+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + shelxl started at 11:52:34 on 31-Mar-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008lsh045 in Pna2(1) CELL 0.71073 9.0662 10.3420 11.7380 90.000 90.000 90.000 ZERR 4.00 0.0003 0.0004 0.0004 0.000 0.000 0.000 LATT -1 SYMM - X, - Y, 1/2 + Z SYMM 1/2 + X, 1/2 - Y, Z SYMM 1/2 - X, 1/2 + Y, 1/2 + Z SFAC C H N O UNIT 52 48 8 4 V = 1100.59 F(000) = 448.0 Mu = 0.08 mm-1 Cell Wt = 848.98 Rho = 1.281 MERG 2 OMIT -3.00 55.00 EXTI 0.00953 EQIV $1 x-1/2, -y+3/2, z HTAB N1 O1_$1 HTAB N2 O1_$1 FMAP 2 PLAN 5 DFIX 0.88 0.02 N1 H1N N2 H2N SIZE 0.02 0.06 0.48 ACTA HTAB 2.00000 BOND $H WGHT 0.02540 0.53680 L.S. 6 TEMP -153.00 FVAR 0.90498 C1 1 -0.032093 0.674824 0.906172 11.00000 0.02041 0.03309 = 0.02420 -0.00217 0.00283 0.00932 C2 1 0.075757 0.746509 0.963307 11.00000 0.02390 0.02959 = 0.03208 -0.00182 -0.00067 0.00270 AFIX 43 H2 2 0.114113 0.823567 0.930702 11.00000 -1.20000 AFIX 0 C3 1 0.125876 0.703438 1.068258 11.00000 0.03111 0.04574 = 0.02849 -0.00491 -0.00565 0.00628 AFIX 43 H3 2 0.201230 0.750173 1.106562 11.00000 -1.20000 AFIX 0 C4 1 0.067759 0.593421 1.117998 11.00000 0.04571 0.04702 = 0.03180 0.00921 -0.00393 0.01368 AFIX 43 H4 2 0.101645 0.565573 1.190546 11.00000 -1.20000 AFIX 0 C5 1 -0.040295 0.524223 1.061065 11.00000 0.04508 0.03411 = 0.04472 0.01180 0.00322 0.00499 AFIX 43 H5 2 -0.080958 0.448781 1.094913 11.00000 -1.20000 AFIX 0 C6 1 -0.089354 0.564313 0.955211 11.00000 0.02976 0.02850 = 0.03764 0.00161 -0.00301 0.00274 AFIX 43 H6 2 -0.162552 0.515746 0.916189 11.00000 -1.20000 AFIX 0 C7 1 -0.011444 0.765803 0.712670 11.00000 0.01773 0.02467 = 0.02628 -0.00469 -0.00279 0.00172 C8 1 -0.036400 0.845071 0.516017 11.00000 0.02214 0.02861 = 0.02444 -0.00093 0.00056 0.00647 C9 1 0.083695 0.928668 0.510786 11.00000 0.02358 0.02756 = 0.03039 -0.00217 -0.00163 -0.00128 AFIX 43 H9 2 0.129633 0.957366 0.578992 11.00000 -1.20000 AFIX 0 C10 1 0.136217 0.970003 0.406245 11.00000 0.03063 0.02627 = 0.03976 0.00491 0.00439 0.00036 AFIX 43 H10 2 0.219568 1.025564 0.403198 11.00000 -1.20000 AFIX 0 C11 1 0.068581 0.931262 0.305770 11.00000 0.04131 0.03098 = 0.02819 0.00349 0.00391 0.00636 AFIX 43 H11 2 0.105802 0.958849 0.234125 11.00000 -1.20000 AFIX 0 C12 1 -0.053622 0.852008 0.311727 11.00000 0.03841 0.04036 = 0.03105 0.00093 -0.00669 -0.00186 AFIX 43 H12 2 -0.102642 0.827255 0.243601 11.00000 -1.20000 AFIX 0 C13 1 -0.105629 0.808196 0.415276 11.00000 0.02888 0.03486 = 0.03124 -0.00001 -0.00508 -0.00540 AFIX 43 H13 2 -0.189016 0.752644 0.417808 11.00000 -1.20000 AFIX 0 N1 3 -0.090848 0.717054 0.800363 11.00000 0.01497 0.03588 = 0.02370 0.00211 -0.00402 0.00009 N2 3 -0.094075 0.799710 0.620066 11.00000 0.01654 0.03404 = 0.02824 0.00014 -0.00410 -0.00234 O1 4 0.123826 0.778146 0.714789 11.00000 0.01494 0.04531 = 0.02889 -0.00107 -0.00089 -0.00008 H1N 2 -0.182835 0.707219 0.790765 11.00000 0.03862 H2N 2 -0.182627 0.773375 0.620183 11.00000 0.02521 HKLF 4 Covalent radii and connectivity table for 2008lsh045 in Pna2(1) C 0.770 H 0.320 N 0.700 O 0.660 C1 - C6 C2 N1 C2 - C3 C1 C3 - C4 C2 C4 - C3 C5 C5 - C6 C4 C6 - C1 C5 C7 - O1 N1 N2 C8 - C9 C13 N2 C9 - C10 C8 C10 - C9 C11 C11 - C12 C10 C12 - C11 C13 C13 - C12 C8 N1 - C7 C1 N2 - C7 C8 O1 - C7 Operators for generating equivalent atoms: $1 x-1/2, -y+3/2, z Floating origin restraints generated h k l Fo^2 Sigma Why rejected 5 0 0 21.01 4.86 observed but should be systematically absent 10051 Reflections read, of which 665 rejected -11 =< h =< 11, -13 =< k =< 13, -15 =< l =< 15, Max. 2-theta = 54.98 1 Systematic absence violations 0 Inconsistent equivalents 2433 Unique reflections, of which 0 suppressed R(int) = 0.0530 R(sigma) = 0.0550 Friedel opposites not merged Maximum memory for data reduction = 1634 / 24530 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 = 2052 / 192626 wR2 = 0.1075 before cycle 1 for 2433 data and 154 / 154 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.079; Restrained GooF = 1.080 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0254 * P )^2 + 0.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.90536 0.00226 0.170 OSF 2 0.00953 0.00223 -0.002 EXTI Mean shift/esd = 0.062 Maximum = -0.860 for x H1N Max. shift = 0.016 A for H2N Max. dU = 0.001 for H1N Least-squares cycle 2 Maximum vector length = 511 Memory required = 2052 / 192626 wR2 = 0.1075 before cycle 2 for 2433 data and 154 / 154 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.018 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.080; Restrained GooF = 1.079 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0254 * P )^2 + 0.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.90546 0.00225 0.044 OSF 2 0.00953 0.00223 0.001 EXTI Mean shift/esd = 0.025 Maximum = -0.340 for x H1N Max. shift = 0.006 A for H2N Max. dU = 0.001 for H1N Least-squares cycle 3 Maximum vector length = 511 Memory required = 2052 / 192626 wR2 = 0.1075 before cycle 3 for 2433 data and 154 / 154 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.012 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.080; Restrained GooF = 1.079 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0254 * P )^2 + 0.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.90548 0.00225 0.010 OSF 2 0.00953 0.00223 0.003 EXTI Mean shift/esd = 0.004 Maximum = 0.061 for U11 H2N Max. shift = 0.002 A for H1N Max. dU = 0.000 for H2N Least-squares cycle 4 Maximum vector length = 511 Memory required = 2052 / 192626 wR2 = 0.1075 before cycle 4 for 2433 data and 154 / 154 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.012 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.080; Restrained GooF = 1.079 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0254 * P )^2 + 0.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.90549 0.00225 0.003 OSF 2 0.00954 0.00223 0.002 EXTI Mean shift/esd = 0.001 Maximum = -0.012 for y H2N Max. shift = 0.000 A for H1N Max. dU = 0.000 for H2N Least-squares cycle 5 Maximum vector length = 511 Memory required = 2052 / 192626 wR2 = 0.1075 before cycle 5 for 2433 data and 154 / 154 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.012 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.080; Restrained GooF = 1.079 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0254 * P )^2 + 0.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.90549 0.00225 0.000 OSF 2 0.00954 0.00223 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.003 for y H2N Max. shift = 0.000 A for H2N Max. dU = 0.000 for H2N Least-squares cycle 6 Maximum vector length = 511 Memory required = 2052 / 192626 wR2 = 0.1075 before cycle 6 for 2433 data and 154 / 154 parameters Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.012 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.080; Restrained GooF = 1.079 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0254 * P )^2 + 0.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.90549 0.00225 0.000 OSF 2 0.00954 0.00223 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for y H2N Max. shift = 0.000 A for H2N Max. dU = 0.000 for H2N No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 7 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.1141 0.8235 0.9307 43 0.950 0.000 C2 C3 C1 H3 0.2012 0.7502 1.1065 43 0.950 0.000 C3 C4 C2 H4 0.1016 0.5656 1.1906 43 0.950 0.000 C4 C3 C5 H5 -0.0810 0.4488 1.0950 43 0.950 0.000 C5 C6 C4 H6 -0.1625 0.5158 0.9162 43 0.950 0.000 C6 C1 C5 H9 0.1296 0.9574 0.5790 43 0.950 0.000 C9 C10 C8 H10 0.2196 1.0255 0.4032 43 0.950 0.000 C10 C9 C11 H11 0.1057 0.9589 0.2341 43 0.950 0.000 C11 C12 C10 H12 -0.1026 0.8272 0.2436 43 0.950 0.000 C12 C11 C13 H13 -0.1890 0.7527 0.4178 43 0.950 0.000 C13 C12 C8 2008lsh045 in Pna2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 -0.03207 0.67481 0.90619 1.00000 0.02046 0.03291 0.02430 -0.00217 0.00280 0.00932 0.02589 0.00416 0.00024 0.00022 0.00021 0.00000 0.00106 0.00117 0.00121 0.00109 0.00099 0.00096 0.00050 C2 0.07574 0.74647 0.96330 1.00000 0.02389 0.02965 0.03216 -0.00176 -0.00059 0.00268 0.02857 0.00438 0.00025 0.00025 0.00022 0.00000 0.00112 0.00120 0.00128 0.00103 0.00103 0.00101 0.00052 H2 0.11409 0.82352 0.93068 1.00000 0.03428 0.00000 0.00000 C3 0.12586 0.70344 1.06824 1.00000 0.03093 0.04552 0.02878 -0.00486 -0.00566 0.00630 0.03507 0.00476 0.00028 0.00027 0.00022 0.00000 0.00131 0.00152 0.00131 0.00122 0.00111 0.00124 0.00060 H3 0.20125 0.75016 1.10651 1.00000 0.04209 0.00000 0.00000 C4 0.06770 0.59343 1.11803 1.00000 0.04581 0.04716 0.03183 0.00926 -0.00400 0.01370 0.04160 0.00547 0.00032 0.00029 0.00025 0.00000 0.00170 0.00166 0.00146 0.00126 0.00129 0.00140 0.00070 H4 0.10156 0.56561 1.19060 1.00000 0.04992 0.00000 0.00000 C5 -0.04034 0.52426 1.06111 1.00000 0.04498 0.03416 0.04483 0.01187 0.00323 0.00503 0.04132 0.00538 0.00031 0.00029 0.00024 0.00000 0.00157 0.00145 0.00164 0.00127 0.00136 0.00128 0.00067 H5 -0.08104 0.44883 1.09497 1.00000 0.04959 0.00000 0.00000 C6 -0.08936 0.56434 0.95521 1.00000 0.02968 0.02843 0.03767 0.00171 -0.00305 0.00285 0.03193 0.00452 0.00027 0.00024 0.00023 0.00000 0.00124 0.00124 0.00138 0.00108 0.00108 0.00102 0.00056 H6 -0.16255 0.51578 0.91618 1.00000 0.03831 0.00000 0.00000 C7 -0.01146 0.76581 0.71267 1.00000 0.01794 0.02465 0.02625 -0.00478 -0.00275 0.00184 0.02295 0.00380 0.00021 0.00022 0.00022 0.00000 0.00090 0.00108 0.00107 0.00095 0.00110 0.00092 0.00045 C8 -0.03641 0.84507 0.51601 1.00000 0.02208 0.02868 0.02442 -0.00104 0.00048 0.00652 0.02506 0.00430 0.00025 0.00023 0.00022 0.00000 0.00111 0.00128 0.00114 0.00109 0.00107 0.00095 0.00051 C9 0.08367 0.92866 0.51080 1.00000 0.02361 0.02761 0.03043 -0.00219 -0.00163 -0.00124 0.02722 0.00416 0.00025 0.00023 0.00023 0.00000 0.00117 0.00128 0.00123 0.00109 0.00105 0.00097 0.00053 H9 0.12959 0.95738 0.57901 1.00000 0.03266 0.00000 0.00000 C10 0.13618 0.96998 0.40624 1.00000 0.03047 0.02642 0.03957 0.00494 0.00428 0.00027 0.03215 0.00435 0.00026 0.00022 0.00022 0.00000 0.00120 0.00114 0.00141 0.00126 0.00121 0.00101 0.00055 H10 0.21956 1.02551 0.40319 1.00000 0.03858 0.00000 0.00000 C11 0.06855 0.93128 0.30579 1.00000 0.04128 0.03093 0.02835 0.00345 0.00398 0.00633 0.03352 0.00474 0.00030 0.00026 0.00022 0.00000 0.00154 0.00136 0.00146 0.00106 0.00117 0.00120 0.00062 H11 0.10575 0.95892 0.23415 1.00000 0.04022 0.00000 0.00000 C12 -0.05359 0.85201 0.31171 1.00000 0.03855 0.04030 0.03104 0.00082 -0.00659 -0.00201 0.03663 0.00473 0.00030 0.00028 0.00022 0.00000 0.00146 0.00159 0.00147 0.00117 0.00120 0.00123 0.00064 H12 -0.10257 0.82722 0.24358 1.00000 0.04396 0.00000 0.00000 C13 -0.10563 0.80820 0.41530 1.00000 0.02883 0.03493 0.03120 0.00001 -0.00504 -0.00539 0.03165 0.00423 0.00026 0.00024 0.00022 0.00000 0.00122 0.00127 0.00130 0.00120 0.00114 0.00096 0.00055 H13 -0.18903 0.75267 0.41783 1.00000 0.03799 0.00000 0.00000 N1 -0.09090 0.71706 0.80033 1.00000 0.01497 0.03588 0.02365 0.00225 -0.00390 0.00018 0.02483 0.00331 0.00020 0.00021 0.00016 0.00000 0.00095 0.00118 0.00108 0.00086 0.00078 0.00091 0.00046 N2 -0.09412 0.79968 0.62005 1.00000 0.01669 0.03392 0.02804 0.00020 -0.00412 -0.00223 0.02622 0.00348 0.00021 0.00021 0.00018 0.00000 0.00093 0.00108 0.00109 0.00091 0.00084 0.00092 0.00045 O1 0.12384 0.77817 0.71479 1.00000 0.01493 0.04546 0.02890 -0.00113 -0.00093 -0.00007 0.02977 0.00281 0.00015 0.00017 0.00016 0.00000 0.00065 0.00106 0.00082 0.00080 0.00074 0.00075 0.00041 H1N -0.18522 0.70756 0.79080 1.00000 0.04021 0.04082 0.00192 0.00288 0.00235 0.00000 0.00814 H2N -0.18454 0.77197 0.61997 1.00000 0.02656 0.03782 0.00199 0.00235 0.00223 0.00000 0.00687 Final Structure Factor Calculation for 2008lsh045 in Pna2(1) Total number of l.s. parameters = 154 Maximum vector length = 511 Memory required = 1900 / 25046 wR2 = 0.1075 before cycle 7 for 2433 data and 2 / 154 parameters Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.012 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.080; Restrained GooF = 1.079 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0254 * P )^2 + 0.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0500 for 1999 Fo > 4sig(Fo) and 0.0691 for all 2433 data wR2 = 0.1075, GooF = S = 1.080, Restrained GooF = 1.079 for all data Flack x parameter = -0.8049 with esd 2.0909 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 = 16.00 for non-hydrogen and 12.00 for hydrogen atoms Principal mean square atomic displacements U 0.0379 0.0255 0.0143 C1 0.0334 0.0294 0.0228 C2 0.0499 0.0312 0.0241 C3 0.0608 0.0412 0.0228 C4 0.0554 0.0424 0.0261 C5 0.0388 0.0318 0.0253 C6 0.0311 0.0206 0.0171 C7 0.0327 0.0245 0.0179 C8 0.0317 0.0273 0.0226 C9 0.0426 0.0293 0.0245 C10 0.0458 0.0289 0.0259 C11 0.0437 0.0390 0.0272 C12 0.0391 0.0327 0.0232 C13 0.0363 0.0248 0.0134 N1 0.0343 0.0292 0.0151 N2 0.0455 0.0289 0.0149 O1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.018 0.029 0.039 0.049 0.060 0.071 0.084 0.110 0.161 1.000 Number in group 247. 268. 233. 245. 233. 241. 236. 248. 237. 245. GooF 1.141 1.142 1.250 1.082 1.054 1.009 0.986 1.011 0.962 1.120 K 1.574 1.185 1.084 1.011 1.010 0.987 1.005 1.002 1.006 1.010 Resolution(A) 0.77 0.80 0.84 0.88 0.92 0.98 1.06 1.16 1.33 1.67 inf Number in group 252. 236. 247. 241. 247. 238. 245. 240. 243. 244. GooF 1.223 1.161 1.169 1.009 1.071 1.065 1.047 0.786 1.051 1.146 K 1.131 1.055 1.061 1.003 0.995 1.001 1.006 1.004 1.024 1.005 R1 0.248 0.183 0.131 0.100 0.086 0.054 0.043 0.027 0.037 0.024 Recommended weighting scheme: WGHT 0.0237 0.5473 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) 3 6 -3 42.46 13.01 5.36 0.032 1.40 3 6 3 38.38 12.98 3.86 0.032 1.40 6 6 4 72.07 33.61 3.34 0.052 1.06 7 1 -11 6.92 23.49 3.22 0.043 0.82 0 2 -10 331.33 259.12 3.16 0.143 1.14 1 2 14 39.00 13.74 3.06 0.033 0.82 1 12 -6 -2.99 8.00 3.04 0.025 0.79 8 9 1 -0.13 26.29 3.04 0.046 0.80 6 0 12 104.06 56.76 3.02 0.067 0.82 5 7 0 18.29 6.18 3.01 0.022 1.15 0 0 -2 1383.92 1609.54 2.99 0.357 5.87 9 7 1 4.07 40.73 2.98 0.057 0.83 4 11 -5 29.22 12.35 2.95 0.031 0.81 3 3 12 20.06 0.99 2.90 0.009 0.90 8 6 0 2.02 18.61 2.84 0.038 0.95 4 1 -5 571.66 497.85 2.83 0.198 1.61 6 0 0 2351.52 1994.48 2.83 0.397 1.51 1 4 13 87.45 55.92 2.82 0.067 0.85 5 4 -11 -7.33 7.85 2.81 0.025 0.87 10 0 8 57.61 27.48 2.76 0.047 0.77 4 1 14 28.05 1.18 2.75 0.010 0.78 8 6 5 -0.44 17.17 2.75 0.037 0.88 4 3 9 21.73 9.58 2.73 0.028 1.07 1 3 -13 27.83 5.59 2.71 0.021 0.87 5 1 10 58.59 80.82 2.68 0.080 0.98 4 1 5 568.58 497.92 2.67 0.199 1.61 8 5 -4 -3.26 8.06 2.66 0.025 0.94 5 3 9 68.25 91.37 2.66 0.085 1.01 2 1 0 54.23 73.08 2.64 0.076 4.15 2 6 -8 130.72 162.40 2.62 0.113 1.08 6 4 0 10.71 0.18 2.61 0.004 1.30 7 9 3 33.92 14.22 2.61 0.034 0.84 0 0 2 1405.31 1609.21 2.61 0.357 5.87 5 3 -9 68.47 91.25 2.60 0.085 1.01 8 4 8 18.60 5.98 2.60 0.022 0.85 6 6 -7 41.12 59.80 2.59 0.069 0.94 4 8 9 12.71 1.77 2.58 0.012 0.85 9 1 -8 -1.27 14.53 2.58 0.034 0.83 5 5 -10 106.02 71.08 2.57 0.075 0.89 7 3 -8 16.77 7.78 2.55 0.025 0.93 10 0 7 19.58 3.50 2.54 0.017 0.80 3 10 9 13.59 40.39 2.51 0.057 0.78 8 9 2 34.23 11.10 2.51 0.030 0.80 6 6 9 37.40 18.39 2.51 0.038 0.86 3 3 -12 15.66 1.01 2.50 0.009 0.90 8 0 2 94.68 124.26 2.50 0.099 1.11 7 8 3 -3.97 8.45 2.49 0.026 0.89 7 1 3 44.80 30.35 2.48 0.049 1.22 4 0 -2 -4.17 3.62 2.46 0.017 2.11 4 4 -9 48.75 65.77 2.46 0.072 1.04 Bond lengths and angles C1 - Distance Angles C6 1.3806 (0.0034) C2 1.3978 (0.0035) 120.12 (0.24) N1 1.4210 (0.0032) 118.53 (0.22) 121.25 (0.22) C1 - C6 C2 C2 - Distance Angles C3 1.3863 (0.0036) C1 1.3978 (0.0035) 119.02 (0.24) H2 0.9500 120.49 120.49 C2 - C3 C1 C3 - Distance Angles C4 1.3835 (0.0041) C2 1.3863 (0.0036) 120.96 (0.26) H3 0.9500 119.52 119.52 C3 - C4 C2 C4 - Distance Angles C3 1.3835 (0.0041) C5 1.3848 (0.0045) 119.38 (0.26) H4 0.9500 120.31 120.31 C4 - C3 C5 C5 - Distance Angles C6 1.3837 (0.0036) C4 1.3848 (0.0045) 120.39 (0.27) H5 0.9500 119.81 119.81 C5 - C6 C4 C6 - Distance Angles C1 1.3806 (0.0034) C5 1.3837 (0.0036) 120.10 (0.25) H6 0.9500 119.95 119.95 C6 - C1 C5 C7 - Distance Angles O1 1.2336 (0.0023) N1 1.3534 (0.0032) 123.53 (0.23) N2 1.3661 (0.0032) 122.34 (0.24) 114.12 (0.17) C7 - O1 N1 C8 - Distance Angles C9 1.3915 (0.0033) C13 1.3917 (0.0036) 119.06 (0.23) N2 1.4090 (0.0034) 122.38 (0.22) 118.52 (0.21) C8 - C9 C13 C9 - Distance Angles C10 1.3840 (0.0037) C8 1.3915 (0.0033) 119.99 (0.23) H9 0.9500 120.00 120.00 C9 - C10 C8 C10 - Distance Angles C9 1.3840 (0.0037) C11 1.3880 (0.0036) 120.82 (0.22) H10 0.9500 119.59 119.59 C10 - C9 C11 C11 - Distance Angles C12 1.3796 (0.0038) C10 1.3880 (0.0036) 118.89 (0.23) H11 0.9500 120.56 120.56 C11 - C12 C10 C12 - Distance Angles C11 1.3796 (0.0038) C13 1.3806 (0.0037) 120.91 (0.24) H12 0.9500 119.54 119.54 C12 - C11 C13 C13 - Distance Angles C12 1.3806 (0.0037) C8 1.3917 (0.0036) 120.27 (0.22) H13 0.9500 119.87 119.87 C13 - C12 C8 N1 - Distance Angles C7 1.3534 (0.0032) C1 1.4210 (0.0032) 125.42 (0.19) H1N 0.8679 (0.0168) 117.94 (1.92) 116.59 (1.93) N1 - C7 C1 N2 - Distance Angles C7 1.3661 (0.0032) C8 1.4090 (0.0034) 124.85 (0.19) H2N 0.8684 (0.0167) 115.72 (1.75) 117.36 (1.75) N2 - C7 C8 O1 - Distance Angles C7 1.2336 (0.0023) O1 - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.868(17) 1.953(19) 2.775(2) 157(3) N1-H1N...O1_$1 0.868(17) 2.13(2) 2.902(3) 148(2) N2-H2N...O1_$1 Hydrogen bonds with H..A < r(A) + 2.000 Angstroms and 110 deg. D-H d(D-H) d(H..A)