+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + ssf1337 started at 13:27:27 on 07-Aug-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL ssf1337 in P-1 CELL 0.67100 4.8629 7.9978 16.5263 96.951 94.475 107.384 ZERR 2.00 0.0003 0.0005 0.0011 0.001 0.001 0.001 LATT 1 SFAC C H N O UNIT 20 36 4 10 V = 604.44 F(000) = 264.0 Mu = 0.11 mm-1 Cell Wt = 492.53 Rho = 1.353 MERG 2 SHEL 7 0.77 DFIX 0.84 0.02 O1W H1W O1W H2W DANG 1.35 0.02 H1W H2W HTAB O31A O1B HTAB O1W O1A EQIV_$1 -x+1, -y+2, -z HTAB N21 O31B_$1 EQIV_$2 -x+2, -y+1, -z HTAB N23 O1A_$2 EQIV_$3 -x+2, -y, -z+1 HTAB O1W O1W_$3 FMAP 2 PLAN 10 SIZE 0.06 0.06 0.08 ACTA HTAB 2.00000 BOND $H WGHT 0.09430 0.15650 L.S. 4 TEMP -153.00 FVAR 1.10408 MOLE 1 C1 1 0.780684 0.405656 0.337591 11.00000 0.01844 0.01845 = 0.01362 0.00177 0.00500 0.00782 C2 1 0.642911 0.512974 0.393894 11.00000 0.02624 0.02033 = 0.01506 0.00430 0.00883 0.01433 AFIX 23 H2A 2 0.464522 0.520116 0.363265 11.00000 -1.20000 H2B 2 0.778455 0.635121 0.408370 11.00000 -1.20000 AFIX 0 C3 1 0.564307 0.440488 0.472944 11.00000 0.02290 0.02004 = 0.01342 0.00408 0.00732 0.01237 AFIX 23 H3A 2 0.740392 0.430596 0.503698 11.00000 -1.20000 H3B 2 0.421970 0.320251 0.459301 11.00000 -1.20000 AFIX 0 O1A 4 0.863441 0.284360 0.361484 11.00000 0.02803 0.02324 = 0.01707 0.00610 0.00889 0.01570 O1B 4 0.811021 0.445340 0.265381 11.00000 0.03672 0.02922 = 0.01492 0.00841 0.01190 0.02125 MOLE 2 C22 1 0.754061 0.981768 -0.238512 11.00000 0.01993 0.01808 = 0.01968 -0.00008 0.00346 0.00785 C24 1 0.872642 0.796784 -0.163894 11.00000 0.02709 0.02172 = 0.02361 0.00657 0.00567 0.01344 AFIX 43 H24 2 0.949124 0.707801 -0.147949 11.00000 -1.20000 AFIX 0 C25 1 0.732791 0.887828 -0.117656 11.00000 0.02588 0.02089 = 0.01968 0.00489 0.00634 0.01021 AFIX 43 H25 2 0.692163 0.875694 -0.062982 11.00000 -1.20000 AFIX 0 C26 1 0.722141 1.079546 -0.307157 11.00000 0.03266 0.02692 = 0.02206 0.00530 0.00277 0.01246 AFIX 137 H26A 2 0.865645 1.071467 -0.344676 11.00000 -1.50000 H26B 2 0.753230 1.204240 -0.285525 11.00000 -1.50000 H26C 2 0.526371 1.027795 -0.336807 11.00000 -1.50000 AFIX 0 N21 3 0.660203 1.002234 -0.165437 11.00000 0.02185 0.01872 = 0.02046 0.00231 0.00554 0.01135 AFIX 43 H21 2 0.566517 1.077020 -0.150005 11.00000 0.04130 AFIX 0 N23 3 0.883768 0.857070 -0.238614 11.00000 0.02500 0.01968 = 0.02108 0.00291 0.00786 0.01184 AFIX 43 H23 2 0.964153 0.818990 -0.279937 11.00000 0.06516 AFIX 0 MOLE 3 C31 1 0.696359 0.680762 0.135722 11.00000 0.01642 0.01619 = 0.01505 0.00055 0.00342 0.00794 C32 1 0.858769 0.558649 0.101781 11.00000 0.01886 0.01738 = 0.01320 0.00315 0.00484 0.01025 AFIX 23 H32A 2 0.740570 0.435012 0.103719 11.00000 -1.20000 H32B 2 1.041571 0.583241 0.138528 11.00000 -1.20000 AFIX 0 C33 1 0.933097 0.571670 0.014999 11.00000 0.01972 0.01748 = 0.01266 0.00251 0.00432 0.01086 AFIX 23 H33A 2 1.071882 0.690056 0.013333 11.00000 -1.20000 H33B 2 0.755017 0.558064 -0.021971 11.00000 -1.20000 AFIX 0 O31A 4 0.625942 0.667865 0.209488 11.00000 0.03040 0.02770 = 0.01565 0.00531 0.00974 0.01899 AFIX 147 H31 2 0.698171 0.596852 0.229802 11.00000 0.08574 AFIX 0 O31B 4 0.630372 0.785623 0.095038 11.00000 0.02352 0.01956 = 0.01887 0.00377 0.00484 0.01375 MOLE 4 O1W 4 0.789788 0.079292 0.491295 11.00000 0.04768 0.04557 = 0.04012 0.02659 0.01385 0.02373 H1W 2 0.828495 -0.009270 0.473459 11.00000 0.18597 H2W 2 0.809179 0.150736 0.457414 11.00000 0.04803 HKLF 4 Covalent radii and connectivity table for ssf1337 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1A O1B C2 C2 - C1 C3 C3 - C2 C3_$4 O1A - C1 O1B - C1 C22 - N23 N21 C26 C24 - C25 N23 C25 - C24 N21 C26 - C22 N21 - C22 C25 N23 - C22 C24 C31 - O31B O31A C32 C32 - C31 C33 C33 - C32 C33_$2 O31A - C31 O31B - C31 O1W - no bonds found Operators for generating equivalent atoms: $1 -x+1, -y+2, -z $2 -x+2, -y+1, -z $3 -x+2, -y, -z+1 $4 -x+1, -y+1, -z+1 6442 Reflections read, of which 1148 rejected -6 =< h =< 6, -10 =< k =< 10, -21 =< l =< 21, Max. 2-theta = 51.65 0 Systematic absence violations 0 Inconsistent equivalents 2668 Unique reflections, of which 0 suppressed R(int) = 0.0347 R(sigma) = 0.0475 Friedel opposites merged Maximum memory for data reduction = 2013 / 27214 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 = 2492 / 208031 wR2 = 0.1504 before cycle 1 for 2668 data and 167 / 167 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. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.019 0.016 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.051; Restrained GooF = 1.051 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0943 * P )^2 + 0.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.10405 0.00416 -0.006 OSF Mean shift/esd = 0.005 Maximum = -0.074 for x H1W Max. shift = 0.004 A for H1W Max. dU = 0.000 for H2W Least-squares cycle 2 Maximum vector length = 511 Memory required = 2492 / 208031 wR2 = 0.1504 before cycle 2 for 2668 data and 167 / 167 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. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.019 0.016 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.051; Restrained GooF = 1.051 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0943 * P )^2 + 0.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.10404 0.00416 -0.004 OSF Mean shift/esd = 0.004 Maximum = -0.086 for x H1W Max. shift = 0.005 A for H1W Max. dU = 0.000 for H2W Least-squares cycle 3 Maximum vector length = 511 Memory required = 2492 / 208031 wR2 = 0.1504 before cycle 3 for 2668 data and 167 / 167 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. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.019 0.016 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.051; Restrained GooF = 1.051 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0943 * P )^2 + 0.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.10402 0.00416 -0.004 OSF Mean shift/esd = 0.003 Maximum = -0.071 for x H1W Max. shift = 0.004 A for H1W Max. dU = 0.000 for H31 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2492 / 208031 wR2 = 0.1504 before cycle 4 for 2668 data and 167 / 167 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. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.019 0.016 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.051; Restrained GooF = 1.051 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0943 * P )^2 + 0.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.10401 0.00416 -0.003 OSF Mean shift/esd = 0.003 Maximum = -0.060 for x H1W Max. shift = 0.003 A for H1W Max. dU = 0.000 for H31 Largest correlation matrix elements 0.811 y H1W / x H1W 0.516 U12 O1B / U22 O1B 0.510 z H2W / y H2W Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2A 0.4645 0.5201 0.3633 23 0.990 0.000 C2 C1 C3 H2B 0.7785 0.6351 0.4084 23 0.990 0.000 C2 C1 C3 H3A 0.7404 0.4306 0.5037 23 0.990 0.000 C3 C2 C3_$4 H3B 0.4220 0.3202 0.4593 23 0.990 0.000 C3 C2 C3_$4 H24 0.9491 0.7078 -0.1480 43 0.950 0.000 C24 C25 N23 H25 0.6922 0.8757 -0.0630 43 0.950 0.000 C25 C24 N21 H26A 0.8656 1.0714 -0.3447 137 0.980 0.000 C26 C22 H26A H26B 0.7533 1.2042 -0.2855 137 0.980 0.000 C26 C22 H26A H26C 0.5264 1.0278 -0.3368 137 0.980 0.000 C26 C22 H26A H21 0.5665 1.0770 -0.1500 43 0.880 0.000 N21 C22 C25 H23 0.9641 0.8190 -0.2799 43 0.880 0.000 N23 C22 C24 H32A 0.7406 0.4350 0.1037 23 0.990 0.000 C32 C31 C33 H32B 1.0416 0.5832 0.1385 23 0.990 0.000 C32 C31 C33 H33A 1.0719 0.6901 0.0133 23 0.990 0.000 C33 C32 C33_$2 H33B 0.7550 0.5581 -0.0220 23 0.990 0.000 C33 C32 C33_$2 H31 0.6982 0.5969 0.2298 147 0.840 0.000 O31A C31 H31 ssf1337 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.78068 0.40566 0.33759 1.00000 0.01844 0.01845 0.01361 0.00177 0.00500 0.00782 0.01626 0.00273 0.00028 0.00017 0.00008 0.00000 0.00061 0.00062 0.00059 0.00047 0.00046 0.00049 0.00030 C2 0.64291 0.51297 0.39389 1.00000 0.02623 0.02033 0.01505 0.00430 0.00883 0.01433 0.01847 0.00301 0.00031 0.00018 0.00008 0.00000 0.00068 0.00065 0.00062 0.00048 0.00050 0.00053 0.00030 H2A 0.46453 0.52012 0.36327 1.00000 0.02216 0.00000 0.00000 H2B 0.77846 0.63512 0.40837 1.00000 0.02216 0.00000 0.00000 C3 0.56431 0.44049 0.47294 1.00000 0.02289 0.02003 0.01342 0.00408 0.00732 0.01237 0.01710 0.00287 0.00029 0.00017 0.00008 0.00000 0.00064 0.00066 0.00059 0.00048 0.00048 0.00052 0.00030 H3A 0.74039 0.43059 0.50370 1.00000 0.02052 0.00000 0.00000 H3B 0.42197 0.32025 0.45930 1.00000 0.02052 0.00000 0.00000 O1A 0.86344 0.28436 0.36148 1.00000 0.02803 0.02323 0.01707 0.00610 0.00889 0.01569 0.02045 0.00215 0.00022 0.00013 0.00006 0.00000 0.00053 0.00053 0.00049 0.00038 0.00038 0.00041 0.00026 O1B 0.81102 0.44534 0.26538 1.00000 0.03671 0.02921 0.01492 0.00841 0.01190 0.02125 0.02357 0.00234 0.00024 0.00014 0.00006 0.00000 0.00059 0.00058 0.00051 0.00040 0.00041 0.00046 0.00028 C22 0.75406 0.98177 -0.23851 1.00000 0.01993 0.01808 0.01968 -0.00008 0.00346 0.00785 0.01899 0.00276 0.00028 0.00018 0.00008 0.00000 0.00064 0.00064 0.00066 0.00049 0.00050 0.00051 0.00031 C24 0.87264 0.79678 -0.16389 1.00000 0.02709 0.02172 0.02361 0.00657 0.00567 0.01344 0.02242 0.00318 0.00032 0.00019 0.00009 0.00000 0.00071 0.00069 0.00070 0.00053 0.00055 0.00055 0.00032 H24 0.94913 0.70780 -0.14795 1.00000 0.02691 0.00000 0.00000 C25 0.73279 0.88782 -0.11766 1.00000 0.02588 0.02089 0.01968 0.00489 0.00635 0.01022 0.02114 0.00298 0.00030 0.00018 0.00009 0.00000 0.00070 0.00067 0.00067 0.00052 0.00053 0.00054 0.00032 H25 0.69215 0.87569 -0.06298 1.00000 0.02536 0.00000 0.00000 C26 0.72215 1.07955 -0.30716 1.00000 0.03266 0.02692 0.02205 0.00530 0.00276 0.01246 0.02640 0.00331 0.00035 0.00020 0.00009 0.00000 0.00080 0.00077 0.00071 0.00058 0.00058 0.00062 0.00035 H26A 0.86561 1.07143 -0.34468 1.00000 0.03959 0.00000 0.00000 H26B 0.75331 1.20425 -0.28553 1.00000 0.03959 0.00000 0.00000 H26C 0.52636 1.02782 -0.33679 1.00000 0.03959 0.00000 0.00000 N21 0.66020 1.00224 -0.16544 1.00000 0.02185 0.01872 0.02046 0.00231 0.00554 0.01135 0.01911 0.00248 0.00025 0.00015 0.00007 0.00000 0.00057 0.00057 0.00059 0.00043 0.00044 0.00045 0.00029 H21 0.56652 1.07702 -0.15001 1.00000 0.04136 0.00000 0.00568 N23 0.88376 0.85707 -0.23861 1.00000 0.02500 0.01968 0.02108 0.00291 0.00786 0.01184 0.02056 0.00257 0.00026 0.00016 0.00007 0.00000 0.00061 0.00059 0.00061 0.00045 0.00046 0.00047 0.00029 H23 0.96414 0.81899 -0.27994 1.00000 0.06502 0.00000 0.00798 C31 0.69635 0.68076 0.13572 1.00000 0.01642 0.01619 0.01504 0.00054 0.00342 0.00794 0.01532 0.00263 0.00027 0.00017 0.00008 0.00000 0.00060 0.00060 0.00061 0.00046 0.00046 0.00047 0.00029 C32 0.85877 0.55865 0.10178 1.00000 0.01886 0.01737 0.01320 0.00315 0.00484 0.01025 0.01522 0.00271 0.00028 0.00017 0.00007 0.00000 0.00061 0.00061 0.00060 0.00045 0.00046 0.00048 0.00029 H32A 0.74057 0.43501 0.10372 1.00000 0.01826 0.00000 0.00000 H32B 1.04157 0.58324 0.13853 1.00000 0.01826 0.00000 0.00000 C33 0.93310 0.57167 0.01500 1.00000 0.01972 0.01747 0.01266 0.00251 0.00432 0.01085 0.01534 0.00273 0.00028 0.00017 0.00008 0.00000 0.00062 0.00062 0.00059 0.00045 0.00046 0.00050 0.00029 H33A 1.07188 0.69005 0.01333 1.00000 0.01841 0.00000 0.00000 H33B 0.75502 0.55806 -0.02197 1.00000 0.01841 0.00000 0.00000 O31A 0.62594 0.66787 0.20949 1.00000 0.03040 0.02770 0.01565 0.00531 0.00974 0.01899 0.02180 0.00229 0.00023 0.00014 0.00006 0.00000 0.00056 0.00056 0.00049 0.00039 0.00039 0.00044 0.00027 H31 0.69820 0.59687 0.22981 1.00000 0.08590 0.00000 0.01002 O31B 0.63037 0.78562 0.09504 1.00000 0.02352 0.01956 0.01887 0.00377 0.00484 0.01375 0.01888 0.00206 0.00021 0.00013 0.00006 0.00000 0.00050 0.00049 0.00049 0.00037 0.00037 0.00039 0.00026 O1W 0.78981 0.07930 0.49130 1.00000 0.04770 0.04554 0.04009 0.02656 0.01384 0.02370 0.04018 0.00330 0.00031 0.00020 0.00008 0.00000 0.00077 0.00080 0.00073 0.00062 0.00058 0.00063 0.00036 H1W 0.82527 -0.01003 0.47289 1.00000 0.18606 0.09999 0.01114 0.00380 0.00253 0.00000 0.02263 H2W 0.80916 0.15088 0.45743 1.00000 0.04821 0.05019 0.00510 0.00267 0.00129 0.00000 0.00641 Final Structure Factor Calculation for ssf1337 in P-1 Total number of l.s. parameters = 167 Maximum vector length = 511 Memory required = 2325 / 22995 wR2 = 0.1504 before cycle 5 for 2668 data and 0 / 167 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. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.019 0.015 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.051; Restrained GooF = 1.051 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0943 * P )^2 + 0.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0516 for 2332 Fo > 4sig(Fo) and 0.0573 for all 2668 data wR2 = 0.1504, GooF = S = 1.051, Restrained GooF = 1.051 for all data Occupancy sum of asymmetric unit = 17.00 for non-hydrogen and 18.00 for hydrogen atoms Principal mean square atomic displacements U 0.0202 0.0177 0.0110 C1 0.0303 0.0155 0.0096 C2 0.0267 0.0149 0.0097 C3 0.0330 0.0159 0.0125 O1A 0.0432 0.0170 0.0106 O1B 0.0225 0.0205 0.0140 C22 0.0303 0.0219 0.0151 C24 0.0276 0.0183 0.0175 C25 0.0334 0.0250 0.0208 C26 0.0248 0.0207 0.0118 N21 0.0283 0.0206 0.0127 N23 0.0187 0.0168 0.0105 C31 0.0219 0.0135 0.0103 C32 0.0226 0.0134 0.0100 C33 0.0373 0.0178 0.0103 O31A 0.0273 0.0184 0.0110 O31B 0.0632 0.0389 0.0183 O1W Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.027 0.052 0.083 0.115 0.150 0.194 0.248 0.318 0.435 1.000 Number in group 268. 271. 262. 272. 260. 267. 276. 259. 264. 269. GooF 0.917 1.112 1.101 1.063 1.118 1.138 1.027 1.046 0.977 0.994 K 1.496 1.036 1.053 1.030 1.019 1.011 1.007 1.005 1.010 1.002 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.96 1.03 1.13 1.27 1.53 inf Number in group 279. 255. 280. 254. 272. 265. 264. 265. 265. 269. GooF 0.901 0.851 0.903 0.978 0.914 0.934 0.930 1.025 1.166 1.660 K 1.034 1.026 1.016 1.008 1.010 0.989 0.974 1.003 0.995 1.038 R1 0.075 0.065 0.064 0.064 0.061 0.050 0.048 0.046 0.049 0.065 Recommended weighting scheme: WGHT 0.0942 0.1564 Note that in most cases convergence will be faster if fixed weights (e.g. the default WGHT 0.1) are retained until the refinement is virtually complete, and only then should the above recommended values be used. Most Disagreeable Reflections (* if suppressed or used for Rfree) h k l Fo^2 Fc^2 Delta(F^2)/esd Fc/Fc(max) Resolution(A) 2 -3 7 5.22 1.05 5.29 0.033 1.55 2 -2 6 0.02 3.70 4.95 0.062 1.74 2 -1 5 2.42 0.08 4.87 0.009 1.88 -4 7 5 14.20 29.52 4.47 0.176 0.90 -2 2 0 8.82 3.60 4.20 0.062 2.31 -1 2 2 31.43 18.34 4.11 0.139 3.16 -1 0 1 38.32 23.82 3.89 0.158 4.58 -1 0 4 8.47 16.62 3.84 0.132 3.25 -1 -4 17 14.36 26.71 3.79 0.168 0.89 0 -4 4 12.86 23.12 3.69 0.156 1.82 1 -4 3 321.51 221.35 3.66 0.483 1.92 1 -3 3 2.57 0.63 3.48 0.026 2.41 0 -2 4 0.21 2.09 3.48 0.047 3.00 1 -6 4 20.17 32.54 3.44 0.185 1.31 0 1 4 238.28 163.08 3.43 0.415 3.38 2 -4 8 1.90 0.25 3.40 0.016 1.36 -2 1 6 28.18 18.21 3.33 0.139 1.88 2 -6 1 486.66 702.36 3.33 0.861 1.29 -3 6 3 9.59 4.86 3.24 0.072 1.13 1 -4 1 5.72 2.68 3.21 0.053 1.99 -1 7 13 33.64 52.32 3.21 0.235 0.79 -1 1 4 36.78 54.83 3.18 0.240 3.10 2 -6 12 52.32 33.91 3.16 0.189 0.98 1 2 1 1.06 0.01 3.03 0.003 2.46 -1 4 5 12.43 19.80 3.01 0.144 1.61 1 -2 8 399.72 290.84 3.01 0.554 1.80 2 -2 2 11.78 6.90 3.00 0.085 2.21 1 -5 6 362.95 268.09 2.99 0.532 1.45 -1 0 6 2.60 0.91 2.95 0.031 2.47 2 -4 6 6.95 11.99 2.93 0.112 1.51 -4 8 1 117.50 85.40 2.90 0.300 0.87 2 -2 4 102.44 75.12 2.90 0.281 1.99 -2 0 9 104.54 76.49 2.85 0.284 1.51 -4 4 14 194.41 140.38 2.84 0.385 0.83 3 -9 5 34.33 23.43 2.84 0.157 0.85 -1 -1 13 7.45 12.58 2.80 0.115 1.24 0 -7 17 67.18 95.06 2.78 0.317 0.78 0 -3 2 14.57 21.96 2.77 0.152 2.51 -1 4 6 2.12 4.86 2.77 0.072 1.52 3 -5 5 2.06 0.33 2.73 0.019 1.22 -3 7 4 10.37 6.07 2.72 0.080 1.00 -1 0 3 32.23 45.32 2.71 0.219 3.74 2 -4 3 64.30 47.43 2.70 0.224 1.69 -1 9 5 116.53 86.04 2.68 0.301 0.82 0 -4 2 1.92 0.56 2.67 0.024 1.90 0 1 2 205.11 152.90 2.65 0.401 5.16 -3 -1 5 3.04 1.22 2.64 0.036 1.37 0 -5 5 3.65 6.80 2.62 0.085 1.46 -1 -3 3 98.44 74.48 2.60 0.280 1.96 -2 -1 7 531.88 702.89 2.56 0.861 1.66 Bond lengths and angles C1 - Distance Angles O1A 1.2491 (0.0016) O1B 1.2797 (0.0016) 121.60 (0.12) C2 1.5162 (0.0018) 120.90 (0.11) 117.50 (0.12) C1 - O1A O1B C2 - Distance Angles C1 1.5162 (0.0018) C3 1.5224 (0.0017) 115.17 (0.11) H2A 0.9900 108.48 108.48 H2B 0.9900 108.48 108.48 107.50 C2 - C1 C3 H2A C3 - Distance Angles C2 1.5224 (0.0017) C3_$4 1.5278 (0.0024) 111.66 (0.13) H3A 0.9900 109.29 109.29 H3B 0.9900 109.29 109.29 107.95 C3 - C2 C3_$4 H3A O1A - Distance Angles C1 1.2491 (0.0016) O1A - O1B - Distance Angles C1 1.2797 (0.0016) O1B - C22 - Distance Angles N23 1.3297 (0.0017) N21 1.3328 (0.0018) 107.53 (0.12) C26 1.4773 (0.0020) 125.85 (0.13) 126.62 (0.13) C22 - N23 N21 C24 - Distance Angles C25 1.3487 (0.0020) N23 1.3781 (0.0019) 107.14 (0.13) H24 0.9500 126.43 126.43 C24 - C25 N23 C25 - Distance Angles C24 1.3487 (0.0020) N21 1.3820 (0.0018) 106.51 (0.12) H25 0.9500 126.74 126.74 C25 - C24 N21 C26 - Distance Angles C22 1.4773 (0.0020) H26A 0.9800 109.47 H26B 0.9800 109.47 109.47 H26C 0.9800 109.47 109.47 109.47 C26 - C22 H26A H26B N21 - Distance Angles C22 1.3328 (0.0018) C25 1.3820 (0.0018) 109.46 (0.12) H21 0.8800 125.27 125.27 N21 - C22 C25 N23 - Distance Angles C22 1.3297 (0.0017) C24 1.3781 (0.0019) 109.36 (0.12) H23 0.8800 125.32 125.32 N23 - C22 C24 C31 - Distance Angles O31B 1.2337 (0.0016) O31A 1.2994 (0.0015) 121.60 (0.12) C32 1.5132 (0.0017) 121.74 (0.11) 116.66 (0.11) C31 - O31B O31A C32 - Distance Angles C31 1.5132 (0.0017) C33 1.5142 (0.0017) 116.18 (0.10) H32A 0.9900 108.24 108.24 H32B 0.9900 108.24 108.24 107.37 C32 - C31 C33 H32A C33 - Distance Angles C32 1.5142 (0.0017) C33_$2 1.5303 (0.0024) 110.84 (0.13) H33A 0.9900 109.47 109.47 H33B 0.9900 109.47 109.47 108.06 C33 - C32 C33_$2 H33A O31A - Distance Angles C31 1.2994 (0.0015) H31 0.8400 109.47 O31A - C31 O31B - Distance Angles C31 1.2337 (0.0016) O31B - O1W - Distance Angles H1W 0.8135 (0.0184) H2W 0.8387 (0.0154) 111.44 (2.71) O1W - H1W Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.84 1.62 2.4609(14) 174.8 O31A-H31...O1B 0.839(15) 2.008(16) 2.8357(16) 169(2) O1W-H2W...O1A 0.88 1.86 2.7277(15) 167.0 N21-H21...O31B_$1 0.88 1.88 2.7529(15) 173.3 N23-H23...O1A_$2 0.814(18) 2.16(4) 2.723(3) 126(4) O1W-H1W...O1W_$3 Hydrogen bonds with H..A < r(A) + 2.000 Angstroms and 110 deg. D-H d(D-H) d(H..A)