+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2007may0017 started at 11:23:45 on 05-Oct-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2007may0017 in Pna2(1) CELL 0.71073 7.8484 8.3983 24.1255 90.000 90.000 90.000 ZERR 8.00 0.0006 0.0007 0.0018 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 O UNIT 72 80 24 V = 1590.19 F(000) = 704.0 Mu = 0.10 mm-1 Cell Wt = 1329.36 Rho = 1.388 MERG 4 OMIT -3.00 55.00 FMAP 2 PLAN 5 ACTA EQIV $1 x + 1/2, -y - 1/2, z HTAB O4 O1_$1 HTAB O1 O4 DFIX 0.84 0.02 O1 H1O O4 H2O BOND $H L.S. 6 SIZE 0.1 0.08 0.02 TEMP -153.00 WGHT 0.142000 2.635000 FVAR 0.53230 MOLE 1 C1 1 -0.006138 0.074680 0.266208 11.00000 0.03876 0.03058 = 0.04788 -0.00058 -0.00647 -0.00133 AFIX 23 H1A 2 0.079898 0.149556 0.281079 11.00000 -1.20000 H1B 2 -0.120091 0.114306 0.277133 11.00000 -1.20000 AFIX 0 C2 1 0.005967 0.072399 0.203749 11.00000 0.03742 0.02211 = 0.04214 0.00113 0.00387 0.00572 C3 1 0.145806 0.141130 0.176644 11.00000 0.04266 0.02808 = 0.04417 0.00241 0.00582 -0.00647 AFIX 43 H3 2 0.234317 0.189284 0.197632 11.00000 -1.20000 AFIX 0 C4 1 0.155178 0.138943 0.119122 11.00000 0.04926 0.02666 = 0.07058 0.00136 0.01390 -0.00637 AFIX 43 H4 2 0.249741 0.186451 0.100936 11.00000 -1.20000 AFIX 0 C5 1 0.028337 0.068391 0.088355 11.00000 0.06052 0.02998 = 0.03735 -0.00090 0.01157 0.00330 AFIX 43 H5 2 0.034151 0.069380 0.049024 11.00000 -1.20000 AFIX 0 C6 1 -0.107997 -0.004160 0.114795 11.00000 0.05553 0.02376 = 0.03468 0.00058 0.00008 0.00432 C7 1 -0.346348 -0.171090 0.112025 11.00000 0.06104 0.06728 = 0.06142 0.00443 -0.00931 -0.03283 AFIX 23 H7A 2 -0.294217 -0.275705 0.120396 11.00000 -1.20000 H7B 2 -0.447968 -0.190142 0.088636 11.00000 -1.20000 AFIX 0 C8 1 -0.400118 -0.095705 0.164185 11.00000 0.04729 0.07243 = 0.04998 -0.00215 -0.00527 -0.01755 AFIX 23 H8A 2 -0.457838 0.006408 0.155953 11.00000 -1.20000 H8B 2 -0.482598 -0.165753 0.183404 11.00000 -1.20000 AFIX 0 C9 1 -0.118670 -0.001030 0.172148 11.00000 0.03772 0.02818 = 0.03987 0.00065 0.00377 0.00749 O1 3 0.020570 -0.080022 0.290424 11.00000 0.04211 0.03545 = 0.04685 0.00638 -0.00239 -0.00021 O2 3 -0.227530 -0.077069 0.081846 11.00000 0.05267 0.04145 = 0.03389 0.00003 -0.00346 -0.00472 O3 3 -0.255335 -0.066619 0.200111 11.00000 0.03998 0.03854 = 0.03913 0.00270 -0.00149 -0.00544 H1O 2 0.120022 -0.096449 0.279139 11.00000 0.06732 MOLE 2 C10 1 0.471689 -0.044951 0.309572 11.00000 0.04607 0.03592 = 0.04442 0.00158 -0.00462 -0.00993 AFIX 23 H10A 2 0.451980 0.067156 0.298627 11.00000 -1.20000 H10B 2 0.587776 -0.074494 0.297245 11.00000 -1.20000 AFIX 0 C11 1 0.464285 -0.056175 0.372011 11.00000 0.03258 0.02521 = 0.04580 0.00288 0.00141 0.00328 C12 1 0.335856 -0.135519 0.400739 11.00000 0.03327 0.03751 = 0.05694 -0.00714 -0.00390 -0.00104 AFIX 43 H12 2 0.245647 -0.184093 0.380653 11.00000 -1.20000 AFIX 0 C13 1 0.337279 -0.144857 0.457888 11.00000 0.03895 0.04083 = 0.04937 0.00363 0.01263 -0.00039 AFIX 43 H13 2 0.247507 -0.198227 0.476663 11.00000 -1.20000 AFIX 0 C14 1 0.467631 -0.077488 0.487745 11.00000 0.05137 0.03418 = 0.03485 0.00457 0.00291 -0.00172 AFIX 43 H14 2 0.469038 -0.085904 0.527011 11.00000 -1.20000 AFIX 0 C15 1 0.596961 0.002704 0.460510 11.00000 0.03148 0.02645 = 0.04378 -0.00126 0.00412 -0.00035 C16 1 0.835507 0.175881 0.461651 11.00000 0.04539 0.04517 = 0.03947 0.00162 -0.00602 -0.01082 AFIX 23 H16A 2 0.942682 0.191405 0.482605 11.00000 -1.20000 H16B 2 0.780671 0.281110 0.456769 11.00000 -1.20000 AFIX 0 C17 1 0.874013 0.104700 0.406149 11.00000 0.03199 0.04084 = 0.05397 -0.00367 0.00271 -0.00399 AFIX 23 H17A 2 0.957505 0.172470 0.386410 11.00000 -1.20000 H17B 2 0.925262 -0.002045 0.411164 11.00000 -1.20000 AFIX 0 C18 1 0.594802 0.012949 0.402175 11.00000 0.03887 0.02429 = 0.03748 0.00405 -0.00196 -0.00068 O4 3 0.352377 -0.142583 0.281471 11.00000 0.04590 0.02874 = 0.04999 -0.00702 -0.01052 0.00114 O5 3 0.723298 0.071405 0.492158 11.00000 0.05396 0.04205 = 0.03456 0.00134 -0.00179 -0.00363 O6 3 0.723261 0.091399 0.374005 11.00000 0.03847 0.04087 = 0.03688 -0.00013 -0.00236 -0.00609 H2O 2 0.382118 -0.238616 0.284212 11.00000 0.06695 HKLF 4 Covalent radii and connectivity table for 2007may0017 in Pna2(1) C 0.770 H 0.320 O 0.660 C1 - O1 C2 C2 - C9 C3 C1 C3 - C4 C2 C4 - C5 C3 C5 - C4 C6 C6 - O2 C9 C5 C7 - O2 C8 C8 - O3 C7 C9 - O3 C2 C6 O1 - C1 O2 - C6 C7 O3 - C9 C8 C10 - O4 C11 C11 - C18 C12 C10 C12 - C13 C11 C13 - C14 C12 C14 - C13 C15 C15 - O5 C14 C18 C16 - O5 C17 C17 - O6 C16 C18 - O6 C11 C15 O4 - C10 O5 - C15 C16 O6 - C18 C17 Operators for generating equivalent atoms: $1 x+1/2, -y-1/2, z Floating origin restraints generated h k l Fo^2 Sigma Why rejected 0 5 0 7.40 1.42 observed but should be systematically absent 0 2 1 6.39 1.22 observed but should be systematically absent 0 4 1 15.06 2.56 observed but should be systematically absent 0 4 1 11.11 1.75 observed but should be systematically absent 0 4 1 13.53 3.14 observed but should be systematically absent 0 4 1 13.51 2.20 observed but should be systematically absent 0 4 1 16.51 4.05 observed but should be systematically absent 0 1 2 4.44 0.92 observed but should be systematically absent 0 1 2 3.87 0.85 observed but should be systematically absent 0 1 2 3.39 0.79 observed but should be systematically absent 17116 Reflections read, of which 1440 rejected -10 =< h =< 10, -10 =< k =< 10, -31 =< l =< 31, Max. 2-theta = 55.00 10 Systematic absence violations 0 Inconsistent equivalents 1831 Unique reflections, of which 0 suppressed R(int) = 0.0666 R(sigma) = 0.0418 Friedel opposites merged Maximum memory for data reduction = 2324 / 18412 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 = 2957 / 277798 wR2 = 0.2736 before cycle 1 for 1831 data and 225 / 225 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 0.002 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.123; Restrained GooF = 1.122 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1420 * P )^2 + 2.63 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.53230 0.00397 -0.001 OSF Mean shift/esd = 0.001 Maximum = 0.002 for z O5 Max. shift = 0.000 A for H2O Max. dU = 0.000 for H1O Least-squares cycle 2 Maximum vector length = 511 Memory required = 2957 / 277798 wR2 = 0.2736 before cycle 2 for 1831 data and 225 / 225 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 0.002 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.123; Restrained GooF = 1.122 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1420 * P )^2 + 2.63 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.53230 0.00397 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for z C5 Max. shift = 0.000 A for H1O Max. dU = 0.000 for C9 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2957 / 277798 wR2 = 0.2736 before cycle 3 for 1831 data and 225 / 225 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 0.002 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.123; Restrained GooF = 1.122 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1420 * P )^2 + 2.63 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.53230 0.00397 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z O6 Max. shift = 0.000 A for H2O Max. dU = 0.000 for H1O Least-squares cycle 4 Maximum vector length = 511 Memory required = 2957 / 277798 wR2 = 0.2736 before cycle 4 for 1831 data and 225 / 225 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 0.002 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.123; Restrained GooF = 1.122 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1420 * P )^2 + 2.63 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.53230 0.00397 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z C14 Max. shift = 0.000 A for H1O Max. dU = 0.000 for H2O Least-squares cycle 5 Maximum vector length = 511 Memory required = 2957 / 277798 wR2 = 0.2736 before cycle 5 for 1831 data and 225 / 225 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 0.002 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.123; Restrained GooF = 1.122 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1420 * P )^2 + 2.63 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.53230 0.00397 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H2O Max. dU = 0.000 for H1O Least-squares cycle 6 Maximum vector length = 511 Memory required = 2957 / 277798 wR2 = 0.2736 before cycle 6 for 1831 data and 225 / 225 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 0.002 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.123; Restrained GooF = 1.122 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1420 * P )^2 + 2.63 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.53230 0.00397 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H1O Max. dU = 0.000 for H1O Largest correlation matrix elements 0.772 z H1O / x H1O 0.720 y H2O / x H2O Idealized hydrogen atom generation before cycle 7 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1A 0.0799 0.1496 0.2811 23 0.990 0.000 C1 O1 C2 H1B -0.1201 0.1143 0.2771 23 0.990 0.000 C1 O1 C2 H3 0.2343 0.1893 0.1976 43 0.950 0.000 C3 C4 C2 H4 0.2497 0.1865 0.1009 43 0.950 0.000 C4 C5 C3 H5 0.0342 0.0694 0.0490 43 0.950 0.000 C5 C4 C6 H7A -0.2942 -0.2757 0.1204 23 0.990 0.000 C7 O2 C8 H7B -0.4480 -0.1901 0.0886 23 0.990 0.000 C7 O2 C8 H8A -0.4578 0.0064 0.1560 23 0.990 0.000 C8 O3 C7 H8B -0.4826 -0.1658 0.1834 23 0.990 0.000 C8 O3 C7 H10A 0.4520 0.0672 0.2986 23 0.990 0.000 C10 O4 C11 H10B 0.5878 -0.0745 0.2972 23 0.990 0.000 C10 O4 C11 H12 0.2456 -0.1841 0.3807 43 0.950 0.000 C12 C13 C11 H13 0.2475 -0.1982 0.4767 43 0.950 0.000 C13 C14 C12 H14 0.4690 -0.0859 0.5270 43 0.950 0.000 C14 C13 C15 H16A 0.9427 0.1914 0.4826 23 0.990 0.000 C16 O5 C17 H16B 0.7807 0.2811 0.4568 23 0.990 0.000 C16 O5 C17 H17A 0.9575 0.1725 0.3864 23 0.990 0.000 C17 O6 C16 H17B 0.9253 -0.0020 0.4112 23 0.990 0.000 C17 O6 C16 2007may0017 in Pna2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 -0.00614 0.07468 0.26621 1.00000 0.03876 0.03058 0.04788 -0.00058 -0.00647 -0.00133 0.03907 0.01248 0.00098 0.00077 0.00034 0.00000 0.00382 0.00327 0.00407 0.00270 0.00302 0.00267 0.00160 H1A 0.07990 0.14956 0.28108 1.00000 0.04689 0.00000 0.00000 H1B -0.12009 0.11431 0.27713 1.00000 0.04689 0.00000 0.00000 C2 0.00597 0.07240 0.20375 1.00000 0.03742 0.02211 0.04214 0.00113 0.00387 0.00572 0.03389 0.01228 0.00089 0.00069 0.00031 0.00000 0.00356 0.00278 0.00390 0.00249 0.00305 0.00244 0.00149 C3 0.14581 0.14113 0.17664 1.00000 0.04266 0.02808 0.04417 0.00241 0.00582 -0.00647 0.03831 0.01275 0.00095 0.00079 0.00030 0.00000 0.00384 0.00319 0.00422 0.00270 0.00323 0.00285 0.00161 H3 0.23432 0.18928 0.19763 1.00000 0.04597 0.00000 0.00000 C4 0.15518 0.13894 0.11912 1.00000 0.04926 0.02666 0.07058 0.00136 0.01390 -0.00637 0.04883 0.01437 0.00102 0.00082 0.00038 0.00000 0.00450 0.00343 0.00598 0.00340 0.00424 0.00303 0.00209 H4 0.24974 0.18645 0.10094 1.00000 0.05860 0.00000 0.00000 C5 0.02834 0.06839 0.08835 1.00000 0.06052 0.02998 0.03735 -0.00090 0.01157 0.00330 0.04262 0.01447 0.00111 0.00082 0.00033 0.00000 0.00487 0.00346 0.00435 0.00263 0.00365 0.00311 0.00182 H5 0.03415 0.06938 0.04902 1.00000 0.05114 0.00000 0.00000 C6 -0.10800 -0.00416 0.11479 1.00000 0.05553 0.02376 0.03468 0.00058 0.00008 0.00432 0.03799 0.01296 0.00102 0.00075 0.00032 0.00000 0.00445 0.00305 0.00395 0.00247 0.00307 0.00289 0.00163 C7 -0.34635 -0.17109 0.11203 1.00000 0.06104 0.06728 0.06142 0.00443 -0.00931 -0.03283 0.06325 0.01515 0.00122 0.00124 0.00041 0.00000 0.00557 0.00566 0.00580 0.00467 0.00466 0.00485 0.00263 H7A -0.29422 -0.27571 0.12040 1.00000 0.07590 0.00000 0.00000 H7B -0.44797 -0.19014 0.08864 1.00000 0.07590 0.00000 0.00000 C8 -0.40012 -0.09571 0.16418 1.00000 0.04729 0.07243 0.04998 -0.00215 -0.00527 -0.01755 0.05657 0.01475 0.00119 0.00123 0.00038 0.00000 0.00478 0.00565 0.00512 0.00426 0.00379 0.00417 0.00224 H8A -0.45784 0.00641 0.15595 1.00000 0.06788 0.00000 0.00000 H8B -0.48260 -0.16575 0.18340 1.00000 0.06788 0.00000 0.00000 C9 -0.11867 -0.00103 0.17215 1.00000 0.03772 0.02818 0.03987 0.00065 0.00377 0.00749 0.03525 0.01261 0.00095 0.00076 0.00029 0.00000 0.00374 0.00308 0.00420 0.00248 0.00273 0.00266 0.00158 O1 0.02057 -0.08002 0.29042 1.00000 0.04211 0.03545 0.04685 0.00638 -0.00239 -0.00021 0.04147 0.00920 0.00067 0.00055 0.00024 0.00000 0.00296 0.00235 0.00287 0.00223 0.00244 0.00202 0.00120 O2 -0.22753 -0.07707 0.08185 1.00000 0.05267 0.04145 0.03389 0.00003 -0.00346 -0.00472 0.04267 0.00917 0.00072 0.00063 0.00022 0.00000 0.00325 0.00297 0.00296 0.00207 0.00246 0.00225 0.00130 O3 -0.25533 -0.06662 0.20011 1.00000 0.03998 0.03854 0.03913 0.00270 -0.00149 -0.00544 0.03922 0.00868 0.00063 0.00058 0.00023 0.00000 0.00267 0.00243 0.00279 0.00202 0.00227 0.00203 0.00119 H1O 0.12002 -0.09645 0.27914 1.00000 0.06732 0.18187 0.00581 0.01180 0.00449 0.00000 0.03109 C10 0.47169 -0.04495 0.30957 1.00000 0.04607 0.03592 0.04442 0.00158 -0.00462 -0.00993 0.04214 0.01273 0.00108 0.00089 0.00032 0.00000 0.00442 0.00329 0.00413 0.00285 0.00315 0.00305 0.00176 H10A 0.45198 0.06716 0.29863 1.00000 0.05056 0.00000 0.00000 H10B 0.58778 -0.07449 0.29725 1.00000 0.05056 0.00000 0.00000 C11 0.46428 -0.05617 0.37201 1.00000 0.03258 0.02521 0.04580 0.00288 0.00141 0.00328 0.03453 0.01245 0.00087 0.00073 0.00033 0.00000 0.00346 0.00285 0.00414 0.00269 0.00305 0.00236 0.00151 C12 0.33586 -0.13552 0.40074 1.00000 0.03327 0.03751 0.05694 -0.00714 -0.00390 -0.00104 0.04257 0.01297 0.00091 0.00089 0.00035 0.00000 0.00366 0.00371 0.00506 0.00325 0.00326 0.00282 0.00180 H12 0.24565 -0.18409 0.38065 1.00000 0.05109 0.00000 0.00000 C13 0.33728 -0.14486 0.45789 1.00000 0.03895 0.04083 0.04937 0.00363 0.01263 -0.00039 0.04305 0.01461 0.00097 0.00093 0.00034 0.00000 0.00393 0.00386 0.00448 0.00325 0.00320 0.00303 0.00173 H13 0.24751 -0.19823 0.47666 1.00000 0.05166 0.00000 0.00000 C14 0.46763 -0.07749 0.48775 1.00000 0.05137 0.03418 0.03485 0.00457 0.00291 -0.00172 0.04013 0.01340 0.00103 0.00080 0.00032 0.00000 0.00443 0.00358 0.00417 0.00267 0.00331 0.00304 0.00172 H14 0.46904 -0.08590 0.52701 1.00000 0.04816 0.00000 0.00000 C15 0.59696 0.00270 0.46051 1.00000 0.03148 0.02645 0.04378 -0.00126 0.00412 -0.00035 0.03390 0.01199 0.00083 0.00074 0.00033 0.00000 0.00341 0.00308 0.00434 0.00254 0.00282 0.00246 0.00154 C16 0.83551 0.17588 0.46165 1.00000 0.04539 0.04517 0.03947 0.00162 -0.00602 -0.01082 0.04334 0.01280 0.00098 0.00096 0.00031 0.00000 0.00420 0.00402 0.00412 0.00317 0.00318 0.00332 0.00175 H16A 0.94268 0.19141 0.48261 1.00000 0.05201 0.00000 0.00000 H16B 0.78067 0.28111 0.45677 1.00000 0.05201 0.00000 0.00000 C17 0.87401 0.10470 0.40615 1.00000 0.03199 0.04084 0.05397 -0.00367 0.00271 -0.00399 0.04226 0.01293 0.00093 0.00092 0.00034 0.00000 0.00336 0.00368 0.00466 0.00341 0.00333 0.00276 0.00170 H17A 0.95750 0.17247 0.38641 1.00000 0.05072 0.00000 0.00000 H17B 0.92526 -0.00205 0.41116 1.00000 0.05072 0.00000 0.00000 C18 0.59480 0.01295 0.40218 1.00000 0.03887 0.02429 0.03748 0.00405 -0.00196 -0.00068 0.03355 0.01225 0.00092 0.00075 0.00031 0.00000 0.00374 0.00291 0.00396 0.00251 0.00277 0.00255 0.00153 O4 0.35238 -0.14258 0.28147 1.00000 0.04590 0.02874 0.04999 -0.00702 -0.01052 0.00114 0.04154 0.00830 0.00065 0.00053 0.00024 0.00000 0.00275 0.00223 0.00299 0.00216 0.00238 0.00202 0.00121 O5 0.72330 0.07141 0.49216 1.00000 0.05396 0.04205 0.03456 0.00134 -0.00179 -0.00363 0.04352 0.00900 0.00073 0.00058 0.00021 0.00000 0.00324 0.00284 0.00300 0.00218 0.00247 0.00235 0.00130 O6 0.72326 0.09140 0.37400 1.00000 0.03847 0.04087 0.03688 -0.00013 -0.00236 -0.00609 0.03874 0.00833 0.00063 0.00057 0.00023 0.00000 0.00261 0.00241 0.00289 0.00222 0.00227 0.00208 0.00117 H2O 0.38212 -0.23862 0.28421 1.00000 0.06695 0.17124 0.01176 0.00420 0.00481 0.00000 0.02660 Final Structure Factor Calculation for 2007may0017 in Pna2(1) Total number of l.s. parameters = 225 Maximum vector length = 511 Memory required = 2734 / 24024 wR2 = 0.2736 before cycle 7 for 1831 data and 2 / 225 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 0.002 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.123; Restrained GooF = 1.122 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1420 * P )^2 + 2.63 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0938 for 1548 Fo > 4sig(Fo) and 0.1106 for all 1831 data wR2 = 0.2736, GooF = S = 1.123, Restrained GooF = 1.122 for all data Absolute structure cannot be determined reliably Occupancy sum of asymmetric unit = 24.00 for non-hydrogen and 20.00 for hydrogen atoms Principal mean square atomic displacements U 0.0512 0.0358 0.0302 C1 0.0450 0.0365 0.0202 C2 0.0496 0.0407 0.0246 C3 0.0775 0.0446 0.0244 C4 0.0655 0.0337 0.0287 C5 0.0561 0.0347 0.0232 C6 0.0995 0.0595 0.0307 C7 0.0815 0.0523 0.0360 C8 0.0446 0.0372 0.0240 C9 0.0503 0.0416 0.0325 O1 0.0549 0.0399 0.0332 O2 0.0460 0.0381 0.0335 O3 0.0544 0.0422 0.0298 C10 0.0464 0.0334 0.0237 C11 0.0597 0.0365 0.0315 C12 0.0583 0.0409 0.0300 C13 0.0519 0.0390 0.0294 C14 0.0451 0.0302 0.0264 C15 0.0577 0.0396 0.0327 C16 0.0555 0.0409 0.0304 C17 0.0408 0.0367 0.0231 C18 0.0599 0.0383 0.0264 O4 0.0552 0.0411 0.0343 O5 0.0461 0.0375 0.0326 O6 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.011 0.016 0.021 0.026 0.032 0.041 0.051 0.071 0.113 1.000 Number in group 212. 159. 193. 191. 175. 182. 173. 183. 180. 183. GooF 1.265 1.294 1.177 1.023 1.157 1.119 1.126 1.044 0.944 1.033 K 2.442 1.538 1.247 1.154 1.102 1.014 0.996 1.002 0.997 1.023 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.16 1.32 1.67 inf Number in group 188. 184. 182. 178. 185. 181. 185. 181. 184. 183. GooF 1.345 1.371 1.185 1.097 1.145 0.931 1.118 0.978 0.998 0.954 K 1.358 1.222 1.040 1.022 0.985 0.972 1.000 0.991 1.050 1.024 R1 0.269 0.272 0.216 0.170 0.161 0.100 0.098 0.070 0.070 0.050 Recommended weighting scheme: WGHT 0.1223 3.5041 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 0 4 2389.67 7002.83 5.47 0.453 6.03 2 5 0 252.68 106.79 4.39 0.056 1.54 9 5 2 183.77 51.80 4.05 0.039 0.77 0 1 21 18.53 86.00 3.86 0.050 1.14 7 1 2 89.37 33.72 3.60 0.031 1.11 2 8 16 31.89 2.78 3.41 0.009 0.84 9 2 7 58.94 6.52 3.39 0.014 0.83 0 1 19 6.99 51.77 3.24 0.039 1.26 0 0 20 26.12 91.71 3.20 0.052 1.21 4 0 18 1451.09 2668.60 3.15 0.280 1.11 1 3 27 33.03 5.36 3.15 0.013 0.85 7 3 21 42.93 9.13 3.06 0.016 0.77 5 2 8 409.47 720.19 3.03 0.145 1.32 1 3 28 21.03 0.22 2.96 0.003 0.82 9 3 2 28.59 83.52 2.91 0.049 0.83 7 1 0 780.46 478.02 2.89 0.118 1.11 8 6 8 38.13 6.18 2.87 0.013 0.78 4 10 1 38.29 4.04 2.85 0.011 0.77 1 2 29 45.22 14.38 2.84 0.021 0.81 3 3 26 17.44 0.28 2.81 0.003 0.83 5 4 1 86.40 40.25 2.79 0.034 1.26 9 1 9 59.68 15.41 2.77 0.021 0.83 1 2 25 59.61 22.79 2.75 0.026 0.93 0 1 27 33.35 0.99 2.72 0.005 0.89 5 9 8 16.63 0.57 2.67 0.004 0.78 6 3 8 124.13 224.97 2.67 0.081 1.10 1 6 24 41.86 13.43 2.66 0.020 0.81 4 3 1 110.13 59.54 2.65 0.042 1.60 1 4 27 117.93 62.91 2.64 0.043 0.82 2 1 27 33.65 8.02 2.64 0.015 0.87 5 5 3 128.20 70.01 2.63 0.045 1.14 7 1 21 71.42 33.34 2.58 0.031 0.80 4 6 1 1348.01 908.51 2.57 0.163 1.14 7 4 16 88.87 45.23 2.52 0.036 0.83 4 1 22 31.42 9.33 2.51 0.017 0.95 5 4 20 -4.50 9.25 2.51 0.016 0.87 4 0 28 251.69 150.73 2.50 0.066 0.79 7 2 2 78.78 40.59 2.49 0.034 1.08 0 2 14 26.32 63.05 2.48 0.043 1.59 6 6 0 39.85 3.04 2.46 0.009 0.96 1 6 20 -2.18 16.32 2.44 0.022 0.91 5 2 21 -4.60 7.94 2.44 0.015 0.91 4 4 21 14.81 0.79 2.42 0.005 0.90 4 6 14 0.19 14.53 2.41 0.021 0.95 2 4 26 28.96 7.21 2.41 0.015 0.83 9 3 1 -5.51 27.70 2.37 0.028 0.83 7 6 1 12.33 38.21 2.35 0.033 0.87 7 2 21 92.40 51.08 2.29 0.039 0.79 9 1 1 37.41 79.25 2.29 0.048 0.87 3 4 2 290.26 192.86 2.28 0.075 1.62 Bond lengths and angles C1 - Distance Angles O1 1.4399 (0.0081) C2 1.5100 (0.0108) 112.60 (0.57) H1A 0.9900 109.07 109.07 H1B 0.9900 109.07 109.07 107.83 C1 - O1 C2 H1A C2 - Distance Angles C9 1.3851 (0.0104) C3 1.4019 (0.0094) 118.65 (0.67) C1 1.5100 (0.0108) 120.70 (0.65) 120.63 (0.68) C2 - C9 C3 C3 - Distance Angles C4 1.3898 (0.0115) C2 1.4019 (0.0093) 120.12 (0.71) H3 0.9500 119.94 119.94 C3 - C4 C2 C4 - Distance Angles C5 1.3759 (0.0120) C3 1.3898 (0.0115) 120.40 (0.71) H4 0.9500 119.80 119.80 C4 - C5 C3 C5 - Distance Angles C4 1.3759 (0.0120) C6 1.3867 (0.0110) 119.96 (0.77) H5 0.9500 120.02 120.02 C5 - C4 C6 C6 - Distance Angles O2 1.3737 (0.0096) C9 1.3865 (0.0100) 123.00 (0.72) C5 1.3867 (0.0110) 117.17 (0.72) 119.82 (0.75) C6 - O2 C9 C7 - Distance Angles O2 1.4224 (0.0103) C8 1.4705 (0.0135) 112.78 (0.75) H7A 0.9900 109.03 109.03 H7B 0.9900 109.03 109.03 107.80 C7 - O2 C8 H7A C8 - Distance Angles O3 1.4499 (0.0101) C7 1.4705 (0.0135) 111.05 (0.80) H8A 0.9900 109.43 109.43 H8B 0.9900 109.43 109.43 108.03 C8 - O3 C7 H8A C9 - Distance Angles O3 1.3817 (0.0090) C2 1.3851 (0.0104) 117.20 (0.62) C6 1.3865 (0.0100) 121.78 (0.69) 121.00 (0.71) C9 - O3 C2 O1 - Distance Angles C1 1.4399 (0.0081) H1O 0.8381 (0.0210) 98.76 (7.20) O1 - C1 O2 - Distance Angles C6 1.3737 (0.0096) C7 1.4224 (0.0102) 113.52 (0.64) O2 - C6 O3 - Distance Angles C9 1.3817 (0.0090) C8 1.4499 (0.0101) 112.56 (0.59) O3 - C9 C10 - Distance Angles O4 1.4173 (0.0086) C11 1.5104 (0.0108) 114.55 (0.63) H10A 0.9900 108.62 108.62 H10B 0.9900 108.62 108.62 107.58 C10 - O4 C11 H10A C11 - Distance Angles C18 1.3842 (0.0100) C12 1.3930 (0.0104) 118.33 (0.71) C10 1.5104 (0.0108) 118.01 (0.65) 123.64 (0.69) C11 - C18 C12 C12 - Distance Angles C13 1.3810 (0.0117) C11 1.3930 (0.0104) 121.20 (0.71) H12 0.9500 119.40 119.40 C12 - C13 C11 C13 - Distance Angles C14 1.3732 (0.0117) C12 1.3810 (0.0117) 120.42 (0.71) H13 0.9500 119.79 119.79 C13 - C14 C12 C14 - Distance Angles C13 1.3732 (0.0117) C15 1.3840 (0.0102) 119.86 (0.75) H14 0.9500 120.07 120.07 C14 - C13 C15 C15 - Distance Angles O5 1.3781 (0.0090) C14 1.3840 (0.0102) 117.93 (0.72) C18 1.4101 (0.0099) 122.42 (0.61) 119.65 (0.66) C15 - O5 C14 C16 - Distance Angles O5 1.4447 (0.0090) C17 1.4972 (0.0110) 109.64 (0.61) H16A 0.9900 109.74 109.74 H16B 0.9900 109.74 109.74 108.21 C16 - O5 C17 H16A C17 - Distance Angles O6 1.4191 (0.0089) C16 1.4972 (0.0110) 110.60 (0.60) H17A 0.9900 109.53 109.53 H17B 0.9900 109.53 109.53 108.09 C17 - O6 C16 H17A C18 - Distance Angles O6 1.3829 (0.0086) C11 1.3842 (0.0100) 118.75 (0.68) C15 1.4101 (0.0099) 120.72 (0.61) 120.53 (0.64) C18 - O6 C11 O4 - Distance Angles C10 1.4173 (0.0087) H2O 0.8422 (0.0210) 109.47 (7.09) O4 - C10 O5 - Distance Angles C15 1.3781 (0.0090) C16 1.4447 (0.0090) 114.24 (0.57) O5 - C15 O6 - Distance Angles C18 1.3829 (0.0086) C17 1.4191 (0.0089) 112.13 (0.60) O6 - C18 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.84(2) 1.88(4) 2.686(7) 161(9) O4-H2O...O1_$1 0.84(2) 1.87(5) 2.665(7) 159(11) O1-H1O...O4 FMAP and GRID set by program FMAP 2 1 20 GRID -2.941 -2 -1 2.941 2 1 R1 = 0.1106 for 1831 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.50 at 0.1514 0.6932 0.1709 [ 0.93 A from C8 ] Deepest hole -0.38 at 0.3782 0.9584 0.4407 [ 1.01 A from C13 ] Mean = 0.00, Rms deviation from mean = 0.08 e/A^3, Highest memory used = 3020 / 29799 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.3486 -0.1932 0.1709 1.00000 0.05 0.50 0.93 C8 1.12 H8B 1.43 C7 1.47 H7A Q2 1 -0.4127 -0.0770 0.1204 1.00000 0.05 0.48 0.97 C7 1.07 C8 1.16 H8A 1.25 H7B Q3 1 -0.2707 -0.0737 0.2398 1.00000 0.05 0.46 0.97 O3 1.78 H10B 2.10 C8 2.11 C9 Q4 1 0.7243 0.0800 0.5278 1.00000 0.05 0.43 0.86 O5 1.99 C16 2.01 C15 2.24 H16A Q5 1 -0.1874 -0.0859 0.0503 1.00000 0.05 0.37 0.83 O2 1.81 C6 2.07 C7 2.17 H5 Shortest distances between peaks (including symmetry equivalents) 1 2 1.64 1 3 2.04 2 5 2.45 4 5 2.87 Time profile in seconds ----------------------- 0.12: 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. 0.76: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.01: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 1.47: Structure factors and derivatives 1.48: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.04: Apply other restraints 0.73: Solve l.s. equations 0.00: Generate HTAB table 0.05: Other dependent quantities, CIF, tables 0.06: Analysis of variance 0.04: Merge reflections for Fourier and .fcf 0.19: Fourier summations 0.04: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2007may0017 finished at 11:24:10 Total CPU time: 5.0 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++