+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + p-1 started at 16:36:10 on 23-Feb-2010 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL p-1 in P-1 CELL 0.71073 8.0079 8.8634 8.8643 67.429 88.975 75.965 ZERR 2.00 0.0002 0.0003 0.0002 0.002 0.002 0.001 LATT 1 SFAC C H B N O UNIT 6 24 10 2 20 V = 561.64 F(000) = 284.0 Mu = 0.15 mm-1 Cell Wt = 552.37 Rho = 1.633 MERG 2 OMIT -3.00 55.00 OMIT -1 1 2 OMIT -1 0 1 SHEL 7 0.77 FMAP 2 PLAN 5 EQIV $1 -x, -y+1, -z EQIV $2 -x+1, -y, -z+1 EQIV $3 -x+1, -y+1, -z EQIV $4 x, y+1, z EQIV $5 -x+1, -y+1, -z+1 EQIV $6 x+1, y, z HTAB O7 O1_$1 HTAB O8 O3_$2 HTAB O9 O4_$3 HTAB O10 O8_$4 HTAB N1 O6_$5 HTAB N1 O6_$6 HTAB N1 O1_$6 HTAB N1 O9 SIZE 0.14 0.36 0.62 ACTA HTAB BOND $H WGHT 0.03830 0.17890 L.S. 9 TEMP -153.00 FVAR 0.45828 MOLE 1 B1 3 0.269516 0.369253 0.282959 11.00000 0.01275 0.01061 = 0.01206 -0.00416 0.00013 -0.00430 B2 3 0.040707 0.269139 0.191421 11.00000 0.01354 0.01344 = 0.01584 -0.00565 -0.00022 -0.00457 B3 3 0.260086 0.068573 0.394506 11.00000 0.01317 0.01227 = 0.01325 -0.00601 0.00127 -0.00387 B4 3 0.463526 0.563965 0.196254 11.00000 0.01225 0.01207 = 0.01252 -0.00369 -0.00166 -0.00334 B5 3 0.282176 0.575722 0.408778 11.00000 0.01232 0.01157 = 0.01347 -0.00359 -0.00083 -0.00339 O1 5 0.119120 0.394607 0.176066 11.00000 0.01421 0.01190 = 0.01498 -0.00244 -0.00376 -0.00462 O2 5 0.103983 0.107877 0.308616 11.00000 0.01526 0.01215 = 0.01962 -0.00329 -0.00410 -0.00570 O3 5 0.345562 0.188767 0.378010 11.00000 0.01266 0.01013 = 0.01466 -0.00343 -0.00253 -0.00390 O4 5 0.397148 0.443669 0.178425 11.00000 0.01405 0.01310 = 0.01202 -0.00536 0.00243 -0.00643 O5 5 0.412417 0.627441 0.314567 11.00000 0.01723 0.01501 = 0.01543 -0.00751 0.00383 -0.00890 O6 5 0.213837 0.454010 0.395433 11.00000 0.01452 0.01309 = 0.01630 -0.00768 0.00420 -0.00706 O7 5 -0.095785 0.295935 0.088446 11.00000 0.02041 0.01456 = 0.02480 -0.00285 -0.01009 -0.00586 AFIX 147 H7 2 -0.116384 0.394748 0.016557 11.00000 -1.50000 AFIX 0 O8 5 0.328399 -0.095972 0.493326 11.00000 0.01515 0.01131 = 0.02157 -0.00397 -0.00506 -0.00470 AFIX 147 H8 2 0.429757 -0.108482 0.528189 11.00000 -1.50000 AFIX 0 O9 5 0.582389 0.629708 0.097977 11.00000 0.01835 0.01879 = 0.01441 -0.00855 0.00469 -0.01069 AFIX 147 H9 2 0.594582 0.594574 0.021885 11.00000 -1.50000 AFIX 0 O10 5 0.211493 0.644281 0.514720 11.00000 0.02152 0.01653 = 0.02314 -0.01218 0.00898 -0.01114 AFIX 147 H10 2 0.252980 0.725271 0.506490 11.00000 -1.50000 AFIX 0 MOLE 2 C1 1 0.843742 0.866749 0.206104 11.00000 0.01915 0.01640 = 0.01838 -0.00335 -0.00115 -0.00793 AFIX 13 H1 2 0.939656 0.898513 0.247717 11.00000 -1.20000 AFIX 0 C2 1 0.669462 0.986068 0.174596 11.00000 0.02703 0.01934 = 0.02226 -0.00808 0.00152 -0.00027 AFIX 23 H2A 2 0.657614 1.088916 0.197444 11.00000 -1.20000 H2B 2 0.568026 0.937754 0.196372 11.00000 -1.20000 AFIX 0 C3 1 0.770141 0.973211 0.034245 11.00000 0.02922 0.02077 = 0.01698 -0.00259 0.00203 -0.00492 AFIX 23 H3A 2 0.730830 0.916947 -0.030544 11.00000 -1.20000 H3B 2 0.820421 1.068114 -0.029472 11.00000 -1.20000 AFIX 0 N1 4 0.850318 0.685560 0.268835 11.00000 0.01432 0.01634 = 0.01742 -0.00476 0.00099 -0.00560 AFIX 137 H1A 2 0.838781 0.646804 0.378549 11.00000 -1.50000 H1B 2 0.953389 0.627818 0.249795 11.00000 -1.50000 H1C 2 0.762850 0.670013 0.216951 11.00000 -1.50000 AFIX 0 HKLF 4 Covalent radii and connectivity table for p-1 in P-1 C 0.770 H 0.320 B 0.820 N 0.700 O 0.660 B1 - O1 O3 O6 O4 B2 - O7 O1 O2 B3 - O8 O3 O2 B4 - O4 O9 O5 B5 - O10 O6 O5 O1 - B2 B1 O2 - B3 B2 O3 - B3 B1 O4 - B4 B1 O5 - B5 B4 O6 - B5 B1 O7 - B2 O8 - B3 O9 - B4 O10 - B5 C1 - N1 C2 C3 C2 - C1 C3 C3 - C1 C2 N1 - C1 Operators for generating equivalent atoms: $1 -x, -y+1, -z $2 -x+1, -y, -z+1 $3 -x+1, -y+1, -z $4 x, y+1, z $5 -x+1, -y+1, -z+1 $6 x+1, y, z 12383 Reflections read, of which 30 rejected -10 =< h =< 10, -11 =< k =< 11, -11 =< l =< 11, Max. 2-theta = 54.96 0 Systematic absence violations 0 Inconsistent equivalents 2571 Unique reflections, of which 0 suppressed R(int) = 0.0274 R(sigma) = 0.0232 Friedel opposites merged Maximum memory for data reduction = 2030 / 26020 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 = 2501 / 221018 wR2 = 0.0821 before cycle 1 for 2571 data and 177 / 177 parameters GooF = S = 1.078; Restrained GooF = 1.078 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0383 * P )^2 + 0.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.45826 0.00079 -0.026 OSF Mean shift/esd = 0.008 Maximum = -0.026 for U22 O2 Max. shift = 0.000 A for H9 Max. dU = 0.000 for B3 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2501 / 221018 wR2 = 0.0821 before cycle 2 for 2571 data and 177 / 177 parameters GooF = S = 1.077; Restrained GooF = 1.077 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0383 * P )^2 + 0.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.45825 0.00079 -0.015 OSF Mean shift/esd = 0.003 Maximum = -0.015 for OSF Max. shift = 0.000 A for H9 Max. dU = 0.000 for B2 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2501 / 221018 wR2 = 0.0821 before cycle 3 for 2571 data and 177 / 177 parameters GooF = S = 1.078; Restrained GooF = 1.078 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0383 * P )^2 + 0.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.45825 0.00079 -0.001 OSF Mean shift/esd = 0.000 Maximum = 0.001 for tors H9 Max. shift = 0.000 A for H9 Max. dU = 0.000 for N1 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2501 / 221018 wR2 = 0.0821 before cycle 4 for 2571 data and 177 / 177 parameters GooF = S = 1.077; Restrained GooF = 1.077 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0383 * P )^2 + 0.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.45825 0.00079 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H9 Max. dU = 0.000 for B5 Least-squares cycle 5 Maximum vector length = 511 Memory required = 2501 / 221018 wR2 = 0.0821 before cycle 5 for 2571 data and 177 / 177 parameters GooF = S = 1.078; Restrained GooF = 1.078 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0383 * P )^2 + 0.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.45825 0.00079 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y O9 Max. shift = 0.000 A for H9 Max. dU = 0.000 for B2 Least-squares cycle 6 Maximum vector length = 511 Memory required = 2501 / 221018 wR2 = 0.0821 before cycle 6 for 2571 data and 177 / 177 parameters GooF = S = 1.078; Restrained GooF = 1.078 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0383 * P )^2 + 0.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.45825 0.00079 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y O9 Max. shift = 0.000 A for H10 Max. dU = 0.000 for B4 Least-squares cycle 7 Maximum vector length = 511 Memory required = 2501 / 221018 wR2 = 0.0821 before cycle 7 for 2571 data and 177 / 177 parameters GooF = S = 1.077; Restrained GooF = 1.077 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0383 * P )^2 + 0.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.45825 0.00079 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y O9 Max. shift = 0.000 A for H10 Max. dU = 0.000 for C1 Least-squares cycle 8 Maximum vector length = 511 Memory required = 2501 / 221018 wR2 = 0.0821 before cycle 8 for 2571 data and 177 / 177 parameters GooF = S = 1.078; Restrained GooF = 1.078 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0383 * P )^2 + 0.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.45825 0.00079 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y O9 Max. shift = 0.000 A for B1 Max. dU = 0.000 for O10 Least-squares cycle 9 Maximum vector length = 511 Memory required = 2501 / 221018 wR2 = 0.0821 before cycle 9 for 2571 data and 177 / 177 parameters GooF = S = 1.077; Restrained GooF = 1.077 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0383 * P )^2 + 0.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.45825 0.00079 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y O9 Max. shift = 0.000 A for H10 Max. dU = 0.000 for B1 Largest correlation matrix elements -0.554 U23 O10 / U22 O10 -0.510 U23 O6 / U33 O6 -0.503 U23 O6 / U22 O6 -0.526 U23 O9 / U33 O9 -0.507 U23 O5 / U22 O5 -0.502 U23 O5 / U33 O5 -0.521 U23 O10 / U33 O10 -0.506 U23 O4 / U33 O4 -0.510 U23 O9 / U22 O9 -0.506 U23 B3 / U22 B3 Idealized hydrogen atom generation before cycle 10 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H7 -0.1164 0.3947 0.0166 147 0.840 0.000 O7 B2 H7 H8 0.4298 -0.1085 0.5282 147 0.840 0.000 O8 B3 H8 H9 0.5946 0.5946 0.0219 147 0.840 0.000 O9 B4 H9 H10 0.2530 0.7253 0.5065 147 0.840 0.000 O10 B5 H10 H1 0.9397 0.8985 0.2477 13 1.000 0.000 C1 N1 C2 C3 H2A 0.6576 1.0889 0.1974 23 0.990 0.000 C2 C1 C3 H2B 0.5680 0.9378 0.1964 23 0.990 0.000 C2 C1 C3 H3A 0.7308 0.9169 -0.0305 23 0.990 0.000 C3 C1 C2 H3B 0.8204 1.0681 -0.0295 23 0.990 0.000 C3 C1 C2 H1A 0.8388 0.6468 0.3785 137 0.910 0.000 N1 C1 H1A H1B 0.9534 0.6278 0.2498 137 0.910 0.000 N1 C1 H1A H1C 0.7629 0.6700 0.2169 137 0.910 0.000 N1 C1 H1A p-1 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq B1 0.26952 0.36925 0.28296 1.00000 0.01274 0.01060 0.01205 -0.00416 0.00013 -0.00430 0.01162 0.00168 0.00015 0.00015 0.00014 0.00000 0.00054 0.00053 0.00053 0.00043 0.00042 0.00042 0.00023 B2 0.04071 0.26914 0.19142 1.00000 0.01353 0.01343 0.01583 -0.00565 -0.00022 -0.00457 0.01406 0.00176 0.00016 0.00015 0.00015 0.00000 0.00055 0.00057 0.00057 0.00046 0.00044 0.00045 0.00024 B3 0.26009 0.06857 0.39451 1.00000 0.01316 0.01226 0.01324 -0.00601 0.00127 -0.00386 0.01245 0.00173 0.00015 0.00015 0.00015 0.00000 0.00055 0.00055 0.00055 0.00045 0.00043 0.00044 0.00023 B4 0.46353 0.56396 0.19625 1.00000 0.01224 0.01206 0.01251 -0.00369 -0.00167 -0.00333 0.01254 0.00173 0.00015 0.00015 0.00015 0.00000 0.00053 0.00054 0.00054 0.00044 0.00042 0.00043 0.00023 B5 0.28217 0.57572 0.40878 1.00000 0.01231 0.01157 0.01347 -0.00358 -0.00083 -0.00338 0.01277 0.00172 0.00015 0.00015 0.00015 0.00000 0.00054 0.00054 0.00056 0.00045 0.00043 0.00044 0.00024 O1 0.11912 0.39461 0.17607 1.00000 0.01420 0.01189 0.01498 -0.00244 -0.00376 -0.00462 0.01426 0.00109 0.00010 0.00009 0.00009 0.00000 0.00037 0.00037 0.00038 0.00029 0.00029 0.00029 0.00017 O2 0.10398 0.10788 0.30862 1.00000 0.01525 0.01214 0.01961 -0.00329 -0.00410 -0.00569 0.01609 0.00110 0.00010 0.00010 0.00010 0.00000 0.00038 0.00038 0.00041 0.00032 0.00031 0.00030 0.00018 O3 0.34556 0.18877 0.37801 1.00000 0.01266 0.01012 0.01465 -0.00342 -0.00253 -0.00390 0.01269 0.00105 0.00009 0.00009 0.00009 0.00000 0.00036 0.00037 0.00037 0.00029 0.00028 0.00028 0.00017 O4 0.39715 0.44367 0.17843 1.00000 0.01404 0.01310 0.01202 -0.00536 0.00243 -0.00643 0.01237 0.00106 0.00009 0.00009 0.00009 0.00000 0.00037 0.00037 0.00036 0.00029 0.00028 0.00029 0.00017 O5 0.41242 0.62744 0.31457 1.00000 0.01722 0.01501 0.01542 -0.00751 0.00383 -0.00890 0.01453 0.00108 0.00010 0.00009 0.00009 0.00000 0.00039 0.00038 0.00038 0.00031 0.00030 0.00031 0.00018 O6 0.21384 0.45401 0.39543 1.00000 0.01451 0.01309 0.01630 -0.00768 0.00420 -0.00706 0.01341 0.00109 0.00010 0.00009 0.00009 0.00000 0.00037 0.00037 0.00038 0.00030 0.00029 0.00029 0.00017 O7 -0.09579 0.29593 0.08845 1.00000 0.02040 0.01455 0.02479 -0.00284 -0.01009 -0.00586 0.02100 0.00116 0.00011 0.00010 0.00011 0.00000 0.00042 0.00040 0.00045 0.00034 0.00034 0.00033 0.00020 H7 -0.11639 0.39475 0.01656 1.00000 0.03150 0.00000 0.00000 O8 0.32840 -0.09597 0.49333 1.00000 0.01514 0.01131 0.02156 -0.00397 -0.00506 -0.00470 0.01643 0.00112 0.00010 0.00009 0.00010 0.00000 0.00038 0.00038 0.00042 0.00032 0.00031 0.00030 0.00018 H8 0.42976 -0.10848 0.52818 1.00000 0.02465 0.00000 0.00000 O9 0.58239 0.62971 0.09798 1.00000 0.01835 0.01879 0.01440 -0.00854 0.00469 -0.01069 0.01547 0.00110 0.00010 0.00010 0.00009 0.00000 0.00039 0.00040 0.00039 0.00032 0.00030 0.00032 0.00018 H9 0.59456 0.59460 0.02187 1.00000 0.02321 0.00000 0.00000 O10 0.21149 0.64428 0.51472 1.00000 0.02151 0.01652 0.02314 -0.01218 0.00898 -0.01114 0.01793 0.00118 0.00011 0.00010 0.00010 0.00000 0.00042 0.00041 0.00043 0.00034 0.00033 0.00032 0.00018 H10 0.25299 0.72526 0.50650 1.00000 0.02689 0.00000 0.00000 C1 0.84374 0.86675 0.20610 1.00000 0.01915 0.01639 0.01838 -0.00335 -0.00115 -0.00793 0.01838 0.00168 0.00015 0.00014 0.00014 0.00000 0.00056 0.00055 0.00056 0.00044 0.00043 0.00045 0.00024 H1 0.93965 0.89851 0.24772 1.00000 0.02205 0.00000 0.00000 C2 0.66946 0.98607 0.17460 1.00000 0.02702 0.01933 0.02226 -0.00808 0.00153 -0.00027 0.02394 0.00196 0.00017 0.00016 0.00016 0.00000 0.00064 0.00059 0.00060 0.00048 0.00049 0.00049 0.00027 H2A 0.65761 1.08892 0.19744 1.00000 0.02873 0.00000 0.00000 H2B 0.56803 0.93775 0.19637 1.00000 0.02873 0.00000 0.00000 C3 0.77014 0.97321 0.03425 1.00000 0.02921 0.02076 0.01698 -0.00259 0.00204 -0.00492 0.02408 0.00196 0.00017 0.00016 0.00015 0.00000 0.00066 0.00060 0.00058 0.00048 0.00048 0.00050 0.00027 H3A 0.73083 0.91694 -0.03054 1.00000 0.02890 0.00000 0.00000 H3B 0.82042 1.06811 -0.02947 1.00000 0.02890 0.00000 0.00000 N1 0.85032 0.68556 0.26883 1.00000 0.01432 0.01633 0.01741 -0.00475 0.00098 -0.00560 0.01627 0.00139 0.00012 0.00012 0.00012 0.00000 0.00044 0.00047 0.00047 0.00037 0.00035 0.00036 0.00020 H1A 0.83877 0.64680 0.37855 1.00000 0.02441 0.00000 0.00000 H1B 0.95339 0.62782 0.24980 1.00000 0.02441 0.00000 0.00000 H1C 0.76286 0.67001 0.21694 1.00000 0.02441 0.00000 0.00000 Final Structure Factor Calculation for p-1 in P-1 Total number of l.s. parameters = 177 Maximum vector length = 511 Memory required = 2324 / 24017 wR2 = 0.0821 before cycle 10 for 2571 data and 0 / 177 parameters GooF = S = 1.078; Restrained GooF = 1.078 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0383 * P )^2 + 0.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0317 for 2284 Fo > 4sig(Fo) and 0.0361 for all 2571 data wR2 = 0.0821, GooF = S = 1.078, Restrained GooF = 1.078 for all data Occupancy sum of asymmetric unit = 19.00 for non-hydrogen and 12.00 for hydrogen atoms Principal mean square atomic displacements U 0.0141 0.0116 0.0092 B1 0.0170 0.0141 0.0111 B2 0.0137 0.0130 0.0106 B3 0.0160 0.0119 0.0098 B4 0.0160 0.0113 0.0110 B5 0.0220 0.0111 0.0097 O1 0.0262 0.0127 0.0094 O2 0.0187 0.0105 0.0088 O3 0.0160 0.0116 0.0095 O4 0.0204 0.0139 0.0093 O5 0.0187 0.0128 0.0087 O6 0.0384 0.0140 0.0107 O7 0.0278 0.0122 0.0093 O8 0.0235 0.0124 0.0105 O9 0.0295 0.0149 0.0094 O10 0.0260 0.0162 0.0129 C1 0.0322 0.0224 0.0172 C2 0.0310 0.0262 0.0150 C3 0.0202 0.0159 0.0128 N1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.015 0.030 0.046 0.064 0.084 0.108 0.141 0.182 0.276 1.000 Number in group 269. 255. 248. 266. 258. 254. 261. 244. 258. 258. GooF 1.050 1.004 1.204 1.175 1.143 0.964 0.950 1.010 0.984 1.241 K 1.458 1.005 0.954 0.966 0.967 0.993 1.008 1.004 1.022 0.993 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.31 1.64 inf Number in group 262. 262. 255. 249. 269. 245. 258. 255. 258. 258. GooF 1.002 1.036 0.971 0.868 0.984 0.931 0.967 0.924 1.159 1.688 K 1.015 1.024 1.021 1.001 1.009 1.014 1.016 1.012 1.019 0.976 R1 0.072 0.067 0.055 0.041 0.039 0.030 0.025 0.023 0.027 0.031 Recommended weighting scheme: WGHT 0.0382 0.1796 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 -1 1 2.21 0.09 4.56 0.004 2.50 -2 -1 1 3.34 8.65 4.38 0.042 3.37 -2 1 3 12.26 20.83 4.21 0.065 2.34 0 0 4 13.82 7.49 4.05 0.039 2.04 0 1 3 39.95 55.52 4.04 0.107 2.95 -1 2 0 305.90 373.10 4.02 0.277 3.21 -3 0 1 3.69 0.92 3.89 0.014 2.52 3 2 2 29.87 20.45 3.89 0.065 2.28 1 4 1 24.23 15.64 3.86 0.057 2.19 0 2 1 104.17 131.67 3.82 0.164 4.28 0 3 0 959.11 1130.44 3.64 0.481 2.64 -1 0 2 3663.69 4354.76 3.64 0.945 3.74 1 -6 4 34.01 48.43 3.56 0.100 0.92 2 3 1 1108.72 1290.45 3.42 0.514 2.63 0 -9 2 16.86 28.57 3.33 0.077 0.80 -5 -2 2 4.62 8.67 3.10 0.042 1.44 1 2 0 1203.75 1381.86 3.08 0.532 3.96 6 8 2 21.30 29.80 3.05 0.078 0.94 -3 -2 1 719.13 627.74 3.05 0.359 2.26 -2 -4 2 1.87 0.36 2.96 0.009 1.58 1 2 3 334.17 385.29 2.94 0.281 2.73 3 2 5 16.68 10.88 2.93 0.047 1.48 -1 3 2 31.38 23.92 2.92 0.070 2.44 -1 -5 5 2.78 0.55 2.91 0.011 0.98 -1 -1 2 665.52 758.89 2.82 0.394 3.11 3 7 4 9.79 5.95 2.81 0.035 1.20 3 6 11 16.47 24.11 2.81 0.070 0.77 -3 4 3 3.96 1.82 2.79 0.019 1.46 5 9 0 23.66 14.92 2.78 0.055 0.87 4 -5 3 34.21 44.24 2.78 0.095 0.92 -2 -4 1 63.78 52.35 2.76 0.104 1.79 -6 -2 5 -0.39 1.01 2.76 0.014 1.01 -1 -2 2 330.28 377.87 2.74 0.278 2.45 2 1 0 845.73 957.17 2.73 0.443 3.89 4 2 3 24.91 18.33 2.72 0.061 1.67 1 1 0 218.01 272.77 2.71 0.236 6.41 0 -2 1 115.61 135.24 2.67 0.166 3.11 -1 4 5 13.17 9.03 2.66 0.043 1.53 2 0 1 3434.08 3843.47 2.65 0.888 3.39 -1 1 0 1554.62 1742.85 2.65 0.598 4.94 -4 2 1 9.06 5.66 2.62 0.034 1.63 6 7 1 2.89 5.83 2.51 0.035 1.01 -6 6 0 7.42 12.77 2.50 0.051 0.82 -2 2 0 42.07 34.27 2.50 0.084 2.47 3 11 4 11.76 19.78 2.49 0.064 0.80 2 2 2 829.14 925.52 2.47 0.436 2.89 6 2 5 0.86 0.01 2.43 0.001 1.05 -1 2 2 609.89 680.40 2.43 0.373 3.11 1 1 2 230.19 259.96 2.41 0.231 3.91 -5 -1 2 1.24 0.19 2.41 0.006 1.49 Bond lengths and angles B1 - Distance Angles O1 1.4645 (0.0013) O3 1.4666 (0.0013) 110.86 (0.08) O6 1.4676 (0.0013) 108.55 (0.08) 109.39 (0.09) O4 1.4704 (0.0013) 107.81 (0.08) 109.64 (0.08) 110.57 (0.08) B1 - O1 O3 O6 B2 - Distance Angles O7 1.3519 (0.0014) O1 1.3671 (0.0014) 121.52 (0.10) O2 1.3808 (0.0014) 117.66 (0.10) 120.75 (0.10) B2 - O7 O1 B3 - Distance Angles O8 1.3576 (0.0014) O3 1.3621 (0.0014) 121.23 (0.10) O2 1.3722 (0.0014) 117.29 (0.10) 121.45 (0.10) B3 - O8 O3 B4 - Distance Angles O4 1.3607 (0.0014) O9 1.3617 (0.0014) 122.08 (0.10) O5 1.3820 (0.0014) 121.66 (0.10) 116.26 (0.09) B4 - O4 O9 B5 - Distance Angles O10 1.3505 (0.0014) O6 1.3652 (0.0014) 116.20 (0.10) O5 1.3792 (0.0014) 122.79 (0.10) 120.98 (0.10) B5 - O10 O6 O1 - Distance Angles B2 1.3671 (0.0014) B1 1.4645 (0.0013) 123.05 (0.09) O1 - B2 O2 - Distance Angles B3 1.3722 (0.0014) B2 1.3808 (0.0014) 119.04 (0.09) O2 - B3 O3 - Distance Angles B3 1.3621 (0.0014) B1 1.4666 (0.0013) 122.58 (0.09) O3 - B3 O4 - Distance Angles B4 1.3607 (0.0014) B1 1.4704 (0.0013) 123.50 (0.08) O4 - B4 O5 - Distance Angles B5 1.3792 (0.0014) B4 1.3820 (0.0014) 118.80 (0.09) O5 - B5 O6 - Distance Angles B5 1.3652 (0.0014) B1 1.4676 (0.0013) 124.10 (0.08) O6 - B5 O7 - Distance Angles B2 1.3519 (0.0015) H7 0.8400 109.47 O7 - B2 O8 - Distance Angles B3 1.3576 (0.0014) H8 0.8400 109.47 O8 - B3 O9 - Distance Angles B4 1.3617 (0.0014) H9 0.8400 109.47 O9 - B4 O10 - Distance Angles B5 1.3505 (0.0014) H10 0.8400 109.47 O10 - B5 C1 - Distance Angles N1 1.4716 (0.0015) C2 1.4884 (0.0017) 116.77 (0.10) C3 1.4891 (0.0016) 117.71 (0.10) 60.34 (0.08) H1 1.0000 116.71 116.71 116.71 C1 - N1 C2 C3 C2 - Distance Angles C1 1.4884 (0.0017) C3 1.4964 (0.0017) 59.85 (0.08) H2A 0.9900 117.79 117.79 H2B 0.9900 117.79 117.79 114.92 C2 - C1 C3 H2A C3 - Distance Angles C1 1.4891 (0.0016) C2 1.4964 (0.0017) 59.81 (0.08) H3A 0.9900 117.79 117.79 H3B 0.9900 117.79 117.79 114.92 C3 - C1 C2 H3A N1 - Distance Angles C1 1.4716 (0.0015) H1A 0.9100 109.47 H1B 0.9100 109.47 109.47 H1C 0.9100 109.47 109.47 109.47 N1 - C1 H1A H1B Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.84 1.98 2.8082(11) 166.7 O7-H7...O1_$1 0.84 1.85 2.6719(11) 166.7 O8-H8...O3_$2 0.84 1.93 2.7586(11) 169.5 O9-H9...O4_$3 0.84 1.79 2.6299(11) 176.2 O10-H10...O8_$4 0.91 1.94 2.8423(12) 170.3 N1-H1A...O6_$5 0.91 2.32 3.0654(12) 138.5 N1-H1B...O6_$6 0.91 2.48 3.2912(12) 149.1 N1-H1B...O1_$6 0.91 1.98 2.8895(12) 176.8 N1-H1C...O9 Hydrogen bonds with H..A < r(A) + 2.000 Angstroms and 110 deg. D-H d(D-H) d(H..A)