+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2007jmw0004 started at 10:51:22 on 27-Feb-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2007jmw0004 in P2(1)/c CELL 0.71073 15.0606 14.3262 8.1711 90.000 90.000 90.000 ZERR 8.00 0.0007 0.0007 0.0005 0.000 0.000 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H CL N UNIT 72 72 8 16 V = 1763.01 F(000) = 752.0 Mu = 0.37 mm-1 Cell Wt = 1445.06 Rho = 1.361 MERG 2 OMIT -3.00 55.00 OMIT 3 5 0 TWIN 1.00 0.00 0.00 0.00 -1.00 0.00 0.00 0.00 -1.00 2 FMAP 2 PLAN 5 SIZE 0.02 0.08 0.12 ACTA BOND $H L.S. 12 TEMP -153.00 WGHT 0.0384 3.1567 BASF 0.51423 FVAR 0.58345 MOLE 1 C1 1 0.419633 0.163447 0.553342 11.00000 0.01382 0.02724 = 0.03287 0.00339 0.00088 0.00076 C2 1 0.506906 0.153037 0.621254 11.00000 0.02035 0.02087 = 0.03527 0.00126 0.00570 -0.00270 C3 1 0.548437 0.173230 0.771926 11.00000 0.01694 0.02797 = 0.03542 -0.00087 -0.00366 -0.00244 AFIX 43 H3 2 0.516279 0.200375 0.859897 11.00000 -1.20000 AFIX 0 C4 1 0.637031 0.152219 0.786787 11.00000 0.02322 0.03547 = 0.03519 0.00513 -0.00434 -0.00348 AFIX 43 H4 2 0.666363 0.164289 0.887517 11.00000 -1.20000 AFIX 0 C5 1 0.685221 0.113336 0.656614 11.00000 0.01927 0.03403 = 0.04997 0.00536 0.00203 0.00188 AFIX 43 H5 2 0.746603 0.100562 0.671306 11.00000 -1.20000 AFIX 0 C6 1 0.646409 0.093112 0.508339 11.00000 0.02279 0.02960 = 0.03865 0.00055 0.00523 0.00232 AFIX 43 H6 2 0.679404 0.066550 0.420876 11.00000 -1.20000 AFIX 0 C7 1 0.556372 0.113495 0.492772 11.00000 0.02850 0.02222 = 0.03020 0.00814 0.00161 -0.00283 C8 1 0.339713 0.202020 0.633841 11.00000 0.02017 0.03176 = 0.02592 -0.00114 -0.00212 0.00001 AFIX 23 H8A 2 0.292342 0.210946 0.551312 11.00000 -1.20000 H8B 2 0.354000 0.263758 0.681479 11.00000 -1.20000 AFIX 0 C9 1 0.519005 0.073835 0.199279 11.00000 0.03446 0.03792 = 0.03271 -0.00300 -0.00049 0.00391 AFIX 137 H9A 2 0.526756 0.129138 0.130149 11.00000 -1.50000 H9B 2 0.469776 0.036113 0.157124 11.00000 -1.50000 H9C 2 0.573669 0.036731 0.198216 11.00000 -1.50000 AFIX 0 C10 1 -0.079427 0.164152 0.382436 11.00000 0.01947 0.02806 = 0.02512 -0.00289 0.00280 -0.00035 C11 1 0.007222 0.154219 0.316205 11.00000 0.02189 0.02137 = 0.02218 -0.00319 -0.00432 0.00051 C12 1 0.046764 0.169428 0.163777 11.00000 0.02914 0.02656 = 0.02587 -0.00301 -0.00125 0.00324 AFIX 43 H12 2 0.013702 0.194581 0.075127 11.00000 -1.20000 AFIX 0 C13 1 0.135358 0.146775 0.145976 11.00000 0.02746 0.03444 = 0.03449 -0.00293 0.01279 -0.00225 AFIX 43 H13 2 0.163404 0.155621 0.042999 11.00000 -1.20000 AFIX 0 C14 1 0.185184 0.110525 0.278834 11.00000 0.02296 0.02962 = 0.04604 -0.00459 0.00341 -0.00189 AFIX 43 H14 2 0.246263 0.096700 0.262838 11.00000 -1.20000 AFIX 0 C15 1 0.148322 0.094851 0.428825 11.00000 0.02230 0.02302 = 0.04092 -0.00873 -0.01048 0.00209 AFIX 43 H15 2 0.182214 0.070040 0.516704 11.00000 -1.20000 AFIX 0 C16 1 0.057650 0.117109 0.447693 11.00000 0.02090 0.02313 = 0.02427 -0.00176 -0.00087 -0.00071 C17 1 -0.161318 0.200305 0.302309 11.00000 0.01796 0.02969 = 0.03746 0.00306 -0.00676 0.00333 AFIX 23 H17A 2 -0.149129 0.262122 0.253034 11.00000 -1.20000 H17B 2 -0.208766 0.208024 0.385062 11.00000 -1.20000 AFIX 0 C18 1 0.023668 0.083410 0.742026 11.00000 0.04339 0.04030 = 0.01690 -0.00185 -0.00411 0.00288 AFIX 137 H18A 2 0.058585 0.025687 0.742477 11.00000 -1.50000 H18B 2 -0.031127 0.073959 0.804555 11.00000 -1.50000 H18C 2 0.058369 0.133757 0.792042 11.00000 -1.50000 AFIX 0 CL1 3 0.300059 0.125262 0.793383 11.00000 0.02753 0.04171 = 0.03658 0.00197 0.00860 0.00108 CL2 3 -0.198133 0.119362 0.143865 11.00000 0.02778 0.04839 = 0.03933 0.00076 -0.00936 -0.00031 N1 4 0.499613 0.102550 0.364519 11.00000 0.02059 0.02628 = 0.02999 0.00084 0.00082 -0.00123 N2 4 0.416245 0.134009 0.400231 11.00000 0.02491 0.02406 = 0.02839 0.00204 -0.00003 0.00349 N3 4 0.001899 0.108120 0.576087 11.00000 0.03299 0.02874 = 0.02629 -0.00237 -0.00330 0.00497 N4 4 -0.081834 0.137496 0.536312 11.00000 0.02037 0.02865 = 0.03398 -0.00125 0.00460 0.00221 HKLF 4 Covalent radii and connectivity table for 2007jmw0004 in P2(1)/c C 0.770 H 0.320 CL 0.990 N 0.700 C1 - N2 C2 C8 C2 - C7 C3 C1 C3 - C4 C2 C4 - C3 C5 C5 - C6 C4 C6 - C5 C7 C7 - N1 C6 C2 C8 - C1 Cl1 C9 - N1 C10 - N4 C11 C17 C11 - C12 C16 C10 C12 - C13 C11 C13 - C12 C14 C14 - C15 C13 C15 - C14 C16 C16 - N3 C15 C11 C17 - C10 Cl2 C18 - N3 Cl1 - C8 Cl2 - C17 N1 - C7 N2 C9 N2 - C1 N1 N3 - C16 N4 C18 N4 - C10 N3 13946 Reflections read, of which 5 rejected -17 =< h =< 19, -18 =< k =< 18, -10 =< l =< 10, 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) -10 11 2 21.20 1.46 3 8.90 4 11 3 8.66 0.85 6 5.99 2 Inconsistent equivalents 3840 Unique reflections, of which 0 suppressed R(int) = 0.0723 R(sigma) = 0.0725 Friedel opposites merged Maximum memory for data reduction = 2167 / 39553 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 = 2780 / 272585 wR2 = 0.1497 before cycle 1 for 3840 data and 220 / 220 parameters GooF = S = 1.057; Restrained GooF = 1.057 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0384 * P )^2 + 3.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.58406 0.00141 0.434 OSF 2 0.51454 0.00230 0.135 BASF 1 Mean shift/esd = 0.042 Maximum = 0.434 for OSF Max. shift = 0.004 A for H18A Max. dU = 0.000 for Cl1 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2780 / 272585 wR2 = 0.1497 before cycle 2 for 3840 data and 220 / 220 parameters GooF = S = 1.057; Restrained GooF = 1.057 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0384 * P )^2 + 3.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.58418 0.00141 0.080 OSF 2 0.51466 0.00230 0.050 BASF 1 Mean shift/esd = 0.019 Maximum = -0.088 for tors H18A Max. shift = 0.003 A for H18A Max. dU = 0.000 for C2 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2780 / 272585 wR2 = 0.1497 before cycle 3 for 3840 data and 220 / 220 parameters GooF = S = 1.057; Restrained GooF = 1.057 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0384 * P )^2 + 3.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.58419 0.00141 0.008 OSF 2 0.51466 0.00230 0.003 BASF 1 Mean shift/esd = 0.009 Maximum = -0.060 for U33 C11 Max. shift = 0.001 A for H18B Max. dU = 0.000 for C2 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2780 / 272585 wR2 = 0.1497 before cycle 4 for 3840 data and 220 / 220 parameters GooF = S = 1.057; Restrained GooF = 1.057 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0384 * P )^2 + 3.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.58419 0.00141 0.003 OSF 2 0.51466 0.00230 0.001 BASF 1 Mean shift/esd = 0.008 Maximum = -0.058 for U33 C11 Max. shift = 0.001 A for H18C Max. dU = 0.000 for C2 Least-squares cycle 5 Maximum vector length = 511 Memory required = 2780 / 272585 wR2 = 0.1497 before cycle 5 for 3840 data and 220 / 220 parameters GooF = S = 1.057; Restrained GooF = 1.057 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0384 * P )^2 + 3.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.58419 0.00141 0.000 OSF 2 0.51466 0.00230 0.001 BASF 1 Mean shift/esd = 0.007 Maximum = -0.052 for U33 C11 Max. shift = 0.001 A for H18C Max. dU = 0.000 for C2 Least-squares cycle 6 Maximum vector length = 511 Memory required = 2780 / 272585 wR2 = 0.1497 before cycle 6 for 3840 data and 220 / 220 parameters GooF = S = 1.057; Restrained GooF = 1.057 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0384 * P )^2 + 3.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.58419 0.00141 0.002 OSF 2 0.51467 0.00230 0.000 BASF 1 Mean shift/esd = 0.006 Maximum = -0.047 for U33 C11 Max. shift = 0.000 A for H18C Max. dU = 0.000 for C2 Least-squares cycle 7 Maximum vector length = 511 Memory required = 2780 / 272585 wR2 = 0.1497 before cycle 7 for 3840 data and 220 / 220 parameters GooF = S = 1.057; Restrained GooF = 1.057 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0384 * P )^2 + 3.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.58420 0.00141 0.002 OSF 2 0.51467 0.00230 0.000 BASF 1 Mean shift/esd = 0.006 Maximum = -0.043 for U33 C11 Max. shift = 0.000 A for H18C Max. dU = 0.000 for C2 Least-squares cycle 8 Maximum vector length = 511 Memory required = 2780 / 272585 wR2 = 0.1497 before cycle 8 for 3840 data and 220 / 220 parameters GooF = S = 1.057; Restrained GooF = 1.057 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0384 * P )^2 + 3.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.58420 0.00141 0.001 OSF 2 0.51467 0.00230 0.000 BASF 1 Mean shift/esd = 0.005 Maximum = -0.039 for U33 C11 Max. shift = 0.000 A for H18C Max. dU = 0.000 for C2 Least-squares cycle 9 Maximum vector length = 511 Memory required = 2780 / 272585 wR2 = 0.1497 before cycle 9 for 3840 data and 220 / 220 parameters GooF = S = 1.057; Restrained GooF = 1.057 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0384 * P )^2 + 3.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.58420 0.00141 0.001 OSF 2 0.51467 0.00230 0.000 BASF 1 Mean shift/esd = 0.005 Maximum = -0.036 for U33 C11 Max. shift = 0.000 A for H18C Max. dU = 0.000 for C2 Least-squares cycle 10 Maximum vector length = 511 Memory required = 2780 / 272585 wR2 = 0.1497 before cycle 10 for 3840 data and 220 / 220 parameters GooF = S = 1.057; Restrained GooF = 1.057 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0384 * P )^2 + 3.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.58420 0.00141 0.001 OSF 2 0.51467 0.00230 0.000 BASF 1 Mean shift/esd = 0.004 Maximum = -0.033 for U33 C11 Max. shift = 0.000 A for H18C Max. dU = 0.000 for C2 Least-squares cycle 11 Maximum vector length = 511 Memory required = 2780 / 272585 wR2 = 0.1497 before cycle 11 for 3840 data and 220 / 220 parameters GooF = S = 1.057; Restrained GooF = 1.057 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0384 * P )^2 + 3.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.58420 0.00141 0.002 OSF 2 0.51467 0.00230 0.000 BASF 1 Mean shift/esd = 0.004 Maximum = -0.031 for U33 C11 Max. shift = 0.000 A for H18C Max. dU = 0.000 for C2 Least-squares cycle 12 Maximum vector length = 511 Memory required = 2780 / 272585 wR2 = 0.1497 before cycle 12 for 3840 data and 220 / 220 parameters GooF = S = 1.057; Restrained GooF = 1.057 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0384 * P )^2 + 3.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.58421 0.00141 0.001 OSF 2 0.51467 0.00230 0.000 BASF 1 Mean shift/esd = 0.004 Maximum = -0.029 for U33 C11 Max. shift = 0.000 A for H18C Max. dU = 0.000 for C2 Largest correlation matrix elements -0.520 U33 C10 / U33 C1 Idealized hydrogen atom generation before cycle 13 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H3 0.5163 0.2003 0.8601 43 0.950 0.000 C3 C4 C2 H4 0.6664 0.1644 0.8875 43 0.950 0.000 C4 C3 C5 H5 0.7466 0.1006 0.6713 43 0.950 0.000 C5 C6 C4 H6 0.6794 0.0665 0.4211 43 0.950 0.000 C6 C5 C7 H8A 0.2924 0.2110 0.5513 23 0.990 0.000 C8 C1 Cl1 H8B 0.3540 0.2638 0.6815 23 0.990 0.000 C8 C1 Cl1 H9A 0.5267 0.1292 0.1301 137 0.980 0.000 C9 N1 H9A H9B 0.4699 0.0360 0.1570 137 0.980 0.000 C9 N1 H9A H9C 0.5738 0.0369 0.1981 137 0.980 0.000 C9 N1 H9A H12 0.0137 0.1945 0.0753 43 0.950 0.000 C12 C13 C11 H13 0.1634 0.1557 0.0431 43 0.950 0.000 C13 C12 C14 H14 0.2462 0.0966 0.2629 43 0.950 0.000 C14 C15 C13 H15 0.1822 0.0700 0.5167 43 0.950 0.000 C15 C14 C16 H17A -0.1491 0.2622 0.2531 23 0.990 0.000 C17 C10 Cl2 H17B -0.2088 0.2081 0.3852 23 0.990 0.000 C17 C10 Cl2 H18A 0.0580 0.0253 0.7426 137 0.980 0.000 C18 N3 H18A H18B -0.0312 0.0746 0.8047 137 0.980 0.000 C18 N3 H18A H18C 0.0589 0.1335 0.7917 137 0.980 0.000 C18 N3 H18A 2007jmw0004 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.41963 0.16338 0.55348 1.00000 0.01391 0.02741 0.03213 0.00333 0.00080 0.00087 0.02448 0.00794 0.00029 0.00030 0.00060 0.00000 0.00190 0.00234 0.00312 0.00208 0.00187 0.00178 0.00104 C2 0.50694 0.15304 0.62134 1.00000 0.02000 0.02057 0.03699 0.00131 0.00573 -0.00269 0.02585 0.00802 0.00030 0.00029 0.00059 0.00000 0.00215 0.00202 0.00306 0.00189 0.00203 0.00182 0.00101 C3 0.54844 0.17319 0.77205 1.00000 0.01702 0.02822 0.03541 -0.00108 -0.00369 -0.00253 0.02688 0.00753 0.00028 0.00029 0.00062 0.00000 0.00210 0.00231 0.00308 0.00206 0.00195 0.00179 0.00104 H3 0.51626 0.20026 0.86006 1.00000 0.03226 0.00000 0.00000 C4 0.63704 0.15224 0.78685 1.00000 0.02306 0.03580 0.03491 0.00516 -0.00419 -0.00354 0.03126 0.00823 0.00029 0.00032 0.00063 0.00000 0.00246 0.00258 0.00316 0.00222 0.00212 0.00197 0.00112 H4 0.66640 0.16436 0.88754 1.00000 0.03751 0.00000 0.00000 C5 0.68522 0.11333 0.65662 1.00000 0.01919 0.03384 0.05011 0.00510 0.00174 0.00184 0.03438 0.00868 0.00033 0.00032 0.00066 0.00000 0.00253 0.00255 0.00337 0.00217 0.00227 0.00209 0.00123 H5 0.74661 0.10056 0.67129 1.00000 0.04125 0.00000 0.00000 C6 0.64643 0.09310 0.50849 1.00000 0.02265 0.02959 0.03931 0.00075 0.00537 0.00226 0.03052 0.00827 0.00029 0.00032 0.00064 0.00000 0.00232 0.00237 0.00320 0.00210 0.00209 0.00198 0.00108 H6 0.67942 0.06649 0.42106 1.00000 0.03662 0.00000 0.00000 C7 0.55635 0.11352 0.49286 1.00000 0.02801 0.02214 0.03137 0.00821 0.00163 -0.00273 0.02717 0.00841 0.00031 0.00031 0.00064 0.00000 0.00251 0.00225 0.00292 0.00191 0.00203 0.00188 0.00104 C8 0.33971 0.20204 0.63388 1.00000 0.02024 0.03171 0.02618 -0.00092 -0.00212 0.00000 0.02605 0.00796 0.00030 0.00031 0.00056 0.00000 0.00200 0.00237 0.00261 0.00183 0.00176 0.00188 0.00095 H8A 0.29235 0.21097 0.55133 1.00000 0.03126 0.00000 0.00000 H8B 0.35402 0.26378 0.68150 1.00000 0.03126 0.00000 0.00000 C9 0.51902 0.07386 0.19920 1.00000 0.03494 0.03804 0.03176 -0.00330 -0.00033 0.00391 0.03491 0.00855 0.00033 0.00035 0.00063 0.00000 0.00280 0.00275 0.00311 0.00224 0.00212 0.00215 0.00116 H9A 0.52667 0.12918 0.13007 1.00000 0.05237 0.00000 0.00000 H9B 0.46986 0.03604 0.15704 1.00000 0.05237 0.00000 0.00000 H9C 0.57375 0.03687 0.19813 1.00000 0.05237 0.00000 0.00000 C10 -0.07939 0.16415 0.38247 1.00000 0.01929 0.02776 0.02608 -0.00268 0.00256 -0.00055 0.02438 0.00783 0.00030 0.00030 0.00057 0.00000 0.00205 0.00227 0.00291 0.00201 0.00182 0.00183 0.00098 C11 0.00727 0.15421 0.31623 1.00000 0.02227 0.02153 0.02098 -0.00333 -0.00416 0.00063 0.02159 0.00722 0.00031 0.00028 0.00053 0.00000 0.00206 0.00199 0.00249 0.00171 0.00190 0.00179 0.00090 C12 0.04675 0.16940 0.16395 1.00000 0.02904 0.02657 0.02597 -0.00304 -0.00158 0.00337 0.02719 0.00788 0.00031 0.00030 0.00060 0.00000 0.00253 0.00231 0.00278 0.00183 0.00194 0.00196 0.00103 H12 0.01365 0.19451 0.07530 1.00000 0.03263 0.00000 0.00000 C13 0.13536 0.14682 0.14606 1.00000 0.02722 0.03436 0.03479 -0.00280 0.01289 -0.00238 0.03212 0.00852 0.00031 0.00032 0.00064 0.00000 0.00261 0.00246 0.00313 0.00209 0.00217 0.00210 0.00113 H13 0.16341 0.15574 0.04311 1.00000 0.03855 0.00000 0.00000 C14 0.18515 0.11051 0.27892 1.00000 0.02290 0.02954 0.04634 -0.00491 0.00310 -0.00177 0.03293 0.00817 0.00033 0.00030 0.00065 0.00000 0.00248 0.00235 0.00329 0.00211 0.00223 0.00192 0.00114 H14 0.24621 0.09664 0.26289 1.00000 0.03951 0.00000 0.00000 C15 0.14835 0.09483 0.42884 1.00000 0.02261 0.02321 0.04032 -0.00858 -0.01063 0.00207 0.02871 0.00744 0.00029 0.00030 0.00064 0.00000 0.00238 0.00214 0.00331 0.00202 0.00211 0.00192 0.00111 H15 0.18224 0.07002 0.51671 1.00000 0.03445 0.00000 0.00000 C16 0.05764 0.11712 0.44768 1.00000 0.02135 0.02318 0.02331 -0.00178 -0.00062 -0.00081 0.02261 0.00742 0.00029 0.00029 0.00055 0.00000 0.00223 0.00212 0.00273 0.00183 0.00174 0.00177 0.00095 C17 -0.16133 0.20035 0.30240 1.00000 0.01783 0.02967 0.03750 0.00297 -0.00671 0.00329 0.02833 0.00760 0.00030 0.00030 0.00061 0.00000 0.00197 0.00233 0.00296 0.00197 0.00188 0.00178 0.00101 H17A -0.14915 0.26217 0.25314 1.00000 0.03400 0.00000 0.00000 H17B -0.20876 0.20806 0.38518 1.00000 0.03400 0.00000 0.00000 C18 0.02365 0.08341 0.74202 1.00000 0.04300 0.03991 0.01838 -0.00221 -0.00389 0.00295 0.03376 0.00840 0.00034 0.00035 0.00060 0.00000 0.00301 0.00274 0.00271 0.00208 0.00213 0.00223 0.00116 H18A 0.05801 0.02532 0.74264 1.00000 0.05065 0.00000 0.00000 H18B -0.03118 0.07464 0.80475 1.00000 0.05065 0.00000 0.00000 H18C 0.05888 0.13346 0.79170 1.00000 0.05065 0.00000 0.00000 Cl1 0.30007 0.12526 0.79344 1.00000 0.02751 0.04178 0.03677 0.00194 0.00864 0.00106 0.03535 0.00227 0.00009 0.00008 0.00015 0.00000 0.00058 0.00064 0.00076 0.00054 0.00053 0.00052 0.00030 Cl2 -0.19814 0.11936 0.14391 1.00000 0.02779 0.04842 0.03957 0.00073 -0.00936 -0.00033 0.03859 0.00212 0.00009 0.00009 0.00015 0.00000 0.00060 0.00074 0.00080 0.00058 0.00055 0.00060 0.00033 N1 0.49958 0.10253 0.36440 1.00000 0.02028 0.02622 0.03092 0.00110 0.00051 -0.00126 0.02580 0.00669 0.00026 0.00025 0.00049 0.00000 0.00180 0.00189 0.00254 0.00161 0.00173 0.00159 0.00086 N2 0.41623 0.13404 0.40038 1.00000 0.02459 0.02403 0.02885 0.00219 -0.00010 0.00341 0.02582 0.00693 0.00025 0.00025 0.00051 0.00000 0.00195 0.00190 0.00243 0.00160 0.00166 0.00158 0.00086 N3 0.00197 0.10811 0.57595 1.00000 0.03341 0.02888 0.02559 -0.00225 -0.00328 0.00499 0.02929 0.00684 0.00029 0.00026 0.00049 0.00000 0.00214 0.00197 0.00235 0.00163 0.00184 0.00177 0.00088 N4 -0.08183 0.13748 0.53649 1.00000 0.02050 0.02891 0.03333 -0.00109 0.00438 0.00224 0.02758 0.00684 0.00026 0.00026 0.00051 0.00000 0.00185 0.00203 0.00268 0.00171 0.00176 0.00162 0.00092 Final Structure Factor Calculation for 2007jmw0004 in P2(1)/c Total number of l.s. parameters = 220 Maximum vector length = 511 Memory required = 2560 / 22995 wR2 = 0.1497 before cycle 13 for 3840 data and 0 / 220 parameters GooF = S = 1.057; Restrained GooF = 1.057 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0384 * P )^2 + 3.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0656 for 2872 Fo > 4sig(Fo) and 0.0958 for all 3840 data wR2 = 0.1497, GooF = S = 1.057, Restrained GooF = 1.057 for all data Occupancy sum of asymmetric unit = 24.00 for non-hydrogen and 18.00 for hydrogen atoms Principal mean square atomic displacements U 0.0339 0.0257 0.0138 C1 0.0388 0.0226 0.0162 C2 0.0362 0.0288 0.0157 C3 0.0421 0.0302 0.0215 C4 0.0517 0.0325 0.0189 C5 0.0411 0.0299 0.0206 C6 0.0362 0.0289 0.0165 C7 0.0319 0.0267 0.0196 C8 0.0416 0.0332 0.0299 C9 0.0301 0.0246 0.0184 C10 0.0272 0.0212 0.0164 C11 0.0328 0.0258 0.0229 C12 0.0456 0.0332 0.0176 C13 0.0481 0.0283 0.0223 C14 0.0483 0.0210 0.0168 C15 0.0250 0.0224 0.0204 C16 0.0399 0.0304 0.0147 C17 0.0455 0.0381 0.0176 C18 0.0441 0.0397 0.0223 Cl1 0.0486 0.0446 0.0226 Cl2 0.0312 0.0263 0.0200 N1 0.0300 0.0269 0.0205 N2 0.0379 0.0257 0.0243 N3 0.0347 0.0295 0.0186 N4 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.017 0.026 0.036 0.048 0.062 0.077 0.096 0.120 0.173 1.000 Number in group 408. 362. 388. 394. 393. 377. 369. 383. 386. 380. GooF 1.197 1.138 1.097 1.036 1.045 0.986 1.001 0.999 1.068 0.972 K 3.608 1.494 1.201 1.107 1.051 1.008 1.009 0.990 1.002 1.017 Resolution(A) 0.77 0.80 0.84 0.88 0.93 0.99 1.06 1.17 1.33 1.68 inf Number in group 391. 387. 381. 384. 384. 379. 381. 387. 380. 386. GooF 1.138 1.152 1.223 1.032 1.061 1.012 0.932 0.894 0.960 1.114 K 1.118 1.123 1.112 1.048 1.013 1.017 0.986 1.000 1.014 1.016 R1 0.260 0.208 0.186 0.124 0.121 0.082 0.062 0.050 0.047 0.037 Recommended weighting scheme: WGHT 0.0338 3.3052 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) 2 1 0 332.50 680.12 6.08 0.156 6.67 0 0 8 142.57 4.64 5.43 0.013 1.02 -10 9 5 63.29 270.24 4.21 0.098 0.91 0 3 9 83.62 2.95 3.87 0.010 0.89 0 12 0 745.39 500.25 3.67 0.134 1.19 -9 6 4 84.43 15.66 3.61 0.024 1.14 -11 3 5 90.98 194.34 3.57 0.083 1.03 -1 0 4 463.61 684.92 3.57 0.157 2.02 -5 17 1 130.00 13.40 3.53 0.022 0.81 10 8 1 99.23 205.14 3.49 0.086 1.14 1 3 0 24.10 0.05 3.38 0.001 4.55 -8 8 4 8.00 81.91 3.33 0.054 1.10 2 4 8 181.41 94.42 3.32 0.058 0.97 10 1 9 96.23 17.05 3.21 0.025 0.78 3 4 8 886.63 669.57 3.18 0.155 0.96 0 14 0 268.37 164.78 3.10 0.077 1.02 -1 10 7 516.17 360.13 3.10 0.114 0.90 9 4 8 61.17 4.15 3.05 0.012 0.85 9 2 1 592.32 441.00 3.05 0.126 1.60 -18 2 3 298.92 169.02 3.01 0.078 0.79 1 10 8 196.02 56.09 2.96 0.045 0.83 -1 1 10 88.11 24.26 2.93 0.029 0.81 12 6 6 62.41 4.99 2.89 0.013 0.86 15 6 5 199.84 106.10 2.86 0.062 0.81 8 2 1 737.39 575.84 2.83 0.144 1.78 5 14 4 -9.33 39.81 2.78 0.038 0.88 -2 7 5 216.89 331.92 2.77 0.109 1.26 15 9 4 -36.32 36.83 2.76 0.036 0.78 17 5 1 31.14 91.20 2.76 0.057 0.84 7 15 4 41.69 127.44 2.75 0.068 0.80 -6 15 3 103.52 41.21 2.73 0.038 0.85 -8 2 7 168.09 268.50 2.71 0.098 0.98 12 10 4 207.82 35.26 2.71 0.036 0.86 4 6 9 124.00 62.81 2.69 0.047 0.83 12 1 7 83.41 15.82 2.69 0.024 0.85 9 0 8 173.49 31.22 2.69 0.033 0.87 -17 3 4 105.33 195.98 2.67 0.084 0.80 -12 6 6 81.31 4.97 2.67 0.013 0.86 3 4 3 310.26 214.26 2.67 0.088 1.99 10 10 5 473.96 326.16 2.66 0.108 0.88 -9 2 1 551.86 419.04 2.65 0.122 1.60 1 1 10 108.31 22.93 2.65 0.029 0.81 -13 7 3 98.30 23.57 2.62 0.029 0.95 6 2 9 111.63 51.11 2.61 0.043 0.85 -7 17 1 -10.64 64.55 2.58 0.048 0.78 -12 8 5 -26.87 27.88 2.58 0.032 0.87 -5 3 4 78.45 132.30 2.56 0.069 1.59 3 5 3 1002.11 818.06 2.55 0.171 1.84 -13 8 3 0.15 68.87 2.54 0.050 0.92 -9 16 1 -45.56 40.00 2.53 0.038 0.79 Bond lengths and angles C1 - Distance Angles N2 1.3208 (0.0061) C2 1.4347 (0.0065) 111.64 (0.41) C8 1.4789 (0.0063) 120.55 (0.40) 127.80 (0.44) C1 - N2 C2 C2 - Distance Angles C7 1.4058 (0.0067) C3 1.4108 (0.0065) 119.98 (0.42) C1 1.4347 (0.0065) 103.78 (0.42) 136.23 (0.44) C2 - C7 C3 C3 - Distance Angles C4 1.3731 (0.0061) C2 1.4108 (0.0065) 117.56 (0.45) H3 0.9500 121.22 121.22 C3 - C4 C2 C4 - Distance Angles C3 1.3731 (0.0061) C5 1.4034 (0.0071) 121.50 (0.47) H4 0.9500 119.25 119.25 C4 - C3 C5 C5 - Distance Angles C6 1.3749 (0.0070) C4 1.4034 (0.0071) 122.11 (0.44) H5 0.9500 118.95 118.95 C5 - C6 C4 C6 - Distance Angles C5 1.3749 (0.0070) C7 1.3937 (0.0062) 116.75 (0.46) H6 0.9500 121.63 121.63 C6 - C5 C7 C7 - Distance Angles N1 1.3630 (0.0063) C6 1.3937 (0.0062) 131.07 (0.49) C2 1.4058 (0.0067) 106.83 (0.40) 122.10 (0.47) C7 - N1 C6 C8 - Distance Angles C1 1.4789 (0.0063) Cl1 1.8073 (0.0045) 111.19 (0.32) H8A 0.9900 109.40 109.40 H8B 0.9900 109.40 109.40 108.01 C8 - C1 Cl1 H8A C9 - Distance Angles N1 1.4410 (0.0064) H9A 0.9800 109.47 H9B 0.9800 109.47 109.47 H9C 0.9800 109.47 109.47 109.47 C9 - N1 H9A H9B C10 - Distance Angles N4 1.3158 (0.0060) C11 1.4201 (0.0061) 111.16 (0.40) C17 1.4899 (0.0061) 119.87 (0.41) 128.96 (0.43) C10 - N4 C11 C11 - Distance Angles C12 1.3962 (0.0065) C16 1.4183 (0.0061) 120.36 (0.43) C10 1.4201 (0.0061) 135.68 (0.42) 103.92 (0.38) C11 - C12 C16 C12 - Distance Angles C13 1.3809 (0.0063) C11 1.3962 (0.0065) 118.00 (0.44) H12 0.9500 121.00 121.00 C12 - C13 C11 C13 - Distance Angles C12 1.3809 (0.0063) C14 1.4182 (0.0072) 121.05 (0.44) H13 0.9500 119.47 119.47 C13 - C12 C14 C14 - Distance Angles C15 1.3632 (0.0071) C13 1.4182 (0.0072) 122.23 (0.44) H14 0.9500 118.88 118.88 C14 - C15 C13 C15 - Distance Angles C14 1.3632 (0.0071) C16 1.4113 (0.0060) 117.02 (0.43) H15 0.9500 121.49 121.49 C15 - C14 C16 C16 - Distance Angles N3 1.3484 (0.0062) C15 1.4113 (0.0060) 131.68 (0.44) C11 1.4183 (0.0061) 106.98 (0.39) 121.33 (0.42) C16 - N3 C15 C17 - Distance Angles C10 1.4899 (0.0061) Cl2 1.8251 (0.0047) 109.99 (0.31) H17A 0.9900 109.66 109.66 H17B 0.9900 109.66 109.66 108.17 C17 - C10 Cl2 H17A C18 - Distance Angles N3 1.4398 (0.0062) H18A 0.9800 109.47 H18B 0.9800 109.47 109.47 H18C 0.9800 109.47 109.47 109.47 C18 - N3 H18A H18B Cl1 - Distance Angles C8 1.8073 (0.0046) Cl1 - Cl2 - Distance Angles C17 1.8251 (0.0047) Cl2 - N1 - Distance Angles C7 1.3630 (0.0063) N2 1.3661 (0.0052) 111.87 (0.39) C9 1.4410 (0.0064) 128.82 (0.40) 118.85 (0.38) N1 - C7 N2 N2 - Distance Angles C1 1.3208 (0.0061) N1 1.3661 (0.0052) 105.86 (0.38) N2 - C1 N3 - Distance Angles C16 1.3484 (0.0062) N4 1.3689 (0.0055) 111.14 (0.38) C18 1.4398 (0.0062) 127.96 (0.42) 120.44 (0.41) N3 - C16 N4 N4 - Distance Angles C10 1.3158 (0.0060) N3 1.3689 (0.0055) 106.79 (0.37) N4 - C10 FMAP and GRID set by program FMAP 2 3 12 GRID -2.778 -2 -2 2.778 2 2 R1 = 0.0949 for 3840 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.46 at 0.7983 0.1227 0.0275 [ 0.95 A from CL2 ] Deepest hole -0.36 at 0.2719 0.3549 0.2500 [ 0.62 A from CL1 ] Mean = 0.00, Rms deviation from mean = 0.08 e/A^3, Highest memory used = 2920 / 22281 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.2017 0.1227 0.0275 1.00000 0.05 0.46 0.95 CL2 2.37 H4 2.58 C17 2.69 H17B Q2 1 -0.1978 0.1215 0.2738 1.00000 0.05 0.43 1.06 CL2 1.28 C17 1.55 H17B 2.08 C10 Q3 1 0.3075 0.1237 0.9097 1.00000 0.05 0.41 0.96 CL1 2.47 H13 2.56 C8 2.65 H8A Q4 1 0.2966 0.1191 0.6770 1.00000 0.05 0.39 0.96 CL1 1.40 C8 1.67 H8A 2.20 C1 Q5 1 0.4814 0.0980 0.1130 1.00000 0.05 0.32 0.83 H9A 0.97 C9 0.97 H9B 1.78 H9C Shortest distances between peaks (including symmetry equivalents) 3 4 1.91 1 2 2.01 Time profile in seconds ----------------------- 0.04: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.01: Generate connectivity array 0.00: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 0.52: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.05: Set up l.s. refinement 0.00: Generate idealized H-atoms 5.01: Structure factors and derivatives 3.74: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.38: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.10: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.01: Fourier summations 0.03: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2007jmw0004 finished at 10:51:31 Total CPU time: 9.2 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++