+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - DOS/WIN95/NT VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + S92 started at 11:33:55 on 21-Sep-2001 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 01SRC832 in P2(1)/n CELL 0.71073 11.7592 25.9714 12.6411 90 96.581 90 ZERR 4 0.0004 0.0009 0.0005 0 0.002 0 LATT 1 SYMM 1/2-X, 1/2+Y, 1/2-Z SFAC C H O UNIT 168 192 32 V = 3835.19 F(000) = 1456.0 Mu = 0.08 mm-1 Cell Wt = 2723.22 Rho = 1.179 SHEL 7 0.84 ACTA TEMP -153 SIZE 0.1 0.07 0.07 EQIV $1 -x+2, -y, -z+1 HTAB O6 O7_$1 HTAB O8 O5_$1 HTAB FMAP 2 PLAN 20 L.S. 4 WGHT 0.085100 EXTI 0.003666 FVAR 0.13948 MOLE 1 C1 1 0.795398 0.303347 0.677890 11.00000 0.04260 0.03128 = 0.03932 0.00771 0.00945 -0.00035 AFIX 23 H1A 2 0.747914 0.304825 0.608030 11.00000 -1.20000 H1B 2 0.876469 0.308112 0.665922 11.00000 -1.20000 AFIX 0 C2 1 0.760077 0.345126 0.748759 11.00000 0.05022 0.02736 = 0.03917 0.00078 0.00271 0.00464 AFIX 23 H2A 2 0.774329 0.378859 0.716264 11.00000 -1.20000 H2B 2 0.808638 0.343218 0.818001 11.00000 -1.20000 AFIX 0 C3 1 0.635084 0.342477 0.768707 11.00000 0.05113 0.03774 = 0.05019 0.00178 0.01003 0.01052 AFIX 33 H3A 2 0.618151 0.370845 0.815567 11.00000 -1.50000 H3B 2 0.620453 0.309571 0.802600 11.00000 -1.50000 H3C 2 0.586118 0.345306 0.700807 11.00000 -1.50000 AFIX 0 C04 1 0.567464 0.201968 0.809816 11.00000 0.03345 0.03260 = 0.03521 -0.00976 0.00740 -0.00071 AFIX 23 H04A 2 0.533714 0.222385 0.747899 11.00000 -1.20000 H04B 2 0.628913 0.222917 0.848867 11.00000 -1.20000 AFIX 0 C5 1 0.476444 0.192003 0.881836 11.00000 0.03376 0.04102 = 0.03519 -0.00472 0.00816 -0.00380 AFIX 23 H5A 2 0.509486 0.171984 0.944598 11.00000 -1.20000 H5B 2 0.414053 0.171379 0.843346 11.00000 -1.20000 AFIX 0 C6 1 0.428165 0.242416 0.918475 11.00000 0.04790 0.04684 = 0.04571 -0.01167 0.01802 -0.00553 AFIX 33 H6A 2 0.368995 0.235168 0.965068 11.00000 -1.50000 H6B 2 0.394647 0.262024 0.856354 11.00000 -1.50000 H6C 2 0.489734 0.262551 0.957621 11.00000 -1.50000 AFIX 0 C7 1 0.818722 0.199011 1.016589 11.00000 0.05686 0.05105 = 0.03603 0.00352 0.01165 0.01137 AFIX 23 H7A 2 0.864028 0.186717 1.082595 11.00000 -1.20000 H7B 2 0.738302 0.188249 1.019045 11.00000 -1.20000 AFIX 0 C8 1 0.824072 0.255881 1.013038 11.00000 0.04905 0.04402 = 0.04670 -0.00502 0.00177 -0.00334 AFIX 23 H8A 2 0.784648 0.267990 0.944127 11.00000 -1.20000 H8B 2 0.905163 0.266728 1.017069 11.00000 -1.20000 AFIX 0 C9 1 0.768843 0.281376 1.103998 11.00000 0.04826 0.04430 = 0.05228 -0.01059 0.01038 0.00534 AFIX 33 H9A 2 0.773938 0.318894 1.097715 11.00000 -1.50000 H9B 2 0.809062 0.270387 1.172465 11.00000 -1.50000 H9C 2 0.688248 0.271135 1.099918 11.00000 -1.50000 AFIX 0 C10 1 0.620520 0.057600 1.082889 11.00000 0.08258 0.03718 = 0.04864 0.00275 0.03652 -0.00105 AFIX 23 H10A 2 0.686302 0.039346 1.122018 11.00000 -1.20000 H10B 2 0.566720 0.031563 1.048869 11.00000 -1.20000 AFIX 0 C11 1 0.560702 0.090341 1.159838 11.00000 0.09860 0.05209 = 0.05508 -0.00037 0.04392 -0.00627 AFIX 23 H11A 2 0.497883 0.109900 1.119250 11.00000 -1.20000 H11B 2 0.526386 0.067446 1.210172 11.00000 -1.20000 AFIX 0 C12 1 0.640691 0.127367 1.221709 11.00000 0.14489 0.07831 = 0.06668 -0.01972 0.05698 -0.01107 AFIX 33 H12A 2 0.598087 0.148014 1.268748 11.00000 -1.50000 H12B 2 0.674998 0.150125 1.172274 11.00000 -1.50000 H12C 2 0.701220 0.108138 1.264505 11.00000 -1.50000 AFIX 0 C13 1 0.972816 0.093543 0.505164 11.00000 0.03252 0.04328 = 0.03265 -0.00258 0.00298 -0.00323 C14 1 0.920880 0.133789 0.568083 11.00000 0.02887 0.03364 = 0.02956 -0.00009 0.00835 0.00285 C15 1 0.985580 0.158627 0.650702 11.00000 0.02635 0.03455 = 0.02629 0.00366 0.00487 -0.00014 AFIX 43 H15 2 1.062562 0.148214 0.670279 11.00000 -1.20000 AFIX 0 C16 1 0.940351 0.198536 0.705762 11.00000 0.02864 0.02955 = 0.02440 0.00367 0.00421 -0.00219 C17 1 0.826954 0.213040 0.674798 11.00000 0.03150 0.02707 = 0.02609 0.00386 0.01159 0.00220 C18 1 0.757354 0.186927 0.595113 11.00000 0.02469 0.03187 = 0.02419 0.00422 0.00642 -0.00135 C19 1 0.806363 0.147114 0.541665 11.00000 0.03297 0.03290 = 0.02552 -0.00135 0.00535 -0.00402 AFIX 43 H19 2 0.761227 0.128921 0.486744 11.00000 -1.20000 AFIX 0 C20 1 0.430861 0.084651 0.514549 11.00000 0.03678 0.05102 = 0.04248 -0.01753 -0.00409 -0.00423 AFIX 43 H20 2 0.384803 0.069105 0.456571 11.00000 -1.20000 AFIX 0 C21 1 0.436868 0.063402 0.614133 11.00000 0.03573 0.03613 = 0.05429 -0.01062 0.01066 -0.00454 AFIX 43 H21 2 0.397497 0.032124 0.623886 11.00000 -1.20000 AFIX 0 C22 1 0.499379 0.086635 0.701297 11.00000 0.02721 0.03335 = 0.04044 -0.00618 0.00972 -0.00068 C23 1 0.554748 0.133217 0.685075 11.00000 0.02168 0.03269 = 0.03420 -0.00589 0.00692 0.00062 C24 1 0.555818 0.154022 0.583493 11.00000 0.02441 0.03483 = 0.03361 -0.00197 0.00553 0.00531 C25 1 0.493007 0.129443 0.498629 11.00000 0.02906 0.04800 = 0.03519 -0.00867 0.00100 0.00534 AFIX 43 H25 2 0.492113 0.143145 0.428858 11.00000 -1.20000 AFIX 0 C26 1 0.878342 -0.010791 0.688708 11.00000 0.03492 0.02845 = 0.03917 -0.00002 0.00179 0.00220 C27 1 0.820704 0.014982 0.772000 11.00000 0.04103 0.02405 = 0.03011 -0.00026 0.00902 0.00321 C28 1 0.884381 0.033441 0.862892 11.00000 0.03829 0.02662 = 0.03442 0.00274 0.00896 0.00499 AFIX 43 H28 2 0.965132 0.029108 0.871312 11.00000 -1.20000 AFIX 0 C29 1 0.831997 0.058381 0.942662 11.00000 0.04733 0.02101 = 0.02780 0.00589 0.00866 0.00506 C30 1 0.713024 0.064008 0.927060 11.00000 0.04663 0.02350 = 0.02969 0.00151 0.01454 -0.00023 C31 1 0.647389 0.047507 0.833918 11.00000 0.03764 0.02475 = 0.04010 0.00447 0.01032 -0.00301 C32 1 0.702665 0.022388 0.756967 11.00000 0.03831 0.02803 = 0.03142 -0.00107 0.00869 0.00203 AFIX 43 H32 2 0.659542 0.010219 0.693764 11.00000 -1.20000 AFIX 0 C33 1 1.193925 0.120258 0.951896 11.00000 0.03567 0.04466 = 0.04610 -0.01002 -0.00418 0.00520 AFIX 43 H33 2 1.270869 0.108420 0.959386 11.00000 -1.20000 AFIX 0 C34 1 1.113247 0.095568 1.004354 11.00000 0.04847 0.03295 = 0.03504 -0.00533 -0.00803 0.01327 AFIX 43 H34 2 1.134780 0.066006 1.046183 11.00000 -1.20000 AFIX 0 C35 1 1.000200 0.113146 0.997283 11.00000 0.04674 0.03011 = 0.02212 -0.00536 -0.00050 0.00230 C36 1 0.972911 0.157713 0.938690 11.00000 0.03740 0.03282 = 0.02277 -0.00547 -0.00159 0.00710 C37 1 1.051366 0.181757 0.880272 11.00000 0.03265 0.03226 = 0.02669 -0.00622 -0.00001 -0.00268 C38 1 1.162476 0.162336 0.888301 11.00000 0.03083 0.04534 = 0.03402 -0.00380 -0.00246 0.00073 AFIX 43 H38 2 1.217434 0.178265 0.849468 11.00000 -1.20000 AFIX 0 C39 1 0.631828 0.199882 0.565572 11.00000 0.03131 0.03451 = 0.02392 0.00117 0.00370 0.00296 AFIX 23 H39A 2 0.619207 0.210283 0.489791 11.00000 -1.20000 H39B 2 0.610767 0.229288 0.609203 11.00000 -1.20000 AFIX 0 C40 1 0.520757 0.060934 0.808804 11.00000 0.03896 0.03168 = 0.04640 -0.00670 0.01728 -0.00993 AFIX 23 H40A 2 0.474208 0.029178 0.808992 11.00000 -1.20000 H40B 2 0.497435 0.084319 0.864287 11.00000 -1.20000 AFIX 0 C41 1 0.906090 0.081288 1.037662 11.00000 0.05502 0.03462 = 0.02637 0.00221 0.00467 0.00547 AFIX 23 H41A 2 0.858865 0.103248 1.079460 11.00000 -1.20000 H41B 2 0.940009 0.053400 1.084499 11.00000 -1.20000 AFIX 0 C42 1 1.010836 0.223039 0.800455 11.00000 0.02740 0.02892 = 0.02965 -0.00056 0.00258 -0.00329 AFIX 23 H42A 2 1.077547 0.241079 0.776599 11.00000 -1.20000 H42B 2 0.963879 0.248626 0.834010 11.00000 -1.20000 AFIX 0 O1 3 0.781075 0.253958 0.727455 11.00000 0.03319 0.02728 = 0.03104 0.00065 0.00692 0.00117 O2 3 0.617224 0.155977 0.771714 11.00000 0.02908 0.03248 = 0.03001 -0.00353 0.00555 -0.00177 O3 3 0.659579 0.090262 1.003252 11.00000 0.05064 0.03169 = 0.03537 -0.00095 0.01778 -0.00390 O4 3 0.861270 0.175467 0.926990 11.00000 0.03531 0.03585 = 0.03017 -0.00031 0.00748 0.00794 O5 3 0.912578 0.072374 0.428035 11.00000 0.04467 0.06023 = 0.05421 -0.02505 0.01081 -0.00288 O6 3 1.078333 0.083267 0.531203 11.00000 0.04450 0.06214 = 0.04596 -0.01004 0.00868 0.02192 AFIX 147 H6 2 1.099422 0.060736 0.489943 11.00000 -1.50000 AFIX 0 O7 3 0.820377 -0.026241 0.604172 11.00000 0.04150 0.05042 = 0.03886 -0.01149 0.00004 0.00674 O8 3 0.986822 -0.016797 0.707194 11.00000 0.04027 0.05470 = 0.04430 -0.01930 0.00416 0.00794 AFIX 147 H8 2 1.010815 -0.032303 0.655816 11.00000 -1.50000 HKLF 4 Covalent radii and connectivity table for 01SRC832 in P2(1)/n C 0.770 H 0.320 O 0.660 C1 - O1 C2 C2 - C1 C3 C3 - C2 C04 - O2 C5 C5 - C04 C6 C6 - C5 C7 - O4 C8 C8 - C7 C9 C9 - C8 C10 - O3 C11 C11 - C12 C10 C12 - C11 C13 - O5 O6 C14 C14 - C15 C19 C13 C15 - C14 C16 C16 - C15 C17 C42 C17 - O1 C16 C18 C18 - C19 C17 C39 C19 - C14 C18 C20 - C21 C25 C21 - C20 C22 C22 - C21 C23 C40 C23 - O2 C24 C22 C24 - C25 C23 C39 C25 - C24 C20 C26 - O7 O8 C27 C27 - C28 C32 C26 C28 - C27 C29 C29 - C30 C28 C41 C30 - O3 C29 C31 C31 - C32 C30 C40 C32 - C31 C27 C33 - C34 C38 C34 - C33 C35 C35 - C36 C34 C41 C36 - O4 C35 C37 C37 - C38 C36 C42 C38 - C33 C37 C39 - C18 C24 C40 - C22 C31 C41 - C35 C29 C42 - C37 C16 O1 - C17 C1 O2 - C23 C04 O3 - C30 C10 O4 - C36 C7 O5 - C13 O6 - C13 O7 - C26 O8 - C26 Operators for generating equivalent atoms: $1 -x+2, -y, -z+1 23567 Reflections read, of which 697 rejected -13 =< h =< 11, -30 =< k =< 30, -14 =< l =< 15, Max. 2-theta = 50.05 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 0 8 2 104.18 2.90 3 15.19 -1 9 3 235.66 4.02 4 48.52 -2 10 4 30.20 0.91 4 11.58 -1 16 4 67.68 2.14 4 11.84 2 21 5 23.50 0.89 5 5.89 2 9 6 92.46 1.70 6 13.20 6 Inconsistent equivalents 6703 Unique reflections, of which 0 suppressed R(int) = 0.0911 R(sigma) = 0.1302 Friedel opposites merged Maximum memory for data reduction = 4307 / 66246 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 = 5649 / 590154 wR2 = 0.2366 before cycle 1 for 6703 data and 454 / 454 parameters GooF = S = 1.257; Restrained GooF = 1.257 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0851 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.14635 0.00052 13.104 OSF 2 0.00366 0.00111 -0.009 EXTI 50 0.91717 0.00040 -3.227 z C6 66 0.82237 0.00045 -3.769 x C8 69 0.05977 0.00345 3.111 U11 C8 84 0.61883 0.00050 -3.344 x C10 93 0.55874 0.00057 -3.440 x C11 95 1.15822 0.00048 -3.376 z C11 104 1.21978 0.00055 -3.534 z C12 138 0.93917 0.00037 -3.216 x C16 158 0.59382 0.00034 -3.853 z C18 176 0.51256 0.00043 -4.669 z C20 185 0.61175 0.00042 -5.614 z C21 194 0.69944 0.00038 -4.955 z C22 203 0.68368 0.00036 -3.827 z C23 221 0.49707 0.00038 -4.125 z C25 246 0.88261 0.00040 -4.402 x C28 255 0.83031 0.00041 -4.101 x C29 266 0.92587 0.00036 -3.290 z C30 273 0.64620 0.00039 -3.043 x C31 275 0.83259 0.00038 -3.451 z C31 291 1.19109 0.00044 -6.439 x C33 300 1.11101 0.00044 -5.051 x C34 309 0.99833 0.00041 -4.594 x C35 318 0.97123 0.00039 -4.264 x C36 327 1.04964 0.00039 -4.460 x C37 336 1.16049 0.00039 -5.065 x C38 356 0.80707 0.00038 -4.516 z C40 363 0.90428 0.00042 -4.302 x C41 381 0.78024 0.00024 -3.540 x O1 390 0.61620 0.00023 -4.412 x O2 392 0.77074 0.00022 -4.366 z O2 399 0.65790 0.00026 -6.419 x O3 401 1.00187 0.00024 -5.657 z O3 402 0.05725 0.00214 3.089 U11 O3 408 0.85991 0.00025 -5.499 x O4 419 0.42669 0.00029 -4.676 z O5 420 0.05171 0.00223 3.160 U11 O5 426 1.07702 0.00030 -4.355 x O6 445 0.98580 0.00029 -3.518 x O8 446 -0.01756 0.00014 -5.581 y O8 Mean shift/esd = 1.186 Maximum = 13.104 for OSF Max. shift = 0.062 A for H8 Max. dU = 0.004 for C12 Least-squares cycle 2 Maximum vector length = 511 Memory required = 5649 / 590154 wR2 = 0.1966 before cycle 2 for 6703 data and 454 / 454 parameters GooF = S = 1.087; Restrained GooF = 1.087 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0851 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.14676 0.00044 0.941 OSF 2 0.00353 0.00092 -0.132 EXTI 399 0.65722 0.00022 -3.097 x O3 Mean shift/esd = 0.524 Maximum = -3.097 for x O3 Max. shift = 0.048 A for H8 Max. dU = 0.002 for C7 Least-squares cycle 3 Maximum vector length = 511 Memory required = 5649 / 590154 wR2 = 0.1926 before cycle 3 for 6703 data and 454 / 454 parameters GooF = S = 1.064; Restrained GooF = 1.064 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0851 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.14680 0.00043 0.091 OSF 2 0.00354 0.00089 0.001 EXTI Mean shift/esd = 0.052 Maximum = -0.572 for U22 O8 Max. shift = 0.023 A for H8 Max. dU = 0.000 for C7 Least-squares cycle 4 Maximum vector length = 511 Memory required = 5649 / 590154 wR2 = 0.1925 before cycle 4 for 6703 data and 454 / 454 parameters GooF = S = 1.064; Restrained GooF = 1.064 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0851 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.14680 0.00043 0.012 OSF 2 0.00354 0.00089 0.004 EXTI Mean shift/esd = 0.013 Maximum = -0.232 for tors H8 Max. shift = 0.011 A for H8 Max. dU = 0.000 for C12 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 H1A 0.7484 0.3052 0.6070 23 0.990 0.000 C1 O1 C2 H1B 0.8765 0.3083 0.6663 23 0.990 0.000 C1 O1 C2 H2A 0.7728 0.3787 0.7162 23 0.990 0.000 C2 C1 C3 H2B 0.8076 0.3429 0.8175 23 0.990 0.000 C2 C1 C3 H3A 0.6180 0.3708 0.8160 33 0.980 0.000 C3 C2 H3A H3B 0.6200 0.3095 0.8033 33 0.980 0.000 C3 C2 H3A H3C 0.5851 0.3451 0.7014 33 0.980 0.000 C3 C2 H3A H04A 0.5321 0.2224 0.7467 23 0.990 0.000 C04 O2 C5 H04B 0.6272 0.2229 0.8477 23 0.990 0.000 C04 O2 C5 H5A 0.5080 0.1718 0.9433 23 0.990 0.000 C5 C04 C6 H5B 0.4127 0.1710 0.8419 23 0.990 0.000 C5 C04 C6 H6A 0.3671 0.2349 0.9633 33 0.980 0.000 C6 C5 H6A H6B 0.3927 0.2616 0.8544 33 0.980 0.000 C6 C5 H6A H6C 0.4877 0.2624 0.9557 33 0.980 0.000 C6 C5 H6A H7A 0.8652 0.1875 1.0823 23 0.990 0.000 C7 O4 C8 H7B 0.7383 0.1881 1.0211 23 0.990 0.000 C7 O4 C8 H8A 0.7805 0.2675 0.9437 23 0.990 0.000 C8 C7 C9 H8B 0.9021 0.2672 1.0149 23 0.990 0.000 C8 C7 C9 H9A 0.7727 0.3191 1.0971 33 0.980 0.000 C9 C8 H9A H9B 0.8082 0.2706 1.1719 33 0.980 0.000 C9 C8 H9A H9C 0.6868 0.2714 1.1004 33 0.980 0.000 C9 C8 H9A H10A 0.6841 0.0399 1.1221 23 0.990 0.000 C10 O3 C11 H10B 0.5647 0.0315 1.0489 23 0.990 0.000 C10 O3 C11 H11A 0.4956 0.1104 1.1163 23 0.990 0.000 C11 C12 C10 H11B 0.5233 0.0685 1.2084 23 0.990 0.000 C11 C12 C10 H12A 0.5953 0.1490 1.2663 33 0.980 0.000 C12 C11 H12A H12B 0.6719 0.1511 1.1695 33 0.980 0.000 C12 C11 H12A H12C 0.6989 0.1094 1.2620 33 0.980 0.000 C12 C11 H12A H15 1.0609 0.1480 0.6707 43 0.950 0.000 C15 C14 C16 H19 0.7605 0.1295 0.4857 43 0.950 0.000 C19 C14 C18 H20 0.3857 0.0699 0.4535 43 0.950 0.000 C20 C21 C25 H21 0.3989 0.0321 0.6199 43 0.950 0.000 C21 C20 C22 H25 0.4935 0.1434 0.4269 43 0.950 0.000 C25 C24 C20 H28 0.9627 0.0293 0.8718 43 0.950 0.000 C28 C27 C29 H32 0.6591 0.0099 0.6936 43 0.950 0.000 C32 C31 C27 H33 1.2669 0.1078 0.9602 43 0.950 0.000 C33 C34 C38 H34 1.1315 0.0660 1.0470 43 0.950 0.000 C34 C33 C35 H38 1.2149 0.1784 0.8497 43 0.950 0.000 C38 C33 C37 H39A 0.6192 0.2106 0.4888 23 0.990 0.000 C39 C18 C24 H39B 0.6113 0.2294 0.6085 23 0.990 0.000 C39 C18 C24 H40A 0.4733 0.0292 0.8063 23 0.990 0.000 C40 C22 C31 H40B 0.4962 0.0843 0.8618 23 0.990 0.000 C40 C22 C31 H41A 0.8564 0.1033 1.0783 23 0.990 0.000 C41 C35 C29 H41B 0.9375 0.0535 1.0836 23 0.990 0.000 C41 C35 C29 H42A 1.0766 0.2404 0.7766 23 0.990 0.000 C42 C37 C16 H42B 0.9629 0.2486 0.8336 23 0.990 0.000 C42 C37 C16 H6 1.0970 0.0602 0.4899 147 0.840 0.000 O6 C13 H6 H8 1.0080 -0.0369 0.6611 147 0.840 0.000 O8 C26 H8 01SRC832 in P2(1)/n ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.79514 0.30352 0.67724 1.00000 0.04311 0.02692 0.03687 0.00798 0.00634 0.00058 0.03550 0.00669 0.00033 0.00013 0.00030 0.00000 0.00248 0.00209 0.00220 0.00189 0.00179 0.00165 0.00094 H1A 0.74842 0.30516 0.60701 1.00000 0.04260 0.00000 0.00000 H1B 0.87648 0.30831 0.66626 1.00000 0.04260 0.00000 0.00000 C2 0.75884 0.34487 0.74839 1.00000 0.05432 0.02409 0.03788 0.00173 -0.00014 0.00369 0.03918 0.00661 0.00033 0.00014 0.00030 0.00000 0.00284 0.00201 0.00218 0.00189 0.00188 0.00176 0.00099 H2A 0.77281 0.37870 0.71618 1.00000 0.04702 0.00000 0.00000 H2B 0.80762 0.34294 0.81751 1.00000 0.04702 0.00000 0.00000 C3 0.63451 0.34235 0.76910 1.00000 0.05918 0.03472 0.04550 -0.00031 0.00580 0.01344 0.04648 0.00737 0.00035 0.00015 0.00032 0.00000 0.00308 0.00223 0.00243 0.00210 0.00207 0.00193 0.00109 H3A 0.61803 0.37079 0.81597 1.00000 0.06972 0.00000 0.00000 H3B 0.62003 0.30950 0.80326 1.00000 0.06972 0.00000 0.00000 H3C 0.58509 0.34515 0.70145 1.00000 0.06972 0.00000 0.00000 C04 0.56589 0.20193 0.80854 1.00000 0.04071 0.02982 0.03458 -0.00959 0.00862 -0.00096 0.03471 0.00650 0.00032 0.00014 0.00029 0.00000 0.00243 0.00208 0.00214 0.00184 0.00177 0.00172 0.00093 H04A 0.53208 0.22237 0.74669 1.00000 0.04165 0.00000 0.00000 H04B 0.62719 0.22291 0.84773 1.00000 0.04165 0.00000 0.00000 C5 0.47486 0.19173 0.88043 1.00000 0.03784 0.04189 0.03737 -0.00272 0.00721 -0.00359 0.03881 0.00680 0.00032 0.00015 0.00030 0.00000 0.00245 0.00236 0.00219 0.00196 0.00182 0.00176 0.00098 H5A 0.50798 0.17181 0.94330 1.00000 0.04657 0.00000 0.00000 H5B 0.41268 0.17100 0.84191 1.00000 0.04657 0.00000 0.00000 C6 0.42630 0.24214 0.91669 1.00000 0.05391 0.04060 0.04747 -0.01248 0.02164 -0.00177 0.04610 0.00717 0.00035 0.00015 0.00032 0.00000 0.00284 0.00242 0.00248 0.00211 0.00208 0.00195 0.00108 H6A 0.36712 0.23491 0.96328 1.00000 0.06915 0.00000 0.00000 H6B 0.39273 0.26163 0.85442 1.00000 0.06915 0.00000 0.00000 H6C 0.48774 0.26239 0.95574 1.00000 0.06915 0.00000 0.00000 C7 0.81811 0.19933 1.01679 1.00000 0.07234 0.05132 0.03995 0.00620 0.02187 0.02011 0.05334 0.00860 0.00041 0.00016 0.00033 0.00000 0.00326 0.00280 0.00249 0.00227 0.00221 0.00225 0.00119 H7A 0.86518 0.18755 1.08226 1.00000 0.06401 0.00000 0.00000 H7B 0.73831 0.18812 1.02113 1.00000 0.06401 0.00000 0.00000 C8 0.82146 0.25588 1.01239 1.00000 0.06645 0.04451 0.04373 -0.00538 0.00145 -0.00051 0.05194 0.00755 0.00039 0.00016 0.00033 0.00000 0.00315 0.00258 0.00246 0.00226 0.00216 0.00213 0.00115 H8A 0.78051 0.26750 0.94375 1.00000 0.06233 0.00000 0.00000 H8B 0.90212 0.26720 1.01486 1.00000 0.06233 0.00000 0.00000 C9 0.76744 0.28157 1.10367 1.00000 0.05168 0.04170 0.05319 -0.01209 0.00830 0.00632 0.04868 0.00746 0.00037 0.00016 0.00033 0.00000 0.00277 0.00242 0.00260 0.00221 0.00209 0.00199 0.00110 H9A 0.77270 0.31907 1.09711 1.00000 0.07302 0.00000 0.00000 H9B 0.80824 0.27063 1.17192 1.00000 0.07302 0.00000 0.00000 H9C 0.68683 0.27144 1.10036 1.00000 0.07302 0.00000 0.00000 C10 0.61812 0.05782 1.08240 1.00000 0.09100 0.03949 0.04628 0.00249 0.03584 -0.00818 0.05676 0.00851 0.00042 0.00016 0.00035 0.00000 0.00363 0.00255 0.00255 0.00227 0.00244 0.00230 0.00125 H10A 0.68405 0.03994 1.12215 1.00000 0.06811 0.00000 0.00000 H10B 0.56467 0.03151 1.04893 1.00000 0.06811 0.00000 0.00000 C11 0.55806 0.09098 1.15772 1.00000 0.10587 0.05454 0.05453 0.00050 0.04427 -0.00512 0.06893 0.00951 0.00047 0.00019 0.00038 0.00000 0.00416 0.00299 0.00292 0.00268 0.00286 0.00277 0.00145 H11A 0.49556 0.11037 1.11625 1.00000 0.08271 0.00000 0.00000 H11B 0.52326 0.06845 1.20839 1.00000 0.08271 0.00000 0.00000 C12 0.63799 0.12839 1.21925 1.00000 0.15625 0.08082 0.06440 -0.02564 0.05283 -0.01895 0.09738 0.01032 0.00057 0.00023 0.00043 0.00000 0.00585 0.00397 0.00345 0.00340 0.00363 0.00389 0.00199 H12A 0.59531 0.14902 1.26626 1.00000 0.14607 0.00000 0.00000 H12B 0.67185 0.15114 1.16952 1.00000 0.14607 0.00000 0.00000 H12C 0.69887 0.10937 1.26204 1.00000 0.14607 0.00000 0.00000 C13 0.97148 0.09361 0.50428 1.00000 0.03522 0.03950 0.03264 -0.00095 0.00893 0.00156 0.03540 0.00717 0.00035 0.00015 0.00029 0.00000 0.00262 0.00233 0.00219 0.00203 0.00191 0.00189 0.00094 C14 0.91935 0.13359 0.56668 1.00000 0.03329 0.03212 0.02942 -0.00324 0.00846 0.00029 0.03123 0.00630 0.00031 0.00013 0.00028 0.00000 0.00241 0.00212 0.00200 0.00179 0.00171 0.00168 0.00089 C15 0.98410 0.15857 0.65057 1.00000 0.02758 0.03122 0.03146 0.00446 0.00430 0.00099 0.03002 0.00621 0.00030 0.00013 0.00027 0.00000 0.00210 0.00202 0.00203 0.00188 0.00161 0.00163 0.00086 H15 1.06088 0.14802 0.67074 1.00000 0.03602 0.00000 0.00000 C16 0.93866 0.19862 0.70537 1.00000 0.02870 0.02734 0.02268 0.00169 0.00632 -0.00240 0.02598 0.00588 0.00029 0.00013 0.00025 0.00000 0.00228 0.00195 0.00188 0.00169 0.00155 0.00159 0.00084 C17 0.82575 0.21300 0.67455 1.00000 0.03818 0.02485 0.02327 0.00400 0.01542 0.00094 0.02784 0.00637 0.00030 0.00013 0.00026 0.00000 0.00247 0.00192 0.00189 0.00170 0.00171 0.00164 0.00086 C18 0.75705 0.18702 0.59344 1.00000 0.02852 0.02853 0.02170 0.00278 0.00586 -0.00175 0.02602 0.00592 0.00028 0.00013 0.00026 0.00000 0.00222 0.00197 0.00185 0.00173 0.00159 0.00158 0.00084 C19 0.80585 0.14752 0.54080 1.00000 0.03706 0.03072 0.02144 -0.00028 0.00513 -0.00639 0.02960 0.00625 0.00031 0.00013 0.00027 0.00000 0.00244 0.00203 0.00178 0.00175 0.00160 0.00170 0.00087 H19 0.76054 0.12954 0.48567 1.00000 0.03552 0.00000 0.00000 C20 0.43183 0.08517 0.51171 1.00000 0.04789 0.04483 0.04472 -0.01394 -0.00278 -0.00343 0.04644 0.00715 0.00035 0.00016 0.00035 0.00000 0.00275 0.00256 0.00258 0.00228 0.00202 0.00206 0.00108 H20 0.38568 0.06985 0.45351 1.00000 0.05573 0.00000 0.00000 C21 0.43780 0.06360 0.61082 1.00000 0.03798 0.03533 0.06124 -0.01317 0.00911 -0.00693 0.04458 0.00699 0.00033 0.00015 0.00035 0.00000 0.00251 0.00227 0.00300 0.00232 0.00208 0.00181 0.00107 H21 0.39890 0.03213 0.61988 1.00000 0.05350 0.00000 0.00000 C22 0.49958 0.08667 0.69882 1.00000 0.03427 0.03295 0.03791 -0.00519 0.00772 -0.00071 0.03477 0.00640 0.00030 0.00014 0.00029 0.00000 0.00234 0.00214 0.00221 0.00198 0.00177 0.00175 0.00092 C23 0.55393 0.13332 0.68323 1.00000 0.02203 0.03083 0.03223 -0.00528 0.00520 0.00153 0.02820 0.00603 0.00028 0.00013 0.00028 0.00000 0.00203 0.00208 0.00205 0.00182 0.00158 0.00157 0.00085 C24 0.55610 0.15442 0.58219 1.00000 0.02642 0.03369 0.03215 -0.00148 0.00558 0.00429 0.03058 0.00615 0.00028 0.00014 0.00028 0.00000 0.00216 0.00209 0.00209 0.00187 0.00161 0.00162 0.00087 C25 0.49373 0.12967 0.49659 1.00000 0.03712 0.04644 0.03341 -0.00403 -0.00313 0.00580 0.03955 0.00652 0.00031 0.00015 0.00030 0.00000 0.00244 0.00252 0.00220 0.00203 0.00181 0.00194 0.00100 H25 0.49347 0.14338 0.42689 1.00000 0.04746 0.00000 0.00000 C26 0.87781 -0.01131 0.68857 1.00000 0.03776 0.02594 0.03808 -0.00257 0.00329 0.00519 0.03401 0.00706 0.00035 0.00013 0.00031 0.00000 0.00273 0.00206 0.00237 0.00187 0.00193 0.00173 0.00094 C27 0.81958 0.01464 0.77116 1.00000 0.04513 0.02314 0.02738 0.00116 0.00594 0.00061 0.03175 0.00643 0.00033 0.00013 0.00028 0.00000 0.00270 0.00192 0.00204 0.00174 0.00179 0.00169 0.00090 C28 0.88191 0.03346 0.86275 1.00000 0.04525 0.02179 0.03693 0.00398 0.00423 0.00469 0.03469 0.00657 0.00033 0.00013 0.00029 0.00000 0.00249 0.00193 0.00226 0.00188 0.00189 0.00169 0.00094 H28 0.96269 0.02926 0.87183 1.00000 0.04163 0.00000 0.00000 C29 0.82953 0.05828 0.94159 1.00000 0.05096 0.02049 0.02579 0.00365 0.00724 0.00296 0.03219 0.00649 0.00034 0.00013 0.00027 0.00000 0.00283 0.00191 0.00202 0.00173 0.00179 0.00170 0.00092 C30 0.71157 0.06430 0.92537 1.00000 0.05500 0.01784 0.03112 0.00219 0.01828 0.00016 0.03362 0.00689 0.00035 0.00013 0.00029 0.00000 0.00286 0.00185 0.00213 0.00176 0.00194 0.00173 0.00093 C31 0.64560 0.04754 0.83216 1.00000 0.04655 0.02190 0.03689 0.00191 0.01361 -0.00302 0.03443 0.00669 0.00032 0.00013 0.00030 0.00000 0.00259 0.00193 0.00224 0.00184 0.00189 0.00169 0.00092 C32 0.70202 0.02226 0.75670 1.00000 0.05054 0.02336 0.02852 0.00030 0.00699 -0.00271 0.03395 0.00667 0.00034 0.00013 0.00029 0.00000 0.00282 0.00195 0.00204 0.00177 0.00182 0.00174 0.00094 H32 0.65910 0.00986 0.69359 1.00000 0.04074 0.00000 0.00000 C33 1.19010 0.11988 0.95266 1.00000 0.04037 0.04175 0.04047 -0.00951 -0.00681 0.01160 0.04175 0.00666 0.00035 0.00015 0.00031 0.00000 0.00258 0.00244 0.00229 0.00220 0.00197 0.00199 0.00103 H33 1.26686 0.10781 0.96022 1.00000 0.05010 0.00000 0.00000 C34 1.11000 0.09544 1.00489 1.00000 0.05544 0.03140 0.03059 -0.00305 -0.00790 0.00901 0.04014 0.00660 0.00036 0.00015 0.00030 0.00000 0.00301 0.00217 0.00213 0.00194 0.00201 0.00203 0.00103 H34 1.13151 0.06597 1.04700 1.00000 0.04817 0.00000 0.00000 C35 0.99743 0.11298 0.99749 1.00000 0.05384 0.02989 0.02047 -0.00508 0.00153 0.00423 0.03495 0.00633 0.00034 0.00014 0.00027 0.00000 0.00285 0.00214 0.00186 0.00177 0.00173 0.00190 0.00096 C36 0.97055 0.15778 0.93856 1.00000 0.03896 0.02879 0.02031 -0.00243 -0.00385 0.00672 0.02992 0.00604 0.00032 0.00013 0.00026 0.00000 0.00245 0.00206 0.00182 0.00178 0.00163 0.00174 0.00088 C37 1.04896 0.18160 0.88060 1.00000 0.03170 0.03049 0.02342 -0.00660 -0.00438 0.00135 0.02912 0.00593 0.00031 0.00013 0.00027 0.00000 0.00237 0.00202 0.00189 0.00175 0.00164 0.00168 0.00088 C38 1.15968 0.16249 0.88827 1.00000 0.03452 0.04430 0.03744 -0.00661 -0.00159 -0.00267 0.03920 0.00630 0.00032 0.00015 0.00030 0.00000 0.00250 0.00243 0.00224 0.00210 0.00175 0.00191 0.00099 H38 1.21487 0.17839 0.84968 1.00000 0.04704 0.00000 0.00000 C39 0.63205 0.20004 0.56453 1.00000 0.03286 0.03571 0.02890 0.00392 0.00260 0.00366 0.03256 0.00626 0.00029 0.00014 0.00028 0.00000 0.00240 0.00217 0.00203 0.00179 0.00165 0.00169 0.00092 H39A 0.61923 0.21059 0.48884 1.00000 0.03908 0.00000 0.00000 H39B 0.61130 0.22938 0.60847 1.00000 0.03908 0.00000 0.00000 C40 0.51994 0.06091 0.80651 1.00000 0.04038 0.02844 0.04848 -0.00649 0.01700 -0.01082 0.03818 0.00658 0.00031 0.00014 0.00031 0.00000 0.00255 0.00204 0.00250 0.00196 0.00189 0.00173 0.00098 H40A 0.47328 0.02918 0.80634 1.00000 0.04582 0.00000 0.00000 H40B 0.49623 0.08430 0.86181 1.00000 0.04582 0.00000 0.00000 C41 0.90381 0.08136 1.03666 1.00000 0.05477 0.03210 0.02651 0.00360 0.00299 0.00977 0.03792 0.00651 0.00033 0.00014 0.00028 0.00000 0.00271 0.00214 0.00201 0.00185 0.00181 0.00187 0.00098 H41A 0.85643 0.10331 1.07833 1.00000 0.04550 0.00000 0.00000 H41B 0.93755 0.05348 1.08362 1.00000 0.04550 0.00000 0.00000 C42 1.00942 0.22273 0.80034 1.00000 0.03278 0.02847 0.03167 0.00044 0.00511 -0.00125 0.03086 0.00595 0.00030 0.00013 0.00027 0.00000 0.00222 0.00199 0.00201 0.00178 0.00165 0.00161 0.00087 H42A 1.07662 0.24045 0.77664 1.00000 0.03704 0.00000 0.00000 H42B 0.96292 0.24860 0.83363 1.00000 0.03704 0.00000 0.00000 O1 0.77986 0.25391 0.72672 1.00000 0.03642 0.02294 0.03043 0.00150 0.00682 0.00178 0.02970 0.00390 0.00019 0.00008 0.00017 0.00000 0.00152 0.00129 0.00129 0.00117 0.00108 0.00103 0.00060 O2 0.61582 0.15609 0.77041 1.00000 0.03380 0.02905 0.03026 -0.00377 0.00523 -0.00294 0.03092 0.00388 0.00019 0.00009 0.00018 0.00000 0.00146 0.00132 0.00133 0.00122 0.00109 0.00108 0.00060 O3 0.65720 0.09063 1.00138 1.00000 0.05964 0.02798 0.03590 0.00103 0.02142 -0.00277 0.03994 0.00445 0.00022 0.00009 0.00019 0.00000 0.00182 0.00137 0.00142 0.00129 0.00127 0.00120 0.00068 O4 0.85927 0.17541 0.92630 1.00000 0.04123 0.03374 0.03240 0.00135 0.00864 0.00792 0.03545 0.00429 0.00021 0.00009 0.00018 0.00000 0.00167 0.00143 0.00142 0.00123 0.00115 0.00121 0.00064 O5 0.91184 0.07286 0.42624 1.00000 0.05477 0.06224 0.05070 -0.02705 0.00936 -0.00665 0.05565 0.00490 0.00024 0.00011 0.00023 0.00000 0.00192 0.00201 0.00180 0.00163 0.00151 0.00145 0.00083 O6 1.07641 0.08328 0.53022 1.00000 0.05242 0.06115 0.04393 -0.01107 0.00858 0.02105 0.05226 0.00517 0.00025 0.00011 0.00021 0.00000 0.00205 0.00205 0.00168 0.00151 0.00141 0.00149 0.00079 H6 1.09698 0.06021 0.48989 1.00000 0.07839 0.00000 0.00000 O7 0.82040 -0.02636 0.60349 1.00000 0.04616 0.05171 0.03555 -0.01310 -0.00171 0.00815 0.04497 0.00459 0.00022 0.00010 0.00020 0.00000 0.00176 0.00176 0.00156 0.00143 0.00131 0.00130 0.00073 O8 0.98517 -0.01780 0.70791 1.00000 0.04981 0.05385 0.04603 -0.02392 0.00286 0.01026 0.05010 0.00471 0.00025 0.00011 0.00021 0.00000 0.00208 0.00189 0.00174 0.00147 0.00141 0.00141 0.00078 H8 1.00796 -0.03693 0.66107 1.00000 0.07515 0.00000 0.00000 Final Structure Factor Calculation for 01SRC832 in P2(1)/n Total number of l.s. parameters = 454 Maximum vector length = 511 Memory required = 5195 / 21973 wR2 = 0.1925 before cycle 5 for 6703 data and 0 / 454 parameters GooF = S = 1.063; Restrained GooF = 1.063 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0851 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0726 for 3374 Fo > 4sig(Fo) and 0.1671 for all 6703 data wR2 = 0.1925, GooF = S = 1.063, Restrained GooF = 1.063 for all data Occupancy sum of asymmetric unit = 50.00 for non-hydrogen and 48.00 for hydrogen atoms Principal mean square atomic displacements U 0.0439 0.0402 0.0224 C1 0.0569 0.0373 0.0234 C2 0.0653 0.0455 0.0287 C3 0.0448 0.0375 0.0218 C04 0.0454 0.0368 0.0343 C5 0.0682 0.0440 0.0261 C6 0.0882 0.0407 0.0311 C7 0.0681 0.0492 0.0385 C8 0.0615 0.0535 0.0311 C9 0.1022 0.0420 0.0261 C10 0.1203 0.0547 0.0318 C11 0.1742 0.0812 0.0368 C12 0.0401 0.0383 0.0278 C13 0.0366 0.0327 0.0243 C14 0.0359 0.0273 0.0268 C15 0.0307 0.0275 0.0197 C16 0.0439 0.0254 0.0142 C17 0.0303 0.0288 0.0190 C18 0.0410 0.0269 0.0209 C19 0.0607 0.0501 0.0285 C20 0.0673 0.0386 0.0278 C21 0.0422 0.0332 0.0289 C22 0.0369 0.0274 0.0204 C23 0.0358 0.0327 0.0232 C24 0.0526 0.0374 0.0286 C25 0.0414 0.0371 0.0235 C26 0.0452 0.0272 0.0228 C27 0.0462 0.0378 0.0201 C28 0.0514 0.0266 0.0186 C29 0.0596 0.0240 0.0172 C30 0.0510 0.0317 0.0206 C31 0.0509 0.0280 0.0230 C32 0.0645 0.0316 0.0292 C33 0.0654 0.0286 0.0264 C34 0.0555 0.0311 0.0182 C35 0.0457 0.0255 0.0185 C36 0.0400 0.0297 0.0177 C37 0.0485 0.0407 0.0284 C38 0.0388 0.0324 0.0264 C39 0.0597 0.0330 0.0219 C40 0.0586 0.0312 0.0240 C41 0.0337 0.0310 0.0279 C42 0.0377 0.0289 0.0226 O1 0.0365 0.0305 0.0257 O2 0.0661 0.0294 0.0243 O3 0.0471 0.0316 0.0277 O4 0.0849 0.0532 0.0288 O5 0.0805 0.0488 0.0274 O6 0.0660 0.0407 0.0282 O7 0.0790 0.0474 0.0239 O8 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.008 0.015 0.023 0.031 0.041 0.053 0.069 0.092 0.138 1.000 Number in group 723. 659. 715. 620. 656. 694. 657. 642. 668. 669. GooF 0.825 0.822 0.937 0.965 1.052 1.188 1.168 1.198 1.215 1.178 K 5.009 1.864 1.169 1.056 0.980 1.012 1.009 0.994 1.019 1.024 Resolution(A) 0.84 0.87 0.90 0.95 1.00 1.06 1.14 1.25 1.43 1.78 inf Number in group 671. 679. 662. 683. 673. 658. 669. 676. 658. 674. GooF 0.863 0.868 0.869 0.922 1.036 1.024 1.075 1.052 1.211 1.536 K 1.168 1.163 1.094 1.009 1.006 1.024 1.029 1.024 1.034 1.011 R1 0.466 0.400 0.342 0.253 0.182 0.130 0.101 0.099 0.084 0.059 Recommended weighting scheme: WGHT 0.1053 0.0000 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) -5 7 1 288.53 131.65 6.22 0.049 1.98 0 0 2 3372.59 6380.74 4.90 0.340 6.28 5 6 1 353.52 589.48 4.85 0.103 2.00 -4 2 1 606.82 401.24 4.33 0.085 2.85 1 2 1 1938.77 2888.80 4.16 0.229 6.87 3 1 6 1249.12 860.17 4.04 0.125 1.76 2 2 0 3040.48 4476.33 4.04 0.285 5.33 2 14 1 102.33 204.98 3.95 0.061 1.74 3 0 3 568.04 387.35 3.95 0.084 2.70 5 8 1 252.21 153.02 3.91 0.053 1.85 2 6 2 1211.50 835.46 3.89 0.123 2.96 -1 2 3 330.43 195.96 3.88 0.060 3.90 -2 1 1 702.23 493.78 3.81 0.095 5.42 3 4 1 466.61 322.94 3.80 0.076 3.15 2 5 2 270.82 412.09 3.78 0.086 3.19 4 3 2 876.25 1266.75 3.78 0.151 2.44 5 17 10 580.97 74.89 3.71 0.037 0.87 -4 15 2 190.92 313.35 3.69 0.075 1.47 1 9 1 716.53 1036.49 3.62 0.137 2.72 -3 1 2 460.84 668.29 3.60 0.110 3.46 0 1 7 286.97 168.61 3.60 0.055 1.79 -4 3 5 387.77 260.22 3.58 0.069 1.97 -5 0 1 166.19 44.97 3.51 0.029 2.35 3 10 3 162.52 62.62 3.48 0.034 1.87 5 1 6 142.57 77.09 3.46 0.037 1.47 6 17 4 86.19 195.61 3.43 0.059 1.10 4 10 5 327.29 213.57 3.39 0.062 1.48 2 19 3 257.58 144.01 3.33 0.051 1.26 -4 4 1 1575.95 1167.97 3.33 0.145 2.66 -7 17 8 -15.42 127.70 3.31 0.048 0.95 4 4 3 0.00 65.04 3.28 0.034 2.15 -2 11 4 23.21 136.60 3.26 0.050 1.83 -10 10 3 285.05 488.83 3.22 0.094 1.06 1 4 3 637.10 864.67 3.18 0.125 3.28 4 14 1 370.05 522.53 3.15 0.097 1.54 1 4 0 1878.52 2526.17 3.14 0.214 5.68 0 4 0 5556.22 7581.53 3.14 0.370 6.49 -3 5 6 266.57 165.13 3.11 0.055 1.82 4 4 1 246.73 167.45 3.07 0.055 2.55 0 6 3 1799.76 1349.20 3.05 0.156 3.01 -1 4 13 211.80 59.82 3.05 0.033 0.96 1 9 3 1072.71 1442.51 3.04 0.162 2.30 -3 22 5 450.88 693.58 3.02 0.112 1.04 4 2 7 66.30 128.14 3.01 0.048 1.45 6 16 1 63.81 146.33 3.00 0.051 1.23 7 14 3 55.78 128.02 2.98 0.048 1.16 5 3 2 1614.02 1240.49 2.97 0.150 2.05 -1 4 1 388.58 539.48 2.97 0.099 5.28 8 15 4 0.05 108.50 2.96 0.044 1.02 1 3 6 394.37 289.41 2.96 0.072 1.97 Bond lengths and angles C1 - Distance Angles O1 1.4522 (0.0040) C2 1.4943 (0.0051) 108.69 (0.29) C1 - O1 C2 - Distance Angles C1 1.4943 (0.0051) C3 1.5159 (0.0054) 114.87 (0.31) C2 - C1 C3 - Distance Angles C2 1.5159 (0.0054) C3 - C04 - Distance Angles O2 1.4350 (0.0041) C5 1.5049 (0.0052) 113.81 (0.30) C04 - O2 C5 - Distance Angles C04 1.5049 (0.0052) C6 1.5200 (0.0052) 110.38 (0.32) C5 - C04 C6 - Distance Angles C5 1.5200 (0.0052) C6 - C7 - Distance Angles O4 1.4337 (0.0045) C8 1.4705 (0.0058) 112.93 (0.34) C7 - O4 C8 - Distance Angles C7 1.4705 (0.0058) C9 1.5324 (0.0057) 113.03 (0.37) C8 - C7 C9 - Distance Angles C8 1.5324 (0.0057) C9 - C10 - Distance Angles O3 1.4472 (0.0046) C11 1.5170 (0.0061) 108.56 (0.33) C10 - O3 C11 - Distance Angles C12 1.5049 (0.0070) C10 1.5170 (0.0061) 112.50 (0.44) C11 - C12 C12 - Distance Angles C11 1.5049 (0.0070) C12 - C13 - Distance Angles O5 1.2637 (0.0044) O6 1.2686 (0.0042) 123.22 (0.35) C14 1.4787 (0.0051) 119.27 (0.35) 117.45 (0.33) C13 - O5 O6 C14 - Distance Angles C15 1.3928 (0.0048) C19 1.3854 (0.0048) 119.08 (0.32) C13 1.4787 (0.0051) 120.62 (0.33) 120.29 (0.32) C14 - C15 C19 C15 - Distance Angles C14 1.3928 (0.0048) C16 1.3901 (0.0048) 121.34 (0.32) C15 - C14 C16 - Distance Angles C15 1.3901 (0.0048) C17 1.3912 (0.0047) 118.06 (0.30) C42 1.5156 (0.0046) 119.77 (0.30) 122.05 (0.30) C16 - C15 C17 C17 - Distance Angles O1 1.3917 (0.0040) C16 1.3912 (0.0047) 118.79 (0.29) C18 1.4033 (0.0047) 119.43 (0.30) 121.77 (0.31) C17 - O1 C16 C18 - Distance Angles C19 1.3828 (0.0048) C17 1.4033 (0.0047) 118.20 (0.31) C39 1.5118 (0.0047) 119.68 (0.30) 122.11 (0.30) C18 - C19 C17 C19 - Distance Angles C14 1.3854 (0.0048) C18 1.3828 (0.0048) 121.45 (0.31) C19 - C14 C20 - Distance Angles C21 1.3668 (0.0058) C25 1.3907 (0.0056) 119.59 (0.37) C20 - C21 C21 - Distance Angles C20 1.3668 (0.0058) C22 1.3926 (0.0052) 121.55 (0.37) C21 - C20 C22 - Distance Angles C21 1.3926 (0.0052) C23 1.3943 (0.0050) 117.81 (0.35) C40 1.5111 (0.0052) 122.92 (0.34) 118.96 (0.32) C22 - C21 C23 C23 - Distance Angles O2 1.3820 (0.0040) C24 1.3926 (0.0049) 119.98 (0.30) C22 1.3943 (0.0050) 117.84 (0.31) 121.89 (0.33) C23 - O2 C24 C24 - Distance Angles C25 1.3928 (0.0049) C23 1.3926 (0.0049) 117.88 (0.34) C39 1.5156 (0.0050) 120.86 (0.33) 121.04 (0.31) C24 - C25 C23 C25 - Distance Angles C24 1.3928 (0.0049) C20 1.3907 (0.0056) 120.93 (0.37) C25 - C24 C26 - Distance Angles O7 1.2643 (0.0042) O8 1.2694 (0.0042) 123.03 (0.34) C27 1.4754 (0.0052) 119.82 (0.35) 117.15 (0.33) C26 - O7 O8 C27 - Distance Angles C28 1.3864 (0.0050) C32 1.3877 (0.0051) 118.89 (0.33) C26 1.4754 (0.0052) 120.54 (0.35) 120.53 (0.32) C27 - C28 C32 C28 - Distance Angles C27 1.3864 (0.0050) C29 1.3889 (0.0051) 121.84 (0.36) C28 - C27 C29 - Distance Angles C30 1.3876 (0.0051) C28 1.3889 (0.0051) 117.66 (0.33) C41 1.5250 (0.0050) 123.01 (0.32) 119.13 (0.35) C29 - C30 C28 C30 - Distance Angles O3 1.3930 (0.0043) C29 1.3876 (0.0051) 118.91 (0.32) C31 1.4036 (0.0052) 118.56 (0.34) 122.42 (0.33) C30 - O3 C29 C31 - Distance Angles C32 1.3879 (0.0051) C30 1.4036 (0.0052) 117.51 (0.35) C40 1.5164 (0.0052) 119.49 (0.33) 122.66 (0.33) C31 - C32 C30 C32 - Distance Angles C31 1.3879 (0.0051) C27 1.3877 (0.0051) 121.62 (0.34) C32 - C31 C33 - Distance Angles C34 1.3669 (0.0057) C38 1.3957 (0.0053) 120.34 (0.37) C33 - C34 C34 - Distance Angles C33 1.3669 (0.0057) C35 1.3928 (0.0053) 121.19 (0.36) C34 - C33 C35 - Distance Angles C36 1.3983 (0.0049) C34 1.3928 (0.0053) 117.58 (0.36) C41 1.5021 (0.0054) 120.07 (0.35) 121.73 (0.33) C35 - C36 C34 C36 - Distance Angles O4 1.3783 (0.0041) C35 1.3983 (0.0049) 119.35 (0.34) C37 1.3873 (0.0051) 118.19 (0.30) 121.95 (0.34) C36 - O4 C35 C37 - Distance Angles C38 1.3863 (0.0050) C36 1.3873 (0.0051) 118.62 (0.33) C42 1.5094 (0.0048) 121.00 (0.34) 119.89 (0.31) C37 - C38 C36 C38 - Distance Angles C33 1.3957 (0.0053) C37 1.3863 (0.0050) 120.04 (0.37) C38 - C33 C39 - Distance Angles C18 1.5118 (0.0047) C24 1.5156 (0.0050) 111.26 (0.28) C39 - C18 C40 - Distance Angles C22 1.5111 (0.0052) C31 1.5164 (0.0052) 110.11 (0.30) C40 - C22 C41 - Distance Angles C35 1.5021 (0.0054) C29 1.5250 (0.0050) 109.29 (0.29) C41 - C35 C42 - Distance Angles C37 1.5094 (0.0048) C16 1.5156 (0.0046) 109.80 (0.27) C42 - C37 O1 - Distance Angles C17 1.3917 (0.0040) C1 1.4522 (0.0040) 113.54 (0.25) O1 - C17 O2 - Distance Angles C23 1.3820 (0.0040) C04 1.4350 (0.0041) 115.12 (0.25) O2 - C23 O3 - Distance Angles C30 1.3930 (0.0043) C10 1.4472 (0.0046) 114.03 (0.27) O3 - C30 O4 - Distance Angles C36 1.3783 (0.0041) C7 1.4337 (0.0045) 117.21 (0.28) O4 - C36 O5 - Distance Angles C13 1.2637 (0.0044) O5 - O6 - Distance Angles C13 1.2686 (0.0042) O6 - O7 - Distance Angles C26 1.2643 (0.0042) O7 - O8 - Distance Angles C26 1.2694 (0.0042) O8 - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.84 1.84 2.643(4) 160.4 O6-H6...O7_$1 0.84 1.79 2.619(4) 167.0 O8-H8...O5_$1 Hydrogen bonds with H..A < r(A) + 2.000 Angstroms and 110 deg. D-H d(D-H) d(H..A)