+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2009src0013pbca started at 12:24:09 on 13-Jan-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2009src0013pbca in Pbca CELL 0.71073 15.5741 14.8047 18.4602 90.000 90.000 90.000 ZERR 16.00 0.0006 0.0004 0.0008 0.000 0.000 0.000 LATT 1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM - X, 1/2 + Y, 1/2 - Z SYMM 1/2 + X, 1/2 - Y, - Z SFAC C H N O ZN UNIT 120 152 72 8 16 V = 4256.37 F(000) = 1920.0 Mu = 2.28 mm-1 Cell Wt = 3777.06 Rho = 1.474 MERG 2 OMIT -3.00 55.00 OMIT 2 1 0 OMIT 1 2 1 SHEL 7 0.77 FMAP 2 PLAN 10 SIZE 0.10 0.22 0.38 ACTA BOND $H WGHT 0.04790 2.63000 L.S. 4 TEMP -153.00 FVAR 0.21501 0.79075 PART 1 C52 1 0.268918 1.161134 0.606885 21.00000 0.04595 AFIX 43 H52 2 0.290570 1.189176 0.649416 21.00000 -1.20000 AFIX 0 C54 1 0.148228 1.136513 0.527023 21.00000 0.05908 AFIX 137 H54A 2 0.193402 1.112459 0.495500 21.00000 -1.50000 H54B 2 0.119511 1.187033 0.502738 21.00000 -1.50000 H54C 2 0.106246 1.088919 0.537361 21.00000 -1.50000 AFIX 0 C55 1 0.127212 1.212051 0.643431 21.00000 0.10555 AFIX 137 H55A 2 0.158907 1.228618 0.687325 21.00000 -1.50000 H55B 2 0.080132 1.171103 0.656166 21.00000 -1.50000 H55C 2 0.103761 1.266632 0.620832 21.00000 -1.50000 AFIX 0 N53 3 0.185102 1.167033 0.592706 21.00000 0.04813 O51 4 0.320287 1.119936 0.566168 21.00000 0.05393 PART 2 SAME C52 > O51 C62 1 0.243624 1.159940 0.545997 -21.00000 0.07273 AFIX 43 H62 2 0.232033 1.148984 0.496242 -21.00000 -1.20000 AFIX 0 C64 1 0.107661 1.239037 0.570201 -21.00000 0.10596 AFIX 137 H64A 2 0.116230 1.274079 0.525747 -21.00000 -1.50000 H64B 2 0.090290 1.279596 0.609513 -21.00000 -1.50000 H64C 2 0.062739 1.193766 0.562217 -21.00000 -1.50000 AFIX 0 C65 1 0.203813 1.199338 0.667756 -21.00000 0.12815 AFIX 137 H65A 2 0.156439 1.171717 0.694777 -21.00000 -1.50000 H65B 2 0.210340 1.262499 0.682660 -21.00000 -1.50000 H65C 2 0.257087 1.166425 0.677830 -21.00000 -1.50000 AFIX 0 N63 3 0.185017 1.195366 0.589101 -21.00000 0.02927 O61 4 0.316132 1.141057 0.573610 -21.00000 0.03597 MOLE 1 PART 0 C2 1 0.104707 0.844456 0.551893 11.00000 0.02033 0.03378 = 0.01891 -0.00292 -0.00264 -0.00289 AFIX 43 H2 2 0.061536 0.810833 0.527507 11.00000 -1.20000 AFIX 0 C4 1 0.220293 0.917134 0.573324 11.00000 0.03594 0.06933 = 0.03386 -0.01392 0.00429 -0.02417 AFIX 43 H4 2 0.274751 0.945354 0.568288 11.00000 -1.20000 AFIX 0 C5 1 0.174406 0.911685 0.635210 11.00000 0.03640 0.07433 = 0.02783 -0.02130 0.00283 -0.02335 AFIX 43 H5 2 0.190888 0.936198 0.680691 11.00000 -1.20000 AFIX 0 N1 3 0.100392 0.865142 0.621705 11.00000 0.02037 0.03623 = 0.01977 -0.00190 -0.00100 -0.00448 N3 3 0.175454 0.875280 0.518919 11.00000 0.02583 0.03402 = 0.02047 -0.00202 -0.00251 -0.00356 MOLE 2 C22 1 0.097521 0.736202 0.807635 11.00000 0.02800 0.03304 = 0.01960 -0.00233 -0.00113 0.00195 AFIX 43 H22 2 0.099114 0.683377 0.778450 11.00000 -1.20000 AFIX 0 C24 1 0.071279 0.629190 0.344431 11.00000 0.04185 0.03241 = 0.02842 0.00171 -0.00973 -0.00987 AFIX 43 H24 2 0.051169 0.568693 0.347001 11.00000 -1.20000 AFIX 0 C25 1 0.116603 0.672134 0.396079 11.00000 0.04239 0.03176 = 0.02947 0.01053 -0.01163 -0.00045 AFIX 43 H25 2 0.133820 0.646599 0.441001 11.00000 -1.20000 AFIX 0 N21 3 0.134032 0.758525 0.373689 11.00000 0.02695 0.03340 = 0.01996 0.00057 -0.00254 0.00060 N23 3 0.058901 0.812585 0.787304 11.00000 0.02536 0.03512 = 0.02128 0.00184 -0.00165 0.00103 MOLE 3 C32 1 -0.143211 0.732143 0.641203 11.00000 0.02370 0.04073 = 0.02121 -0.00136 -0.00002 0.00304 AFIX 43 H32 2 -0.178957 0.777584 0.661472 11.00000 -1.20000 AFIX 0 C34 1 -0.031068 0.656162 0.611029 11.00000 0.01992 0.04009 = 0.04171 0.00056 -0.00128 0.00557 AFIX 43 H34 2 0.026631 0.636412 0.605747 11.00000 -1.20000 AFIX 0 N31 3 0.326370 0.837832 0.396108 11.00000 0.02417 0.03338 = 0.02525 -0.00013 0.00125 -0.00038 N33 3 -0.057575 0.732546 0.647516 11.00000 0.02304 0.03311 = 0.02429 0.00279 -0.00255 0.00214 MOLE 4 C42 1 -0.094312 0.987754 0.637868 11.00000 0.02571 0.03233 = 0.01925 -0.00020 0.00298 -0.00213 AFIX 43 H42 2 -0.058696 0.990502 0.596148 11.00000 -1.20000 AFIX 0 C43 1 0.398769 0.885778 0.415923 11.00000 0.02760 0.03226 = 0.04429 -0.00001 0.00230 -0.00211 AFIX 43 H43 2 0.399173 0.939571 0.443979 11.00000 -1.20000 AFIX 0 C44 1 0.197045 0.987057 0.288029 11.00000 0.03757 0.04505 = 0.03787 0.01265 0.01880 0.00814 AFIX 43 H44 2 0.247907 0.964081 0.266407 11.00000 -1.20000 AFIX 0 C45 1 -0.142740 0.951697 0.742388 11.00000 0.04276 0.04628 = 0.02897 0.01187 0.01744 0.01381 AFIX 43 H45 2 -0.149288 0.924857 0.788804 11.00000 -1.20000 AFIX 0 N41 3 -0.077056 0.935263 0.694820 11.00000 0.02693 0.03355 = 0.01885 0.00300 0.00057 -0.00001 N43 3 0.166099 0.964044 0.355092 11.00000 0.02583 0.03149 = 0.02847 0.00496 0.00182 0.00376 MOLE 5 ZN1 5 0.203210 0.859157 0.415703 11.00000 0.02209 0.03074 = 0.02013 0.00056 -0.00025 0.00074 ZN2 5 0.007705 0.834447 0.691341 11.00000 0.02258 0.03471 = 0.01928 0.00210 -0.00241 0.00087 HKLF 4 1.0 0.00 1.00 0.00 1.00 0.00 0.00 0.00 0.00 -1.00 Covalent radii and connectivity table for 2009src0013pbca in Pbca C 0.770 H 0.320 N 0.700 O 0.660 ZN 1.330 C52_a - O51_a N53_a C54_a - N53_a C55_a - N53_a N53_a - C52_a C54_a C55_a O51_a - C52_a C62_b - O61_b N63_b C64_b - N63_b C65_b - N63_b N63_b - C62_b C64_b C65_b O61_b - C62_b C2 - N1 N3 C4 - C5 N3 C5 - C4 N1 N1 - C2 C5 Zn2 N3 - C2 C4 Zn1 C22 - N23 N21_$2 C24 - C25 N23_$1 C25 - C24 N21 N21 - C22_$1 C25 Zn1 N23 - C22 C24_$2 Zn2 C32 - N31_$4 N33 C34 - C43_$4 N33 N31 - C32_$3 C43 Zn1 N33 - C32 C34 Zn2 C42 - N43_$5 N41 C43 - C34_$3 N31 C44 - C45_$5 N43 C45 - C44_$5 N41 N41 - C42 C45 Zn2 N43 - C42_$5 C44 Zn1 Zn1 - N3 N31 N21 N43 Zn2 - N23 N1 N33 N41 Operators for generating equivalent atoms: $1 x, -y+3/2, z-1/2 $2 x, -y+3/2, z+1/2 $3 x+1/2, -y+3/2, -z+1 $4 x-1/2, -y+3/2, -z+1 $5 -x, -y+2, -z+1 33526 Reflections read, of which 2127 rejected -20 =< h =< 19, -16 =< k =< 19, -22 =< l =< 23, Max. 2-theta = 54.97 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Su of mean(Fo^2) 4 14 0 6.46 1.10 3 7.07 3 13 2 0.23 0.10 11 2.22 14 10 3 0.93 0.36 6 4.02 11 9 8 0.85 0.35 5 4.59 4 Inconsistent equivalents 4866 Unique reflections, of which 0 suppressed R(int) = 0.0956 R(sigma) = 0.0738 Friedel opposites merged Maximum memory for data reduction = 3214 / 48696 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 = 3932 / 303763 wR2 = 0.1143 before cycle 1 for 4866 data and 244 / 244 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 8. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.031 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.014; Restrained GooF = 1.013 for 8 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0479 * P )^2 + 2.63 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.21500 0.00037 -0.015 OSF 2 0.79072 0.00766 -0.003 FVAR 2 Mean shift/su = 0.002 Maximum = 0.020 for U13 Zn2 Max. shift = 0.004 A for H65A_b Max. dU = 0.000 for C62_b Least-squares cycle 2 Maximum vector length = 511 Memory required = 3932 / 303763 wR2 = 0.1143 before cycle 2 for 4866 data and 244 / 244 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 8. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.031 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.014; Restrained GooF = 1.014 for 8 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0479 * P )^2 + 2.63 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.21500 0.00037 -0.004 OSF 2 0.79069 0.00766 -0.004 FVAR 2 Mean shift/su = 0.001 Maximum = 0.016 for z O61_b Max. shift = 0.004 A for H65A_b Max. dU = 0.000 for C62_b Least-squares cycle 3 Maximum vector length = 511 Memory required = 3932 / 303763 wR2 = 0.1143 before cycle 3 for 4866 data and 244 / 244 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 8. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.031 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.014; Restrained GooF = 1.013 for 8 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0479 * P )^2 + 2.63 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.21500 0.00037 0.001 OSF 2 0.79068 0.00766 -0.002 FVAR 2 Mean shift/su = 0.001 Maximum = 0.012 for z O61_b Max. shift = 0.003 A for H65A_b Max. dU = 0.000 for O61_b Least-squares cycle 4 Maximum vector length = 511 Memory required = 3932 / 303763 wR2 = 0.1143 before cycle 4 for 4866 data and 244 / 244 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 8. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.031 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.014; Restrained GooF = 1.013 for 8 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0479 * P )^2 + 2.63 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.21500 0.00037 0.000 OSF 2 0.79066 0.00766 -0.002 FVAR 2 Mean shift/su = 0.000 Maximum = 0.007 for tors H65A_b Max. shift = 0.002 A for H65A_b Max. dU = 0.000 for C65_b Largest correlation matrix elements -0.678 y N63_b / U11 N53_a -0.617 x O61_b / x O51_a 0.507 U11 O61_b / y O51_a -0.675 U11 O61_b / U11 O51_a 0.588 z N63_b / z C65_b 0.506 U11 C52_a / FVAR 2 -0.659 z O61_b / z O51_a 0.564 U11 N63_b / y N53_a -0.637 y O61_b / U11 O51_a 0.517 U11 C54_a / FVAR 2 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H52 0.2906 1.1892 0.6494 43 0.950 0.000 C52_a O51_a N53_a H54A 0.1934 1.1125 0.4955 137 0.980 0.000 C54_a N53_a H54A_a H54B 0.1195 1.1870 0.5027 137 0.980 0.000 C54_a N53_a H54A_a H54C 0.1062 1.0889 0.5374 137 0.980 0.000 C54_a N53_a H54A_a H55A 0.1589 1.2286 0.6873 137 0.980 0.000 C55_a N53_a H55A_a H55B 0.0801 1.1711 0.6562 137 0.980 0.000 C55_a N53_a H55A_a H55C 0.1037 1.2666 0.6208 137 0.980 0.000 C55_a N53_a H55A_a H62 0.2321 1.1490 0.4962 43 0.950 0.000 C62_b O61_b N63_b H64A 0.1162 1.2740 0.5257 137 0.980 0.000 C64_b N63_b H64A_b H64B 0.0903 1.2796 0.6095 137 0.980 0.000 C64_b N63_b H64A_b H64C 0.0627 1.1938 0.5622 137 0.980 0.000 C64_b N63_b H64A_b H65A 0.1564 1.1718 0.6948 137 0.980 0.000 C65_b N63_b H65A_b H65B 0.2104 1.2625 0.6827 137 0.980 0.000 C65_b N63_b H65A_b H65C 0.2571 1.1664 0.6778 137 0.980 0.000 C65_b N63_b H65A_b H2 0.0615 0.8108 0.5275 43 0.950 0.000 C2 N1 N3 H4 0.2747 0.9454 0.5683 43 0.950 0.000 C4 C5 N3 H5 0.1909 0.9362 0.6807 43 0.950 0.000 C5 C4 N1 H22 0.0991 0.6834 0.7785 43 0.950 0.000 C22 N23 N21_$2 H24 0.0512 0.5687 0.3470 43 0.950 0.000 C24 C25 N23_$1 H25 0.1338 0.6466 0.4410 43 0.950 0.000 C25 C24 N21 H32 -0.1790 0.7776 0.6615 43 0.950 0.000 C32 N31_$4 N33 H34 0.0266 0.6364 0.6057 43 0.950 0.000 C34 C43_$4 N33 H42 -0.0587 0.9905 0.5961 43 0.950 0.000 C42 N43_$5 N41 H43 0.3992 0.9396 0.4440 43 0.950 0.000 C43 C34_$3 N31 H44 0.2479 0.9641 0.2664 43 0.950 0.000 C44 C45_$5 N43 H45 -0.1493 0.9249 0.7888 43 0.950 0.000 C45 C44_$5 N41 2009src0013pbca in Pbca ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C52_a 0.26891 1.16114 0.60689 0.79066 0.04595 0.01073 0.00038 0.00038 0.00035 0.00766 0.00168 H52_a 0.29057 1.18917 0.64942 0.79066 0.05514 0.00766 0.00000 C54_a 0.14823 1.13651 0.52702 0.79066 0.05906 0.01103 0.00043 0.00041 0.00037 0.00766 0.00203 H54A_a 0.19340 1.11246 0.49550 0.79066 0.08859 0.00766 0.00000 H54B_a 0.11951 1.18703 0.50273 0.79066 0.08859 0.00766 0.00000 H54C_a 0.10625 1.08892 0.53736 0.79066 0.08859 0.00766 0.00000 C55_a 0.12721 1.21205 0.64343 0.79066 0.10552 0.01750 0.00062 0.00063 0.00057 0.00766 0.00329 H55A_a 0.15891 1.22864 0.68732 0.79066 0.15828 0.00766 0.00000 H55B_a 0.08014 1.17110 0.65618 0.79066 0.15828 0.00766 0.00000 H55C_a 0.10375 1.26662 0.62082 0.79066 0.15828 0.00766 0.00000 N53_a 0.18510 1.16703 0.59271 0.79066 0.04813 0.01052 0.00036 0.00047 0.00032 0.00766 0.00196 O51_a 0.32028 1.11994 0.56615 0.79066 0.05389 0.01072 0.00035 0.00042 0.00036 0.00766 0.00215 C62_b 0.24364 1.15994 0.54601 0.20934 0.07283 0.04254 0.00133 0.00168 0.00125 0.00766 0.00913 H62_b 0.23208 1.14899 0.49625 0.20934 0.08740 0.00766 0.00000 C64_b 0.10766 1.23903 0.57019 0.20934 0.10603 0.05622 0.00164 0.00214 0.00183 0.00766 0.01258 H64A_b 0.11623 1.27405 0.52573 0.20934 0.15905 0.00766 0.00000 H64B_b 0.09029 1.27960 0.60949 0.20934 0.15905 0.00766 0.00000 H64C_b 0.06274 1.19375 0.56223 0.20934 0.15905 0.00766 0.00000 C65_b 0.20380 1.19934 0.66776 0.20934 0.12820 0.05995 0.00246 0.00292 0.00130 0.00766 0.01533 H65A_b 0.15640 1.17176 0.69478 0.20934 0.19230 0.00766 0.00000 H65B_b 0.21037 1.26250 0.68265 0.20934 0.19230 0.00766 0.00000 H65C_b 0.25705 1.16639 0.67785 0.20934 0.19230 0.00766 0.00000 N63_b 0.18502 1.19537 0.58910 0.20934 0.02930 0.03328 0.00100 0.00147 0.00095 0.00766 0.00536 O61_b 0.31614 1.14105 0.57367 0.20934 0.03606 0.03519 0.00109 0.00140 0.00119 0.00766 0.00583 C2 0.10471 0.84446 0.55189 1.00000 0.02033 0.03377 0.01891 -0.00292 -0.00264 -0.00289 0.02434 0.00618 0.00022 0.00024 0.00020 0.00000 0.00182 0.00209 0.00208 0.00164 0.00148 0.00153 0.00083 H2 0.06154 0.81083 0.52751 1.00000 0.02920 0.00000 0.00000 C4 0.22029 0.91713 0.57332 1.00000 0.03594 0.06934 0.03385 -0.01392 0.00429 -0.02417 0.04638 0.00714 0.00028 0.00033 0.00024 0.00000 0.00238 0.00316 0.00276 0.00238 0.00200 0.00218 0.00121 H4 0.27475 0.94535 0.56829 1.00000 0.05565 0.00000 0.00000 C5 0.17441 0.91168 0.63521 1.00000 0.03640 0.07432 0.02783 -0.02130 0.00283 -0.02335 0.04618 0.00693 0.00026 0.00032 0.00025 0.00000 0.00237 0.00327 0.00256 0.00237 0.00199 0.00220 0.00120 H5 0.19089 0.93620 0.68069 1.00000 0.05542 0.00000 0.00000 N1 0.10039 0.86514 0.62171 1.00000 0.02037 0.03622 0.01977 -0.00190 -0.00100 -0.00448 0.02545 0.00499 0.00018 0.00020 0.00017 0.00000 0.00159 0.00173 0.00179 0.00145 0.00127 0.00129 0.00070 N3 0.17545 0.87528 0.51892 1.00000 0.02583 0.03402 0.02047 -0.00201 -0.00251 -0.00356 0.02678 0.00508 0.00019 0.00020 0.00017 0.00000 0.00165 0.00174 0.00182 0.00144 0.00136 0.00133 0.00072 C22 0.09752 0.73620 0.80764 1.00000 0.02799 0.03304 0.01960 -0.00233 -0.00113 0.00195 0.02688 0.00638 0.00022 0.00025 0.00020 0.00000 0.00198 0.00209 0.00214 0.00172 0.00165 0.00162 0.00085 H22 0.09911 0.68338 0.77845 1.00000 0.03225 0.00000 0.00000 C24 0.07128 0.62919 0.34443 1.00000 0.04185 0.03241 0.02842 0.00171 -0.00973 -0.00987 0.03422 0.00666 0.00026 0.00027 0.00022 0.00000 0.00238 0.00212 0.00245 0.00186 0.00192 0.00183 0.00097 H24 0.05117 0.56869 0.34700 1.00000 0.04107 0.00000 0.00000 C25 0.11660 0.67213 0.39608 1.00000 0.04239 0.03176 0.02947 0.01053 -0.01164 -0.00045 0.03454 0.00689 0.00027 0.00026 0.00023 0.00000 0.00236 0.00212 0.00243 0.00183 0.00190 0.00184 0.00097 H25 0.13382 0.64660 0.44100 1.00000 0.04145 0.00000 0.00000 N21 0.13403 0.75853 0.37369 1.00000 0.02695 0.03339 0.01996 0.00057 -0.00254 0.00060 0.02677 0.00514 0.00018 0.00020 0.00017 0.00000 0.00165 0.00177 0.00185 0.00145 0.00137 0.00135 0.00072 N23 0.05890 0.81258 0.78730 1.00000 0.02536 0.03511 0.02128 0.00184 -0.00165 0.00103 0.02725 0.00532 0.00019 0.00021 0.00017 0.00000 0.00167 0.00183 0.00180 0.00145 0.00134 0.00137 0.00073 C32 -0.14321 0.73214 0.64120 1.00000 0.02369 0.04073 0.02121 -0.00135 -0.00002 0.00304 0.02854 0.00648 0.00022 0.00026 0.00021 0.00000 0.00195 0.00229 0.00218 0.00179 0.00163 0.00166 0.00088 H32 -0.17896 0.77758 0.66147 1.00000 0.03425 0.00000 0.00000 C34 -0.03107 0.65616 0.61103 1.00000 0.01992 0.04009 0.04171 0.00057 -0.00128 0.00557 0.03390 0.00707 0.00025 0.00026 0.00024 0.00000 0.00189 0.00235 0.00267 0.00199 0.00179 0.00168 0.00097 H34 0.02663 0.63641 0.60575 1.00000 0.04068 0.00000 0.00000 N31 0.32637 0.83783 0.39611 1.00000 0.02417 0.03338 0.02525 -0.00014 0.00125 -0.00038 0.02760 0.00539 0.00019 0.00021 0.00017 0.00000 0.00161 0.00178 0.00187 0.00144 0.00137 0.00136 0.00073 N33 -0.05757 0.73255 0.64752 1.00000 0.02305 0.03311 0.02429 0.00279 -0.00255 0.00214 0.02681 0.00521 0.00018 0.00020 0.00017 0.00000 0.00162 0.00178 0.00188 0.00142 0.00136 0.00130 0.00072 C42 -0.09431 0.98775 0.63787 1.00000 0.02571 0.03233 0.01924 -0.00020 0.00298 -0.00212 0.02576 0.00604 0.00022 0.00023 0.00021 0.00000 0.00196 0.00200 0.00206 0.00169 0.00159 0.00158 0.00083 H42 -0.05870 0.99050 0.59615 1.00000 0.03091 0.00000 0.00000 C43 0.39877 0.88578 0.41592 1.00000 0.02760 0.03226 0.04428 -0.00002 0.00230 -0.00211 0.03472 0.00716 0.00024 0.00027 0.00024 0.00000 0.00217 0.00206 0.00280 0.00199 0.00189 0.00170 0.00098 H43 0.39917 0.93957 0.44398 1.00000 0.04166 0.00000 0.00000 C44 0.19704 0.98706 0.28803 1.00000 0.03757 0.04505 0.03787 0.01265 0.01880 0.00814 0.04016 0.00801 0.00026 0.00028 0.00024 0.00000 0.00234 0.00250 0.00270 0.00208 0.00199 0.00199 0.00107 H44 0.24791 0.96408 0.26641 1.00000 0.04819 0.00000 0.00000 C45 -0.14274 0.95170 0.74239 1.00000 0.04276 0.04627 0.02897 0.01187 0.01744 0.01381 0.03933 0.00786 0.00026 0.00028 0.00024 0.00000 0.00238 0.00243 0.00247 0.00203 0.00198 0.00204 0.00105 H45 -0.14929 0.92486 0.78880 1.00000 0.04720 0.00000 0.00000 N41 -0.07706 0.93526 0.69482 1.00000 0.02692 0.03355 0.01884 0.00300 0.00057 -0.00001 0.02644 0.00518 0.00019 0.00020 0.00016 0.00000 0.00158 0.00172 0.00176 0.00143 0.00137 0.00135 0.00070 N43 0.16610 0.96404 0.35509 1.00000 0.02583 0.03149 0.02847 0.00495 0.00181 0.00376 0.02859 0.00541 0.00019 0.00020 0.00018 0.00000 0.00162 0.00173 0.00195 0.00149 0.00144 0.00136 0.00073 Zn1 0.20321 0.85916 0.41570 1.00000 0.02208 0.03074 0.02012 0.00056 -0.00025 0.00074 0.02432 0.00072 0.00003 0.00003 0.00002 0.00000 0.00023 0.00025 0.00025 0.00020 0.00018 0.00017 0.00014 Zn2 0.00771 0.83445 0.69134 1.00000 0.02258 0.03471 0.01928 0.00210 -0.00241 0.00087 0.02552 0.00073 0.00003 0.00003 0.00002 0.00000 0.00023 0.00026 0.00025 0.00019 0.00018 0.00018 0.00014 Final Structure Factor Calculation for 2009src0013pbca in Pbca Total number of l.s. parameters = 244 Maximum vector length = 511 Memory required = 3688 / 24017 wR2 = 0.1143 before cycle 5 for 4866 data and 0 / 244 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 8. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.031 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.014; Restrained GooF = 1.013 for 8 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0479 * P )^2 + 2.63 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0473 for 3217 Fo > 4sig(Fo) and 0.0889 for all 4866 data wR2 = 0.1143, GooF = S = 1.014, Restrained GooF = 1.013 for all data Occupancy sum of asymmetric unit = 27.00 for non-hydrogen and 19.00 for hydrogen atoms Principal mean square atomic displacements U 0.0347 0.0223 0.0160 C2 0.0860 0.0308 0.0224 C4 0.0920 0.0298 0.0167 C5 0.0375 0.0209 0.0180 N1 0.0354 0.0261 0.0188 N3 0.0342 0.0273 0.0191 C22 0.0517 0.0290 0.0219 C24 0.0512 0.0355 0.0169 C25 0.0335 0.0277 0.0191 N21 0.0354 0.0259 0.0204 N23 0.0413 0.0232 0.0211 C32 0.0419 0.0414 0.0184 C34 0.0334 0.0261 0.0233 N31 0.0341 0.0262 0.0201 N33 0.0330 0.0262 0.0181 C42 0.0446 0.0330 0.0265 C43 0.0666 0.0354 0.0185 C44 0.0690 0.0320 0.0169 C45 0.0341 0.0270 0.0182 N41 0.0367 0.0253 0.0238 N43 0.0308 0.0221 0.0201 Zn1 0.0350 0.0238 0.0177 Zn2 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.011 0.021 0.032 0.045 0.057 0.074 0.093 0.121 0.170 1.000 Number in group 524. 477. 476. 503. 480. 485. 459. 497. 475. 490. GooF 0.822 0.846 1.006 1.058 1.076 1.160 1.142 1.003 0.993 0.996 K 1.838 0.969 1.048 0.962 0.968 0.962 0.997 1.003 1.018 0.998 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.32 1.65 inf Number in group 502. 491. 477. 490. 484. 475. 488. 488. 486. 485. GooF 0.882 0.915 0.931 0.994 1.072 0.986 1.051 1.007 1.012 1.245 K 1.018 0.994 0.998 1.004 1.011 1.008 1.016 1.028 1.023 0.975 R1 0.254 0.206 0.175 0.142 0.095 0.074 0.068 0.045 0.034 0.030 Recommended weighting scheme: WGHT 0.0478 2.6641 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)/su Fc/Fc(max) Resolution(A) 1 1 2 8569.71 18344.60 6.04 0.293 7.00 5 14 5 483.46 990.87 4.57 0.068 0.97 1 6 3 470.61 265.27 4.19 0.035 2.27 7 6 5 260.04 107.65 3.72 0.022 1.51 5 6 3 837.31 559.85 3.66 0.051 1.85 3 15 2 264.55 587.05 3.62 0.052 0.96 2 7 6 240.07 417.08 3.61 0.044 1.70 5 3 4 311.20 166.68 3.40 0.028 2.29 11 1 18 219.79 817.12 3.38 0.062 0.83 3 3 6 435.46 246.88 3.36 0.034 2.33 9 9 7 2815.51 3689.03 3.35 0.131 1.09 3 2 2 207.41 116.52 3.32 0.023 3.86 4 0 0 6338.10 5030.46 3.29 0.153 3.89 8 13 4 330.17 772.47 3.28 0.060 0.96 6 15 1 2884.15 1844.06 3.27 0.093 0.92 7 8 9 348.33 666.78 3.27 0.056 1.17 1 3 8 6230.88 5170.50 3.21 0.155 2.07 10 10 6 2758.06 1928.39 3.21 0.095 1.01 9 6 20 1082.85 1848.19 3.19 0.093 0.77 3 4 1 1925.05 2384.47 3.12 0.106 2.97 0 10 16 1835.72 479.59 3.10 0.047 0.91 8 1 17 658.55 1055.80 3.09 0.070 0.95 11 7 7 77.29 287.53 3.07 0.037 1.07 9 0 4 1136.92 784.45 3.07 0.061 1.62 5 2 6 692.49 487.94 3.02 0.048 2.10 7 9 15 1287.26 1850.90 2.97 0.093 0.90 5 0 6 5310.19 4218.65 2.95 0.140 2.19 4 4 15 3554.61 4388.17 2.92 0.143 1.12 6 1 4 380.33 245.94 2.92 0.034 2.24 16 1 4 895.15 1306.87 2.92 0.078 0.95 8 5 11 -59.26 120.20 2.89 0.024 1.17 8 13 6 835.32 394.29 2.89 0.043 0.94 6 6 5 534.52 731.99 2.88 0.058 1.61 16 7 5 949.40 1543.08 2.86 0.085 0.86 11 11 5 249.13 585.00 2.85 0.052 0.94 16 3 5 1229.09 1774.16 2.84 0.091 0.92 6 10 9 352.12 671.83 2.84 0.056 1.09 1 3 10 878.45 606.39 2.83 0.053 1.72 3 4 11 598.02 363.63 2.81 0.041 1.47 9 7 15 185.92 630.42 2.81 0.054 0.91 14 0 16 -214.02 341.63 2.79 0.040 0.80 4 1 7 3489.72 2904.66 2.79 0.116 2.16 13 12 5 658.33 1157.17 2.78 0.073 0.84 7 6 17 -42.77 485.25 2.78 0.048 0.91 2 4 20 932.84 1495.22 2.77 0.084 0.89 4 2 19 906.98 1531.85 2.75 0.085 0.94 16 9 6 1563.28 2176.07 2.75 0.101 0.81 11 10 2 188.63 424.30 2.73 0.045 1.02 13 2 5 12941.30 11020.00 2.73 0.227 1.13 3 6 3 30.57 128.85 2.72 0.025 2.10 Bond lengths and angles C52_a - Distance Angles O51_a 1.2559 (0.0083) N53_a 1.3342 (0.0076) 122.51 (0.66) H52_a 0.9500 118.74 118.74 C52_a - O51_a N53_a C54_a - Distance Angles N53_a 1.4157 (0.0081) H54A_a 0.9800 109.47 H54B_a 0.9800 109.47 109.47 H54C_a 0.9800 109.47 109.47 109.47 C54_a - N53_a H54A_a H54B_a C55_a - Distance Angles N53_a 1.4608 (0.0098) H55A_a 0.9800 109.47 H55B_a 0.9800 109.47 109.47 H55C_a 0.9800 109.47 109.47 109.47 C55_a - N53_a H55A_a H55B_a N53_a - Distance Angles C52_a 1.3342 (0.0076) C54_a 1.4157 (0.0081) 122.96 (0.59) C55_a 1.4608 (0.0098) 120.53 (0.68) 116.38 (0.65) N53_a - C52_a C54_a O51_a - Distance Angles C52_a 1.2559 (0.0083) O51_a - C62_b - Distance Angles O61_b 1.2704 (0.0177) N63_b 1.3196 (0.0167) 117.39 (2.06) H62_b 0.9500 121.31 121.30 C62_b - O61_b N63_b C64_b - Distance Angles N63_b 1.4111 (0.0175) H64A_b 0.9800 109.47 H64B_b 0.9800 109.47 109.47 H64C_b 0.9800 109.47 109.47 109.47 C64_b - N63_b H64A_b H64B_b C65_b - Distance Angles N63_b 1.4824 (0.0182) H65A_b 0.9800 109.47 H65B_b 0.9800 109.47 109.47 H65C_b 0.9800 109.47 109.47 109.47 C65_b - N63_b H65A_b H65B_b N63_b - Distance Angles C62_b 1.3196 (0.0168) C64_b 1.4111 (0.0175) 128.58 (1.93) C65_b 1.4824 (0.0182) 118.02 (1.85) 113.12 (1.93) N63_b - C62_b C64_b O61_b - Distance Angles C62_b 1.2704 (0.0177) O61_b - C2 - Distance Angles N1 1.3263 (0.0046) N3 1.3389 (0.0045) 113.87 (0.32) H2 0.9500 123.06 123.06 C2 - N1 N3 C4 - Distance Angles C5 1.3499 (0.0059) N3 1.3712 (0.0050) 108.86 (0.36) H4 0.9500 125.57 125.57 C4 - C5 N3 C5 - Distance Angles C4 1.3499 (0.0060) N1 1.3659 (0.0046) 108.81 (0.37) H5 0.9500 125.59 125.59 C5 - C4 N1 N1 - Distance Angles C2 1.3263 (0.0046) C5 1.3659 (0.0046) 104.54 (0.31) Zn2 1.9856 (0.0030) 127.81 (0.24) 127.65 (0.27) N1 - C2 C5 N3 - Distance Angles C2 1.3389 (0.0044) C4 1.3712 (0.0050) 103.89 (0.32) Zn1 1.9683 (0.0032) 125.41 (0.25) 130.69 (0.27) N3 - C2 C4 C22 - Distance Angles N23 1.3347 (0.0045) N21_$2 1.3477 (0.0046) 113.30 (0.33) H22 0.9500 123.35 123.35 C22 - N23 N21_$2 C24 - Distance Angles C25 1.3459 (0.0054) N23_$1 1.3756 (0.0049) 108.70 (0.34) H24 0.9500 125.65 125.65 C24 - C25 N23_$1 C25 - Distance Angles C24 1.3459 (0.0054) N21 1.3713 (0.0047) 109.32 (0.35) H25 0.9500 125.34 125.34 C25 - C24 N21 N21 - Distance Angles C22_$1 1.3477 (0.0046) C25 1.3713 (0.0047) 104.08 (0.31) Zn1 1.9955 (0.0030) 122.43 (0.25) 133.32 (0.26) N21 - C22_$1 C25 N23 - Distance Angles C22 1.3347 (0.0045) C24_$2 1.3756 (0.0050) 104.61 (0.31) Zn2 1.9694 (0.0031) 125.07 (0.26) 130.04 (0.26) N23 - C22 C24_$2 C32 - Distance Angles N31_$4 1.3312 (0.0047) N33 1.3388 (0.0044) 113.77 (0.34) H32 0.9500 123.12 123.12 C32 - N31_$4 N33 C34 - Distance Angles C43_$4 1.3517 (0.0054) N33 1.3795 (0.0048) 108.32 (0.33) H34 0.9500 125.84 125.84 C34 - C43_$4 N33 N31 - Distance Angles C32_$3 1.3312 (0.0047) C43 1.3817 (0.0048) 104.26 (0.31) Zn1 1.9773 (0.0030) 124.34 (0.25) 131.39 (0.26) N31 - C32_$3 C43 N33 - Distance Angles C32 1.3388 (0.0044) C34 1.3795 (0.0048) 104.59 (0.31) Zn2 1.9910 (0.0030) 123.19 (0.26) 131.82 (0.24) N33 - C32 C34 C42 - Distance Angles N43_$5 1.3327 (0.0043) N41 1.3347 (0.0046) 113.82 (0.33) H42 0.9500 123.09 123.09 C42 - N43_$5 N41 C43 - Distance Angles C34_$3 1.3517 (0.0054) N31 1.3817 (0.0048) 109.04 (0.35) H43 0.9500 125.48 125.48 C43 - C34_$3 N31 C44 - Distance Angles C45_$5 1.3611 (0.0055) N43 1.3715 (0.0049) 108.63 (0.34) H44 0.9500 125.68 125.68 C44 - C45_$5 N43 C45 - Distance Angles C44_$5 1.3611 (0.0055) N41 1.3699 (0.0047) 108.53 (0.36) H45 0.9500 125.73 125.73 C45 - C44_$5 N41 N41 - Distance Angles C42 1.3347 (0.0046) C45 1.3699 (0.0047) 104.54 (0.31) Zn2 1.9936 (0.0030) 122.95 (0.25) 130.40 (0.26) N41 - C42 C45 N43 - Distance Angles C42_$5 1.3327 (0.0043) C44 1.3715 (0.0050) 104.47 (0.31) Zn1 1.9993 (0.0030) 127.14 (0.26) 126.62 (0.25) N43 - C42_$5 C44 Zn1 - Distance Angles N3 1.9683 (0.0032) N31 1.9773 (0.0031) 114.17 (0.13) N21 1.9955 (0.0030) 110.38 (0.12) 109.48 (0.13) N43 1.9993 (0.0030) 112.59 (0.13) 107.58 (0.12) 101.90 (0.13) Zn1 - N3 N31 N21 Zn2 - Distance Angles N23 1.9694 (0.0031) N1 1.9856 (0.0030) 109.00 (0.12) N33 1.9910 (0.0030) 116.60 (0.13) 106.35 (0.12) N41 1.9936 (0.0030) 111.23 (0.13) 109.32 (0.12) 104.02 (0.12) Zn2 - N23 N1 N33 FMAP and GRID set by program FMAP 2 1 20 GRID -1.471 -2 -1 1.471 2 1 R1 = 0.0869 for 4866 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.57 at 0.1300 0.2611 0.1285 [ 0.49 A from C55 ] Deepest hole -0.56 at 0.0096 0.1692 0.2624 [ 0.90 A from ZN2 ] Mean = 0.00, Rms deviation from mean = 0.11 e/A^3, Highest memory used = 4159 / 37041 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.1300 1.2389 0.6285 1.00000 0.05 0.57 0.49 C55 0.60 H55C 0.93 H64B 1.13 C64 Q2 1 0.1074 1.1725 0.6494 1.00000 0.05 0.55 0.44 H55B 0.67 C55 1.13 H65A 1.35 H55A Q3 1 0.2955 1.1391 0.7035 1.00000 0.05 0.50 0.86 H65C 1.24 H52 1.81 C65 1.86 C52 Q4 1 -0.1019 0.8391 0.8081 1.00000 0.05 0.43 1.51 H45 1.70 H55C 1.77 H64B 1.86 H55A Q5 1 0.1240 1.1229 0.6967 1.00000 0.05 0.43 0.88 H65A 1.24 H55B 1.65 C55 1.67 H55A Q6 1 0.3050 1.1454 0.5493 1.00000 0.05 0.42 0.49 O61 0.54 O51 0.98 C62 1.22 C52 Q7 1 0.1507 0.9649 0.4733 1.00000 0.05 0.41 1.62 N3 2.03 H42 2.06 ZN1 2.20 N43 Q8 1 0.1341 1.0703 0.6584 1.00000 0.05 0.41 1.68 H65A 1.71 H55B 2.04 N53 2.12 C55 Q9 1 0.0183 0.6381 0.8227 1.00000 0.05 0.40 1.64 H22 1.66 H55B 1.93 C22 2.54 N21 Q10 1 0.2024 0.6331 0.4625 1.00000 0.05 0.39 1.16 H25 1.22 H62 1.76 H54A 1.80 C62 Shortest distances between peaks (including symmetry equivalents) 5 8 1.06 1 2 1.11 2 5 1.17 2 8 1.58 6 10 1.62 1 4 1.94 2 9 2.09 1 5 2.13 5 9 2.26 1 8 2.56 2 4 2.59 8 9 2.60 3 5 2.68 3 8 2.84 3 6 2.85 1 9 2.89 Time profile in seconds ----------------------- 0.06: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: 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. 1.52: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 2.28: Structure factors and derivatives 1.88: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.17: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.09: Analysis of variance 0.05: Merge reflections for Fourier and .fcf 0.09: Fourier summations 0.05: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2009src0013pbca finished at 12:24:15 Total CPU time: 6.2 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++