+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 02src191 started at 14:14:51 on 29-Jul-2004 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL DIRDIF output for 02SRC191 in P-1 CELL 0.71073 11.6573 12.1713 12.4865 86.561 85.943 77.228 ZERR 2.00 0.0013 0.0012 0.0015 0.004 0.005 0.009 LATT 1 SFAC C H N O SB I CU CL UNIT 66.66 51.32 2 4 2 4 2 1.32 V = 1721.69 F(000) = 891.7 Mu = 3.27 mm-1 Cell Wt = 1869.31 Rho = 1.803 MERG 2 OMIT -3.00 55.00 OMIT -1 1 0 OMIT 0 1 0 OMIT -3 0 1 OMIT 5 3 0 OMIT 0 2 1 OMIT -1 2 2 OMIT 6 2 0 OMIT 1 0 0 OMIT -1 2 0 OMIT 1 2 1 OMIT 1 2 4 EXTI 0.00000 FMAP 2 PLAN 10 SIZE 0.06 0.12 0.18 BOND $H WGHT 0.05730 7.13200 L.S. 4 TEMP -153.00 FVAR 0.15653 MOLE 1 C1 1 0.462425 0.176897 0.516347 11.00000 0.02843 0.03682 = 0.04364 0.00397 -0.00086 -0.01744 C2 1 0.438062 0.199056 0.401319 11.00000 0.04179 0.04237 = 0.04396 -0.00408 -0.00559 -0.01529 C3 1 0.529456 0.154715 0.321554 11.00000 0.04047 0.06359 = 0.03951 -0.02034 -0.00190 -0.01716 C4 1 0.509907 0.186581 0.213774 11.00000 0.04225 0.14145 = 0.05884 -0.02966 -0.00402 -0.00816 AFIX 43 H4 2 0.439368 0.236527 0.193108 11.00000 -1.20000 AFIX 0 C5 1 0.600538 0.140691 0.136821 11.00000 0.03415 0.21348 = 0.05090 -0.02972 -0.01169 -0.00830 AFIX 43 H5 2 0.589441 0.158342 0.062603 11.00000 -1.20000 AFIX 0 C6 1 0.703353 0.071738 0.166945 11.00000 0.04171 0.17200 = 0.06863 -0.06169 0.00659 -0.01463 AFIX 43 H6 2 0.764317 0.045874 0.113891 11.00000 -1.20000 AFIX 0 C7 1 0.719794 0.039181 0.273406 11.00000 0.03540 0.08288 = 0.05375 -0.02592 -0.00590 -0.01356 AFIX 43 H7 2 0.789900 -0.012160 0.293017 11.00000 -1.20000 AFIX 0 C8 1 0.633348 0.081747 0.352199 11.00000 0.03084 0.04729 = 0.06119 -0.01834 0.00272 -0.01075 C9 1 0.653908 0.050787 0.465345 11.00000 0.03437 0.03739 = 0.05760 0.00106 -0.00528 -0.01301 C10 1 0.567352 0.103451 0.546937 11.00000 0.03272 0.04042 = 0.04590 -0.01057 0.00726 -0.00722 C11 1 0.587272 0.084648 0.657820 11.00000 0.03675 0.03440 = 0.04948 0.01072 -0.00303 -0.00377 C12 1 0.502091 0.141473 0.736680 11.00000 0.04433 0.05466 = 0.04783 0.01682 -0.00839 -0.01366 C13 1 0.522235 0.122591 0.854828 11.00000 0.04897 0.07089 = 0.04444 0.01371 0.00149 0.00630 AFIX 137 H13A 2 0.456935 0.169602 0.896154 11.00000 -1.50000 H13B 2 0.596312 0.142883 0.869191 11.00000 -1.50000 H13C 2 0.526563 0.043002 0.876007 11.00000 -1.50000 AFIX 0 C14 1 0.399817 0.212244 0.701943 11.00000 0.03450 0.04459 = 0.04556 0.00574 0.00252 -0.01586 AFIX 43 H14 2 0.342728 0.248742 0.753811 11.00000 -1.20000 AFIX 0 C15 1 0.377925 0.231744 0.591374 11.00000 0.03473 0.03218 = 0.03261 -0.00534 -0.00496 -0.01501 C16 1 0.253788 0.477823 0.442518 11.00000 0.03354 0.03517 = 0.04055 0.00201 0.00175 -0.00998 C17 1 0.335578 0.535675 0.472384 11.00000 0.05802 0.04151 = 0.06531 0.00828 -0.02374 -0.02436 AFIX 43 H17 2 0.373868 0.514412 0.537509 11.00000 -1.20000 AFIX 0 C18 1 0.360946 0.622097 0.409209 11.00000 0.03760 0.04677 = 0.12300 0.01311 -0.00419 -0.02671 AFIX 43 H18 2 0.415307 0.662937 0.430990 11.00000 -1.20000 AFIX 0 C19 1 0.307649 0.651538 0.312209 11.00000 0.04969 0.04998 = 0.06976 0.01450 -0.01678 -0.01376 AFIX 43 H19 2 0.327228 0.711153 0.267047 11.00000 -1.20000 AFIX 0 C20 1 0.227293 0.594896 0.281863 11.00000 0.04807 0.04451 = 0.05417 0.01499 -0.00704 -0.00629 AFIX 43 H20 2 0.190053 0.615661 0.216155 11.00000 -1.20000 AFIX 0 C21 1 0.200243 0.506826 0.347444 11.00000 0.04579 0.03549 = 0.04449 -0.00139 -0.00976 -0.00865 AFIX 43 H21 2 0.144793 0.466752 0.326527 11.00000 -1.20000 AFIX 0 C22 1 0.096487 0.256680 0.484578 11.00000 0.02384 0.03091 = 0.04004 -0.00242 -0.00444 0.00317 C23 1 0.105767 0.219922 0.378673 11.00000 0.03248 0.04052 = 0.03741 0.00269 -0.00410 -0.00225 AFIX 43 H23 2 0.162607 0.239325 0.326932 11.00000 -1.20000 AFIX 0 C24 1 0.029975 0.155205 0.352848 11.00000 0.03679 0.03743 = 0.04725 0.00167 0.00042 -0.00347 AFIX 43 H24 2 0.035713 0.128105 0.282457 11.00000 -1.20000 AFIX 0 C25 1 -0.054329 0.128694 0.426928 11.00000 0.03562 0.04727 = 0.04777 -0.01016 -0.00516 -0.00731 AFIX 43 H25 2 -0.103721 0.081187 0.408269 11.00000 -1.20000 AFIX 0 C26 1 -0.066669 0.170028 0.525529 11.00000 0.04308 0.06981 = 0.05232 -0.00208 0.00318 -0.02791 AFIX 43 H26 2 -0.128858 0.156121 0.574154 11.00000 -1.20000 AFIX 0 C27 1 0.010837 0.233423 0.557852 11.00000 0.04557 0.04857 = 0.03026 -0.00362 0.00204 -0.01166 AFIX 43 H27 2 0.004083 0.259528 0.628698 11.00000 -1.20000 AFIX 0 C28 1 0.144307 0.412255 0.681258 11.00000 0.03615 0.03995 = 0.02802 0.00680 -0.00741 -0.01293 C29 1 0.113786 0.529055 0.687004 11.00000 0.05621 0.02925 = 0.03585 -0.00111 -0.01311 0.00126 AFIX 43 H29 2 0.134948 0.575444 0.628347 11.00000 -1.20000 AFIX 0 C30 1 0.053770 0.577518 0.776085 11.00000 0.07569 0.03640 = 0.05105 0.00542 -0.02126 -0.00556 AFIX 43 H30 2 0.036820 0.657293 0.779456 11.00000 -1.20000 AFIX 0 C31 1 0.017368 0.514394 0.860621 11.00000 0.07268 0.04503 = 0.02899 -0.00360 -0.00056 0.00529 AFIX 43 H31 2 -0.026462 0.549998 0.920918 11.00000 -1.20000 AFIX 0 C32 1 0.044796 0.399266 0.857401 11.00000 0.06201 0.05427 = 0.03671 -0.00204 -0.00183 -0.00958 AFIX 43 H32 2 0.020050 0.354879 0.916024 11.00000 -1.20000 AFIX 0 C33 1 0.108490 0.346657 0.769221 11.00000 0.04759 0.05014 = 0.04537 -0.00313 -0.00690 -0.00606 AFIX 43 H33 2 0.127907 0.266690 0.768115 11.00000 -1.20000 AFIX 0 N1 3 0.684560 0.015351 0.692154 11.00000 0.04189 0.05825 = 0.06166 0.01957 -0.00027 -0.00077 AFIX 93 H1A 2 0.738179 -0.019927 0.645488 11.00000 -1.20000 H1B 2 0.695041 0.004972 0.761441 11.00000 -1.20000 AFIX 0 O1 4 0.341511 0.257405 0.376890 11.00000 0.03494 0.04868 = 0.04228 -0.00563 -0.00460 -0.00444 O2 4 0.743713 -0.015840 0.487975 11.00000 0.05030 0.04888 = 0.06627 0.00233 0.00636 -0.00660 SB1 5 0.222943 0.338447 0.539289 11.00000 0.03293 0.03685 = 0.03649 0.00125 -0.00380 -0.00737 MOLE 2 I1 6 0.066223 -0.113398 0.136419 11.00000 0.06119 0.05226 = 0.05090 0.01713 -0.01947 -0.02148 I2 6 0.217541 0.178630 0.063734 11.00000 0.04380 0.04988 = 0.04456 0.00577 -0.00750 -0.01290 CU1 7 0.069536 0.068971 0.020656 11.00000 0.04046 0.04848 = 0.04069 0.00358 -0.00286 -0.01024 MOLE 3 C34 1 0.670024 0.522586 1.054789 10.33000 0.06345 0.02142 = 0.17332 0.03434 0.03544 -0.02025 AFIX 23 H34A 2 0.730646 0.562765 1.073125 10.33000 -1.20000 H34B 2 0.632998 0.561530 0.989916 10.33000 -1.20000 AFIX 0 CL1 8 0.740463 0.382579 1.023544 10.33000 0.08516 0.09841 = 0.08036 -0.01066 -0.00403 -0.02533 CL2 8 0.570406 0.531943 1.152977 10.33000 0.10471 0.16731 = 0.21956 -0.12530 0.04030 -0.05734 HKLF 4 Covalent radii and connectivity table for DIRDIF output for 02SRC191 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 SB 1.410 I 1.330 CU 1.280 CL 0.990 C1 - C15 C10 C2 C2 - O1 C3 C1 C3 - C8 C4 C2 C4 - C3 C5 C5 - C6 C4 C6 - C5 C7 C7 - C6 C8 C8 - C7 C3 C9 C9 - O2 C10 C8 C10 - C1 C11 C9 C11 - N1 C10 C12 C12 - C14 C11 C13 C13 - C12 C14 - C12 C15 C15 - C1 C14 Sb1 C16 - C21 C17 Sb1 C17 - C18 C16 C18 - C17 C19 C19 - C20 C18 C20 - C19 C21 C21 - C16 C20 C22 - C27 C23 Sb1 C23 - C24 C22 C24 - C23 C25 C25 - C26 C24 C26 - C25 C27 C27 - C22 C26 C28 - C29 C33 Sb1 C29 - C30 C28 C30 - C29 C31 C31 - C30 C32 C32 - C31 C33 C33 - C32 C28 N1 - C11 O1 - C2 Sb1 O2 - C9 Sb1 - C28 C15 C16 C22 O1 I1 - Cu1_$1 Cu1 I2 - Cu1 Cu1 - I2 I1_$1 I1 Cu1_$1 C34 - Cl2 Cl1 Cl1 - C34 Cl2 - C34 Operators for generating equivalent atoms: $1 -x, -y, -z 18254 Reflections read, of which 43 rejected -14 =< h =< 13, -15 =< k =< 15, -16 =< l =< 16, Max. 2-theta = 54.99 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 1 1 0 81.51 1.16 3 98.41 5 -2 1 70.52 1.93 3 21.77 3 -1 1 452.17 11.13 3 118.59 5 0 1 123.58 3.27 3 22.45 0 1 1 277.09 14.08 2 294.92 9 2 2 50.88 1.10 2 53.46 12 4 3 21.82 2.34 2 13.23 4 -1 4 125.87 2.26 6 15.44 7 1 6 107.26 3.09 2 66.15 8 1 8 33.35 1.92 2 16.75 10 Inconsistent equivalents 6303 Unique reflections, of which 0 suppressed R(int) = 0.0697 R(sigma) = 0.0897 Friedel opposites merged Maximum memory for data reduction = 3567 / 64854 Default effective X-H distances for T = -153.0 C AFIX m = 1 2 3 4 4[N] 3[N] 15[B] 8[O] 9 9[N] 16 d(X-H) = 1.00 0.99 0.98 0.95 0.88 0.91 1.12 0.84 0.95 0.88 0.95 Note that these distances are chosen to give the best fit to the X-ray data and so avoid the introduction of systematic error. The true internuclear distances are longer and do not vary with temperature ! The apparent variation with temperature is caused by libration. Least-squares cycle 1 Maximum vector length = 511 Memory required = 4602 / 502688 wR2 = 0.1455 before cycle 1 for 6303 data and 390 / 390 parameters GooF = S = 1.039; Restrained GooF = 1.039 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0573 * P )^2 + 7.13 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.15688 0.00037 0.936 OSF 2 0.00000 0.00028 -4.637 EXTI Mean shift/esd = 0.047 Maximum = -4.637 for EXTI Max. shift = 0.004 A for C34 Max. dU =-0.001 for C34 Least-squares cycle 2 Maximum vector length = 511 Memory required = 4602 / 502688 wR2 = 0.1455 before cycle 2 for 6303 data and 390 / 390 parameters GooF = S = 1.040; Restrained GooF = 1.040 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0573 * P )^2 + 7.13 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.15682 0.00037 -0.149 OSF 2 0.00000 0.00028 -6.176 EXTI Mean shift/esd = 0.027 Maximum = -6.176 for EXTI Max. shift = 0.002 A for C34 Max. dU = 0.000 for C34 Least-squares cycle 3 Maximum vector length = 511 Memory required = 4602 / 502688 wR2 = 0.1455 before cycle 3 for 6303 data and 390 / 390 parameters GooF = S = 1.039; Restrained GooF = 1.039 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0573 * P )^2 + 7.13 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.15681 0.00037 -0.044 OSF 2 0.00000 0.00028 -6.176 EXTI Mean shift/esd = 0.017 Maximum = -6.176 for EXTI Max. shift = 0.001 A for C34 Max. dU = 0.000 for C34 Least-squares cycle 4 Maximum vector length = 511 Memory required = 4602 / 502688 wR2 = 0.1455 before cycle 4 for 6303 data and 390 / 390 parameters GooF = S = 1.039; Restrained GooF = 1.039 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0573 * P )^2 + 7.13 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.15680 0.00037 -0.026 OSF 2 0.00000 0.00028 -6.177 EXTI Mean shift/esd = 0.016 Maximum = -6.177 for EXTI Max. shift = 0.001 A for C34 Max. dU = 0.000 for C34 Largest correlation matrix elements -0.597 U23 Cl2 / U22 Cl2 0.576 EXTI / OSF -0.517 z Cl2 / y Cl2 -0.588 U23 Cl2 / U33 Cl2 -0.548 U12 Cl2 / U13 Cl2 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H4 0.4393 0.2362 0.1932 43 0.950 0.000 C4 C3 C5 H5 0.5896 0.1586 0.0626 43 0.950 0.000 C5 C6 C4 H6 0.7641 0.0458 0.1138 43 0.950 0.000 C6 C5 C7 H7 0.7899 -0.0122 0.2930 43 0.950 0.000 C7 C6 C8 H13A 0.4569 0.1697 0.8961 137 0.980 0.000 C13 C12 H13A H13B 0.5963 0.1430 0.8691 137 0.980 0.000 C13 C12 H13A H13C 0.5267 0.0431 0.8760 137 0.980 0.000 C13 C12 H13A H14 0.3428 0.2489 0.7538 43 0.950 0.000 C14 C12 C15 H17 0.3737 0.5144 0.5376 43 0.950 0.000 C17 C18 C16 H18 0.4153 0.6630 0.4309 43 0.950 0.000 C18 C17 C19 H19 0.3272 0.7111 0.2669 43 0.950 0.000 C19 C20 C18 H20 0.1900 0.6157 0.2163 43 0.950 0.000 C20 C19 C21 H21 0.1449 0.4667 0.3264 43 0.950 0.000 C21 C16 C20 H23 0.1625 0.2394 0.3270 43 0.950 0.000 C23 C24 C22 H24 0.0357 0.1281 0.2825 43 0.950 0.000 C24 C23 C25 H25 -0.1037 0.0812 0.4082 43 0.950 0.000 C25 C26 C24 H26 -0.1289 0.1561 0.5742 43 0.950 0.000 C26 C25 C27 H27 0.0041 0.2596 0.6287 43 0.950 0.000 C27 C22 C26 H29 0.1350 0.5754 0.6283 43 0.950 0.000 C29 C30 C28 H30 0.0370 0.6574 0.7795 43 0.950 0.000 C30 C29 C31 H31 -0.0265 0.5500 0.9209 43 0.950 0.000 C31 C30 C32 H32 0.0201 0.3548 0.9160 43 0.950 0.000 C32 C31 C33 H33 0.1280 0.2667 0.7681 43 0.950 0.000 C33 C32 C28 H1A 0.7381 -0.0200 0.6454 93 0.880 0.000 N1 C11 C10 H1B 0.6951 0.0050 0.7614 93 0.880 0.000 N1 C11 C10 H34A 0.7305 0.5627 1.0740 23 0.990 0.001 C34 Cl2 Cl1 H34B 0.6330 0.5619 0.9906 23 0.990 0.001 C34 Cl2 Cl1 DIRDIF output for 02SRC191 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.46246 0.17686 0.51636 1.00000 0.02858 0.03674 0.04374 0.00387 -0.00086 -0.01732 0.03507 0.01302 0.00070 0.00073 0.00069 0.00000 0.00493 0.00553 0.00540 0.00410 0.00401 0.00411 0.00208 C2 0.43809 0.19903 0.40134 1.00000 0.04153 0.04203 0.04379 -0.00417 -0.00540 -0.01519 0.04127 0.01364 0.00084 0.00080 0.00072 0.00000 0.00587 0.00600 0.00565 0.00434 0.00455 0.00471 0.00224 C3 0.52948 0.15469 0.32157 1.00000 0.04063 0.06339 0.03927 -0.02000 -0.00212 -0.01703 0.04616 0.01355 0.00080 0.00086 0.00074 0.00000 0.00588 0.00703 0.00570 0.00470 0.00456 0.00509 0.00244 C4 0.50993 0.18645 0.21389 1.00000 0.04211 0.14071 0.05933 -0.02941 -0.00395 -0.00784 0.08152 0.01867 0.00099 0.00127 0.00094 0.00000 0.00660 0.01257 0.00792 0.00754 0.00582 0.00695 0.00402 H4 0.43929 0.23625 0.19325 1.00000 0.09782 0.00000 0.00000 C5 0.60059 0.14078 0.13682 1.00000 0.03395 0.21375 0.05104 -0.03003 -0.01186 -0.00777 0.10112 0.02054 0.00100 0.00150 0.00096 0.00000 0.00715 0.01750 0.00762 0.00871 0.00576 0.00852 0.00541 H5 0.58956 0.15865 0.06262 1.00000 0.12135 0.00000 0.00000 C6 0.70324 0.07178 0.16693 1.00000 0.04177 0.17219 0.06833 -0.06162 0.00671 -0.01507 0.09355 0.01911 0.00103 0.00138 0.00105 0.00000 0.00747 0.01495 0.00903 0.00897 0.00634 0.00815 0.00489 H6 0.76414 0.04584 0.11385 1.00000 0.11226 0.00000 0.00000 C7 0.71983 0.03915 0.27345 1.00000 0.03542 0.08376 0.05348 -0.02606 -0.00557 -0.01376 0.05634 0.01467 0.00084 0.00097 0.00083 0.00000 0.00571 0.00843 0.00697 0.00571 0.00503 0.00527 0.00285 H7 0.78995 -0.01218 0.29304 1.00000 0.06761 0.00000 0.00000 C8 0.63336 0.08175 0.35221 1.00000 0.03088 0.04757 0.06101 -0.01841 0.00267 -0.01098 0.04571 0.01408 0.00077 0.00082 0.00081 0.00000 0.00534 0.00637 0.00671 0.00491 0.00477 0.00452 0.00241 C9 0.65392 0.05077 0.46532 1.00000 0.03461 0.03722 0.05766 0.00103 -0.00509 -0.01322 0.04234 0.01416 0.00081 0.00080 0.00078 0.00000 0.00567 0.00601 0.00647 0.00455 0.00465 0.00464 0.00229 C10 0.56736 0.10352 0.54694 1.00000 0.03254 0.04016 0.04573 -0.01009 0.00740 -0.00726 0.03972 0.01406 0.00074 0.00076 0.00073 0.00000 0.00514 0.00585 0.00573 0.00432 0.00427 0.00418 0.00219 C11 0.58725 0.08475 0.65778 1.00000 0.03670 0.03446 0.04946 0.01056 -0.00272 -0.00408 0.04128 0.01496 0.00078 0.00075 0.00075 0.00000 0.00537 0.00571 0.00595 0.00435 0.00453 0.00425 0.00227 C12 0.50211 0.14153 0.73661 1.00000 0.04409 0.05494 0.04770 0.01658 -0.00843 -0.01386 0.04893 0.01576 0.00084 0.00087 0.00076 0.00000 0.00598 0.00679 0.00599 0.00485 0.00474 0.00489 0.00254 C13 0.52227 0.12268 0.85478 1.00000 0.04895 0.07065 0.04448 0.01394 0.00104 0.00586 0.05849 0.01793 0.00089 0.00095 0.00074 0.00000 0.00623 0.00780 0.00607 0.00519 0.00479 0.00521 0.00293 H13A 0.45694 0.16966 0.89610 1.00000 0.08774 0.00000 0.00000 H13B 0.59632 0.14305 0.86913 1.00000 0.08774 0.00000 0.00000 H13C 0.52668 0.04309 0.87596 1.00000 0.08774 0.00000 0.00000 C14 0.39986 0.21231 0.70192 1.00000 0.03434 0.04449 0.04583 0.00546 0.00242 -0.01562 0.04100 0.01406 0.00075 0.00078 0.00072 0.00000 0.00521 0.00606 0.00567 0.00438 0.00423 0.00435 0.00225 H14 0.34280 0.24885 0.75379 1.00000 0.04920 0.00000 0.00000 C15 0.37796 0.23173 0.59137 1.00000 0.03505 0.03221 0.03255 -0.00511 -0.00498 -0.01529 0.03174 0.01180 0.00070 0.00069 0.00064 0.00000 0.00490 0.00525 0.00485 0.00374 0.00387 0.00389 0.00195 C16 0.25379 0.47789 0.44250 1.00000 0.03398 0.03562 0.04021 0.00201 0.00200 -0.01025 0.03655 0.01374 0.00073 0.00074 0.00068 0.00000 0.00488 0.00553 0.00523 0.00395 0.00398 0.00397 0.00207 C17 0.33550 0.53566 0.47247 1.00000 0.05792 0.04201 0.06529 0.00844 -0.02389 -0.02421 0.05247 0.01475 0.00087 0.00083 0.00083 0.00000 0.00649 0.00645 0.00675 0.00503 0.00517 0.00508 0.00265 H17 0.37371 0.51442 0.53763 1.00000 0.06296 0.00000 0.00000 C18 0.36093 0.62218 0.40917 1.00000 0.03732 0.04644 0.12321 0.01301 -0.00392 -0.02642 0.06704 0.01861 0.00086 0.00091 0.00106 0.00000 0.00589 0.00718 0.01057 0.00675 0.00623 0.00502 0.00341 H18 0.41530 0.66302 0.43093 1.00000 0.08045 0.00000 0.00000 C19 0.30764 0.65156 0.31217 1.00000 0.04974 0.04985 0.07017 0.01453 -0.01666 -0.01390 0.05619 0.01681 0.00088 0.00090 0.00087 0.00000 0.00653 0.00701 0.00734 0.00538 0.00551 0.00521 0.00279 H19 0.32723 0.71113 0.26695 1.00000 0.06743 0.00000 0.00000 C20 0.22729 0.59492 0.28194 1.00000 0.04826 0.04459 0.05440 0.01485 -0.00722 -0.00633 0.05017 0.01671 0.00084 0.00083 0.00079 0.00000 0.00602 0.00651 0.00629 0.00490 0.00478 0.00480 0.00256 H20 0.18997 0.61575 0.21628 1.00000 0.06021 0.00000 0.00000 C21 0.20027 0.50682 0.34738 1.00000 0.04590 0.03555 0.04468 -0.00128 -0.01000 -0.00854 0.04176 0.01425 0.00079 0.00075 0.00071 0.00000 0.00567 0.00583 0.00561 0.00431 0.00443 0.00435 0.00225 H21 0.14490 0.46668 0.32640 1.00000 0.05011 0.00000 0.00000 C22 0.09647 0.25667 0.48458 1.00000 0.02378 0.03086 0.03995 -0.00247 -0.00454 0.00324 0.03280 0.01299 0.00067 0.00069 0.00067 0.00000 0.00447 0.00524 0.00526 0.00381 0.00380 0.00360 0.00199 C23 0.10572 0.21996 0.37872 1.00000 0.03268 0.04062 0.03690 0.00282 -0.00384 -0.00228 0.03772 0.01388 0.00074 0.00074 0.00068 0.00000 0.00499 0.00585 0.00537 0.00410 0.00390 0.00414 0.00215 H23 0.16253 0.23942 0.32698 1.00000 0.04527 0.00000 0.00000 C24 0.02996 0.15518 0.35285 1.00000 0.03710 0.03709 0.04723 0.00147 0.00061 -0.00341 0.04149 0.01511 0.00075 0.00075 0.00076 0.00000 0.00530 0.00587 0.00570 0.00428 0.00439 0.00431 0.00225 H24 0.03575 0.12805 0.28246 1.00000 0.04979 0.00000 0.00000 C25 -0.05435 0.12868 0.42691 1.00000 0.03546 0.04702 0.04838 -0.01043 -0.00533 -0.00720 0.04342 0.01463 0.00077 0.00081 0.00076 0.00000 0.00526 0.00622 0.00614 0.00464 0.00446 0.00436 0.00231 H25 -0.10375 0.08119 0.40825 1.00000 0.05210 0.00000 0.00000 C26 -0.06669 0.17005 0.52559 1.00000 0.04312 0.06925 0.05261 -0.00198 0.00298 -0.02784 0.05288 0.01548 0.00084 0.00092 0.00083 0.00000 0.00576 0.00754 0.00662 0.00542 0.00469 0.00523 0.00265 H26 -0.12886 0.15613 0.57424 1.00000 0.06346 0.00000 0.00000 C27 0.01083 0.23347 0.55784 1.00000 0.04542 0.04825 0.03071 -0.00342 0.00183 -0.01140 0.04141 0.01438 0.00077 0.00078 0.00070 0.00000 0.00565 0.00625 0.00500 0.00413 0.00423 0.00456 0.00224 H27 0.00408 0.25963 0.62867 1.00000 0.04969 0.00000 0.00000 C28 0.14429 0.41224 0.68129 1.00000 0.03607 0.03994 0.02851 0.00688 -0.00763 -0.01282 0.03420 0.01298 0.00072 0.00075 0.00063 0.00000 0.00493 0.00603 0.00466 0.00385 0.00369 0.00403 0.00206 C29 0.11384 0.52907 0.68700 1.00000 0.05610 0.02962 0.03594 -0.00095 -0.01321 0.00102 0.04167 0.01399 0.00081 0.00076 0.00072 0.00000 0.00605 0.00593 0.00546 0.00411 0.00452 0.00436 0.00229 H29 0.13503 0.57543 0.62832 1.00000 0.05001 0.00000 0.00000 C30 0.05386 0.57759 0.77610 1.00000 0.07556 0.03620 0.05076 0.00511 -0.02098 -0.00542 0.05467 0.01606 0.00095 0.00088 0.00080 0.00000 0.00742 0.00624 0.00671 0.00503 0.00565 0.00520 0.00276 H30 0.03700 0.65736 0.77952 1.00000 0.06561 0.00000 0.00000 C31 0.01737 0.51439 0.86059 1.00000 0.07231 0.04535 0.02914 -0.00356 -0.00021 0.00529 0.05181 0.01634 0.00091 0.00087 0.00072 0.00000 0.00716 0.00703 0.00537 0.00445 0.00475 0.00518 0.00266 H31 -0.02654 0.54998 0.92086 1.00000 0.06217 0.00000 0.00000 C32 0.04481 0.39923 0.85739 1.00000 0.06176 0.05453 0.03681 -0.00196 -0.00189 -0.00920 0.05162 0.01589 0.00089 0.00091 0.00077 0.00000 0.00659 0.00772 0.00571 0.00479 0.00487 0.00529 0.00262 H32 0.02005 0.35484 0.91601 1.00000 0.06195 0.00000 0.00000 C33 0.10850 0.34665 0.76924 1.00000 0.04759 0.05144 0.04484 -0.00310 -0.00692 -0.00622 0.04842 0.01517 0.00082 0.00089 0.00075 0.00000 0.00584 0.00662 0.00609 0.00480 0.00473 0.00479 0.00246 H33 0.12795 0.26668 0.76815 1.00000 0.05811 0.00000 0.00000 N1 0.68457 0.01534 0.69211 1.00000 0.04210 0.05824 0.06141 0.01926 0.00011 -0.00095 0.05653 0.01414 0.00067 0.00070 0.00068 0.00000 0.00496 0.00587 0.00557 0.00438 0.00408 0.00418 0.00232 H1A 0.73815 -0.01997 0.64543 1.00000 0.06783 0.00000 0.00000 H1B 0.69507 0.00495 0.76139 1.00000 0.06783 0.00000 0.00000 O1 0.34152 0.25732 0.37691 1.00000 0.03506 0.04873 0.04225 -0.00572 -0.00431 -0.00451 0.04248 0.00918 0.00052 0.00053 0.00046 0.00000 0.00373 0.00413 0.00367 0.00291 0.00287 0.00310 0.00151 O2 0.74374 -0.01587 0.48796 1.00000 0.05012 0.04846 0.06662 0.00235 0.00635 -0.00660 0.05639 0.01134 0.00060 0.00058 0.00055 0.00000 0.00450 0.00455 0.00475 0.00352 0.00357 0.00364 0.00182 Sb1 0.22295 0.33845 0.53929 1.00000 0.03302 0.03692 0.03659 0.00129 -0.00382 -0.00737 0.03559 0.00091 0.00005 0.00005 0.00005 0.00000 0.00035 0.00040 0.00036 0.00026 0.00025 0.00026 0.00020 I1 0.06623 -0.11340 0.13641 1.00000 0.06131 0.05238 0.05100 0.01716 -0.01948 -0.02149 0.05350 0.00103 0.00006 0.00006 0.00005 0.00000 0.00046 0.00047 0.00042 0.00031 0.00032 0.00033 0.00024 I2 0.21755 0.17862 0.06373 1.00000 0.04389 0.04997 0.04464 0.00579 -0.00753 -0.01289 0.04584 0.00097 0.00005 0.00005 0.00005 0.00000 0.00039 0.00045 0.00039 0.00029 0.00028 0.00030 0.00022 Cu1 0.06954 0.06896 0.02066 1.00000 0.04058 0.04854 0.04076 0.00361 -0.00285 -0.01022 0.04342 0.00177 0.00009 0.00010 0.00009 0.00000 0.00068 0.00077 0.00067 0.00053 0.00051 0.00053 0.00032 C34 0.66986 0.52265 1.05539 0.33000 0.06252 0.02173 0.16861 0.03294 0.03300 -0.02013 0.08605 0.06967 0.00293 0.00256 0.00365 0.00000 0.02181 0.01882 0.03988 0.02136 0.02390 0.01549 0.01404 H34A 0.73048 0.56268 1.07405 0.33000 0.10327 0.00000 0.00000 H34B 0.63300 0.56189 0.99056 0.33000 0.10327 0.00000 0.00000 Cl1 0.74046 0.38256 1.02358 0.33000 0.08533 0.09861 0.08059 -0.01039 -0.00390 -0.02567 0.08709 0.01638 0.00092 0.00096 0.00082 0.00000 0.00690 0.00817 0.00681 0.00559 0.00532 0.00584 0.00292 Cl2 0.57053 0.53182 1.15287 0.33000 0.10413 0.16687 0.22028 -0.12543 0.04040 -0.05667 0.15717 0.02079 0.00121 0.00146 0.00150 0.00000 0.00949 0.01465 0.01738 0.01336 0.01039 0.00965 0.00717 Final Structure Factor Calculation for DIRDIF output for 02SRC191 in P-1 Total number of l.s. parameters = 390 Maximum vector length = 511 Memory required = 4212 / 27083 wR2 = 0.1455 before cycle 5 for 6303 data and 0 / 390 parameters GooF = S = 1.039; Restrained GooF = 1.039 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0573 * P )^2 + 7.13 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0574 for 4004 Fo > 4sig(Fo) and 0.1092 for all 6303 data wR2 = 0.1455, GooF = S = 1.039, Restrained GooF = 1.039 for all data Occupancy sum of asymmetric unit = 40.99 for non-hydrogen and 25.66 for hydrogen atoms Principal mean square atomic displacements U 0.0474 0.0394 0.0184 C1 0.0468 0.0451 0.0319 C2 0.0721 0.0402 0.0262 C3 0.1515 0.0511 0.0420 C4 0.2248 0.0505 0.0280 C5 may be split into 0.5968 0.1583 0.1349 and 0.6044 0.1232 0.1387 0.1965 0.0481 0.0360 C6 0.0957 0.0431 0.0302 C7 0.0712 0.0362 0.0297 C8 0.0584 0.0398 0.0288 C9 0.0535 0.0385 0.0272 C10 0.0584 0.0380 0.0275 C11 0.0716 0.0424 0.0328 C12 0.0957 0.0437 0.0362 C13 0.0532 0.0440 0.0258 C14 0.0403 0.0349 0.0201 C15 0.0440 0.0371 0.0286 C16 0.0849 0.0426 0.0299 C17 0.1277 0.0547 0.0186 C18 0.0830 0.0460 0.0396 C19 0.0685 0.0503 0.0317 C20 0.0523 0.0375 0.0355 C21 0.0418 0.0377 0.0189 C22 0.0470 0.0370 0.0292 C23 0.0515 0.0397 0.0333 C24 0.0567 0.0393 0.0342 C25 0.0738 0.0542 0.0306 C26 0.0488 0.0455 0.0298 C27 0.0469 0.0318 0.0239 C28 0.0651 0.0335 0.0264 C29 0.0847 0.0478 0.0315 C30 0.0869 0.0399 0.0286 C31 0.0643 0.0537 0.0368 C32 0.0565 0.0473 0.0415 C33 0.0892 0.0441 0.0363 N1 0.0528 0.0404 0.0342 O1 0.0755 0.0483 0.0454 O2 0.0399 0.0349 0.0320 Sb1 0.0814 0.0465 0.0326 I1 0.0568 0.0424 0.0383 I2 0.0519 0.0404 0.0380 Cu1 0.1976 0.0582 0.0023 C34 0.1013 0.0827 0.0773 Cl1 0.3153 0.0890 0.0672 Cl2 may be split into 0.5776 0.5193 1.1675 and 0.5635 0.5444 1.1383 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.012 0.025 0.038 0.053 0.069 0.088 0.114 0.152 0.223 1.000 Number in group 637. 657. 604. 653. 623. 606. 643. 624. 622. 634. GooF 0.974 1.042 0.986 1.019 1.074 1.044 1.141 1.060 0.948 1.126 K 0.216 1.225 0.952 1.000 1.024 1.021 1.008 0.986 1.002 1.041 Resolution(A) 0.77 0.81 0.86 0.91 0.97 1.04 1.12 1.23 1.42 1.77 inf Number in group 635. 630. 625. 640. 633. 628. 620. 634. 626. 632. GooF 0.912 0.907 0.994 0.935 0.977 0.924 1.019 1.088 1.077 1.478 K 1.112 1.137 1.071 1.009 1.007 0.998 1.020 1.015 1.018 1.032 R1 0.389 0.272 0.224 0.166 0.119 0.091 0.072 0.058 0.047 0.043 Recommended weighting scheme: WGHT 0.0547 7.4406 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) 7 -7 5 413.44 1147.17 5.50 0.103 0.98 0 3 1 8745.88 5960.34 5.16 0.235 3.82 0 1 2 154.94 0.13 5.11 0.001 5.62 -1 -1 1 22984.41 16585.06 4.83 0.393 7.15 3 0 1 570.66 263.44 4.82 0.049 3.68 3 0 0 554.59 5.76 4.71 0.007 3.78 0 2 2 1329.59 788.51 4.65 0.086 4.39 3 6 1 264.88 20.73 4.55 0.014 1.93 -2 0 2 875.62 497.15 4.54 0.068 4.07 1 -1 1 265.93 27.17 4.51 0.016 6.41 2 1 12 137.41 1047.55 4.49 0.099 1.03 3 3 0 13203.18 9607.64 4.40 0.299 3.09 1 5 0 125.29 0.13 4.33 0.001 2.43 1 -2 2 1754.92 1179.95 4.31 0.105 3.80 -1 -1 3 3541.60 2516.46 4.28 0.153 3.67 -4 4 11 -458.71 946.96 4.23 0.094 0.96 -2 -4 1 263.37 69.76 4.16 0.025 2.78 3 1 5 218.17 1.20 4.16 0.003 2.17 0 2 0 112.76 319.79 4.11 0.055 5.93 1 5 2 169.77 26.60 4.05 0.016 2.31 0 3 0 15056.78 11303.04 4.02 0.324 3.95 1 -3 1 636.93 355.56 3.98 0.057 3.35 -2 -3 1 10246.13 7827.75 3.90 0.270 3.42 0 -2 1 10629.59 8100.99 3.77 0.274 5.26 2 -2 3 169.66 50.33 3.75 0.022 2.78 0 -1 5 141.03 339.21 3.74 0.056 2.41 -2 0 3 1769.03 1203.87 3.69 0.106 3.26 7 7 1 370.58 142.53 3.65 0.036 1.33 -5 -1 4 155.85 30.67 3.62 0.017 1.80 -2 3 4 990.09 639.70 3.60 0.077 2.15 6 0 3 615.40 307.77 3.58 0.053 1.76 7 -2 5 23571.54 17380.63 3.55 0.402 1.30 -3 0 2 1571.95 1104.93 3.49 0.101 3.15 -5 7 11 939.35 39.71 3.46 0.019 0.83 2 0 12 -274.01 372.33 3.42 0.059 1.03 -1 0 1 19971.09 27373.78 3.41 0.504 8.15 -5 -2 1 1458.64 1038.76 3.41 0.098 2.22 2 2 5 1370.04 917.71 3.38 0.092 2.27 2 1 0 3721.39 2880.23 3.37 0.164 5.62 -1 -1 2 1671.68 2268.04 3.36 0.145 4.98 -2 4 0 381.09 208.98 3.32 0.044 2.42 5 6 0 218.42 42.59 3.26 0.020 1.68 1 -6 1 91.74 2.71 3.21 0.005 1.85 5 4 2 487.71 293.65 3.21 0.052 1.98 7 -1 4 6337.04 4729.16 3.19 0.210 1.42 2 2 3 151.96 45.22 3.18 0.020 3.23 2 -9 4 -4.54 193.56 3.16 0.042 1.13 2 7 0 698.81 1049.99 3.13 0.099 1.73 1 1 0 3294.16 16004.91 3.12 0.386 9.27 -1 2 9 92.15 300.98 3.04 0.053 1.33 Bond lengths and angles C1 - Distance Angles C15 1.3954 (0.0119) C10 1.4073 (0.0119) 122.27 (0.78) C2 1.4810 (0.0119) 117.27 (0.78) 120.46 (0.80) C1 - C15 C10 C2 - Distance Angles O1 1.2382 (0.0102) C3 1.4417 (0.0130) 122.27 (0.82) C1 1.4810 (0.0119) 119.11 (0.82) 118.59 (0.84) C2 - O1 C3 C3 - Distance Angles C8 1.3966 (0.0131) C4 1.3969 (0.0146) 121.74 (0.92) C2 1.4417 (0.0129) 120.40 (0.87) 117.86 (0.93) C3 - C8 C4 C4 - Distance Angles C3 1.3969 (0.0146) C5 1.4187 (0.0161) 116.82 (1.13) H4 0.9500 121.59 121.59 C4 - C3 C5 C5 - Distance Angles C6 1.3638 (0.0176) C4 1.4187 (0.0161) 121.43 (1.15) H5 0.9500 119.28 119.28 C5 - C6 C4 C6 - Distance Angles C5 1.3638 (0.0176) C7 1.3796 (0.0160) 120.89 (1.08) H6 0.9500 119.56 119.56 C6 - C5 C7 C7 - Distance Angles C6 1.3796 (0.0160) C8 1.3935 (0.0131) 119.77 (1.05) H7 0.9500 120.12 120.12 C7 - C6 C8 C8 - Distance Angles C7 1.3935 (0.0131) C3 1.3966 (0.0130) 119.27 (0.94) C9 1.4623 (0.0132) 119.42 (0.90) 121.30 (0.84) C8 - C7 C3 C9 - Distance Angles O2 1.2137 (0.0103) C10 1.4545 (0.0129) 122.29 (0.88) C8 1.4623 (0.0132) 118.99 (0.87) 118.70 (0.85) C9 - O2 C10 C10 - Distance Angles C1 1.4073 (0.0119) C11 1.4162 (0.0123) 118.64 (0.79) C9 1.4545 (0.0129) 120.02 (0.82) 121.33 (0.83) C10 - C1 C11 C11 - Distance Angles N1 1.3364 (0.0110) C10 1.4162 (0.0123) 121.57 (0.86) C12 1.4393 (0.0135) 118.32 (0.83) 120.11 (0.79) C11 - N1 C10 C12 - Distance Angles C14 1.3874 (0.0126) C11 1.4393 (0.0136) 118.78 (0.83) C13 1.5065 (0.0127) 120.51 (0.92) 120.70 (0.84) C12 - C14 C11 C13 - Distance Angles C12 1.5065 (0.0127) H13A 0.9800 109.47 H13B 0.9800 109.47 109.47 H13C 0.9800 109.47 109.47 109.47 C13 - C12 H13A H13B C14 - Distance Angles C12 1.3874 (0.0126) C15 1.4179 (0.0114) 121.97 (0.87) H14 0.9500 119.01 119.01 C14 - C12 C15 C15 - Distance Angles C1 1.3954 (0.0119) C14 1.4179 (0.0114) 118.22 (0.78) Sb1 2.0983 (0.0081) 119.94 (0.59) 121.84 (0.63) C15 - C1 C14 C16 - Distance Angles C21 1.3717 (0.0116) C17 1.3855 (0.0122) 120.09 (0.83) Sb1 2.1054 (0.0083) 120.81 (0.64) 118.95 (0.66) C16 - C21 C17 C17 - Distance Angles C18 1.3515 (0.0133) C16 1.3855 (0.0122) 120.12 (0.93) H17 0.9500 119.94 119.94 C17 - C18 C16 C18 - Distance Angles C17 1.3515 (0.0133) C19 1.3918 (0.0149) 120.13 (0.96) H18 0.9500 119.93 119.93 C18 - C17 C19 C19 - Distance Angles C20 1.3645 (0.0138) C18 1.3918 (0.0149) 120.09 (0.94) H19 0.9500 119.96 119.96 C19 - C20 C18 C20 - Distance Angles C19 1.3645 (0.0138) C21 1.3873 (0.0123) 119.80 (0.91) H20 0.9500 120.10 120.10 C20 - C19 C21 C21 - Distance Angles C16 1.3717 (0.0117) C20 1.3873 (0.0123) 119.74 (0.86) H21 0.9500 120.13 120.13 C21 - C16 C20 C22 - Distance Angles C27 1.3703 (0.0115) C23 1.4099 (0.0117) 121.19 (0.79) Sb1 2.1223 (0.0082) 117.64 (0.62) 120.99 (0.60) C22 - C27 C23 C23 - Distance Angles C24 1.3729 (0.0122) C22 1.4099 (0.0117) 117.84 (0.81) H23 0.9500 121.08 121.08 C23 - C24 C22 C24 - Distance Angles C23 1.3729 (0.0122) C25 1.3787 (0.0122) 121.35 (0.90) H24 0.9500 119.32 119.32 C24 - C23 C25 C25 - Distance Angles C26 1.3452 (0.0131) C24 1.3787 (0.0122) 120.04 (0.90) H25 0.9500 119.98 119.98 C25 - C26 C24 C26 - Distance Angles C25 1.3452 (0.0131) C27 1.4043 (0.0129) 121.06 (0.88) H26 0.9500 119.47 119.47 C26 - C25 C27 C27 - Distance Angles C22 1.3703 (0.0115) C26 1.4043 (0.0129) 118.32 (0.84) H27 0.9500 120.84 120.84 C27 - C22 C26 C28 - Distance Angles C29 1.3923 (0.0122) C33 1.4124 (0.0121) 117.79 (0.83) Sb1 2.0947 (0.0087) 120.41 (0.60) 121.42 (0.68) C28 - C29 C33 C29 - Distance Angles C30 1.3644 (0.0134) C28 1.3923 (0.0122) 120.60 (0.86) H29 0.9500 119.70 119.70 C29 - C30 C28 C30 - Distance Angles C29 1.3644 (0.0135) C31 1.3673 (0.0131) 121.71 (0.97) H30 0.9500 119.14 119.14 C30 - C29 C31 C31 - Distance Angles C30 1.3673 (0.0132) C32 1.3694 (0.0137) 119.28 (0.93) H31 0.9500 120.36 120.36 C31 - C30 C32 C32 - Distance Angles C31 1.3694 (0.0137) C33 1.3896 (0.0134) 120.65 (0.93) H32 0.9500 119.68 119.68 C32 - C31 C33 C33 - Distance Angles C32 1.3896 (0.0133) C28 1.4124 (0.0121) 119.92 (0.94) H33 0.9500 120.04 120.04 C33 - C32 C28 N1 - Distance Angles C11 1.3364 (0.0110) H1A 0.8800 120.00 H1B 0.8800 120.00 120.00 N1 - C11 H1A O1 - Distance Angles C2 1.2382 (0.0102) Sb1 2.4974 (0.0059) 111.08 (0.54) O1 - C2 O2 - Distance Angles C9 1.2137 (0.0103) O2 - Sb1 - Distance Angles C28 2.0947 (0.0087) C15 2.0983 (0.0081) 102.71 (0.31) C16 2.1054 (0.0083) 102.87 (0.34) 113.24 (0.31) C22 2.1223 (0.0083) 104.69 (0.32) 115.69 (0.30) 115.37 (0.32) O1 2.4974 (0.0059) 172.28 (0.26) 72.29 (0.26) 74.48 (0.28) 82.91 (0.26) Sb1 - C28 C15 C16 C22 I1 - Distance Angles Cu1_$1 2.5646 (0.0012) Cu1 2.5812 (0.0013) 62.56 (0.05) I1 - Cu1_$1 I2 - Distance Angles Cu1 2.5066 (0.0013) I2 - Cu1 - Distance Angles I2 2.5066 (0.0013) I1_$1 2.5646 (0.0012) 125.83 (0.05) I1 2.5812 (0.0013) 116.54 (0.04) 117.44 (0.05) Cu1_$1 2.6718 (0.0023) 173.50 (0.07) 59.02 (0.04) 58.42 (0.04) Cu1 - I2 I1_$1 I1 C34 - Distance Angles Cl2 1.6108 (0.0377) Cl1 1.7768 (0.0354) 114.65 (1.77) H34A 0.9900 108.62 108.62 H34B 0.9900 108.59 108.58 107.57 C34 - Cl2 Cl1 H34A Cl1 - Distance Angles C34 1.7768 (0.0355) Cl1 - Cl2 - Distance Angles C34 1.6108 (0.0378) Cl2 - FMAP and GRID set by program FMAP 2 3 31 GRID -1.786 -2 -2 1.786 2 2 R1 = 0.1076 for 6303 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 1.37 at 0.0995 0.8424 0.0746 [ 0.98 A from I1 ] Deepest hole -0.78 at 0.8417 0.5635 0.4159 [ 1.24 A from C28 ] Mean = 0.00, Rms deviation from mean = 0.18 e/A^3, Highest memory used = 4018 / 30461 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.0995 -0.1576 0.0746 1.00000 0.05 1.37 0.98 I1 2.39 CU1 2.75 CU1 3.02 H32 Q2 1 0.5000 0.5000 1.0000 0.50000 0.05 1.36 1.86 H34B 2.22 CL2 2.22 C34 2.88 CL1 Q3 1 0.5003 0.5881 1.2543 1.00000 0.05 1.35 1.57 CL2 2.23 H19 2.29 C19 2.43 C18 Q4 1 -0.0604 0.2705 0.3364 1.00000 0.05 1.29 1.57 C24 1.68 H30 1.95 H29 1.97 H24 Q5 1 0.2485 0.1409 0.0043 1.00000 0.05 1.28 0.91 I2 2.43 CU1 2.78 H13A 2.82 H6 Q6 1 0.1952 0.3666 0.6055 1.00000 0.05 1.10 0.92 SB1 1.18 C28 2.24 C33 2.26 C29 Q7 1 -0.0756 -0.0436 0.3889 1.00000 0.05 1.00 1.51 H25 1.99 H7 2.25 C25 2.28 C26 Q8 1 0.1515 -0.1944 -0.0086 1.00000 0.05 0.90 2.18 I1 2.37 CL1 2.51 H6 2.70 CU1 Q9 1 0.7676 0.0014 0.4083 1.00000 0.05 0.84 1.04 O2 1.46 H7 1.48 C9 1.81 C7 Q10 1 0.5025 0.5881 0.6241 1.00000 0.05 0.83 2.27 H17 2.43 C17 2.61 H17 2.71 H18 Shortest distances between peaks (including symmetry equivalents) 1 8 1.22 7 9 1.79 3 10 2.56 Time profile in seconds ----------------------- 0.20: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.02: 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. 2.67: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.03: Set up l.s. refinement 0.02: Generate idealized H-atoms 2.81: Structure factors and derivatives 6.88: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.97: Solve l.s. equations 0.00: Generate HTAB table 0.00: Other dependent quantities, CIF, tables 0.16: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.13: Fourier summations 0.03: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 02src191 finished at 14:15:06 Total CPU time: 13.9 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++