+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 07skc0014 started at 12:11:35 on 05-Aug-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 07skc0014 in P-1 CELL 0.71073 6.7452 8.7155 11.3058 101.834 91.509 92.367 ZERR 1.00 0.0003 0.0005 0.0006 0.003 0.003 0.003 LATT 1 SFAC C H N O UNIT 22 36 4 12 V = 649.55 F(000) = 292.0 Mu = 0.11 mm-1 Cell Wt = 548.55 Rho = 1.402 MERG 2 OMIT -3.00 55.00 SHEL 7 0.77 EQIV_$1 x, y-1, z HTAB N21 O1A_$1 EQIV_$2 -x+2, -y+2, -z+1 HTAB O31B O4B_$2 EQIV_$3 -x, -y+1, -z HTAB N24 O1B_$3 EQIV_$4 x-1, y, z HTAB N24 O4A_$4 FMAP 2 PLAN 10 SIZE 0.02 0.07 0.16 ACTA BOND $H WGHT 0.00000 1.63390 L.S. 4 TEMP -153.00 FVAR 0.83629 MOLE 1 C1 1 0.406318 0.964238 0.127335 11.00000 0.01779 0.01732 = 0.01781 0.00434 0.00103 0.00255 C2 1 0.506672 0.814207 0.129911 11.00000 0.01759 0.01605 = 0.01965 0.00124 0.00096 0.00140 AFIX 43 H2 2 0.463227 0.722160 0.072990 11.00000 -1.20000 AFIX 0 C3 1 0.652986 0.804665 0.208029 11.00000 0.01733 0.01616 = 0.02224 0.00402 0.00338 0.00179 AFIX 43 H3 2 0.699390 0.897710 0.262860 11.00000 -1.20000 AFIX 0 C4 1 0.749202 0.654269 0.214309 11.00000 0.01594 0.01707 = 0.02277 0.00541 0.00318 0.00197 O1A 4 0.472985 1.088324 0.198317 11.00000 0.01939 0.01531 = 0.02257 0.00194 -0.00311 0.00241 O1B 4 0.258814 0.957766 0.055753 11.00000 0.02052 0.01916 = 0.02507 0.00154 -0.00640 0.00540 O4A 4 0.692559 0.531439 0.140058 11.00000 0.02007 0.01332 = 0.03227 0.00116 -0.00183 0.00437 O4B 4 0.883292 0.660406 0.296059 11.00000 0.02365 0.02043 = 0.03276 0.00442 -0.00893 0.00486 MOLE 2 C22 1 0.071336 0.298261 0.322277 11.00000 0.01547 0.02199 = 0.01762 0.00607 0.00377 0.00247 AFIX 23 H22A 2 0.006838 0.397596 0.354156 11.00000 -1.20000 H22B 2 0.100318 0.247030 0.390863 11.00000 -1.20000 AFIX 0 C23 1 -0.066815 0.192388 0.231440 11.00000 0.01909 0.01452 = 0.02227 0.00679 -0.00015 0.00139 AFIX 23 H23A 2 -0.006924 0.089775 0.204591 11.00000 -1.20000 H23B 2 -0.193698 0.174031 0.269549 11.00000 -1.20000 AFIX 0 N24 3 -0.105631 0.264765 0.124797 11.00000 0.01678 0.01573 = 0.02044 0.00009 -0.00332 0.00422 AFIX 23 H24A 2 -0.183471 0.195814 0.068056 11.00000 -1.20000 H24B 2 -0.174588 0.354140 0.148718 11.00000 -1.20000 AFIX 0 C25 1 0.081442 0.305458 0.069027 11.00000 0.01947 0.01913 = 0.01882 0.00563 0.00294 0.00464 AFIX 23 H25A 2 0.050072 0.358989 0.002069 11.00000 -1.20000 H25B 2 0.148782 0.208210 0.034970 11.00000 -1.20000 AFIX 0 C26 1 0.218221 0.411291 0.161529 11.00000 0.01792 0.01723 = 0.02096 0.00573 0.00227 0.00026 AFIX 23 H26A 2 0.343750 0.434330 0.123729 11.00000 -1.20000 H26B 2 0.155119 0.511797 0.191540 11.00000 -1.20000 AFIX 0 C27 1 0.402736 0.429483 0.356245 11.00000 0.02238 0.01844 = 0.02859 -0.00036 -0.00488 -0.00333 AFIX 137 H27A 2 0.525646 0.451726 0.317241 11.00000 -1.50000 H27B 2 0.432561 0.371963 0.420009 11.00000 -1.50000 H27C 2 0.343229 0.528402 0.391707 11.00000 -1.50000 AFIX 0 N21 3 0.261193 0.332861 0.264814 11.00000 0.01485 0.01264 = 0.01925 0.00265 -0.00012 0.00117 AFIX 13 H21 2 0.318196 0.238110 0.234363 11.00000 0.04021 AFIX 0 MOLE 3 C31 1 0.740690 1.120332 0.555242 11.00000 0.02489 0.02125 = 0.01608 0.00155 -0.00041 0.00664 C32 1 0.574521 1.000910 0.539179 11.00000 0.02639 0.01825 = 0.02257 0.00526 -0.00029 0.00140 AFIX 43 H32 2 0.575104 0.922942 0.586845 11.00000 -1.20000 AFIX 0 O31A 4 0.749775 1.226308 0.499879 11.00000 0.02806 0.02371 = 0.02639 0.00818 -0.00393 -0.00068 O31B 4 0.876610 1.099896 0.636491 11.00000 0.02989 0.02397 = 0.03114 0.00937 -0.01166 -0.00350 AFIX 147 H31B 2 0.957732 1.177743 0.650983 11.00000 0.06008 AFIX 0 HKLF 4 Covalent radii and connectivity table for 07skc0014 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1B O1A C2 C2 - C3 C1 C3 - C2 C4 C4 - O4A O4B C3 O1A - C1 O1B - C1 O4A - C4 O4B - C4 C22 - N21 C23 C23 - N24 C22 N24 - C25 C23 C25 - N24 C26 C26 - N21 C25 C27 - N21 N21 - C27 C26 C22 C31 - O31A O31B C32 C32 - C32_$5 C31 O31A - C31 O31B - C31 Operators for generating equivalent atoms: $1 x, y-1, z $2 -x+2, -y+2, -z+1 $3 -x, -y+1, -z $4 x-1, y, z $5 -x+1, -y+2, -z+1 8728 Reflections read, of which 23 rejected -8 =< h =< 8, -11 =< k =< 11, -14 =< l =< 14, Max. 2-theta = 54.97 0 Systematic absence violations 0 Inconsistent equivalents 2952 Unique reflections, of which 0 suppressed R(int) = 0.0569 R(sigma) = 0.0723 Friedel opposites merged Maximum memory for data reduction = 2082 / 29303 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 = 2594 / 218795 wR2 = 0.1551 before cycle 1 for 2952 data and 176 / 176 parameters GooF = S = 1.070; Restrained GooF = 1.070 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 1.63 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.83629 0.00210 0.002 OSF Mean shift/esd = 0.001 Maximum = 0.004 for U12 O1A Max. shift = 0.000 A for H31B Max. dU = 0.000 for H31B Least-squares cycle 2 Maximum vector length = 511 Memory required = 2594 / 218795 wR2 = 0.1551 before cycle 2 for 2952 data and 176 / 176 parameters GooF = S = 1.070; Restrained GooF = 1.070 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 1.63 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.83629 0.00210 -0.001 OSF Mean shift/esd = 0.000 Maximum = 0.001 for U12 O1A Max. shift = 0.000 A for C31 Max. dU = 0.000 for C3 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2594 / 218795 wR2 = 0.1551 before cycle 3 for 2952 data and 176 / 176 parameters GooF = S = 1.070; Restrained GooF = 1.070 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 1.63 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.83629 0.00210 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y C31 Max. shift = 0.000 A for C31 Max. dU = 0.000 for H31B Least-squares cycle 4 Maximum vector length = 511 Memory required = 2594 / 218795 wR2 = 0.1551 before cycle 4 for 2952 data and 176 / 176 parameters GooF = S = 1.070; Restrained GooF = 1.070 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 1.63 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.83629 0.00210 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y O31B Max. shift = 0.000 A for O31B Max. dU = 0.000 for H31B 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 H2 0.4632 0.7222 0.0730 43 0.950 0.000 C2 C3 C1 H3 0.6994 0.8977 0.2629 43 0.950 0.000 C3 C2 C4 H22A 0.0068 0.3976 0.3542 23 0.990 0.000 C22 N21 C23 H22B 0.1003 0.2470 0.3909 23 0.990 0.000 C22 N21 C23 H23A -0.0069 0.0898 0.2046 23 0.990 0.000 C23 N24 C22 H23B -0.1937 0.1740 0.2695 23 0.990 0.000 C23 N24 C22 H24A -0.1835 0.1958 0.0681 23 0.920 0.000 N24 C25 C23 H24B -0.1746 0.3541 0.1487 23 0.920 0.000 N24 C25 C23 H25A 0.0501 0.3590 0.0021 23 0.990 0.000 C25 N24 C26 H25B 0.1488 0.2082 0.0350 23 0.990 0.000 C25 N24 C26 H26A 0.3438 0.4343 0.1237 23 0.990 0.000 C26 N21 C25 H26B 0.1551 0.5118 0.1915 23 0.990 0.000 C26 N21 C25 H27A 0.5256 0.4517 0.3172 137 0.980 0.000 C27 N21 H27A H27B 0.4326 0.3720 0.4200 137 0.980 0.000 C27 N21 H27A H27C 0.3432 0.5284 0.3917 137 0.980 0.000 C27 N21 H27A H21 0.3182 0.2381 0.2344 13 0.930 0.000 N21 C27 C26 C22 H32 0.5751 0.9229 0.5868 43 0.950 0.000 C32 C32_$5 C31 H31B 0.9577 1.1777 0.6510 147 0.840 0.000 O31B C31 H31B 07skc0014 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.40632 0.96424 0.12733 1.00000 0.01779 0.01732 0.01781 0.00434 0.00103 0.00255 0.01748 0.00566 0.00043 0.00034 0.00026 0.00000 0.00143 0.00147 0.00146 0.00121 0.00118 0.00118 0.00061 C2 0.50667 0.81421 0.12991 1.00000 0.01759 0.01605 0.01965 0.00124 0.00096 0.00140 0.01809 0.00578 0.00043 0.00035 0.00027 0.00000 0.00141 0.00145 0.00148 0.00119 0.00117 0.00117 0.00061 H2 0.46323 0.72216 0.07299 1.00000 0.02171 0.00000 0.00000 C3 0.65299 0.80466 0.20803 1.00000 0.01733 0.01616 0.02224 0.00402 0.00338 0.00179 0.01849 0.00596 0.00043 0.00035 0.00028 0.00000 0.00141 0.00145 0.00150 0.00121 0.00119 0.00116 0.00062 H3 0.69939 0.89771 0.26286 1.00000 0.02219 0.00000 0.00000 C4 0.74920 0.65427 0.21431 1.00000 0.01594 0.01707 0.02277 0.00541 0.00318 0.00197 0.01833 0.00583 0.00042 0.00035 0.00027 0.00000 0.00140 0.00148 0.00154 0.00125 0.00120 0.00117 0.00062 O1A 0.47298 1.08832 0.19832 1.00000 0.01939 0.01531 0.02257 0.00194 -0.00311 0.00241 0.01940 0.00386 0.00030 0.00023 0.00019 0.00000 0.00104 0.00104 0.00111 0.00088 0.00087 0.00085 0.00047 O1B 0.25881 0.95777 0.05575 1.00000 0.02052 0.01916 0.02507 0.00154 -0.00640 0.00540 0.02202 0.00396 0.00031 0.00024 0.00019 0.00000 0.00108 0.00110 0.00117 0.00092 0.00091 0.00089 0.00049 O4A 0.69256 0.53144 0.14006 1.00000 0.02007 0.01332 0.03227 0.00116 -0.00183 0.00437 0.02234 0.00405 0.00030 0.00024 0.00020 0.00000 0.00107 0.00103 0.00125 0.00092 0.00094 0.00085 0.00049 O4B 0.88329 0.66041 0.29606 1.00000 0.02365 0.02043 0.03276 0.00442 -0.00893 0.00486 0.02584 0.00416 0.00032 0.00025 0.00021 0.00000 0.00115 0.00116 0.00128 0.00100 0.00099 0.00094 0.00053 C22 0.07134 0.29826 0.32228 1.00000 0.01547 0.02198 0.01762 0.00607 0.00377 0.00247 0.01797 0.00572 0.00042 0.00036 0.00026 0.00000 0.00136 0.00154 0.00145 0.00123 0.00114 0.00119 0.00062 H22A 0.00684 0.39760 0.35416 1.00000 0.02157 0.00000 0.00000 H22B 0.10032 0.24703 0.39086 1.00000 0.02157 0.00000 0.00000 C23 -0.06682 0.19239 0.23144 1.00000 0.01908 0.01452 0.02227 0.00679 -0.00015 0.00139 0.01820 0.00564 0.00044 0.00034 0.00027 0.00000 0.00144 0.00143 0.00153 0.00121 0.00120 0.00117 0.00062 H23A -0.00692 0.08978 0.20459 1.00000 0.02184 0.00000 0.00000 H23B -0.19370 0.17403 0.26955 1.00000 0.02184 0.00000 0.00000 N24 -0.10563 0.26476 0.12480 1.00000 0.01678 0.01573 0.02044 0.00009 -0.00332 0.00422 0.01815 0.00468 0.00035 0.00029 0.00022 0.00000 0.00120 0.00124 0.00130 0.00104 0.00101 0.00099 0.00054 H24A -0.18347 0.19581 0.06806 1.00000 0.02178 0.00000 0.00000 H24B -0.17459 0.35414 0.14872 1.00000 0.02178 0.00000 0.00000 C25 0.08144 0.30546 0.06903 1.00000 0.01947 0.01913 0.01882 0.00563 0.00294 0.00464 0.01875 0.00581 0.00043 0.00036 0.00027 0.00000 0.00144 0.00148 0.00149 0.00123 0.00118 0.00121 0.00062 H25A 0.05007 0.35899 0.00207 1.00000 0.02250 0.00000 0.00000 H25B 0.14878 0.20821 0.03497 1.00000 0.02250 0.00000 0.00000 C26 0.21822 0.41129 0.16153 1.00000 0.01792 0.01723 0.02096 0.00573 0.00227 0.00026 0.01843 0.00566 0.00043 0.00035 0.00027 0.00000 0.00143 0.00146 0.00152 0.00123 0.00119 0.00118 0.00062 H26A 0.34375 0.43433 0.12373 1.00000 0.02212 0.00000 0.00000 H26B 0.15512 0.51180 0.19154 1.00000 0.02212 0.00000 0.00000 C27 0.40274 0.42948 0.35625 1.00000 0.02238 0.01844 0.02859 -0.00036 -0.00488 -0.00333 0.02411 0.00572 0.00046 0.00037 0.00030 0.00000 0.00157 0.00154 0.00171 0.00133 0.00134 0.00129 0.00070 H27A 0.52565 0.45173 0.31724 1.00000 0.03616 0.00000 0.00000 H27B 0.43256 0.37196 0.42001 1.00000 0.03616 0.00000 0.00000 H27C 0.34323 0.52840 0.39171 1.00000 0.03616 0.00000 0.00000 N21 0.26119 0.33286 0.26481 1.00000 0.01485 0.01264 0.01925 0.00265 -0.00012 0.00117 0.01567 0.00451 0.00034 0.00028 0.00022 0.00000 0.00116 0.00118 0.00126 0.00100 0.00098 0.00096 0.00052 H21 0.31820 0.23811 0.23436 1.00000 0.04021 0.00000 0.01104 C31 0.74069 1.12033 0.55524 1.00000 0.02489 0.02125 0.01608 0.00155 -0.00041 0.00664 0.02093 0.00597 0.00046 0.00036 0.00027 0.00000 0.00159 0.00157 0.00146 0.00126 0.00123 0.00130 0.00066 C32 0.57452 1.00091 0.53918 1.00000 0.02639 0.01825 0.02257 0.00526 -0.00029 0.00140 0.02226 0.00599 0.00046 0.00037 0.00028 0.00000 0.00159 0.00150 0.00158 0.00128 0.00128 0.00128 0.00066 H32 0.57510 0.92294 0.58684 1.00000 0.02672 0.00000 0.00000 O31A 0.74978 1.22631 0.49988 1.00000 0.02806 0.02371 0.02639 0.00818 -0.00393 -0.00068 0.02576 0.00424 0.00033 0.00026 0.00020 0.00000 0.00123 0.00119 0.00120 0.00100 0.00098 0.00098 0.00053 O31B 0.87661 1.09990 0.63649 1.00000 0.02989 0.02397 0.03114 0.00937 -0.01166 -0.00350 0.02817 0.00442 0.00035 0.00027 0.00021 0.00000 0.00127 0.00126 0.00131 0.00106 0.00105 0.00105 0.00055 H31B 0.95773 1.17774 0.65098 1.00000 0.06008 0.00000 0.01489 Final Structure Factor Calculation for 07skc0014 in P-1 Total number of l.s. parameters = 176 Maximum vector length = 511 Memory required = 2418 / 22995 wR2 = 0.1551 before cycle 5 for 2952 data and 0 / 176 parameters GooF = S = 1.070; Restrained GooF = 1.070 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 1.63 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0761 for 2106 Fo > 4sig(Fo) and 0.1131 for all 2952 data wR2 = 0.1551, GooF = S = 1.070, Restrained GooF = 1.070 for all data Occupancy sum of asymmetric unit = 19.00 for non-hydrogen and 18.00 for hydrogen atoms Principal mean square atomic displacements U 0.0193 0.0175 0.0156 C1 0.0215 0.0177 0.0150 C2 0.0234 0.0167 0.0154 C3 0.0236 0.0165 0.0149 C4 0.0265 0.0170 0.0147 O1A 0.0337 0.0188 0.0135 O1B 0.0350 0.0205 0.0116 O4A 0.0407 0.0222 0.0146 O4B 0.0230 0.0179 0.0130 C22 0.0230 0.0191 0.0125 C23 0.0267 0.0152 0.0125 N24 0.0237 0.0172 0.0154 C25 0.0217 0.0183 0.0153 C26 0.0335 0.0250 0.0138 C27 0.0197 0.0148 0.0125 N21 0.0297 0.0176 0.0155 C31 0.0268 0.0224 0.0176 C32 0.0331 0.0237 0.0205 O31A 0.0446 0.0219 0.0181 O31B Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.008 0.016 0.024 0.033 0.043 0.056 0.072 0.094 0.136 1.000 Number in group 320. 295. 282. 288. 291. 301. 291. 292. 295. 297. GooF 1.169 1.103 1.125 1.111 1.029 1.111 1.037 0.964 1.040 0.984 K 8.741 2.129 1.408 1.105 1.059 1.026 1.000 0.991 1.004 1.005 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.15 1.32 1.66 inf Number in group 295. 305. 289. 298. 290. 300. 289. 294. 297. 295. GooF 1.182 1.151 1.123 1.111 1.166 1.091 0.999 0.958 0.838 1.031 K 1.069 1.111 1.069 1.035 1.049 1.018 1.007 1.008 1.006 0.999 R1 0.245 0.242 0.199 0.193 0.157 0.122 0.077 0.066 0.052 0.032 Recommended weighting scheme: WGHT 0.0000 1.6340 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 4 11 60.60 132.61 3.66 0.095 0.84 -1 -9 1 56.82 14.04 3.52 0.031 0.94 3 7 7 29.67 0.05 3.51 0.002 0.80 0 -2 1 176.20 246.56 3.45 0.129 4.28 -1 -9 4 30.54 72.88 3.32 0.070 0.94 -4 -2 10 -0.46 20.42 3.32 0.037 0.95 1 -1 4 25.69 8.65 3.27 0.024 2.57 5 5 5 17.60 0.21 3.20 0.004 0.89 -6 -4 4 80.90 37.06 3.12 0.050 0.96 5 -8 7 108.68 46.42 3.08 0.056 0.80 2 -8 2 -0.65 14.63 3.07 0.032 1.05 4 -4 10 29.03 0.20 3.03 0.004 0.90 0 1 1 408.49 520.45 2.98 0.188 6.16 0 -8 11 69.76 30.01 2.90 0.045 0.82 8 3 1 17.17 46.37 2.90 0.056 0.79 0 -3 6 12.74 1.72 2.88 0.011 1.72 3 -1 12 39.35 1.98 2.87 0.012 0.86 -4 8 2 31.41 2.20 2.87 0.012 0.89 5 -5 5 6.19 32.26 2.86 0.047 1.01 -5 6 7 37.09 5.55 2.86 0.019 0.80 -1 1 1 8.08 0.78 2.85 0.007 4.67 1 -1 1 111.75 157.05 2.82 0.103 5.07 4 2 7 69.84 39.01 2.81 0.051 1.05 -5 -9 3 -1.08 17.41 2.78 0.034 0.77 -1 2 0 13860.99 14717.98 2.77 1.000 3.68 -2 3 10 42.77 4.30 2.76 0.017 0.94 -1 5 2 8.52 0.26 2.70 0.004 1.52 -2 6 1 19.52 5.62 2.69 0.020 1.29 -3 -2 8 89.74 139.09 2.67 0.097 1.20 -2 -5 8 388.16 490.75 2.66 0.183 1.13 -3 -2 13 40.15 0.07 2.66 0.002 0.82 1 1 12 295.84 220.10 2.66 0.122 0.88 6 -6 3 21.49 3.07 2.66 0.014 0.90 -1 7 5 24.95 0.49 2.65 0.006 0.98 0 -6 13 40.61 80.36 2.64 0.074 0.81 -1 1 2 4884.57 5305.42 2.63 0.600 3.68 -5 -3 10 116.44 172.60 2.63 0.108 0.86 2 -9 4 13.53 0.04 2.62 0.002 0.93 0 2 0 150.58 198.95 2.57 0.116 4.26 5 3 3 256.80 193.17 2.56 0.115 1.10 1 -10 8 40.52 9.07 2.56 0.025 0.80 0 -8 10 17.33 1.87 2.56 0.011 0.86 -6 -6 8 -6.86 30.79 2.55 0.046 0.79 1 -10 7 -4.46 14.08 2.54 0.031 0.82 6 5 0 27.80 8.01 2.53 0.023 0.92 -1 -1 2 8277.28 8986.49 2.53 0.781 4.10 5 -7 3 57.52 17.18 2.52 0.034 0.93 -4 -3 5 19.42 43.09 2.51 0.054 1.27 8 0 1 58.44 22.52 2.50 0.039 0.84 0 10 2 18.27 1.60 2.47 0.010 0.82 Bond lengths and angles C1 - Distance Angles O1B 1.2579 (0.0034) O1A 1.2652 (0.0035) 124.13 (0.26) C2 1.5022 (0.0039) 117.65 (0.26) 118.20 (0.25) C1 - O1B O1A C2 - Distance Angles C3 1.3236 (0.0040) C1 1.5022 (0.0039) 122.87 (0.28) H2 0.9500 118.57 118.57 C2 - C3 C1 C3 - Distance Angles C2 1.3236 (0.0040) C4 1.5001 (0.0040) 123.28 (0.28) H3 0.9500 118.36 118.36 C3 - C2 C4 C4 - Distance Angles O4A 1.2560 (0.0035) O4B 1.2676 (0.0035) 124.27 (0.26) C3 1.5001 (0.0039) 118.83 (0.26) 116.90 (0.27) C4 - O4A O4B O1A - Distance Angles C1 1.2652 (0.0035) O1A - O1B - Distance Angles C1 1.2579 (0.0034) O1B - O4A - Distance Angles C4 1.2560 (0.0035) O4A - O4B - Distance Angles C4 1.2676 (0.0035) O4B - C22 - Distance Angles N21 1.4984 (0.0036) C23 1.5048 (0.0041) 110.37 (0.24) H22A 0.9900 109.58 109.58 H22B 0.9900 109.58 109.58 108.12 C22 - N21 C23 H22A C23 - Distance Angles N24 1.4930 (0.0036) C22 1.5048 (0.0041) 110.38 (0.24) H23A 0.9900 109.58 109.58 H23B 0.9900 109.58 109.58 108.12 C23 - N24 C22 H23A N24 - Distance Angles C25 1.4874 (0.0038) C23 1.4930 (0.0036) 111.93 (0.22) H24A 0.9200 109.23 109.23 H24B 0.9200 109.23 109.23 107.91 N24 - C25 C23 H24A C25 - Distance Angles N24 1.4874 (0.0038) C26 1.5096 (0.0041) 110.71 (0.24) H25A 0.9900 109.50 109.50 H25B 0.9900 109.50 109.50 108.07 C25 - N24 C26 H25A C26 - Distance Angles N21 1.4969 (0.0036) C25 1.5096 (0.0041) 109.72 (0.24) H26A 0.9900 109.72 109.72 H26B 0.9900 109.72 109.72 108.20 C26 - N21 C25 H26A C27 - Distance Angles N21 1.4879 (0.0037) H27A 0.9800 109.47 H27B 0.9800 109.47 109.47 H27C 0.9800 109.47 109.47 109.47 C27 - N21 H27A H27B N21 - Distance Angles C27 1.4879 (0.0037) C26 1.4969 (0.0036) 111.91 (0.23) C22 1.4984 (0.0036) 110.43 (0.23) 109.77 (0.21) H21 0.9300 108.21 108.21 108.21 N21 - C27 C26 C22 C31 - Distance Angles O31A 1.2178 (0.0037) O31B 1.3237 (0.0035) 123.98 (0.30) C32 1.4792 (0.0045) 123.28 (0.28) 112.74 (0.27) C31 - O31A O31B C32 - Distance Angles C32_$5 1.3198 (0.0060) C31 1.4792 (0.0045) 122.18 (0.38) H32 0.9500 118.91 118.91 C32 - C32_$5 C31 O31A - Distance Angles C31 1.2178 (0.0037) O31A - O31B - Distance Angles C31 1.3237 (0.0035) H31B 0.8400 109.47 O31B - C31 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.93 1.70 2.608(3) 165.7 N21-H21...O1A_$1 0.84 1.73 2.563(3) 171.2 O31B-H31B...O4B_$2 0.92 1.77 2.664(3) 161.9 N24-H24A...O1B_$3 0.92 1.84 2.719(3) 160.0 N24-H24B...O4A_$4 FMAP and GRID set by program FMAP 2 1 18 GRID -3.333 -2 -2 3.333 2 2 R1 = 0.1131 for 2952 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.32 at 0.4688 0.2504 0.1026 [ 1.82 A from H26A ] Deepest hole -0.31 at 0.0989 0.8077 0.3838 [ 0.58 A from H31B ] Mean = 0.00, Rms deviation from mean = 0.08 e/A^3, Highest memory used = 2450 / 17826 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.4688 0.2504 0.1026 1.00000 0.05 0.32 1.82 H26A 1.84 H21 1.95 O1A 2.11 H2 Q2 1 0.3010 0.9380 0.1202 1.00000 0.05 0.29 0.73 C1 0.83 O1B 1.79 O1A 1.81 C2 Q3 1 -0.4256 0.2260 0.1066 1.00000 0.05 0.29 1.72 H24A 1.86 O1A 1.98 H24B 2.17 N24 Q4 1 0.3679 0.4812 0.1827 1.00000 0.05 0.28 0.72 H26A 1.15 C26 1.47 H26B 1.87 N21 Q5 1 0.4486 0.8860 0.1307 1.00000 0.05 0.28 0.75 C2 0.76 C1 1.45 H2 1.72 O1B Q6 1 0.2100 0.6422 0.2638 1.00000 0.05 0.28 1.29 H26B 2.06 H31B 2.11 C26 2.12 H27C Q7 1 0.0669 -0.0999 0.1441 1.00000 0.05 0.28 1.75 H23A 1.77 O1B 2.36 C1 2.46 H25B Q8 1 -0.0409 0.2602 0.4663 1.00000 0.05 0.27 1.29 H22B 1.51 O31A 1.90 C22 1.94 H22A Q9 1 0.7426 1.3220 0.5817 1.00000 0.05 0.27 1.11 O31A 1.43 H27C 1.72 C31 2.19 H31B Q10 1 0.2524 0.3870 0.2108 1.00000 0.05 0.27 0.67 C26 0.85 N21 1.30 H26A 1.35 H26B Shortest distances between peaks (including symmetry equivalents) 1 3 0.75 2 5 1.12 4 10 1.20 2 7 1.64 6 9 1.73 4 6 1.90 8 9 2.00 1 10 2.16 1 4 2.17 6 10 2.21 5 7 2.59 3 5 2.66 3 4 2.68 1 5 2.74 3 10 2.79 2 3 2.83 1 2 2.95 4 9 2.99 Time profile in seconds ----------------------- 0.06: 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 0.02: Analyse other restraints etc. 0.41: 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 0.39: Structure factors and derivatives 0.66: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.09: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.08: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.05: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 07skc0014 finished at 12:11:37 Total CPU time: 1.8 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++