+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2007src1588 started at 17:06:20 on 23-Nov-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2007src1588 in C222(1) CELL 0.71073 7.4019 15.8155 26.8034 90.000 90.000 90.000 ZERR 8.00 0.0002 0.0003 0.0004 0.000 0.000 0.000 LATT -7 SYMM - X, - Y, 1/2 + Z SYMM - X, Y, 1/2 - Z SYMM X, - Y, - Z SFAC C H N O UNIT 136 168 8 32 V = 3137.73 F(000) = 1296.0 Mu = 0.09 mm-1 Cell Wt = 2426.78 Rho = 1.284 MERG 2 OMIT -3.00 55.00 OMIT 2 0 2 OMIT 2 0 3 OMIT 0 0 4 OMIT 1 1 0 FMAP 2 PLAN 20 BOND TEMP -153 SIZE 0.4 0.35 0.2 ACTA WGHT 0.04060 0.88710 L.S. 4 FVAR 0.19771 C1 1 0.068040 0.300010 0.002409 11.00000 0.02589 0.02315 = 0.02406 -0.00168 -0.00349 -0.00425 C2 1 -0.078653 0.408858 0.041231 11.00000 0.02832 0.02483 = 0.02932 -0.00256 -0.00368 0.00261 AFIX 23 H2A 2 -0.207743 0.399099 0.043612 11.00000 -1.20000 H2B 2 -0.055741 0.468984 0.044543 11.00000 -1.20000 AFIX 0 C3 1 0.022426 0.359162 0.081517 11.00000 0.02297 0.01548 = 0.02238 -0.00096 0.00201 0.00054 AFIX 13 H3 2 -0.062283 0.342141 0.107760 11.00000 -1.20000 AFIX 0 C4 1 0.185107 0.404597 0.105074 11.00000 0.02765 0.01840 = 0.01785 0.00075 -0.00131 -0.00249 AFIX 13 H4 2 0.243719 0.364496 0.127766 11.00000 -1.20000 AFIX 0 C5 1 0.325415 0.431152 0.066304 11.00000 0.03098 0.02967 = 0.02507 0.00411 -0.00180 -0.00965 AFIX 137 H5A 2 0.271036 0.469297 0.042838 11.00000 -1.50000 H5B 2 0.368904 0.382022 0.049036 11.00000 -1.50000 H5C 2 0.424457 0.458819 0.082682 11.00000 -1.50000 AFIX 0 C6 1 0.122299 0.480178 0.136390 11.00000 0.04307 0.02450 = 0.03206 -0.00910 -0.00230 -0.00103 AFIX 137 H6A 2 0.222190 0.501714 0.155374 11.00000 -1.50000 H6B 2 0.028082 0.462456 0.158673 11.00000 -1.50000 H6C 2 0.077289 0.523699 0.114738 11.00000 -1.50000 AFIX 0 C7 1 0.154140 0.211209 0.073759 11.00000 0.02102 0.01704 = 0.02186 -0.00133 0.00117 -0.00155 AFIX 13 H7 2 0.284659 0.213067 0.079799 11.00000 -1.20000 AFIX 0 C8 1 0.075572 0.126890 0.060652 11.00000 0.03341 0.01865 = 0.02482 -0.00393 0.00131 -0.00424 AFIX 23 H8A 2 0.157398 0.079133 0.058417 11.00000 -1.20000 H8B 2 -0.024343 0.125678 0.037246 11.00000 -1.20000 AFIX 0 C9 1 0.041592 0.164368 0.111587 11.00000 0.02417 0.01925 = 0.02331 -0.00151 0.00282 -0.00272 AFIX 13 H9 2 -0.080222 0.186897 0.116924 11.00000 -1.20000 AFIX 0 C10 1 0.129872 0.127071 0.156609 11.00000 0.03877 0.01776 = 0.02556 -0.00064 -0.00072 -0.00105 AFIX 23 H10A 2 0.049643 0.086690 0.172454 11.00000 -1.20000 H10B 2 0.240227 0.098058 0.147235 11.00000 -1.20000 AFIX 0 C11 1 0.231153 0.173632 0.235784 11.00000 0.03623 0.02235 = 0.02593 0.00443 -0.00213 -0.00099 C12 1 0.274495 0.247894 0.267673 11.00000 0.02115 0.02241 = 0.02093 0.00253 0.00278 -0.00093 C13 1 0.243938 0.330350 0.251575 11.00000 0.02463 0.02461 = 0.02078 0.00311 0.00190 0.00059 AFIX 43 H13 2 0.194170 0.340283 0.220260 11.00000 -1.20000 AFIX 0 C14 1 0.288166 0.397777 0.282530 11.00000 0.03594 0.02184 = 0.02658 0.00212 0.00118 0.00051 AFIX 43 H14 2 0.268430 0.453046 0.272010 11.00000 -1.20000 AFIX 0 C15 1 0.361995 0.382104 0.329256 11.00000 0.03124 0.03350 = 0.02437 -0.00423 0.00088 -0.00302 AFIX 43 H15 2 0.391960 0.427263 0.349880 11.00000 -1.20000 AFIX 0 C16 1 0.391680 0.300071 0.345603 11.00000 0.02321 0.03760 = 0.01914 0.00246 0.00039 -0.00178 AFIX 43 H16 2 0.440408 0.290356 0.377067 11.00000 -1.20000 AFIX 0 C17 1 0.348330 0.232588 0.314792 11.00000 0.02280 0.02736 = 0.02339 0.00718 0.00396 -0.00028 AFIX 43 H17 2 0.368316 0.177413 0.325447 11.00000 -1.20000 AFIX 0 N1 3 0.074464 0.285095 0.052158 11.00000 0.02605 0.01599 = 0.01887 -0.00206 0.00003 -0.00064 O1 4 0.119116 0.255239 -0.031476 11.00000 0.04581 0.03346 = 0.02056 -0.00606 -0.00057 0.00119 O2 4 -0.008807 0.377385 -0.005879 11.00000 0.03624 0.02602 = 0.02356 0.00053 -0.00735 0.00094 O3 4 0.169917 0.196018 0.190508 11.00000 0.03353 0.01852 = 0.02156 0.00076 -0.00231 -0.00091 O4 4 0.248565 0.101274 0.248717 11.00000 0.11119 0.01963 = 0.04248 0.00665 -0.03023 -0.00121 HKLF 4 Covalent radii and connectivity table for 2007src1588 in C222(1) C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1 N1 O2 C2 - O2 C3 C3 - N1 C2 C4 C4 - C5 C6 C3 C5 - C4 C6 - C4 C7 - N1 C8 C9 C8 - C7 C9 C9 - C10 C7 C8 C10 - O3 C9 C11 - O4 O3 C12 C12 - C13 C17 C11 C13 - C14 C12 C14 - C15 C13 C15 - C16 C14 C16 - C15 C17 C17 - C16 C12 N1 - C1 C7 C3 O1 - C1 O2 - C1 C2 O3 - C11 C10 O4 - C11 h k l Fo^2 Sigma Why rejected -4 1 -5 1.84 0.43 observed but should be systematically absent -2 1 6 0.95 0.23 observed but should be systematically absent 58093 Reflections read, of which 29944 rejected -9 =< h =< 9, -20 =< k =< 20, -34 =< l =< 34, Max. 2-theta = 55.00 2 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 3 3 1 8.04 0.20 10 2.35 1 9 1 4.74 0.20 8 3.65 4 2 4 4.87 0.13 14 1.15 -5 5 6 9.75 0.32 8 1.78 4 Inconsistent equivalents 3609 Unique reflections, of which 0 suppressed R(int) = 0.0493 R(sigma) = 0.0280 Friedel opposites not merged Maximum memory for data reduction = 2078 / 42524 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 = 2657 / 249120 wR2 = 0.0784 before cycle 1 for 3609 data and 201 / 201 parameters GooF = S = 1.040; Restrained GooF = 1.040 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0406 * P )^2 + 0.89 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19797 0.00028 0.937 OSF Mean shift/esd = 0.114 Maximum = 0.937 for OSF Max. shift = 0.003 A for H6C Max. dU = 0.000 for O4 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2657 / 249120 wR2 = 0.0784 before cycle 2 for 3609 data and 201 / 201 parameters GooF = S = 1.040; Restrained GooF = 1.040 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0406 * P )^2 + 0.89 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19804 0.00028 0.237 OSF Mean shift/esd = 0.039 Maximum = 0.237 for OSF Max. shift = 0.001 A for H6C Max. dU = 0.000 for O4 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2657 / 249120 wR2 = 0.0784 before cycle 3 for 3609 data and 201 / 201 parameters GooF = S = 1.039; Restrained GooF = 1.039 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0406 * P )^2 + 0.89 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19804 0.00028 0.004 OSF Mean shift/esd = 0.001 Maximum = 0.008 for tors H6A Max. shift = 0.000 A for H6B Max. dU = 0.000 for O4 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2657 / 249120 wR2 = 0.0784 before cycle 4 for 3609 data and 201 / 201 parameters GooF = S = 1.039; Restrained GooF = 1.039 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0406 * P )^2 + 0.89 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19804 0.00028 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.002 for x C14 Max. shift = 0.000 A for H6B Max. dU = 0.000 for C11 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2A -0.2105 0.3989 0.0437 23 0.990 0.000 C2 O2 C3 H2B -0.0553 0.4702 0.0446 23 0.990 0.000 C2 O2 C3 H3 -0.0640 0.3418 0.1083 13 1.000 0.000 C3 N1 C2 C4 H4 0.2449 0.3637 0.1282 13 1.000 0.000 C4 C5 C6 C3 H5A 0.2699 0.4700 0.0423 137 0.980 0.000 C5 C4 H5A H5B 0.3701 0.3810 0.0487 137 0.980 0.000 C5 C4 H5A H5C 0.4264 0.4595 0.0830 137 0.980 0.000 C5 C4 H5A H6A 0.2243 0.5023 0.1557 137 0.980 0.000 C6 C4 H6A H6B 0.0264 0.4621 0.1592 137 0.980 0.000 C6 C4 H6A H6C 0.0758 0.5245 0.1143 137 0.980 0.000 C6 C4 H6A H7 0.2874 0.2131 0.0799 13 1.000 0.000 C7 N1 C8 C9 H8A 0.1590 0.0781 0.0584 23 0.990 0.000 C8 C7 C9 H8B -0.0264 0.1257 0.0367 23 0.990 0.000 C8 C7 C9 H9 -0.0827 0.1874 0.1170 13 1.000 0.000 C9 C10 C7 C8 H10A 0.0480 0.0858 0.1728 23 0.990 0.000 C10 O3 C9 H10B 0.2425 0.0974 0.1470 23 0.990 0.000 C10 O3 C9 H13 0.1930 0.3405 0.2196 43 0.950 0.000 C13 C14 C12 H14 0.2681 0.4542 0.2718 43 0.950 0.000 C14 C15 C13 H15 0.3925 0.4282 0.3503 43 0.950 0.000 C15 C16 C14 H16 0.4415 0.2901 0.3778 43 0.950 0.000 C16 C15 C17 H17 0.3688 0.1762 0.3257 43 0.950 0.000 C17 C16 C12 2007src1588 in C222(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.06806 0.30001 0.00241 1.00000 0.02590 0.02327 0.02412 -0.00167 -0.00354 -0.00433 0.02443 0.00214 0.00018 0.00008 0.00005 0.00000 0.00060 0.00058 0.00056 0.00048 0.00051 0.00049 0.00025 C2 -0.07870 0.40888 0.04123 1.00000 0.02856 0.02503 0.02921 -0.00246 -0.00368 0.00268 0.02760 0.00232 0.00020 0.00009 0.00005 0.00000 0.00067 0.00064 0.00060 0.00049 0.00053 0.00052 0.00028 H2A -0.21046 0.39893 0.04366 1.00000 0.03312 0.00000 0.00000 H2B -0.05529 0.47025 0.04461 1.00000 0.03312 0.00000 0.00000 C3 0.02238 0.35917 0.08153 1.00000 0.02304 0.01554 0.02251 -0.00102 0.00187 0.00064 0.02037 0.00204 0.00017 0.00007 0.00004 0.00000 0.00060 0.00052 0.00056 0.00042 0.00047 0.00044 0.00024 H3 -0.06405 0.34179 0.10831 1.00000 0.02444 0.00000 0.00000 C4 0.18511 0.40459 0.10508 1.00000 0.02777 0.01849 0.01796 0.00060 -0.00117 -0.00260 0.02141 0.00204 0.00018 0.00007 0.00004 0.00000 0.00065 0.00055 0.00051 0.00043 0.00047 0.00047 0.00025 H4 0.24491 0.36368 0.12824 1.00000 0.02569 0.00000 0.00000 C5 0.32548 0.43115 0.06629 1.00000 0.03112 0.02988 0.02508 0.00416 -0.00166 -0.00971 0.02869 0.00236 0.00020 0.00009 0.00005 0.00000 0.00071 0.00068 0.00059 0.00048 0.00052 0.00055 0.00029 H5A 0.26989 0.46998 0.04229 1.00000 0.04304 0.00000 0.00000 H5B 0.37008 0.38098 0.04872 1.00000 0.04304 0.00000 0.00000 H5C 0.42645 0.45951 0.08300 1.00000 0.04304 0.00000 0.00000 C6 0.12224 0.48019 0.13639 1.00000 0.04323 0.02441 0.03225 -0.00914 -0.00225 -0.00086 0.03330 0.00241 0.00022 0.00008 0.00005 0.00000 0.00087 0.00070 0.00067 0.00052 0.00063 0.00056 0.00032 H6A 0.22431 0.50234 0.15566 1.00000 0.04995 0.00000 0.00000 H6B 0.02641 0.46205 0.15923 1.00000 0.04995 0.00000 0.00000 H6C 0.07582 0.52452 0.11429 1.00000 0.04995 0.00000 0.00000 C7 0.15418 0.21121 0.07375 1.00000 0.02129 0.01714 0.02187 -0.00141 0.00127 -0.00154 0.02010 0.00203 0.00017 0.00007 0.00004 0.00000 0.00053 0.00056 0.00053 0.00042 0.00046 0.00046 0.00023 H7 0.28736 0.21310 0.07992 1.00000 0.02412 0.00000 0.00000 C8 0.07556 0.12689 0.06064 1.00000 0.03362 0.01868 0.02498 -0.00397 0.00146 -0.00440 0.02576 0.00223 0.00020 0.00008 0.00004 0.00000 0.00069 0.00058 0.00057 0.00046 0.00053 0.00052 0.00027 H8A 0.15905 0.07814 0.05836 1.00000 0.03091 0.00000 0.00000 H8B -0.02641 0.12567 0.03675 1.00000 0.03091 0.00000 0.00000 C9 0.04156 0.16437 0.11159 1.00000 0.02443 0.01923 0.02332 -0.00144 0.00276 -0.00287 0.02233 0.00209 0.00018 0.00007 0.00004 0.00000 0.00065 0.00053 0.00056 0.00045 0.00049 0.00047 0.00025 H9 -0.08273 0.18736 0.11704 1.00000 0.02679 0.00000 0.00000 C10 0.12990 0.12702 0.15661 1.00000 0.03913 0.01779 0.02560 -0.00079 -0.00083 -0.00110 0.02750 0.00225 0.00021 0.00008 0.00005 0.00000 0.00078 0.00058 0.00060 0.00047 0.00055 0.00054 0.00028 H10A 0.04803 0.08581 0.17279 1.00000 0.03301 0.00000 0.00000 H10B 0.24254 0.09742 0.14704 1.00000 0.03301 0.00000 0.00000 C11 0.23115 0.17364 0.23578 1.00000 0.03625 0.02241 0.02598 0.00445 -0.00211 -0.00092 0.02821 0.00235 0.00020 0.00008 0.00005 0.00000 0.00074 0.00061 0.00062 0.00046 0.00057 0.00055 0.00028 C12 0.27450 0.24789 0.26768 1.00000 0.02118 0.02244 0.02104 0.00256 0.00281 -0.00093 0.02155 0.00218 0.00017 0.00008 0.00004 0.00000 0.00056 0.00059 0.00052 0.00044 0.00048 0.00047 0.00024 C13 0.24390 0.33035 0.25156 1.00000 0.02467 0.02467 0.02094 0.00303 0.00198 0.00056 0.02343 0.00223 0.00018 0.00007 0.00005 0.00000 0.00063 0.00057 0.00052 0.00047 0.00048 0.00051 0.00025 H13 0.19303 0.34048 0.21958 1.00000 0.02811 0.00000 0.00000 C14 0.28818 0.39778 0.28252 1.00000 0.03589 0.02205 0.02659 0.00208 0.00110 0.00047 0.02818 0.00242 0.00020 0.00009 0.00005 0.00000 0.00076 0.00062 0.00061 0.00047 0.00054 0.00054 0.00029 H14 0.26809 0.45424 0.27176 1.00000 0.03381 0.00000 0.00000 C15 0.36199 0.38210 0.32927 1.00000 0.03115 0.03362 0.02440 -0.00404 0.00101 -0.00305 0.02973 0.00236 0.00020 0.00009 0.00005 0.00000 0.00074 0.00075 0.00061 0.00051 0.00054 0.00059 0.00030 H15 0.39254 0.42823 0.35035 1.00000 0.03567 0.00000 0.00000 C16 0.39171 0.30006 0.34561 1.00000 0.02316 0.03758 0.01935 0.00244 0.00039 -0.00185 0.02670 0.00229 0.00017 0.00009 0.00004 0.00000 0.00063 0.00072 0.00055 0.00050 0.00048 0.00054 0.00027 H16 0.44150 0.29013 0.37775 1.00000 0.03204 0.00000 0.00000 C17 0.34835 0.23257 0.31479 1.00000 0.02295 0.02756 0.02347 0.00708 0.00402 -0.00032 0.02466 0.00230 0.00018 0.00009 0.00004 0.00000 0.00062 0.00067 0.00057 0.00047 0.00051 0.00051 0.00027 H17 0.36878 0.17620 0.32567 1.00000 0.02959 0.00000 0.00000 N1 0.07447 0.28509 0.05216 1.00000 0.02622 0.01607 0.01887 -0.00211 0.00006 -0.00064 0.02039 0.00173 0.00015 0.00006 0.00003 0.00000 0.00052 0.00048 0.00045 0.00036 0.00041 0.00041 0.00021 O1 0.11912 0.25524 -0.03147 1.00000 0.04589 0.03355 0.02063 -0.00611 -0.00047 0.00122 0.03336 0.00168 0.00014 0.00007 0.00003 0.00000 0.00063 0.00055 0.00042 0.00037 0.00043 0.00045 0.00024 O2 -0.00880 0.37737 -0.00587 1.00000 0.03629 0.02615 0.02364 0.00053 -0.00736 0.00098 0.02869 0.00157 0.00013 0.00006 0.00003 0.00000 0.00054 0.00046 0.00043 0.00035 0.00039 0.00041 0.00021 O3 0.16993 0.19603 0.19051 1.00000 0.03361 0.01854 0.02163 0.00071 -0.00238 -0.00095 0.02459 0.00152 0.00013 0.00006 0.00003 0.00000 0.00050 0.00042 0.00042 0.00032 0.00036 0.00038 0.00020 O4 0.24858 0.10128 0.24871 1.00000 0.11147 0.01978 0.04255 0.00659 -0.03021 -0.00120 0.05793 0.00212 0.00023 0.00006 0.00005 0.00000 0.00120 0.00046 0.00056 0.00048 0.00070 0.00065 0.00040 Final Structure Factor Calculation for 2007src1588 in C222(1) Total number of l.s. parameters = 201 Maximum vector length = 511 Memory required = 2458 / 25046 wR2 = 0.0784 before cycle 5 for 3609 data and 2 / 201 parameters GooF = S = 1.039; Restrained GooF = 1.039 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0406 * P )^2 + 0.89 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0339 for 3401 Fo > 4sig(Fo) and 0.0375 for all 3609 data wR2 = 0.0784, GooF = S = 1.039, Restrained GooF = 1.039 for all data Flack x parameter = -0.1933 with esd 0.7374 Expected values are 0 (within 3 esd's) for correct and +1 for inverted absolute structure. Note that this rough estimate ignores correlation with other parameters; if the above value differs significantly from zero, it is ESSENTIAL to test the inverted structure or refine x as a full-matrix parameter using TWIN and BASF Absolute structure cannot be determined reliably Occupancy sum of asymmetric unit = 22.00 for non-hydrogen and 21.00 for hydrogen atoms Principal mean square atomic displacements U 0.0299 0.0254 0.0180 C1 0.0340 0.0252 0.0235 C2 0.0247 0.0211 0.0153 C3 0.0286 0.0181 0.0175 C4 0.0413 0.0249 0.0199 C5 0.0437 0.0379 0.0182 C6 0.0236 0.0203 0.0164 C7 0.0354 0.0257 0.0161 C8 0.0278 0.0212 0.0180 C9 0.0392 0.0256 0.0176 C10 0.0369 0.0283 0.0194 C11 0.0248 0.0227 0.0171 C12 0.0273 0.0241 0.0189 C13 0.0361 0.0272 0.0212 C14 0.0369 0.0294 0.0229 C15 0.0381 0.0230 0.0189 C16 0.0334 0.0243 0.0163 C17 0.0263 0.0200 0.0149 N1 0.0461 0.0358 0.0182 O1 0.0397 0.0263 0.0201 O2 0.0341 0.0213 0.0184 O3 0.1229 0.0336 0.0173 O4 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.035 0.053 0.068 0.081 0.099 0.119 0.146 0.183 0.260 1.000 Number in group 377. 368. 354. 349. 368. 351. 365. 356. 358. 363. GooF 1.149 1.092 1.012 1.006 1.022 0.989 0.958 1.047 0.957 1.131 K 1.709 1.249 1.003 0.998 0.996 1.000 1.007 1.002 1.007 0.981 Resolution(A) 0.77 0.79 0.83 0.87 0.91 0.97 1.04 1.15 1.32 1.65 inf Number in group 368. 366. 354. 358. 360. 363. 356. 369. 354. 361. GooF 1.047 0.991 1.003 1.021 0.890 0.909 0.943 0.872 1.162 1.437 K 1.012 1.007 1.018 1.014 1.008 0.999 0.995 0.987 1.019 0.982 R1 0.076 0.070 0.064 0.054 0.034 0.029 0.025 0.020 0.029 0.034 Recommended weighting scheme: WGHT 0.0390 0.8765 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 10 1 347.28 704.93 7.23 0.163 1.45 0 10 7 445.47 596.75 4.60 0.150 1.46 2 0 17 174.23 113.85 4.46 0.066 1.45 -1 1 3 16617.25 20718.91 4.41 0.885 5.36 0 2 2 136.36 272.74 3.81 0.102 6.81 1 1 3 17446.83 20711.21 3.74 0.885 5.36 1 3 14 1988.63 1683.65 3.53 0.252 1.75 0 8 28 34.41 6.15 3.52 0.015 0.86 0 8 0 5358.06 4549.04 3.50 0.415 1.98 0 2 5 252.25 325.60 3.49 0.111 4.44 0 4 14 46.76 24.75 3.48 0.031 1.72 1 1 2 10940.14 12842.93 3.45 0.697 6.00 0 2 16 867.44 719.90 3.45 0.165 1.64 6 2 0 249.50 186.61 3.33 0.084 1.22 -2 10 1 422.50 704.48 3.32 0.163 1.45 0 4 5 8.54 22.49 3.31 0.029 3.18 1 11 15 118.63 167.31 3.29 0.080 1.11 5 1 0 31.05 12.40 3.28 0.022 1.47 1 1 1 2121.39 2519.53 3.24 0.309 6.50 0 4 1 10086.60 11668.96 3.23 0.664 3.91 2 0 8 758.04 636.01 3.19 0.155 2.48 1 19 12 1390.17 1155.30 3.18 0.209 0.78 7 5 13 497.19 381.31 3.18 0.120 0.90 0 10 2 342.95 432.37 3.17 0.128 1.57 -1 3 14 1955.76 1682.28 3.17 0.252 1.75 4 16 8 74.67 120.36 3.13 0.067 0.84 4 16 1 223.93 162.21 3.04 0.078 0.87 0 2 4 13539.02 15490.75 3.02 0.765 5.11 0 2 3 8776.82 10092.72 2.99 0.618 5.92 1 7 5 4247.47 53.96 2.94 0.045 2.00 1 1 4 10205.03 11651.46 2.92 0.664 4.74 0 12 0 658.11 507.63 2.91 0.138 1.32 1 1 5 16290.97 18516.82 2.90 0.836 4.19 2 18 9 110.00 72.82 2.87 0.052 0.82 -1 1 4 10222.57 11635.29 2.87 0.663 4.74 8 6 8 1.25 30.24 2.83 0.034 0.84 0 0 14 1802.57 1568.46 2.82 0.243 1.91 2 0 7 697.98 816.96 2.80 0.176 2.66 -3 9 17 144.63 189.96 2.79 0.085 1.06 3 15 1 65.40 32.32 2.79 0.035 0.97 -1 1 1 2190.83 2518.39 2.79 0.308 6.50 0 0 8 12.95 29.57 2.77 0.033 3.35 -3 3 27 72.53 108.20 2.76 0.064 0.91 -1 11 15 127.68 167.73 2.75 0.080 1.11 3 7 9 247.46 195.13 2.73 0.086 1.45 0 10 1 2048.26 0.33 2.72 0.004 1.58 -1 1 2 10997.18 12840.08 2.70 0.697 6.00 7 1 19 42.52 16.95 2.70 0.025 0.84 1 11 4 192.78 149.83 2.69 0.075 1.38 -3 15 1 61.41 32.39 2.68 0.035 0.97 Bond lengths and angles C1 - Distance Angles O1 1.2120 (0.0016) N1 1.3548 (0.0016) 128.68 (0.13) O2 1.3675 (0.0016) 122.05 (0.12) 109.28 (0.11) C1 - O1 N1 C2 - Distance Angles O2 1.4527 (0.0016) C3 1.5312 (0.0017) 105.24 (0.10) C2 - O2 C3 - Distance Angles N1 1.4632 (0.0014) C2 1.5312 (0.0017) 99.23 (0.09) C4 1.5380 (0.0016) 112.86 (0.10) 115.61 (0.10) C3 - N1 C2 C4 - Distance Angles C5 1.5286 (0.0018) C6 1.5332 (0.0017) 111.36 (0.11) C3 1.5380 (0.0016) 112.43 (0.10) 110.56 (0.11) C4 - C5 C6 C5 - Distance Angles C4 1.5286 (0.0018) C5 - C6 - Distance Angles C4 1.5332 (0.0017) C6 - C7 - Distance Angles N1 1.4313 (0.0015) C8 1.4969 (0.0016) 118.17 (0.10) C9 1.5074 (0.0016) 116.45 (0.10) 60.34 (0.08) C7 - N1 C8 C8 - Distance Angles C7 1.4969 (0.0016) C9 1.5099 (0.0016) 60.18 (0.08) C8 - C7 C9 - Distance Angles C10 1.4943 (0.0018) C7 1.5074 (0.0016) 119.71 (0.12) C8 1.5099 (0.0016) 120.16 (0.11) 59.48 (0.08) C9 - C10 C7 C10 - Distance Angles O3 1.4506 (0.0015) C9 1.4943 (0.0018) 107.32 (0.10) C10 - O3 C11 - Distance Angles O4 1.2026 (0.0015) O3 1.3429 (0.0015) 123.20 (0.13) C12 1.4876 (0.0017) 124.22 (0.12) 112.57 (0.10) C11 - O4 O3 C12 - Distance Angles C13 1.3923 (0.0016) C17 1.3972 (0.0017) 120.43 (0.12) C11 1.4876 (0.0017) 121.74 (0.11) 117.83 (0.11) C12 - C13 C17 C13 - Distance Angles C14 1.3904 (0.0018) C12 1.3923 (0.0016) 119.67 (0.12) C13 - C14 C14 - Distance Angles C15 1.3894 (0.0018) C13 1.3904 (0.0018) 119.60 (0.13) C14 - C15 C15 - Distance Angles C16 1.3871 (0.0020) C14 1.3894 (0.0018) 120.94 (0.13) C15 - C16 C16 - Distance Angles C15 1.3871 (0.0020) C17 1.3874 (0.0019) 119.67 (0.12) C16 - C15 C17 - Distance Angles C16 1.3874 (0.0019) C12 1.3972 (0.0017) 119.69 (0.12) C17 - C16 N1 - Distance Angles C1 1.3548 (0.0016) C7 1.4313 (0.0015) 123.68 (0.10) C3 1.4632 (0.0014) 112.39 (0.10) 123.00 (0.09) N1 - C1 C7 O1 - Distance Angles C1 1.2120 (0.0016) O1 - O2 - Distance Angles C1 1.3675 (0.0016) C2 1.4527 (0.0016) 108.30 (0.09) O2 - C1 O3 - Distance Angles C11 1.3429 (0.0015) C10 1.4506 (0.0015) 115.87 (0.10) O3 - C11 O4 - Distance Angles C11 1.2026 (0.0015) O4 - FMAP and GRID set by program FMAP 2 1 12 GRID -2.778 -2 -1 2.778 2 1 R1 = 0.0357 for 2036 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.15 at 0.2486 0.7181 0.2491 [ 0.67 A from C12 ] Deepest hole -0.15 at 0.0036 0.3991 0.4011 [ 0.81 A from C3 ] Mean = 0.00, Rms deviation from mean = 0.04 e/A^3, Highest memory used = 3515 / 35508 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.2514 0.2181 0.2509 1.00000 0.05 0.15 0.67 C12 0.83 C11 1.76 O3 1.78 C13 Q2 1 0.2852 0.2406 0.2903 1.00000 0.05 0.15 0.62 C12 0.82 C17 1.52 H17 1.78 C13 Q3 1 0.0603 0.2599 -0.0648 1.00000 0.05 0.12 1.00 O1 1.73 H16 1.91 C1 2.10 H7 Q4 1 0.2539 0.2843 0.2601 1.00000 0.05 0.12 0.63 C12 0.77 C13 1.47 H13 1.82 C17 Q5 1 0.1526 0.3410 0.1966 1.00000 0.05 0.12 0.68 H13 1.63 C13 1.99 H4 2.30 O3 Q6 1 0.3664 0.3414 0.3322 1.00000 0.05 0.11 0.65 C15 0.77 C16 1.47 H15 1.57 H16 Q7 1 0.2757 0.3819 0.1869 1.00000 0.05 0.11 1.25 H13 1.61 H4 1.93 C13 2.12 H6A Q8 1 -0.1176 0.2021 0.0293 1.00000 0.05 0.11 1.40 H8B 2.03 N1 2.04 C8 2.06 O1 Q9 1 0.0968 0.2000 0.1018 1.00000 0.05 0.11 0.74 C9 0.88 C7 1.40 H9 1.54 H7 Q10 1 0.5761 0.2207 0.3678 1.00000 0.05 0.11 1.51 H16 1.73 H7 1.95 C16 2.03 H17 Q11 1 0.3329 0.0415 0.2729 1.00000 0.05 0.10 1.31 O4 1.97 H14 2.06 H6A 2.43 C11 Q12 1 0.0959 0.1418 0.1310 1.00000 0.05 0.10 0.75 C9 0.77 C10 1.36 H10B 1.47 H10A Q13 1 0.3763 0.3353 0.4203 1.00000 0.05 0.10 1.43 H16 1.86 H2A 1.93 O1 2.08 C16 Q14 1 0.1623 0.4774 0.2384 1.00000 0.05 0.10 1.24 H14 1.96 C14 2.10 O4 2.23 H13 Q15 1 0.0259 0.5000 0.0000 0.50000 0.05 0.10 1.42 H2B 1.96 O2 1.97 C2 2.18 H5A Q16 1 -0.0247 0.3141 0.2025 1.00000 0.05 0.10 1.73 H13 2.05 C13 2.27 C12 2.38 O3 Q17 1 0.2474 0.4755 0.2191 1.00000 0.05 0.10 1.46 H14 1.76 H6A 2.12 C14 2.17 O4 Q18 1 0.3585 0.1430 0.3734 1.00000 0.05 0.10 1.39 H17 1.96 H6C 2.12 C17 2.17 H9 Q19 1 0.4740 0.2126 0.0956 1.00000 0.05 0.10 1.44 H7 1.55 H16 2.09 O1 2.32 C16 Q20 1 0.2859 0.3848 0.3097 1.00000 0.05 0.10 0.76 C14 0.77 C15 1.50 H14 1.51 H15 Shortest distances between peaks (including symmetry equivalents) 14 17 0.81 10 19 1.06 11 14 1.06 1 4 1.07 2 4 1.09 6 20 1.09 3 19 1.13 1 2 1.14 5 7 1.15 9 12 1.21 11 17 1.22 5 16 1.39 3 13 1.63 7 17 1.73 18 19 1.85 4 16 2.03 10 18 2.03 2 6 2.04 4 5 2.06 4 20 2.09 3 10 2.09 7 14 2.21 16 20 2.26 2 16 2.26 13 19 2.27 4 6 2.29 5 17 2.32 3 18 2.34 2 20 2.34 6 13 2.36 5 14 2.43 14 14 2.48 4 7 2.50 7 16 2.50 8 9 2.51 1 5 2.54 16 16 2.57 9 10 2.58 14 20 2.58 1 16 2.58 4 16 2.62 3 8 2.63 6 10 2.64 10 12 2.73 6 16 2.73 10 13 2.73 11 11 2.76 2 18 2.76 6 7 2.77 11 14 2.80 9 19 2.80 17 20 2.83 1 16 2.86 7 11 2.86 5 16 2.89 1 11 2.92 3 8 2.99 Time profile in seconds ----------------------- 0.09: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.01: Generate connectivity array 0.01: 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. 7.70: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.04: OSF, H-atoms from difference map 0.01: Set up l.s. refinement 0.00: Generate idealized H-atoms 2.27: Structure factors and derivatives 1.57: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.24: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.08: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.10: Fourier summations 0.04: Peaksearch 0.01: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2007src1588 finished at 17:06:53 Total CPU time: 12.2 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++