+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2006cgl0741 started at 16:00:10 on 21-Jul-2006 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2006cgl0741 in P-1 CELL 0.71073 7.0558 13.6319 14.1191 106.205 95.292 104.352 ZERR 2.00 0.0003 0.0003 0.0005 0.002 0.002 0.002 LATT 1 SFAC C H N BR UNIT 40 26 4 14 V = 1244.22 F(000) = 784.0 Mu = 11.30 mm-1 Cell Wt = 1681.39 Rho = 2.244 MERG 2 EQIV $1 -x+1, -y, -z OMIT -3.00 55.00 OMIT 0 1 0 OMIT 0 -1 0 OMIT 0 0 1 OMIT 0 -1 1 FMAP 2 PLAN 5 SIZE 0.34 0.2 0.16 ACTA HTAB N1 N2_$1 BOND $H L.S. 6 TEMP -153.00 WGHT 0.031300 3.885400 EXTI 0.001862 FVAR 0.27412 MOLE 1 C1 1 0.547747 0.060654 -0.236540 11.00000 0.02117 0.02064 = 0.03353 0.00879 0.00663 0.00855 C2 1 0.511320 -0.045178 -0.241871 11.00000 0.02285 0.01932 = 0.02805 0.00773 0.00209 0.00441 AFIX 43 H2 2 0.462146 -0.067936 -0.188798 11.00000 -1.20000 AFIX 0 C3 1 0.618335 -0.088297 -0.395225 11.00000 0.02377 0.02949 = 0.02378 0.00257 -0.00112 0.01107 AFIX 43 H3 2 0.638237 -0.141376 -0.450185 11.00000 -1.20000 AFIX 0 C4 1 0.666623 0.016315 -0.393914 11.00000 0.02937 0.03491 = 0.02831 0.01543 0.00571 0.01279 AFIX 43 H4 2 0.723296 0.036903 -0.446382 11.00000 -1.20000 AFIX 0 C5 1 0.629830 0.091155 -0.313233 11.00000 0.02656 0.02461 = 0.04231 0.01545 0.00697 0.00790 AFIX 43 H5 2 0.661271 0.163863 -0.310684 11.00000 -1.20000 AFIX 0 C6 1 0.508519 0.136381 -0.146995 11.00000 0.02571 0.02514 = 0.03791 0.01141 0.00327 0.00532 C7 1 0.393548 0.198597 -0.146835 11.00000 0.02751 0.02504 = 0.03702 0.01166 0.00455 0.00802 C8 1 0.359494 0.276874 -0.058039 11.00000 0.03316 0.02022 = 0.03193 0.01013 0.00960 0.00977 C9 1 0.167557 0.268138 -0.037762 11.00000 0.02381 0.02648 = 0.04341 0.00734 0.00396 0.00324 AFIX 43 H9 2 0.059655 0.210920 -0.079608 11.00000 -1.20000 AFIX 0 C10 1 0.133676 0.342217 0.042792 11.00000 0.02158 0.02851 = 0.03202 0.00688 0.00344 0.01085 AFIX 43 H10 2 0.002473 0.335665 0.056307 11.00000 -1.20000 AFIX 0 C11 1 0.290828 0.426768 0.104614 11.00000 0.02302 0.02194 = 0.02520 0.01050 0.00266 0.01103 C12 1 0.483346 0.435245 0.085727 11.00000 0.02785 0.02170 = 0.02709 0.01052 0.00411 0.00696 AFIX 43 H12 2 0.591286 0.492082 0.128048 11.00000 -1.20000 AFIX 0 C13 1 0.516944 0.360100 0.004590 11.00000 0.02822 0.01913 = 0.03873 0.00959 0.01315 0.00832 AFIX 43 H13 2 0.648401 0.365608 -0.008199 11.00000 -1.20000 AFIX 0 C14 1 0.256045 0.508295 0.190575 11.00000 0.02184 0.01800 = 0.03275 0.00762 0.00741 0.01093 C15 1 0.353078 0.537425 0.283928 11.00000 0.03077 0.01607 = 0.02737 0.00647 0.01107 0.00782 C16 1 0.493406 0.483413 0.316672 11.00000 0.03593 0.01955 = 0.02142 0.00962 0.00449 0.00904 C17 1 0.431583 0.373865 0.301159 11.00000 0.03240 0.01565 = 0.02906 0.00762 0.00453 0.00712 AFIX 43 H17 2 0.297852 0.335246 0.271150 11.00000 -1.20000 AFIX 0 C18 1 0.742757 0.375469 0.368537 11.00000 0.03184 0.03501 = 0.03490 0.01781 -0.00382 0.00907 AFIX 43 H18 2 0.830803 0.337817 0.385116 11.00000 -1.20000 AFIX 0 C19 1 0.813694 0.483823 0.387994 11.00000 0.03930 0.04399 = 0.04702 0.02559 -0.01118 0.00420 AFIX 43 H19 2 0.947905 0.520660 0.418460 11.00000 -1.20000 AFIX 0 C20 1 0.686513 0.537997 0.362484 11.00000 0.03621 0.02421 = 0.03977 0.01615 -0.00539 -0.00221 AFIX 43 H20 2 0.732124 0.613094 0.376523 11.00000 -1.20000 AFIX 0 N1 3 0.544041 -0.115451 -0.320047 11.00000 0.02100 0.01732 = 0.02795 0.00640 -0.00315 0.00746 AFIX 3 H1N 2 0.515411 -0.182751 -0.322258 11.00000 -1.20000 AFIX 0 N2 3 0.554159 0.321247 0.327091 11.00000 0.04162 0.01974 = 0.02976 0.01045 0.00341 0.01234 BR1 4 0.640928 0.133537 -0.024035 11.00000 0.03060 0.02442 = 0.02593 0.01033 -0.00075 0.01093 BR2 4 0.246641 0.190327 -0.271460 11.00000 0.03447 0.03458 = 0.02753 0.01117 0.00073 0.02035 BR3 4 0.067152 0.576277 0.156105 11.00000 0.03242 0.03792 = 0.04066 0.01630 0.01099 0.02373 BR4 4 0.318054 0.650547 0.387519 11.00000 0.05522 0.02158 = 0.03239 0.00709 0.01657 0.01374 MOLE 2 BR5 4 0.966151 0.196984 0.492233 11.00000 0.03626 0.02957 = 0.03258 0.00905 0.00900 0.01302 BR6 4 0.982814 0.136313 0.299525 11.00000 0.02204 0.03003 = 0.03531 0.01190 0.00130 0.01184 BR7 4 1.004656 0.073923 0.121453 11.00000 0.06553 0.08369 = 0.03004 0.01783 0.00327 0.04398 HKLF 4 1.0 1.00 0.00 0.00 0.00 1.00 0.00 0.00 0.00 1.00 Covalent radii and connectivity table for 2006cgl0741 in P-1 C 0.770 H 0.320 N 0.700 BR 1.140 C1 - C2 C5 C6 C2 - N1 C1 C3 - N1 C4 C4 - C3 C5 C5 - C1 C4 C6 - C7 C1 Br1 C7 - C6 C8 Br2 C8 - C13 C9 C7 C9 - C10 C8 C10 - C9 C11 C11 - C12 C10 C14 C12 - C13 C11 C13 - C12 C8 C14 - C15 C11 Br3 C15 - C14 C16 Br4 C16 - C20 C17 C15 C17 - N2 C16 C18 - N2 C19 C19 - C18 C20 C20 - C16 C19 N1 - C2 C3 N2 - C18 C17 Br1 - C6 Br2 - C7 Br3 - C14 Br4 - C15 Br5 - Br6 Br6 - Br7 Br5 Br7 - Br6 Operators for generating equivalent atoms: $1 -x+1, -y, -z 22349 Reflections read, of which 27 rejected -9 =< h =< 9, -17 =< k =< 17, -18 =< l =< 18, Max. 2-theta = 55.00 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 2 7 2 3.77 0.50 2 3.39 -4 3 11 -3.59 3.43 5 29.74 -4 4 13 9.73 5.30 3 39.05 3 Inconsistent equivalents 5676 Unique reflections, of which 0 suppressed R(int) = 0.0561 R(sigma) = 0.0567 Friedel opposites merged Maximum memory for data reduction = 2217 / 57330 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 = 2894 / 327023 wR2 = 0.0895 before cycle 1 for 5676 data and 263 / 263 parameters GooF = S = 1.020; Restrained GooF = 1.020 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0313 * P )^2 + 3.89 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.27412 0.00041 -0.011 OSF 2 0.00186 0.00022 0.000 EXTI Mean shift/esd = 0.002 Maximum = -0.014 for U13 Br1 Max. shift = 0.000 A for H3 Max. dU = 0.000 for C4 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2894 / 327023 wR2 = 0.0895 before cycle 2 for 5676 data and 263 / 263 parameters GooF = S = 1.020; Restrained GooF = 1.020 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0313 * P )^2 + 3.89 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.27412 0.00041 0.001 OSF 2 0.00186 0.00022 0.001 EXTI Mean shift/esd = 0.001 Maximum = 0.005 for U23 Br4 Max. shift = 0.000 A for C18 Max. dU = 0.000 for C10 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2894 / 327023 wR2 = 0.0895 before cycle 3 for 5676 data and 263 / 263 parameters GooF = S = 1.020; Restrained GooF = 1.020 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0313 * P )^2 + 3.89 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.27412 0.00041 0.001 OSF 2 0.00186 0.00022 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.001 for OSF Max. shift = 0.000 A for C1 Max. dU = 0.000 for C8 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2894 / 327023 wR2 = 0.0895 before cycle 4 for 5676 data and 263 / 263 parameters GooF = S = 1.020; Restrained GooF = 1.020 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0313 * P )^2 + 3.89 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.27412 0.00041 0.000 OSF 2 0.00186 0.00022 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for y Br4 Max. shift = 0.000 A for C19 Max. dU = 0.000 for C20 Least-squares cycle 5 Maximum vector length = 511 Memory required = 2894 / 327023 wR2 = 0.0895 before cycle 5 for 5676 data and 263 / 263 parameters GooF = S = 1.020; Restrained GooF = 1.020 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0313 * P )^2 + 3.89 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.27412 0.00041 0.000 OSF 2 0.00186 0.00022 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for y Br4 Max. shift = 0.000 A for C9 Max. dU = 0.000 for C5 Least-squares cycle 6 Maximum vector length = 511 Memory required = 2894 / 327023 wR2 = 0.0895 before cycle 6 for 5676 data and 263 / 263 parameters GooF = S = 1.020; Restrained GooF = 1.020 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0313 * P )^2 + 3.89 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.27412 0.00041 0.000 OSF 2 0.00186 0.00022 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for y Br4 Max. shift = 0.000 A for C5 Max. dU = 0.000 for C9 Largest correlation matrix elements 0.588 EXTI / OSF 0.546 U12 Br7 / U11 Br7 0.509 U12 Br2 / U22 Br2 0.571 U12 Br7 / U22 Br7 0.543 U12 Br3 / U22 Br3 Idealized hydrogen atom generation before cycle 7 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.4621 -0.0679 -0.1888 43 0.950 0.000 C2 N1 C1 H3 0.6382 -0.1414 -0.4502 43 0.950 0.000 C3 N1 C4 H4 0.7233 0.0369 -0.4464 43 0.950 0.000 C4 C3 C5 H5 0.6613 0.1639 -0.3107 43 0.950 0.000 C5 C1 C4 H9 0.0597 0.2109 -0.0796 43 0.950 0.000 C9 C10 C8 H10 0.0025 0.3357 0.0563 43 0.950 0.000 C10 C9 C11 H12 0.5913 0.4921 0.1280 43 0.950 0.000 C12 C13 C11 H13 0.6484 0.3656 -0.0082 43 0.950 0.000 C13 C12 C8 H17 0.2979 0.3352 0.2712 43 0.950 0.000 C17 N2 C16 H18 0.8308 0.3378 0.3851 43 0.950 0.000 C18 N2 C19 H19 0.9479 0.5207 0.4185 43 0.950 0.000 C19 C18 C20 H20 0.7321 0.6131 0.3765 43 0.950 0.000 C20 C16 C19 2006cgl0741 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.54775 0.06065 -0.23654 1.00000 0.02117 0.02064 0.03353 0.00879 0.00663 0.00855 0.02443 0.01131 0.00073 0.00038 0.00040 0.00000 0.00256 0.00246 0.00294 0.00213 0.00217 0.00200 0.00109 C2 0.51132 -0.04518 -0.24187 1.00000 0.02285 0.01932 0.02805 0.00773 0.00209 0.00441 0.02380 0.01061 0.00072 0.00037 0.00039 0.00000 0.00261 0.00245 0.00279 0.00209 0.00211 0.00200 0.00108 H2 0.46215 -0.06794 -0.18880 1.00000 0.02857 0.00000 0.00000 C3 0.61834 -0.08830 -0.39523 1.00000 0.02377 0.02949 0.02378 0.00257 -0.00112 0.01107 0.02662 0.01109 0.00074 0.00040 0.00039 0.00000 0.00269 0.00279 0.00275 0.00219 0.00216 0.00219 0.00116 H3 0.63824 -0.14138 -0.45018 1.00000 0.03194 0.00000 0.00000 C4 0.66662 0.01632 -0.39391 1.00000 0.02937 0.03491 0.02831 0.01543 0.00571 0.01279 0.02896 0.01208 0.00079 0.00042 0.00041 0.00000 0.00290 0.00295 0.00291 0.00235 0.00228 0.00233 0.00117 H4 0.72330 0.03690 -0.44638 1.00000 0.03475 0.00000 0.00000 C5 0.62983 0.09116 -0.31323 1.00000 0.02656 0.02461 0.04231 0.01545 0.00697 0.00790 0.02992 0.01225 0.00077 0.00042 0.00043 0.00000 0.00283 0.00267 0.00335 0.00241 0.00242 0.00219 0.00121 H5 0.66127 0.16386 -0.31068 1.00000 0.03590 0.00000 0.00000 C6 0.50852 0.13638 -0.14700 1.00000 0.02571 0.02514 0.03791 0.01141 0.00327 0.00532 0.02978 0.01191 0.00078 0.00041 0.00043 0.00000 0.00279 0.00269 0.00322 0.00234 0.00235 0.00219 0.00120 C7 0.39355 0.19860 -0.14683 1.00000 0.02751 0.02504 0.03702 0.01166 0.00455 0.00802 0.02942 0.01199 0.00079 0.00041 0.00042 0.00000 0.00282 0.00270 0.00318 0.00232 0.00236 0.00224 0.00119 C8 0.35949 0.27687 -0.05804 1.00000 0.03316 0.02022 0.03193 0.01013 0.00960 0.00977 0.02735 0.01182 0.00080 0.00039 0.00040 0.00000 0.00297 0.00252 0.00301 0.00218 0.00235 0.00217 0.00116 C9 0.16756 0.26814 -0.03776 1.00000 0.02381 0.02648 0.04341 0.00734 0.00396 0.00324 0.03288 0.01231 0.00079 0.00042 0.00044 0.00000 0.00282 0.00281 0.00346 0.00244 0.00243 0.00219 0.00127 H9 0.05966 0.21092 -0.07961 1.00000 0.03945 0.00000 0.00000 C10 0.13368 0.34222 0.04279 1.00000 0.02158 0.02851 0.03202 0.00688 0.00344 0.01085 0.02732 0.01144 0.00076 0.00040 0.00039 0.00000 0.00262 0.00273 0.00298 0.00226 0.00221 0.00215 0.00115 H10 0.00247 0.33566 0.05631 1.00000 0.03278 0.00000 0.00000 C11 0.29083 0.42677 0.10461 1.00000 0.02302 0.02194 0.02520 0.01050 0.00266 0.01103 0.02196 0.01095 0.00072 0.00037 0.00037 0.00000 0.00257 0.00248 0.00268 0.00205 0.00205 0.00202 0.00105 C12 0.48335 0.43524 0.08573 1.00000 0.02785 0.02170 0.02709 0.01052 0.00411 0.00696 0.02500 0.01160 0.00077 0.00039 0.00039 0.00000 0.00276 0.00252 0.00280 0.00212 0.00220 0.00209 0.00110 H12 0.59129 0.49208 0.12805 1.00000 0.03000 0.00000 0.00000 C13 0.51694 0.36010 0.00459 1.00000 0.02822 0.01913 0.03873 0.00959 0.01315 0.00832 0.02779 0.01182 0.00079 0.00038 0.00041 0.00000 0.00282 0.00247 0.00321 0.00222 0.00238 0.00211 0.00117 H13 0.64840 0.36561 -0.00820 1.00000 0.03335 0.00000 0.00000 C14 0.25604 0.50830 0.19057 1.00000 0.02184 0.01800 0.03275 0.00762 0.00741 0.01093 0.02310 0.01115 0.00072 0.00037 0.00039 0.00000 0.00254 0.00237 0.00293 0.00208 0.00217 0.00198 0.00107 C15 0.35308 0.53742 0.28393 1.00000 0.03077 0.01607 0.02737 0.00647 0.01107 0.00782 0.02419 0.01124 0.00077 0.00037 0.00038 0.00000 0.00280 0.00233 0.00282 0.00202 0.00223 0.00204 0.00109 C16 0.49341 0.48341 0.31667 1.00000 0.03593 0.01955 0.02142 0.00962 0.00449 0.00904 0.02477 0.01119 0.00078 0.00037 0.00037 0.00000 0.00298 0.00246 0.00263 0.00203 0.00222 0.00216 0.00111 C17 0.43158 0.37387 0.30116 1.00000 0.03240 0.01565 0.02906 0.00762 0.00453 0.00712 0.02558 0.01146 0.00080 0.00037 0.00038 0.00000 0.00291 0.00237 0.00286 0.00206 0.00227 0.00208 0.00112 H17 0.29785 0.33525 0.27115 1.00000 0.03070 0.00000 0.00000 C18 0.74276 0.37547 0.36854 1.00000 0.03184 0.03501 0.03490 0.01781 -0.00382 0.00907 0.03319 0.01213 0.00083 0.00043 0.00042 0.00000 0.00308 0.00310 0.00323 0.00254 0.00250 0.00247 0.00129 H18 0.83080 0.33782 0.38512 1.00000 0.03983 0.00000 0.00000 C19 0.81369 0.48382 0.38799 1.00000 0.03930 0.04399 0.04702 0.02559 -0.01118 0.00420 0.04373 0.01390 0.00094 0.00049 0.00048 0.00000 0.00349 0.00358 0.00380 0.00299 0.00290 0.00275 0.00156 H19 0.94791 0.52066 0.41846 1.00000 0.05248 0.00000 0.00000 C20 0.68651 0.53800 0.36248 1.00000 0.03621 0.02421 0.03977 0.01615 -0.00539 -0.00221 0.03494 0.01208 0.00084 0.00043 0.00044 0.00000 0.00320 0.00279 0.00337 0.00247 0.00259 0.00232 0.00134 H20 0.73212 0.61309 0.37652 1.00000 0.04193 0.00000 0.00000 N1 0.54404 -0.11545 -0.32005 1.00000 0.02100 0.01732 0.02795 0.00640 -0.00315 0.00746 0.02237 0.00860 0.00058 0.00031 0.00030 0.00000 0.00214 0.00201 0.00239 0.00175 0.00178 0.00166 0.00091 H1N 0.51541 -0.18275 -0.32226 1.00000 0.02684 0.00000 0.00000 N2 0.55416 0.32125 0.32709 1.00000 0.04162 0.01974 0.02976 0.01045 0.00341 0.01234 0.02932 0.00990 0.00069 0.00032 0.00033 0.00000 0.00276 0.00216 0.00249 0.00185 0.00206 0.00196 0.00102 Br1 0.64093 0.13354 -0.02404 1.00000 0.03060 0.02442 0.02593 0.01033 -0.00075 0.01093 0.02627 0.00112 0.00008 0.00004 0.00004 0.00000 0.00028 0.00026 0.00027 0.00020 0.00021 0.00021 0.00013 Br2 0.24664 0.19033 -0.27146 1.00000 0.03447 0.03458 0.02753 0.01117 0.00073 0.02035 0.03023 0.00121 0.00008 0.00004 0.00004 0.00000 0.00030 0.00030 0.00029 0.00023 0.00022 0.00024 0.00014 Br3 0.06715 0.57628 0.15611 1.00000 0.03242 0.03792 0.04066 0.01630 0.01099 0.02373 0.03326 0.00133 0.00008 0.00004 0.00004 0.00000 0.00030 0.00031 0.00033 0.00025 0.00024 0.00024 0.00015 Br4 0.31805 0.65055 0.38752 1.00000 0.05522 0.02158 0.03239 0.00709 0.01657 0.01374 0.03555 0.00130 0.00009 0.00004 0.00004 0.00000 0.00038 0.00027 0.00031 0.00022 0.00026 0.00024 0.00016 Br5 0.96615 0.19698 0.49223 1.00000 0.03626 0.02957 0.03258 0.00905 0.00900 0.01302 0.03206 0.00125 0.00008 0.00004 0.00004 0.00000 0.00031 0.00028 0.00031 0.00023 0.00024 0.00023 0.00015 Br6 0.98281 0.13631 0.29953 1.00000 0.02204 0.03003 0.03531 0.01190 0.00130 0.01184 0.02819 0.00115 0.00007 0.00004 0.00004 0.00000 0.00026 0.00028 0.00030 0.00023 0.00021 0.00021 0.00014 Br7 1.00466 0.07392 0.12145 1.00000 0.06553 0.08369 0.03004 0.01783 0.00327 0.04398 0.05583 0.00174 0.00011 0.00006 0.00005 0.00000 0.00047 0.00053 0.00034 0.00033 0.00031 0.00041 0.00021 Final Structure Factor Calculation for 2006cgl0741 in P-1 Total number of l.s. parameters = 263 Maximum vector length = 511 Memory required = 2631 / 22995 wR2 = 0.0895 before cycle 7 for 5676 data and 0 / 263 parameters GooF = S = 1.020; Restrained GooF = 1.020 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0313 * P )^2 + 3.89 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0402 for 4147 Fo > 4sig(Fo) and 0.0710 for all 5676 data wR2 = 0.0895, GooF = S = 1.020, Restrained GooF = 1.020 for all data Occupancy sum of asymmetric unit = 29.00 for non-hydrogen and 13.00 for hydrogen atoms Principal mean square atomic displacements U 0.0338 0.0222 0.0173 C1 0.0294 0.0232 0.0188 C2 0.0382 0.0227 0.0189 C3 0.0371 0.0283 0.0215 C4 0.0426 0.0263 0.0208 C5 0.0389 0.0271 0.0234 C6 0.0374 0.0275 0.0233 C7 0.0360 0.0277 0.0183 C8 0.0460 0.0308 0.0218 C9 0.0353 0.0281 0.0185 C10 0.0264 0.0261 0.0134 C11 0.0290 0.0270 0.0190 C12 0.0423 0.0229 0.0181 C13 0.0334 0.0236 0.0122 C14 0.0354 0.0219 0.0153 C15 0.0362 0.0229 0.0152 C16 0.0329 0.0292 0.0147 C17 0.0477 0.0334 0.0185 C18 0.0735 0.0364 0.0213 C19 0.0580 0.0284 0.0184 C20 0.0346 0.0191 0.0134 N1 0.0429 0.0298 0.0153 N2 0.0357 0.0267 0.0164 Br1 0.0449 0.0300 0.0157 Br2 0.0471 0.0370 0.0157 Br3 0.0579 0.0295 0.0192 Br4 0.0376 0.0326 0.0260 Br5 0.0371 0.0309 0.0166 Br6 0.0978 0.0445 0.0252 Br7 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.012 0.023 0.035 0.048 0.063 0.080 0.101 0.132 0.188 1.000 Number in group 587. 578. 567. 541. 571. 580. 573. 546. 566. 567. GooF 0.913 0.996 1.063 1.066 1.019 1.056 1.056 0.980 1.032 1.012 K 2.359 1.113 1.100 1.005 1.004 0.985 1.000 1.000 1.005 1.005 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.32 1.66 inf Number in group 590. 545. 574. 566. 562. 577. 560. 570. 562. 570. GooF 1.055 0.966 0.995 1.000 1.019 0.902 0.910 0.924 0.989 1.359 K 1.010 1.023 1.014 0.994 1.005 1.011 1.010 1.017 1.012 0.994 R1 0.213 0.163 0.143 0.112 0.075 0.058 0.041 0.035 0.031 0.027 Recommended weighting scheme: WGHT 0.0315 3.7904 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) 0 -14 4 331.35 606.47 5.32 0.064 0.94 -1 1 0 396.44 149.40 5.18 0.032 6.80 -1 0 1 160.62 4.65 4.87 0.006 6.48 -1 -5 2 51.76 172.33 4.53 0.034 2.28 -1 1 17 -121.30 381.01 4.38 0.050 0.78 0 -3 2 1362.53 1828.27 4.32 0.110 4.18 1 -2 3 490.20 308.24 4.15 0.045 3.69 -4 -7 12 194.03 524.13 4.15 0.059 0.93 0 -4 5 2835.75 3503.30 4.02 0.153 2.45 -9 7 2 4111.49 524.58 3.97 0.059 0.77 -4 -7 13 1588.68 2226.20 3.92 0.122 0.89 2 -4 3 563.18 373.08 3.83 0.050 2.47 -1 -1 4 238.56 122.25 3.75 0.029 3.25 -3 9 8 1448.17 1876.18 3.73 0.112 0.97 -7 10 3 485.93 1127.57 3.71 0.087 0.87 8 -11 4 206.02 760.16 3.63 0.071 0.78 -5 12 1 38.53 254.78 3.59 0.041 0.96 2 -2 3 1398.97 1747.81 3.48 0.108 2.69 -6 -9 1 335.34 0.97 3.48 0.003 0.78 0 -3 4 3042.29 3824.71 3.42 0.160 3.13 1 -1 2 3111.59 3712.08 3.34 0.157 4.75 -2 -8 11 12.98 213.17 3.32 0.038 1.07 -5 7 0 158.74 25.57 3.30 0.013 1.26 0 -4 3 20172.80 24479.80 3.30 0.404 3.05 1 0 0 3393.70 2791.53 3.29 0.136 6.73 -8 -3 1 1346.34 764.63 3.28 0.071 0.79 -1 -6 17 1097.52 204.14 3.27 0.037 0.83 -8 10 5 -98.92 906.56 3.27 0.078 0.77 1 -3 4 369.76 537.37 3.25 0.060 2.90 4 3 0 325.17 187.03 3.21 0.035 1.43 -3 -3 1 190.51 94.76 3.19 0.025 1.83 2 -1 2 94.92 30.54 3.15 0.014 3.00 1 -3 1 1166.15 932.04 3.15 0.079 4.18 1 3 3 2096.53 1737.45 3.14 0.108 2.26 -8 5 3 1746.61 0.20 3.09 0.001 0.87 -7 0 10 -30.00 155.44 3.08 0.032 0.85 2 -6 2 317.74 205.36 3.06 0.037 2.09 0 3 2 692.89 895.25 3.05 0.077 3.13 0 5 6 2472.98 2075.47 3.04 0.118 1.45 7 -7 7 957.79 1356.36 3.03 0.095 0.86 -1 -14 5 3497.41 4913.87 2.99 0.181 0.90 5 -5 6 344.02 533.34 2.98 0.060 1.16 4 4 8 346.00 99.63 2.97 0.026 0.93 1 11 4 3919.24 3244.06 2.92 0.147 0.94 -1 -4 17 3342.91 2501.39 2.91 0.129 0.83 4 -5 14 2069.56 2965.21 2.89 0.141 0.84 0 -1 3 105.33 45.48 2.88 0.017 4.68 -4 -2 6 571.76 755.65 2.87 0.071 1.42 -3 -1 6 9.48 94.52 2.83 0.025 1.73 3 12 0 503.68 106.99 2.81 0.027 0.86 Bond lengths and angles C1 - Distance Angles C2 1.3802 (0.0067) C5 1.3887 (0.0075) 117.41 (0.47) C6 1.4894 (0.0074) 118.72 (0.48) 123.77 (0.45) C1 - C2 C5 C2 - Distance Angles N1 1.3251 (0.0062) C1 1.3802 (0.0067) 120.86 (0.49) H2 0.9500 119.57 119.57 C2 - N1 C1 C3 - Distance Angles N1 1.3282 (0.0067) C4 1.3760 (0.0073) 120.34 (0.47) H3 0.9500 119.83 119.83 C3 - N1 C4 C4 - Distance Angles C3 1.3760 (0.0073) C5 1.3939 (0.0075) 117.96 (0.52) H4 0.9500 121.02 121.02 C4 - C3 C5 C5 - Distance Angles C1 1.3887 (0.0075) C4 1.3939 (0.0075) 120.76 (0.49) H5 0.9500 119.62 119.62 C5 - C1 C4 C6 - Distance Angles C7 1.3106 (0.0075) C1 1.4894 (0.0074) 126.58 (0.53) Br1 1.9091 (0.0056) 120.56 (0.45) 112.83 (0.36) C6 - C7 C1 C7 - Distance Angles C6 1.3106 (0.0075) C8 1.4846 (0.0073) 126.75 (0.53) Br2 1.9179 (0.0055) 119.08 (0.44) 114.16 (0.37) C7 - C6 C8 C8 - Distance Angles C13 1.3918 (0.0073) C9 1.3931 (0.0074) 119.44 (0.47) C7 1.4846 (0.0073) 120.76 (0.48) 119.79 (0.47) C8 - C13 C9 C9 - Distance Angles C10 1.3781 (0.0074) C8 1.3931 (0.0074) 120.23 (0.49) H9 0.9500 119.89 119.89 C9 - C10 C8 C10 - Distance Angles C9 1.3781 (0.0074) C11 1.3951 (0.0069) 120.42 (0.49) H10 0.9500 119.79 119.79 C10 - C9 C11 C11 - Distance Angles C12 1.3913 (0.0070) C10 1.3951 (0.0069) 119.72 (0.45) C14 1.4852 (0.0067) 119.27 (0.44) 121.01 (0.45) C11 - C12 C10 C12 - Distance Angles C13 1.3905 (0.0070) C11 1.3913 (0.0070) 119.66 (0.47) H12 0.9500 120.17 120.17 C12 - C13 C11 C13 - Distance Angles C12 1.3905 (0.0070) C8 1.3918 (0.0072) 120.52 (0.49) H13 0.9500 119.74 119.74 C13 - C12 C8 C14 - Distance Angles C15 1.3305 (0.0071) C11 1.4852 (0.0067) 124.47 (0.43) Br3 1.9017 (0.0047) 121.08 (0.36) 114.36 (0.35) C14 - C15 C11 C15 - Distance Angles C14 1.3305 (0.0071) C16 1.4843 (0.0069) 123.58 (0.43) Br4 1.8908 (0.0047) 122.24 (0.37) 114.17 (0.36) C15 - C14 C16 C16 - Distance Angles C20 1.3765 (0.0074) C17 1.3947 (0.0066) 117.75 (0.47) C15 1.4843 (0.0069) 122.11 (0.45) 120.14 (0.47) C16 - C20 C17 C17 - Distance Angles N2 1.3388 (0.0064) C16 1.3947 (0.0066) 122.28 (0.49) H17 0.9500 118.86 118.86 C17 - N2 C16 C18 - Distance Angles N2 1.3367 (0.0069) C19 1.3745 (0.0080) 122.27 (0.51) H18 0.9500 118.86 118.86 C18 - N2 C19 C19 - Distance Angles C18 1.3745 (0.0080) C20 1.3776 (0.0081) 118.75 (0.55) H19 0.9500 120.62 120.62 C19 - C18 C20 C20 - Distance Angles C16 1.3765 (0.0074) C19 1.3776 (0.0081) 120.06 (0.51) H20 0.9500 119.97 119.97 C20 - C16 C19 N1 - Distance Angles C2 1.3251 (0.0062) C3 1.3282 (0.0067) 122.57 (0.43) H1N 0.8800 118.72 118.71 N1 - C2 C3 N2 - Distance Angles C18 1.3367 (0.0069) C17 1.3388 (0.0064) 118.83 (0.44) N2 - C18 Br1 - Distance Angles C6 1.9091 (0.0056) Br1 - Br2 - Distance Angles C7 1.9179 (0.0055) Br2 - Br3 - Distance Angles C14 1.9017 (0.0047) Br3 - Br4 - Distance Angles C15 1.8908 (0.0047) Br4 - Br5 - Distance Angles Br6 2.6367 (0.0008) Br5 - Br6 - Distance Angles Br7 2.4518 (0.0009) Br5 2.6367 (0.0008) 177.52 (0.03) Br6 - Br7 Br7 - Distance Angles Br6 2.4518 (0.0009) Br7 - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.88 1.81 2.689(6) 177.6 N1-H1N...N2_$1 FMAP and GRID set by program FMAP 2 1 20 GRID -2.941 -2 -2 2.941 2 2 R1 = 0.0694 for 5676 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 1.35 at 0.0390 0.5949 0.7641 [ 2.45 A from C14 ] Deepest hole -1.25 at 0.4162 0.6604 0.4182 [ 0.74 A from BR4 ] Mean = 0.00, Rms deviation from mean = 0.15 e/A^3, Highest memory used = 2887 / 28153 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.0390 0.4051 0.2359 1.00000 0.05 1.35 2.45 C14 2.52 H10 2.55 C19 2.59 C18 Q2 1 0.1783 0.6262 0.3604 1.00000 0.05 1.21 0.96 BR4 2.10 C15 2.26 H19 2.68 C14 Q3 1 0.9770 0.1788 0.3581 1.00000 0.05 0.93 0.88 BR6 1.85 BR5 2.57 H18 3.12 H3 Q4 1 0.9709 0.1224 0.1474 1.00000 0.05 0.75 0.77 BR7 2.09 BR6 3.11 H2 3.15 H17 Q5 1 0.4677 0.1846 -0.0963 1.00000 0.05 0.75 0.94 C7 0.95 C6 1.62 C8 1.90 BR1 Shortest distances between peaks (including symmetry equivalents) 3 4 2.85 1 2 2.96 Time profile in seconds ----------------------- 0.01: 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 0.01: Analyse other restraints etc. 0.65: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 1.89: Structure factors and derivatives 4.41: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.01: Apply other restraints 0.31: Solve l.s. equations 0.00: Generate HTAB table 0.01: Other dependent quantities, CIF, tables 0.16: Analysis of variance 0.05: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.05: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2006cgl0741 finished at 16:00:19 Total CPU time: 7.5 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++