0 C18 1.801 50.1 104.3 102.7 0 14 1.005 41.6 40.9 90.4 83.0 0 18 1.819 46.5 69.1 53.6 96.3 37.2 18 0.50 -0.3941 0.8756 0.1573 1.000 2.5 0 C15 1.921 0 C13 1.489 89.7 0 C12 1.844 94.9 47.6 0 C14 1.497 45.9 54.9 89.6 0 14 1.186 101.7 27.2 23.6 79.0 0 16 1.664 91.3 158.2 153.7 112.7 166.7 0 17 1.819 75.8 16.0 43.7 48.5 30.8 161.1 0 10 1.966 106.0 163.1 123.0 141.5 138.8 31.3 166.3 20 0.50 -0.4337 0.7935 0.2967 1.000 1.3 0 C15 1.910 0 C14 1.877 43.0 0 C17 1.687 48.5 89.5 0 H17A 1.212 77.8 112.2 32.4 0 H14 1.583 69.4 29.3 109.1 118.6 Code Atom x y z Height Symmetry Transformation 1 BR1 -0.1641 0.2207 0.1096 0.8 0.0000-X -0.5000+Y 0.5000-Z 2 BR1 -0.1641 1.2207 0.1096 4.8 0.0000-X 0.5000+Y 0.5000-Z 3 CU1 0.0148 0.2416 0.1891 1.1 0.0000-X -0.5000+Y 0.5000-Z 4 CL5 -0.4666 0.7981 0.0147 2.7 0.0000-X 0.5000+Y 0.5000-Z 5 CL5 -0.5334 1.2019 -0.0147 4.2 -1.0000+X 1.5000-Y -0.5000+Z 6 CL3 0.2185 0.8143 0.1895 4.0 0.0000+X 0.0000+Y 0.0000+Z 7 CL3 -0.2185 0.3143 0.3105 0.0 0.0000-X -0.5000+Y 0.5000-Z 8 CL3 -0.7815 0.6857 -0.3105 2.9 -1.0000+X 1.5000-Y -0.5000+Z 9 CL2 -0.1189 1.0168 -0.0841 5.1 0.0000-X 2.0000-Y 0.0000-Z 10 CL2 -0.1189 0.4832 0.4159 0.5 0.0000-X -0.5000+Y 0.5000-Z 11 CL6 -0.5484 0.8684 0.4019 0.7 0.0000-X 1.0000-Y 1.0000-Z 12 CL6 -0.5484 0.6316 -0.0981 2.3 0.0000-X 0.5000+Y 0.5000-Z 13 CL6 -0.4516 0.3684 0.0981 0.6 -1.0000+X 0.5000-Y -0.5000+Z 14 CL4 -0.4117 1.1397 0.4350 2.1 -1.0000+X 1.0000+Y 0.0000+Z 15 CL4 0.4117 0.8603 0.5650 2.9 1.0000-X 1.0000-Y 1.0000-Z 16 CL4 -0.5883 0.6397 0.0650 1.4 0.0000-X 0.5000+Y 0.5000-Z 17 CL4 -0.4117 0.3603 -0.0650 1.5 -1.0000+X 0.5000-Y -0.5000+Z 18 C20 -0.5691 0.7096 -0.0196 2.2 0.0000-X 0.5000+Y 0.5000-Z 19 N1 -0.0585 0.8777 0.3565 2.5 0.0000-X 0.5000+Y 0.5000-Z 20 D2 0.3666 0.7518 0.4603 2.8 1.0000-X 1.0000-Y 1.0000-Z 21 D2 -0.6334 0.7482 -0.0397 2.2 0.0000-X 0.5000+Y 0.5000-Z 22 D1 0.1989 0.6604 0.5580 1.4 0.0000+X 1.5000-Y 0.5000+Z 23 H12 0.2696 0.4977 0.3799 1.9 0.0000-X -0.5000+Y 0.5000-Z 24 H8 0.1935 0.9425 0.3566 3.6 0.0000-X 0.5000+Y 0.5000-Z 25 H18A 0.3547 0.6239 0.3196 3.0 0.0000-X -0.5000+Y 0.5000-Z 26 H14 -0.3882 0.5928 -0.2067 3.2 0.0000+X 1.5000-Y -0.5000+Z 27 H2 -0.1018 0.7939 0.4437 1.6 0.0000-X 0.5000+Y 0.5000-Z 28 H7A 0.0179 0.9207 0.2352 3.6 0.0000-X 0.5000+Y 0.5000-Z 29 1 -0.4361 0.3556 0.1214 0.4 -1.0000-X 1.0000-Y 0.0000-Z 30 1 -0.5639 0.8556 0.3786 0.7 0.0000+X 1.5000-Y 0.5000+Z 31 2 -0.4248 0.4212 -0.0355 1.5 -1.0000-X 1.0000-Y 0.0000-Z 32 3 -0.5083 0.3986 0.0652 0.7 -1.0000-X 1.0000-Y 0.0000-Z 33 3 -0.4917 0.8986 0.4348 0.9 0.0000+X 1.5000-Y 0.5000+Z 34 4 -0.4253 0.3423 -0.0868 1.5 -1.0000-X 1.0000-Y 0.0000-Z 35 4 -0.4253 1.1577 0.4132 2.2 -1.0000-X 0.5000+Y 0.5000-Z Molecule 2 scale 0.883 inches = 2.242 cm per Angstrom CL1 BR1 16 10 CL5 7 11 4 C20 CL4 2 13 1 12 CL6 3 15 3 CL6 2 CL4 Atom Peak x y z Sof Height Distances and Angles CL5 0.00 0.4666 0.2981 0.4853 1.000 2.5 0 C20 1.735 19 11 0.497 90.5 17 7 0.858 38.2 123.6 18 10 0.981 82.3 149.1 44.1 23 16 1.970 87.3 158.9 49.4 10.4 21 13 2.963 67.0 25.3 103.6 143.4 152.1 6 H18B 3.254 87.2 58.3 119.7 150.1 142.4 51.1 22 15 3.263 60.5 33.6 90.2 122.2 132.2 23.9 74.8 5 H16B 3.305 131.3 59.9 128.8 103.4 107.0 84.0 104.5 77.0 2 CL1 3.770 83.7 148.2 66.3 61.0 52.3 130.3 90.1 141.3 141.8 CL6 0.00 0.5484 0.1316 0.5981 1.000 4.2 0 C20 1.713 11 1 0.414 108.7 20 12 0.836 63.5 127.1 14 3 0.882 94.5 149.3 81.0 22 15 1.448 128.1 87.7 140.6 61.8 21 13 1.830 103.8 56.0 167.3 99.7 45.7 9 H14 3.154 142.0 77.3 142.9 72.1 15.3 47.2 13 2 3.174 115.3 135.7 71.9 32.4 69.7 115.3 71.7 7 H17A 3.256 100.3 72.8 156.6 83.7 36.8 16.7 44.1 103.4 8 H9 3.286 113.1 99.8 51.2 88.7 111.7 141.3 102.2 58.4 146.1 4 CL4 3.888 125.6 125.2 77.6 40.5 65.9 111.2 65.3 10.5 101.7 54.8 CL4 0.00 0.5883 0.1397 0.4350 1.000 4.0 0 C20 1.729 16 4 0.422 106.1 12 2 0.960 86.0 141.2 17 7 2.004 36.1 71.1 107.5 20 12 2.211 43.8 143.1 43.5 74.1 23 16 2.360 75.8 30.4 135.3 40.7 114.1 10 H18C 3.005 159.6 53.6 111.1 124.3 154.5 84.0 15 3 3.268 111.9 117.0 29.2 121.4 72.0 127.4 82.8 3 CL6 3.888 114.3 107.3 37.0 117.0 77.9 117.7 77.8 10.1 1 BR1 4.114 58.6 115.1 102.7 82.3 71.4 101.8 124.4 127.3 137.3 C20 0.00 0.5691 0.2096 0.5196 1.000 3.9 0 CL5 1.735 0 CL6 1.713 110.8 0 CL4 1.729 110.6 113.0 0 D2 0.958 108.1 110.5 103.6 17 7 1.187 26.6 129.4 84.7 110.3 20 12 1.535 132.3 29.2 85.1 111.5 138.2 19 11 1.809 15.9 95.2 122.1 112.4 41.3 118.9 18 10 1.876 31.2 131.2 79.9 111.4 4.8 136.8 45.6 11 1 1.887 111.2 12.0 122.0 99.6 133.9 36.9 95.3 136.7 16 4 1.890 99.0 123.0 12.4 104.2 72.7 96.3 111.5 68.0 133.0 12 2 1.918 123.3 83.1 29.9 117.8 102.8 55.9 126.9 98.4 92.6 40.4 14 3 1.987 98.3 26.3 98.3 136.7 108.6 34.0 85.4 109.0 37.7 104.9 D2 0.00 0.6334 0.2482 0.5397 1.000 4.4 0 C20 0.958 1 BR1 2.630 157.5 23 16 2.935 58.1 135.1 Code Atom x y z Height Symmetry Transformation 1 BR1 0.8359 0.2793 0.6096 6.5 1.0000-X 1.0000-Y 1.0000-Z 2 CL1 0.6629 0.4424 0.3979 3.6 1.0000-X -0.5000+Y 0.5000-Z 3 CL6 0.4516 -0.1316 0.4019 3.4 1.0000-X 0.0000-Y 1.0000-Z 4 CL4 0.4117 -0.1397 0.5650 3.6 1.0000-X 0.0000-Y 1.0000-Z 5 H16B 0.2105 0.2757 0.4622 0.0 0.0000-X -0.5000+Y 0.5000-Z 6 H18B 0.5569 0.4162 0.6662 3.6 1.0000+X 1.5000-Y 0.5000+Z 7 H17A 0.3772 0.2716 0.6598 2.3 0.0000-X 1.0000-Y 1.0000-Z 8 H9 0.6712 -0.0935 0.6132 6.1 1.0000+X 0.5000-Y 0.5000+Z 9 H14 0.3882 0.0928 0.7067 3.1 0.0000-X 1.0000-Y 1.0000-Z 10 H18C 0.5879 0.0876 0.2564 3.5 1.0000+X -1.0000+Y 0.0000+Z 11 1 0.5639 0.1444 0.6214 4.4 0.0000-X -0.5000+Y 0.5000-Z 12 2 0.5752 0.0788 0.4645 4.1 0.0000-X -0.5000+Y 0.5000-Z 13 2 0.4248 -0.0788 0.5355 3.4 1.0000+X 0.5000-Y 0.5000+Z 14 3 0.4917 0.1014 0.5652 3.6 0.0000-X -0.5000+Y 0.5000-Z 15 3 0.5083 -0.1014 0.4348 4.0 1.0000+X 0.5000-Y 0.5000+Z 16 4 0.5747 0.1577 0.4132 3.7 0.0000-X -0.5000+Y 0.5000-Z 17 7 0.5073 0.2579 0.4668 2.9 0.0000-X -0.5000+Y 0.5000-Z 18 10 0.4740 0.2785 0.4294 2.4 0.0000-X -0.5000+Y 0.5000-Z 19 11 0.4534 0.2897 0.5101 2.5 0.0000-X -0.5000+Y 0.5000-Z 20 12 0.5758 0.1032 0.5635 4.4 0.0000-X -0.5000+Y 0.5000-Z 21 13 0.4860 0.2186 0.6584 3.5 0.0000-X -0.5000+Y 0.5000-Z 22 15 0.4550 0.1250 0.6282 3.4 0.0000-X -0.5000+Y 0.5000-Z 23 16 0.4879 0.2854 0.3715 2.3 0.0000-X -0.5000+Y 0.5000-Z Molecule 3 scale 0.819 inches = 2.079 cm per Angstrom CU1 N2 CU1 CL2 BR1 CL2 CL3 9 C19 1 6 CL1 5 19 BR1 CL5 Atom Peak x y z Sof Height Distances and Angles CL3 0.31 0.2185 0.8143 0.1895 1.000 2.5 0 C19 1.762 0 6 1.077 76.3 12 H5 3.006 114.9 145.8 11 H7A 3.241 98.7 127.8 84.1 9 H8 3.290 117.8 88.5 110.9 47.3 13 1 3.640 118.4 44.8 123.7 104.1 56.8 1 BR1 3.758 162.7 110.8 68.6 64.4 48.8 66.1 3 CU1 4.203 132.7 141.7 54.3 40.0 57.5 97.8 34.2 CL1 0.59 0.3371 0.9424 0.1021 1.000 4.7 0 C19 1.732 0 5 0.996 95.3 0 19 2.019 124.5 30.1 0 6 2.239 53.1 42.3 71.5 5 CL5 3.770 120.2 92.6 72.1 109.0 CL2 0.17 0.1189 0.9832 0.0841 1.000 3.8 0 C19 1.750 8 H16A 3.129 101.2 11 H7A 3.221 99.7 158.5 10 H17C 3.270 98.8 65.1 106.4 7 N2 3.489 106.8 131.7 34.2 72.2 6 CL2 3.588 129.6 71.0 99.4 119.4 115.0 4 CU1 4.140 145.8 91.6 68.0 58.1 45.2 84.5 C19 0.00 0.2161 0.8868 0.0979 1.000 3.5 0 CL3 1.762 0 CL1 1.732 112.6 0 CL2 1.750 108.9 110.4 0 D1 0.874 102.4 111.2 111.2 0 6 1.834 34.8 77.8 123.3 117.3 D1 0.00 0.1989 0.8396 0.0580 1.000 3.2 0 C19 0.874 2 BR1 2.771 151.0 5 0.67 0.3720 0.9197 0.1612 1.000 4.5 0 CL1 0.996 0 19 1.261 126.5 0 6 1.646 113.6 117.5 6 0.66 0.2975 0.8445 0.2021 1.000 3.2 0 CL3 1.077 0 CL1 2.239 118.0 0 C19 1.834 68.9 49.1 0 5 1.646 141.9 24.0 73.0 9 0.57 0.4642 1.0171 0.2883 1.000 5.3 0 19 1.947 19 0.50 0.4696 0.9213 0.1976 1.000 4.9 0 CL1 2.019 0 5 1.261 23.4 0 9 1.947 107.7 97.2 Code Atom x y z Height Symmetry Transformation 1 BR1 0.1641 0.7207 0.3904 0.6 0.0000+X 0.0000+Y 0.0000+Z 2 BR1 0.1641 0.7793 -0.1096 3.1 0.0000+X 1.5000-Y -0.5000+Z 3 CU1 -0.0148 0.7416 0.3109 0.0 0.0000+X 0.0000+Y 0.0000+Z 4 CU1 0.0148 1.2416 0.1891 5.0 0.0000-X 0.5000+Y 0.5000-Z 5 CL5 0.5334 0.7981 0.0147 5.0 1.0000-X 0.5000+Y 0.5000-Z 6 CL2 -0.1189 1.0168 -0.0841 3.4 0.0000-X 2.0000-Y 0.0000-Z 7 N2 0.0983 1.0473 0.2856 3.4 0.0000-X 0.5000+Y 0.5000-Z 8 H16A 0.1682 1.1189 -0.0587 5.9 0.0000-X 2.0000-Y 0.0000-Z 9 H8 0.1935 0.9425 0.3566 2.8 0.0000-X 0.5000+Y 0.5000-Z 10 H17C 0.2713 1.1843 0.1514 6.2 0.0000-X 0.5000+Y 0.5000-Z 11 H7A 0.0179 0.9207 0.2352 2.0 0.0000-X 0.5000+Y 0.5000-Z 12 H5 0.0826 0.6222 0.1592 0.2 0.0000+X 0.0000+Y 0.0000+Z 13 1 0.4361 0.8556 0.3786 3.4 1.0000+X 1.5000-Y 0.5000+Z Time profile in seconds ----------------------- 0.32: Read and process instructions 0.00: Fit rigid groups 0.05: Interpret restraints etc. 0.06: Generate connectivity array 0.06: 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 3.32: Analyse other restraints etc. 26.93: Read intensity data, sort/merge etc. 0.03: Set up constraints 0.00: OSF, H-atoms from difference map 0.20: Set up l.s. refinement 0.02: Generate idealized H-atoms 41.57: Structure factors and derivatives 136.09: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.48: Apply other restraints 9.96: Solve l.s. equations 0.00: Generate HTAB table 0.55: Other dependent quantities, CIF, tables 4.23: Analysis of variance 0.43: Merge reflections for Fourier and .fcf 2.95: Fourier summations 1.29: Peaksearch 0.77: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 00skl038 finished at 12:16:51 Total CPU time: 229.4 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++