+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 04src0422 started at 12:55:58 on 20-Nov-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 04src0422 in C2/c CELL 0.71073 23.5068 18.1213 21.0066 90.000 118.687 90.000 ZERR 2.00 0.0047 0.0036 0.0042 0.000 0.030 0.000 LATT 7 SYMM - X, Y, 1/2 - Z SFAC C H N O CL ZN UNIT 232 248 104 120 24 12 V = 7849.90 F(000) = 4096.0 Mu = 1.21 mm-1 Cell Wt = 8048.58 Rho = 1.703 MERG 2 OMIT -3.00 55.00 OMIT -2 0 4 OMIT -4 0 2 OMIT -6 0 6 OMIT -3 3 3 OMIT -2 4 5 OMIT 0 4 5 OMIT 0 12 1 EXTI 0.00110 SHEL 7 0.77 DELU 0.01 SIMU 0.01 FMAP 2 PLAN 5 SIZE 0.07 0.20 0.22 ACTA BOND $H WGHT 0.07360 181.32001 L.S. 20 TEMP -153.00 FVAR 0.19646 0.41844 0.53526 ZN1 6 0.000000 0.941001 0.750000 10.50000 0.04385 0.03660 = 0.04961 0.00000 0.02682 0.00000 ZN2 6 0.000000 1.184937 0.750000 10.50000 0.02115 0.03583 = 0.04385 0.00000 0.01407 0.00000 ZN3 6 0.000000 1.429917 0.750000 10.50000 0.05275 0.03408 = 0.05313 0.00000 0.01990 0.00000 MOLE 1 C1 1 0.010543 0.817593 0.863433 11.00000 0.10396 0.04819 = 0.07741 0.00125 0.06904 0.00621 AFIX 43 H1 2 0.054203 0.833669 0.890882 11.00000 -1.20000 AFIX 0 C2 1 -0.010509 0.758793 0.888832 11.00000 0.11492 0.05888 = 0.09167 0.01059 0.07388 0.00493 AFIX 43 H2 2 0.017532 0.735294 0.933500 11.00000 -1.20000 AFIX 0 C3 1 -0.072570 0.736030 0.847619 11.00000 0.11927 0.06439 = 0.10981 0.00307 0.07787 -0.01396 AFIX 43 H3 2 -0.087366 0.694808 0.863540 11.00000 -1.20000 AFIX 0 C4 1 -0.114219 0.769325 0.785024 11.00000 0.10440 0.05266 = 0.10528 -0.00890 0.07510 -0.01936 AFIX 43 H4 2 -0.157628 0.752568 0.757196 11.00000 -1.20000 AFIX 0 C5 1 -0.091140 0.829130 0.762816 11.00000 0.08607 0.04637 = 0.08488 -0.02113 0.06613 -0.01978 C6 1 -0.131652 0.871248 0.697608 11.00000 0.06413 0.05979 = 0.07453 -0.02842 0.05094 -0.03329 C7 1 -0.199745 0.860116 0.647348 11.00000 0.06542 0.08925 = 0.08665 -0.03586 0.04989 -0.04390 AFIX 43 H7 2 -0.222240 0.820566 0.655104 11.00000 -1.20000 AFIX 0 C8 1 -0.231642 0.904756 0.589949 11.00000 0.05510 0.11056 = 0.07827 -0.03332 0.03301 -0.04302 AFIX 43 H8 2 -0.275854 0.895459 0.556346 11.00000 -1.20000 AFIX 0 C9 1 -0.199683 0.964994 0.579684 11.00000 0.04157 0.09950 = 0.06659 -0.02617 0.02371 -0.02947 AFIX 43 H9 2 -0.221798 0.997903 0.540093 11.00000 -1.20000 AFIX 0 C10 1 -0.134589 0.975140 0.629231 11.00000 0.03634 0.06988 = 0.05488 -0.02081 0.02543 -0.01958 C11 1 -0.095524 1.038246 0.627189 11.00000 0.02882 0.05816 = 0.04614 -0.00983 0.01531 -0.00602 C12 1 0.062024 1.082352 0.687527 11.00000 0.02830 0.04038 = 0.04023 0.00132 0.01830 0.00323 C13 1 0.112357 1.138269 0.728414 11.00000 0.02368 0.05379 = 0.04469 -0.00507 0.01679 -0.00463 C14 1 0.172654 1.140428 0.732311 11.00000 0.02946 0.08297 = 0.06323 -0.01772 0.02468 -0.00608 AFIX 43 H14 2 0.184569 1.105790 0.706843 11.00000 -1.20000 AFIX 0 C15 1 0.215011 1.194982 0.774735 11.00000 0.03293 0.09714 = 0.07566 -0.01969 0.02598 -0.01265 AFIX 43 H15 2 0.256103 1.199440 0.776729 11.00000 -1.20000 AFIX 0 C16 1 0.198399 1.243650 0.814713 11.00000 0.03345 0.08273 = 0.06452 -0.01831 0.01838 -0.01951 AFIX 43 H16 2 0.228626 1.278715 0.846752 11.00000 -1.20000 AFIX 0 C17 1 0.136713 1.238942 0.805993 11.00000 0.02903 0.05565 = 0.04089 -0.00264 0.01338 -0.01186 C18 1 0.108620 1.292349 0.836241 11.00000 0.03141 0.04522 = 0.03208 0.00150 0.00745 -0.00810 C19 1 -0.025727 1.334623 0.852051 11.00000 0.04310 0.04535 = 0.04570 -0.01038 0.01641 -0.00265 C20 1 -0.070820 1.399102 0.833329 11.00000 0.04797 0.04785 = 0.06696 -0.01377 0.02773 -0.00758 C21 1 -0.110976 1.411893 0.862688 11.00000 0.06169 0.06284 = 0.09362 -0.01352 0.04758 -0.00530 AFIX 43 H21 2 -0.109770 1.380420 0.899483 11.00000 -1.20000 AFIX 0 C22 1 -0.152560 1.470219 0.838458 11.00000 0.07011 0.06835 = 0.12102 -0.01199 0.05282 0.00438 AFIX 43 H22 2 -0.180248 1.480224 0.858684 11.00000 -1.20000 AFIX 0 C23 1 -0.154168 1.514798 0.784147 11.00000 0.06270 0.05911 = 0.11284 -0.01641 0.03476 0.00941 AFIX 43 H23 2 -0.183745 1.554911 0.766071 11.00000 -1.20000 AFIX 0 C24 1 -0.111784 1.500525 0.755700 11.00000 0.05346 0.04393 = 0.08114 -0.01597 0.02040 0.00164 C25 1 -0.110119 1.540555 0.698167 11.00000 0.06852 0.03706 = 0.07372 -0.01178 0.00894 0.00753 C26 1 -0.152528 1.598414 0.660758 11.00000 0.08742 0.04476 = 0.08245 -0.01398 -0.00232 0.01959 AFIX 43 H26 2 -0.184758 1.613152 0.673153 11.00000 -1.20000 AFIX 0 C27 1 -0.147199 1.633897 0.605754 11.00000 0.09881 0.04132 = 0.08562 -0.00153 -0.01078 0.01248 AFIX 43 H27 2 -0.175222 1.673957 0.580990 11.00000 -1.20000 AFIX 0 C28 1 -0.100430 1.611081 0.586066 11.00000 0.09933 0.04775 = 0.08303 0.01245 -0.00172 -0.00145 AFIX 43 H28 2 -0.096174 1.635582 0.548590 11.00000 -1.20000 AFIX 0 C29 1 -0.059640 1.550193 0.623928 11.00000 0.08048 0.04820 = 0.07401 0.01108 0.00926 -0.00122 AFIX 43 H29 2 -0.029359 1.532061 0.609914 11.00000 -1.20000 AFIX 0 N1 3 -0.028117 0.852049 0.802275 11.00000 0.08936 0.04027 = 0.07379 -0.00653 0.06152 -0.00828 N2 3 -0.101979 0.929774 0.685653 11.00000 0.04667 0.05453 = 0.05727 -0.02452 0.03173 -0.02572 N3 3 -0.124012 1.097999 0.588397 11.00000 0.02803 0.08820 = 0.05556 0.01344 -0.00236 0.00165 AFIX 93 H3A 2 -0.100421 1.136066 0.589226 11.00000 -1.20000 H3B 2 -0.166494 1.099555 0.561844 11.00000 -1.20000 AFIX 0 N4 3 -0.032500 1.028918 0.669090 11.00000 0.02511 0.04084 = 0.04750 -0.00350 0.01661 -0.00087 N5 3 0.005003 1.094109 0.683017 11.00000 0.02150 0.03837 = 0.03869 -0.00096 0.01093 -0.00116 N6 3 0.077293 1.021577 0.663573 11.00000 0.03167 0.04949 = 0.05024 -0.00623 0.02448 0.00023 AFIX 93 H6A 2 0.048407 0.986264 0.643268 11.00000 -1.20000 H6B 2 0.116283 1.016670 0.668025 11.00000 -1.20000 AFIX 0 N7 3 0.094895 1.186807 0.764060 11.00000 0.02124 0.05026 = 0.04144 -0.00123 0.01299 -0.00793 N8 3 0.140907 1.355366 0.865539 11.00000 0.04157 0.04423 = 0.04941 0.00026 0.01498 -0.01332 AFIX 93 H8A 2 0.122904 1.389921 0.879405 11.00000 -1.20000 H8B 2 0.180028 1.362025 0.870835 11.00000 -1.20000 AFIX 0 N9 3 0.049141 1.277572 0.826173 11.00000 0.03572 0.03823 = 0.03579 0.00017 0.01446 -0.00581 N10 3 0.017288 1.342119 0.828556 11.00000 0.03450 0.04147 = 0.04034 -0.00522 0.01285 -0.00461 N11 3 -0.031514 1.277889 0.888369 11.00000 0.06149 0.06016 = 0.04871 0.00229 0.03507 0.00048 AFIX 93 H11A 2 -0.005074 1.239968 0.899230 11.00000 -1.20000 H11B 2 -0.061797 1.278146 0.901617 11.00000 -1.20000 AFIX 0 N12 3 -0.071542 1.442469 0.782839 11.00000 0.04808 0.04480 = 0.05808 -0.01224 0.01913 0.00165 N13 3 -0.063844 1.518494 0.679115 11.00000 0.06832 0.04092 = 0.07061 0.00543 0.01356 0.00107 MOLE 2 SAME 0.01 O32 O33 O34 O31 CL31 O31 4 0.117545 0.157386 0.563073 11.00000 0.10113 0.09481 = 0.11491 0.00624 0.03393 -0.05360 O32 4 0.223432 0.197848 0.625386 11.00000 0.07901 0.05945 = 0.10541 -0.01411 0.05852 -0.01602 O33 4 0.170252 0.195131 0.498031 11.00000 0.13281 0.15936 = 0.10590 -0.03906 0.07894 -0.00285 O34 4 0.141373 0.279280 0.561300 11.00000 0.12394 0.06571 = 0.11373 -0.00149 0.07172 0.00275 CL31 5 0.163528 0.205977 0.560348 11.00000 0.07654 0.04553 = 0.09334 -0.01210 0.05794 -0.01601 MOLE 3 PART 1 SAME 0.01 O31 > CL31 O41 4 0.223467 0.909888 0.591952 21.00000 0.05005 0.09787 = 0.12495 -0.02493 0.03199 0.00884 O42 4 0.237088 0.880823 0.705064 21.00000 0.11584 0.08880 = 0.13400 0.01025 0.02516 0.00187 O43 4 0.206991 1.000020 0.661808 21.00000 0.05205 0.06955 = 0.10368 -0.00567 0.04421 -0.00650 O44 4 0.133571 0.904632 0.609004 21.00000 0.06422 0.08100 = 0.13811 -0.03076 0.04106 -0.00812 CL41 5 0.200604 0.924374 0.642215 21.00000 0.06793 0.07520 = 0.11792 -0.02186 0.03502 -0.00160 PART 2 SAME 0.01 O31 > CL31 O46 4 0.248789 0.948008 0.606493 -21.00000 0.06266 0.11200 = 0.11546 -0.03922 0.05035 0.00441 O47 4 0.181442 0.861618 0.617260 -21.00000 0.07748 0.07764 = 0.14417 -0.01696 0.02085 0.00326 O48 4 0.202254 0.972356 0.679934 -21.00000 0.04558 0.10815 = 0.10110 -0.03604 0.03738 0.00757 O49 4 0.137886 0.970662 0.555301 -21.00000 0.06333 0.07840 = 0.09974 -0.02151 0.02958 0.00624 CL46 5 0.192772 0.938493 0.614322 -21.00000 0.04204 0.07130 = 0.10016 -0.04327 0.02981 0.01181 MOLE 4 PART 1 SAME 0.01 O31 > CL31 O51 4 0.137391 0.577610 0.488822 31.00000 0.10906 0.04498 = 0.07212 0.00387 0.07390 -0.00889 O52 4 0.235522 0.638473 0.547559 31.00000 0.06541 0.20614 = 0.11021 0.00104 0.04891 -0.00037 O53 4 0.140713 0.701764 0.514998 31.00000 0.12544 0.06814 = 0.08864 -0.01922 0.03376 0.00463 O54 4 0.174392 0.614459 0.607343 31.00000 0.10037 0.11384 = 0.06398 -0.00313 0.05139 0.01757 CL51 5 0.173257 0.633443 0.542037 31.00000 0.05478 0.09197 = 0.05389 -0.00076 0.02940 -0.00049 PART 2 SAME 0.01 O31 > CL31 O56 4 0.056762 0.596791 0.520539 -31.00000 0.07586 0.14510 = 0.13956 0.00227 0.06000 0.01013 O57 4 0.151752 0.561835 0.515576 -31.00000 0.08677 0.03774 = 0.06565 0.03284 0.06567 0.01382 O58 4 0.116196 0.683131 0.495821 -31.00000 0.09304 0.06646 = 0.07326 -0.00928 0.02325 0.01334 O59 4 0.157912 0.632668 0.609440 -31.00000 0.09425 0.10875 = 0.07047 -0.00134 0.03501 0.03430 CL56 5 0.119804 0.616522 0.534299 -31.00000 0.07757 0.08421 = 0.07344 -0.00215 0.04290 0.01086 MOLE 5 PART 0 O101 4 0.061606 0.825659 0.487001 11.00000 0.14351 0.11842 = 0.07430 -0.00636 0.04531 -0.07233 O102 4 0.017247 0.059459 0.474085 11.00000 0.11880 0.08957 = 0.05291 -0.00794 0.03000 -0.06836 PART 1 O103 4 0.002917 0.563291 0.519738 31.00000 0.09377 0.19463 = 0.17179 0.02191 0.03591 0.00851 PART 2 O104 4 0.257601 0.695780 0.515264 -31.00000 0.08396 0.18296 = 0.08958 -0.00302 0.02450 0.02085 HKLF 4 Covalent radii and connectivity table for 04src0422 in C2/c C 0.770 H 0.320 N 0.700 O 0.660 CL 0.990 ZN 1.330 Zn1 - N2 N2_$1 N4_$1 N4 N1_$1 N1 Zn2 - N7 N7_$1 N5 N5_$1 N9 N9_$1 Zn3 - N12_$1 N12 N10_$1 N10 N13_$1 N13 C1 - N1 C2 C2 - C3 C1 C3 - C4 C2 C4 - C3 C5 C5 - N1 C4 C6 C6 - N2 C7 C5 C7 - C8 C6 C8 - C7 C9 C9 - C10 C8 C10 - N2 C9 C11 C11 - N4 N3 C10 C12 - N5 N6 C13 C13 - N7 C14 C12 C14 - C13 C15 C15 - C14 C16 C16 - C17 C15 C17 - N7 C16 C18 C18 - N9 N8 C17 C19 - N11 N10 C20 C20 - N12 C21 C19 C21 - C22 C20 C22 - C21 C23 C23 - C22 C24 C24 - N12 C23 C25 C25 - N13 C26 C24 C26 - C27 C25 C27 - C26 C28 C28 - C27 C29 C29 - N13 C28 N1 - C1 C5 Zn1 N2 - C10 C6 Zn1 N3 - C11 N4 - C11 N5 Zn1 N5 - C12 N4 Zn2 N6 - C12 N7 - C13 C17 Zn2 N8 - C18 N9 - C18 N10 Zn2 N10 - C19 N9 Zn3 N11 - C19 N12 - C20 C24 Zn3 N13 - C29 C25 Zn3 O31 - Cl31 O32 - Cl31 O33 - Cl31 O34 - Cl31 Cl31 - O33 O31 O32 O34 O41_a - Cl41_a O42_a - Cl41_a O43_a - Cl41_a O44_a - Cl41_a Cl41_a - O43_a O42_a O41_a O44_a O46_b - Cl46_b O47_b - Cl46_b O48_b - Cl46_b O49_b - Cl46_b Cl46_b - O46_b O49_b O48_b O47_b O51_a - Cl51_a O52_a - Cl51_a O53_a - Cl51_a O54_a - Cl51_a Cl51_a - O54_a O52_a O53_a O51_a O56_b - Cl56_b O57_b - Cl56_b O58_b - Cl56_b O59_b - Cl56_b Cl56_b - O57_b O56_b O59_b O58_b O101 - no bonds found O102 - no bonds found O103_a - no bonds found O104_b - no bonds found Operators for generating equivalent atoms: $1 -x, y, -z+3/2 h k l Fo^2 Sigma Why rejected -16 0 1 76.92 15.73 observed but should be systematically absent -16 0 1 93.63 13.55 observed but should be systematically absent -14 0 1 58.79 12.97 observed but should be systematically absent -14 0 1 50.09 10.53 observed but should be systematically absent -10 0 1 245.42 26.62 observed but should be systematically absent -10 0 1 325.04 27.50 observed but should be systematically absent -10 0 1 207.98 25.41 observed but should be systematically absent -10 0 1 267.53 22.80 observed but should be systematically absent 4 0 1 14.68 3.33 observed but should be systematically absent 4 0 1 15.96 3.52 observed but should be systematically absent 4 0 1 22.17 3.40 observed but should be systematically absent 16 0 1 107.36 18.12 observed but should be systematically absent 16 0 1 113.94 18.87 observed but should be systematically absent 18 0 1 71.56 17.36 observed but should be systematically absent 18 0 1 82.61 15.31 observed but should be systematically absent -20 0 3 61.53 12.74 observed but should be systematically absent -10 0 3 101.72 12.11 observed but should be systematically absent -10 0 3 126.23 14.01 observed but should be systematically absent -10 0 3 127.49 12.64 observed but should be systematically absent -10 0 3 145.65 16.91 observed but should be systematically absent -4 0 3 17.80 2.99 observed but should be systematically absent -4 0 3 21.48 3.24 observed but should be systematically absent -4 0 3 28.45 5.29 observed but should be systematically absent 2 0 3 89.16 9.34 observed but should be systematically absent 2 0 3 113.94 9.34 observed but should be systematically absent 2 0 3 93.81 8.98 observed but should be systematically absent 2 0 3 90.70 8.83 observed but should be systematically absent 2 0 3 86.58 7.61 observed but should be systematically absent 4 0 3 133.28 12.55 observed but should be systematically absent 4 0 3 115.40 9.58 observed but should be systematically absent 4 0 3 110.37 13.76 observed but should be systematically absent 4 0 3 92.15 9.85 observed but should be systematically absent 4 0 3 132.47 10.57 observed but should be systematically absent 10 0 3 38.17 8.71 observed but should be systematically absent 10 0 3 56.99 9.31 observed but should be systematically absent 10 0 3 42.92 8.33 observed but should be systematically absent 10 0 3 43.16 7.44 observed but should be systematically absent 12 0 3 53.24 8.04 observed but should be systematically absent 12 0 3 55.32 10.32 observed but should be systematically absent -12 0 5 37.22 7.66 observed but should be systematically absent -12 0 5 27.57 6.53 observed but should be systematically absent -10 0 5 87.17 11.38 observed but should be systematically absent -10 0 5 102.69 11.06 observed but should be systematically absent -10 0 5 87.25 11.71 observed but should be systematically absent -10 0 5 106.14 13.47 observed but should be systematically absent -8 0 5 16.10 3.53 observed but should be systematically absent -2 0 5 32.19 4.76 observed but should be systematically absent -2 0 5 28.47 3.91 observed but should be systematically absent -2 0 5 25.89 4.01 observed but should be systematically absent -2 0 5 33.06 4.72 observed but should be systematically absent ** etc. ** 33556 Reflections read, of which 756 rejected -27 =< h =< 30, -21 =< k =< 23, -27 =< l =< 25, Max. 2-theta = 54.97 107 Systematic absence violations 0 Inconsistent equivalents 8912 Unique reflections, of which 0 suppressed R(int) = 0.0631 R(sigma) = 0.0742 Friedel opposites merged Maximum memory for data reduction = 6320 / 108363 Special position constraints for Zn1 x = 0.0000 z = 0.7500 U23 = 0 U12 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for Zn2 x = 0.0000 z = 0.7500 U23 = 0 U12 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for Zn3 x = 0.0000 z = 0.7500 U23 = 0 U12 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof 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. ** Cell contents from UNIT instruction and atom list do not agree ** Unit-cell contents from UNIT instruction and atom list resp. C 232.00 232.00 H 248.00 200.00 N 104.00 104.00 O 120.00 120.00 CL 24.00 24.00 ZN 12.00 12.00 Least-squares cycle 1 Maximum vector length = 511 Memory required = 7995 / 915642 wR2 = 0.2976 before cycle 1 for 8912 data and 658 / 658 parameters Disagreeable restraints before cycle 1 Observed Target Error Sigma Restraint 0.0399 0.0100 SAME/SADI O54_a Cl51_a O51_a Cl51_a 0.0875 0.0200 SAME/SADI O56_b O57_b O31 O34 etc. 0.0746 0.0200 SAME/SADI O32 O34 O52_a O54_a etc. 0.0317 0.0100 SIMU U33 C23 C24 0.1138 0.0200 SIMU U22 O33 Cl31 0.1142 0.0200 SIMU U22 O52_a Cl51_a 0.0707 0.0200 SIMU U11 O53_a Cl51_a 0.0609 0.0200 SIMU U22 O56_b Cl56_b 0.0661 0.0200 SIMU U33 O56_b Cl56_b 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. 425. 0. 0. 0. 194. 534. 0. 0. rms sigma 0.000 0.000 0.000 0.016 0.000 0.000 0.000 0.010 0.016 0.000 0.000 rms deviation 0.000 0.000 0.000 0.023 0.000 0.000 0.000 0.005 0.018 0.000 0.000 GooF = S = 1.089; Restrained GooF = 1.105 for 1153 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0736 * P )^2 + 181.32 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.19646 0.00085 -0.001 OSF 2 0.41844 0.00904 0.000 FVAR 2 3 0.53526 0.00620 0.000 FVAR 3 4 0.00110 0.00020 0.014 EXTI Mean shift/su = 0.001 Maximum = 0.014 for EXTI Max. shift = 0.000 A for O43_a Max. dU = 0.000 for O52_a Least-squares cycle 2 Maximum vector length = 511 Memory required = 7995 / 915642 wR2 = 0.2976 before cycle 2 for 8912 data and 658 / 658 parameters Disagreeable restraints before cycle 2 Observed Target Error Sigma Restraint 0.0398 0.0100 SAME/SADI O54_a Cl51_a O51_a Cl51_a 0.0875 0.0200 SAME/SADI O56_b O57_b O31 O34 etc. 0.0746 0.0200 SAME/SADI O32 O34 O52_a O54_a etc. 0.0317 0.0100 SIMU U33 C23 C24 0.1138 0.0200 SIMU U22 O33 Cl31 0.1142 0.0200 SIMU U22 O52_a Cl51_a 0.0707 0.0200 SIMU U11 O53_a Cl51_a 0.0609 0.0200 SIMU U22 O56_b Cl56_b 0.0661 0.0200 SIMU U33 O56_b Cl56_b 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. 425. 0. 0. 0. 194. 534. 0. 0. rms sigma 0.000 0.000 0.000 0.016 0.000 0.000 0.000 0.010 0.016 0.000 0.000 rms deviation 0.000 0.000 0.000 0.023 0.000 0.000 0.000 0.005 0.018 0.000 0.000 GooF = S = 1.089; Restrained GooF = 1.105 for 1153 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0736 * P )^2 + 181.32 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.19646 0.00085 0.001 OSF 2 0.41844 0.00904 0.000 FVAR 2 3 0.53526 0.00620 0.000 FVAR 3 4 0.00110 0.00020 0.005 EXTI Mean shift/su = 0.000 Maximum = 0.005 for EXTI Max. shift = 0.000 A for O48_b Max. dU = 0.000 for N2 Least-squares cycle 3 Maximum vector length = 511 Memory required = 7995 / 915642 wR2 = 0.2976 before cycle 3 for 8912 data and 658 / 658 parameters Disagreeable restraints before cycle 3 Observed Target Error Sigma Restraint 0.0398 0.0100 SAME/SADI O54_a Cl51_a O51_a Cl51_a 0.0875 0.0200 SAME/SADI O56_b O57_b O31 O34 etc. 0.0746 0.0200 SAME/SADI O32 O34 O52_a O54_a etc. 0.0317 0.0100 SIMU U33 C23 C24 0.1138 0.0200 SIMU U22 O33 Cl31 0.1142 0.0200 SIMU U22 O52_a Cl51_a 0.0707 0.0200 SIMU U11 O53_a Cl51_a 0.0609 0.0200 SIMU U22 O56_b Cl56_b 0.0661 0.0200 SIMU U33 O56_b Cl56_b 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. 425. 0. 0. 0. 194. 534. 0. 0. rms sigma 0.000 0.000 0.000 0.016 0.000 0.000 0.000 0.010 0.016 0.000 0.000 rms deviation 0.000 0.000 0.000 0.023 0.000 0.000 0.000 0.005 0.018 0.000 0.000 GooF = S = 1.089; Restrained GooF = 1.105 for 1153 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0736 * P )^2 + 181.32 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.19646 0.00085 0.001 OSF 2 0.41844 0.00904 0.000 FVAR 2 3 0.53526 0.00620 0.000 FVAR 3 4 0.00110 0.00020 0.001 EXTI Mean shift/su = 0.000 Maximum = 0.001 for y Zn3 Max. shift = 0.000 A for O56_b Max. dU = 0.000 for O58_b Least-squares cycle 4 Maximum vector length = 511 Memory required = 7995 / 915642 wR2 = 0.2976 before cycle 4 for 8912 data and 658 / 658 parameters Disagreeable restraints before cycle 4 Observed Target Error Sigma Restraint 0.0398 0.0100 SAME/SADI O54_a Cl51_a O51_a Cl51_a 0.0875 0.0200 SAME/SADI O56_b O57_b O31 O34 etc. 0.0746 0.0200 SAME/SADI O32 O34 O52_a O54_a etc. 0.0317 0.0100 SIMU U33 C23 C24 0.1138 0.0200 SIMU U22 O33 Cl31 0.1142 0.0200 SIMU U22 O52_a Cl51_a 0.0707 0.0200 SIMU U11 O53_a Cl51_a 0.0609 0.0200 SIMU U22 O56_b Cl56_b 0.0661 0.0200 SIMU U33 O56_b Cl56_b 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. 425. 0. 0. 0. 194. 534. 0. 0. rms sigma 0.000 0.000 0.000 0.016 0.000 0.000 0.000 0.010 0.016 0.000 0.000 rms deviation 0.000 0.000 0.000 0.023 0.000 0.000 0.000 0.005 0.018 0.000 0.000 GooF = S = 1.089; Restrained GooF = 1.105 for 1153 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0736 * P )^2 + 181.32 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.19646 0.00085 0.000 OSF 2 0.41844 0.00904 0.000 FVAR 2 3 0.53526 0.00620 0.000 FVAR 3 4 0.00110 0.00020 0.000 EXTI Mean shift/su = 0.000 Maximum = -0.001 for y Zn2 Max. shift = 0.000 A for O56_b Max. dU = 0.000 for O53_a Least-squares cycle 5 Maximum vector length = 511 Memory required = 7995 / 915642 wR2 = 0.2976 before cycle 5 for 8912 data and 658 / 658 parameters Disagreeable restraints before cycle 5 Observed Target Error Sigma Restraint 0.0398 0.0100 SAME/SADI O54_a Cl51_a O51_a Cl51_a 0.0875 0.0200 SAME/SADI O56_b O57_b O31 O34 etc. 0.0746 0.0200 SAME/SADI O32 O34 O52_a O54_a etc. 0.0317 0.0100 SIMU U33 C23 C24 0.1138 0.0200 SIMU U22 O33 Cl31 0.1142 0.0200 SIMU U22 O52_a Cl51_a 0.0707 0.0200 SIMU U11 O53_a Cl51_a 0.0609 0.0200 SIMU U22 O56_b Cl56_b 0.0661 0.0200 SIMU U33 O56_b Cl56_b 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. 425. 0. 0. 0. 194. 534. 0. 0. rms sigma 0.000 0.000 0.000 0.016 0.000 0.000 0.000 0.010 0.016 0.000 0.000 rms deviation 0.000 0.000 0.000 0.023 0.000 0.000 0.000 0.005 0.018 0.000 0.000 GooF = S = 1.089; Restrained GooF = 1.105 for 1153 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0736 * P )^2 + 181.32 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.19646 0.00085 0.000 OSF 2 0.41844 0.00904 0.000 FVAR 2 3 0.53526 0.00620 0.000 FVAR 3 4 0.00110 0.00020 0.000 EXTI Mean shift/su = 0.000 Maximum = -0.001 for y Zn2 Max. shift = 0.000 A for O103_a Max. dU = 0.000 for O104_b Least-squares cycle 6 Maximum vector length = 511 Memory required = 7995 / 915642 wR2 = 0.2976 before cycle 6 for 8912 data and 658 / 658 parameters Disagreeable restraints before cycle 6 Observed Target Error Sigma Restraint 0.0398 0.0100 SAME/SADI O54_a Cl51_a O51_a Cl51_a 0.0875 0.0200 SAME/SADI O56_b O57_b O31 O34 etc. 0.0746 0.0200 SAME/SADI O32 O34 O52_a O54_a etc. 0.0317 0.0100 SIMU U33 C23 C24 0.1138 0.0200 SIMU U22 O33 Cl31 0.1142 0.0200 SIMU U22 O52_a Cl51_a 0.0707 0.0200 SIMU U11 O53_a Cl51_a 0.0609 0.0200 SIMU U22 O56_b Cl56_b 0.0661 0.0200 SIMU U33 O56_b Cl56_b Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 425. 0. 0. 0. 194. 534. 0. 0. rms sigma 0.000 0.000 0.000 0.016 0.000 0.000 0.000 0.010 0.016 0.000 0.000 rms deviation 0.000 0.000 0.000 0.023 0.000 0.000 0.000 0.005 0.018 0.000 0.000 GooF = S = 1.089; Restrained GooF = 1.105 for 1153 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0736 * P )^2 + 181.32 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.19646 0.00085 0.000 OSF 2 0.41845 0.00904 0.000 FVAR 2 3 0.53526 0.00620 0.000 FVAR 3 4 0.00110 0.00020 0.000 EXTI Mean shift/su = 0.000 Maximum = -0.001 for y Zn2 Max. shift = 0.000 A for O59_b Max. dU = 0.000 for O58_b Least-squares cycle 7 Maximum vector length = 511 Memory required = 7995 / 915642 wR2 = 0.2976 before cycle 7 for 8912 data and 658 / 658 parameters Disagreeable restraints before cycle 7 Observed Target Error Sigma Restraint 0.0398 0.0100 SAME/SADI O54_a Cl51_a O51_a Cl51_a 0.0875 0.0200 SAME/SADI O56_b O57_b O31 O34 etc. 0.0746 0.0200 SAME/SADI O32 O34 O52_a O54_a etc. 0.0317 0.0100 SIMU U33 C23 C24 0.1138 0.0200 SIMU U22 O33 Cl31 0.1142 0.0200 SIMU U22 O52_a Cl51_a 0.0707 0.0200 SIMU U11 O53_a Cl51_a 0.0609 0.0200 SIMU U22 O56_b Cl56_b 0.0661 0.0200 SIMU U33 O56_b Cl56_b Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 425. 0. 0. 0. 194. 534. 0. 0. rms sigma 0.000 0.000 0.000 0.016 0.000 0.000 0.000 0.010 0.016 0.000 0.000 rms deviation 0.000 0.000 0.000 0.023 0.000 0.000 0.000 0.005 0.018 0.000 0.000 GooF = S = 1.089; Restrained GooF = 1.105 for 1153 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0736 * P )^2 + 181.32 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.19646 0.00085 0.000 OSF 2 0.41845 0.00904 0.000 FVAR 2 3 0.53526 0.00620 0.000 FVAR 3 4 0.00110 0.00020 0.000 EXTI Mean shift/su = 0.000 Maximum = -0.001 for y Zn2 Max. shift = 0.000 A for O57_b Max. dU = 0.000 for O53_a Least-squares cycle 8 Maximum vector length = 511 Memory required = 7995 / 915642 wR2 = 0.2976 before cycle 8 for 8912 data and 658 / 658 parameters Disagreeable restraints before cycle 8 Observed Target Error Sigma Restraint 0.0398 0.0100 SAME/SADI O54_a Cl51_a O51_a Cl51_a 0.0875 0.0200 SAME/SADI O56_b O57_b O31 O34 etc. 0.0746 0.0200 SAME/SADI O32 O34 O52_a O54_a etc. 0.0317 0.0100 SIMU U33 C23 C24 0.1138 0.0200 SIMU U22 O33 Cl31 0.1142 0.0200 SIMU U22 O52_a Cl51_a 0.0707 0.0200 SIMU U11 O53_a Cl51_a 0.0609 0.0200 SIMU U22 O56_b Cl56_b 0.0661 0.0200 SIMU U33 O56_b Cl56_b Summary of restraints applied in cycle 8 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 425. 0. 0. 0. 194. 534. 0. 0. rms sigma 0.000 0.000 0.000 0.016 0.000 0.000 0.000 0.010 0.016 0.000 0.000 rms deviation 0.000 0.000 0.000 0.023 0.000 0.000 0.000 0.005 0.018 0.000 0.000 GooF = S = 1.089; Restrained GooF = 1.105 for 1153 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0736 * P )^2 + 181.32 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.19646 0.00085 0.000 OSF 2 0.41845 0.00904 0.000 FVAR 2 3 0.53526 0.00620 0.000 FVAR 3 4 0.00110 0.00020 0.000 EXTI Mean shift/su = 0.000 Maximum = -0.001 for y Zn2 Max. shift = 0.000 A for O103_a Max. dU = 0.000 for O53_a Least-squares cycle 9 Maximum vector length = 511 Memory required = 7995 / 915642 wR2 = 0.2976 before cycle 9 for 8912 data and 658 / 658 parameters Disagreeable restraints before cycle 9 Observed Target Error Sigma Restraint 0.0398 0.0100 SAME/SADI O54_a Cl51_a O51_a Cl51_a 0.0875 0.0200 SAME/SADI O56_b O57_b O31 O34 etc. 0.0746 0.0200 SAME/SADI O32 O34 O52_a O54_a etc. 0.0317 0.0100 SIMU U33 C23 C24 0.1138 0.0200 SIMU U22 O33 Cl31 0.1142 0.0200 SIMU U22 O52_a Cl51_a 0.0707 0.0200 SIMU U11 O53_a Cl51_a 0.0609 0.0200 SIMU U22 O56_b Cl56_b 0.0661 0.0200 SIMU U33 O56_b Cl56_b Summary of restraints applied in cycle 9 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 425. 0. 0. 0. 194. 534. 0. 0. rms sigma 0.000 0.000 0.000 0.016 0.000 0.000 0.000 0.010 0.016 0.000 0.000 rms deviation 0.000 0.000 0.000 0.023 0.000 0.000 0.000 0.005 0.018 0.000 0.000 GooF = S = 1.089; Restrained GooF = 1.105 for 1153 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0736 * P )^2 + 181.32 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.19646 0.00085 0.000 OSF 2 0.41844 0.00904 0.000 FVAR 2 3 0.53526 0.00620 0.000 FVAR 3 4 0.00110 0.00020 0.000 EXTI Mean shift/su = 0.000 Maximum = -0.001 for y Zn2 Max. shift = 0.000 A for O43_a Max. dU = 0.000 for O57_b Least-squares cycle 10 Maximum vector length = 511 Memory required = 7995 / 915642 wR2 = 0.2976 before cycle 10 for 8912 data and 658 / 658 parameters Disagreeable restraints before cycle 10 Observed Target Error Sigma Restraint 0.0398 0.0100 SAME/SADI O54_a Cl51_a O51_a Cl51_a 0.0875 0.0200 SAME/SADI O56_b O57_b O31 O34 etc. 0.0746 0.0200 SAME/SADI O32 O34 O52_a O54_a etc. 0.0317 0.0100 SIMU U33 C23 C24 0.1138 0.0200 SIMU U22 O33 Cl31 0.1142 0.0200 SIMU U22 O52_a Cl51_a 0.0707 0.0200 SIMU U11 O53_a Cl51_a 0.0609 0.0200 SIMU U22 O56_b Cl56_b 0.0661 0.0200 SIMU U33 O56_b Cl56_b Summary of restraints applied in cycle 10 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 425. 0. 0. 0. 194. 534. 0. 0. rms sigma 0.000 0.000 0.000 0.016 0.000 0.000 0.000 0.010 0.016 0.000 0.000 rms deviation 0.000 0.000 0.000 0.023 0.000 0.000 0.000 0.005 0.018 0.000 0.000 GooF = S = 1.089; Restrained GooF = 1.105 for 1153 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0736 * P )^2 + 181.32 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.19646 0.00085 0.000 OSF 2 0.41845 0.00904 0.000 FVAR 2 3 0.53526 0.00620 0.000 FVAR 3 4 0.00110 0.00020 0.000 EXTI Mean shift/su = 0.000 Maximum = -0.001 for y Zn2 Max. shift = 0.000 A for O52_a Max. dU = 0.000 for O52_a Least-squares cycle 11 Maximum vector length = 511 Memory required = 7995 / 915642 wR2 = 0.2976 before cycle 11 for 8912 data and 658 / 658 parameters Disagreeable restraints before cycle 11 Observed Target Error Sigma Restraint 0.0398 0.0100 SAME/SADI O54_a Cl51_a O51_a Cl51_a 0.0875 0.0200 SAME/SADI O56_b O57_b O31 O34 etc. 0.0746 0.0200 SAME/SADI O32 O34 O52_a O54_a etc. 0.0317 0.0100 SIMU U33 C23 C24 0.1138 0.0200 SIMU U22 O33 Cl31 0.1142 0.0200 SIMU U22 O52_a Cl51_a 0.0707 0.0200 SIMU U11 O53_a Cl51_a 0.0609 0.0200 SIMU U22 O56_b Cl56_b 0.0661 0.0200 SIMU U33 O56_b Cl56_b Summary of restraints applied in cycle 11 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 425. 0. 0. 0. 194. 534. 0. 0. rms sigma 0.000 0.000 0.000 0.016 0.000 0.000 0.000 0.010 0.016 0.000 0.000 rms deviation 0.000 0.000 0.000 0.023 0.000 0.000 0.000 0.005 0.018 0.000 0.000 GooF = S = 1.089; Restrained GooF = 1.105 for 1153 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0736 * P )^2 + 181.32 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.19646 0.00085 0.000 OSF 2 0.41845 0.00904 0.000 FVAR 2 3 0.53526 0.00620 0.000 FVAR 3 4 0.00110 0.00020 0.000 EXTI Mean shift/su = 0.000 Maximum = -0.001 for y Zn2 Max. shift = 0.000 A for C4 Max. dU = 0.000 for O53_a Least-squares cycle 12 Maximum vector length = 511 Memory required = 7995 / 915642 wR2 = 0.2976 before cycle 12 for 8912 data and 658 / 658 parameters Disagreeable restraints before cycle 12 Observed Target Error Sigma Restraint 0.0398 0.0100 SAME/SADI O54_a Cl51_a O51_a Cl51_a 0.0875 0.0200 SAME/SADI O56_b O57_b O31 O34 etc. 0.0746 0.0200 SAME/SADI O32 O34 O52_a O54_a etc. 0.0317 0.0100 SIMU U33 C23 C24 0.1138 0.0200 SIMU U22 O33 Cl31 0.1142 0.0200 SIMU U22 O52_a Cl51_a 0.0707 0.0200 SIMU U11 O53_a Cl51_a 0.0609 0.0200 SIMU U22 O56_b Cl56_b 0.0661 0.0200 SIMU U33 O56_b Cl56_b Summary of restraints applied in cycle 12 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 425. 0. 0. 0. 194. 534. 0. 0. rms sigma 0.000 0.000 0.000 0.016 0.000 0.000 0.000 0.010 0.016 0.000 0.000 rms deviation 0.000 0.000 0.000 0.023 0.000 0.000 0.000 0.005 0.018 0.000 0.000 GooF = S = 1.089; Restrained GooF = 1.105 for 1153 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0736 * P )^2 + 181.32 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.19646 0.00085 0.000 OSF 2 0.41845 0.00904 0.000 FVAR 2 3 0.53526 0.00620 0.000 FVAR 3 4 0.00110 0.00020 0.000 EXTI Mean shift/su = 0.000 Maximum = -0.001 for y Zn2 Max. shift = 0.000 A for O58_b Max. dU = 0.000 for O52_a Least-squares cycle 13 Maximum vector length = 511 Memory required = 7995 / 915642 wR2 = 0.2976 before cycle 13 for 8912 data and 658 / 658 parameters Disagreeable restraints before cycle 13 Observed Target Error Sigma Restraint 0.0398 0.0100 SAME/SADI O54_a Cl51_a O51_a Cl51_a 0.0875 0.0200 SAME/SADI O56_b O57_b O31 O34 etc. 0.0746 0.0200 SAME/SADI O32 O34 O52_a O54_a etc. 0.0317 0.0100 SIMU U33 C23 C24 0.1138 0.0200 SIMU U22 O33 Cl31 0.1142 0.0200 SIMU U22 O52_a Cl51_a 0.0707 0.0200 SIMU U11 O53_a Cl51_a 0.0609 0.0200 SIMU U22 O56_b Cl56_b 0.0661 0.0200 SIMU U33 O56_b Cl56_b Summary of restraints applied in cycle 13 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 425. 0. 0. 0. 194. 534. 0. 0. rms sigma 0.000 0.000 0.000 0.016 0.000 0.000 0.000 0.010 0.016 0.000 0.000 rms deviation 0.000 0.000 0.000 0.023 0.000 0.000 0.000 0.005 0.018 0.000 0.000 GooF = S = 1.089; Restrained GooF = 1.105 for 1153 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0736 * P )^2 + 181.32 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.19646 0.00085 0.000 OSF 2 0.41845 0.00904 0.000 FVAR 2 3 0.53526 0.00620 0.000 FVAR 3 4 0.00110 0.00020 0.000 EXTI Mean shift/su = 0.000 Maximum = -0.001 for y Zn2 Max. shift = 0.000 A for O46_b Max. dU = 0.000 for O58_b Least-squares cycle 14 Maximum vector length = 511 Memory required = 7995 / 915642 wR2 = 0.2976 before cycle 14 for 8912 data and 658 / 658 parameters Disagreeable restraints before cycle 14 Observed Target Error Sigma Restraint 0.0398 0.0100 SAME/SADI O54_a Cl51_a O51_a Cl51_a 0.0875 0.0200 SAME/SADI O56_b O57_b O31 O34 etc. 0.0746 0.0200 SAME/SADI O32 O34 O52_a O54_a etc. 0.0317 0.0100 SIMU U33 C23 C24 0.1138 0.0200 SIMU U22 O33 Cl31 0.1142 0.0200 SIMU U22 O52_a Cl51_a 0.0707 0.0200 SIMU U11 O53_a Cl51_a 0.0609 0.0200 SIMU U22 O56_b Cl56_b 0.0661 0.0200 SIMU U33 O56_b Cl56_b Summary of restraints applied in cycle 14 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 425. 0. 0. 0. 194. 534. 0. 0. rms sigma 0.000 0.000 0.000 0.016 0.000 0.000 0.000 0.010 0.016 0.000 0.000 rms deviation 0.000 0.000 0.000 0.023 0.000 0.000 0.000 0.005 0.018 0.000 0.000 GooF = S = 1.089; Restrained GooF = 1.105 for 1153 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0736 * P )^2 + 181.32 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.19646 0.00085 0.000 OSF 2 0.41845 0.00904 0.000 FVAR 2 3 0.53526 0.00620 0.000 FVAR 3 4 0.00110 0.00020 0.000 EXTI Mean shift/su = 0.000 Maximum = -0.001 for y Zn2 Max. shift = 0.000 A for O41_a Max. dU = 0.000 for O52_a Least-squares cycle 15 Maximum vector length = 511 Memory required = 7995 / 915642 wR2 = 0.2976 before cycle 15 for 8912 data and 658 / 658 parameters Disagreeable restraints before cycle 15 Observed Target Error Sigma Restraint 0.0398 0.0100 SAME/SADI O54_a Cl51_a O51_a Cl51_a 0.0875 0.0200 SAME/SADI O56_b O57_b O31 O34 etc. 0.0746 0.0200 SAME/SADI O32 O34 O52_a O54_a etc. 0.0317 0.0100 SIMU U33 C23 C24 0.1138 0.0200 SIMU U22 O33 Cl31 0.1142 0.0200 SIMU U22 O52_a Cl51_a 0.0707 0.0200 SIMU U11 O53_a Cl51_a 0.0609 0.0200 SIMU U22 O56_b Cl56_b 0.0661 0.0200 SIMU U33 O56_b Cl56_b Summary of restraints applied in cycle 15 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 425. 0. 0. 0. 194. 534. 0. 0. rms sigma 0.000 0.000 0.000 0.016 0.000 0.000 0.000 0.010 0.016 0.000 0.000 rms deviation 0.000 0.000 0.000 0.023 0.000 0.000 0.000 0.005 0.018 0.000 0.000 GooF = S = 1.089; Restrained GooF = 1.105 for 1153 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0736 * P )^2 + 181.32 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.19646 0.00085 0.000 OSF 2 0.41845 0.00904 0.000 FVAR 2 3 0.53526 0.00620 0.000 FVAR 3 4 0.00110 0.00020 0.000 EXTI Mean shift/su = 0.000 Maximum = -0.001 for y Zn2 Max. shift = 0.000 A for C23 Max. dU = 0.000 for O52_a Least-squares cycle 16 Maximum vector length = 511 Memory required = 7995 / 915642 wR2 = 0.2976 before cycle 16 for 8912 data and 658 / 658 parameters Disagreeable restraints before cycle 16 Observed Target Error Sigma Restraint 0.0398 0.0100 SAME/SADI O54_a Cl51_a O51_a Cl51_a 0.0875 0.0200 SAME/SADI O56_b O57_b O31 O34 etc. 0.0746 0.0200 SAME/SADI O32 O34 O52_a O54_a etc. 0.0317 0.0100 SIMU U33 C23 C24 0.1138 0.0200 SIMU U22 O33 Cl31 0.1142 0.0200 SIMU U22 O52_a Cl51_a 0.0707 0.0200 SIMU U11 O53_a Cl51_a 0.0609 0.0200 SIMU U22 O56_b Cl56_b 0.0661 0.0200 SIMU U33 O56_b Cl56_b Summary of restraints applied in cycle 16 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 425. 0. 0. 0. 194. 534. 0. 0. rms sigma 0.000 0.000 0.000 0.016 0.000 0.000 0.000 0.010 0.016 0.000 0.000 rms deviation 0.000 0.000 0.000 0.023 0.000 0.000 0.000 0.005 0.018 0.000 0.000 GooF = S = 1.089; Restrained GooF = 1.105 for 1153 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0736 * P )^2 + 181.32 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.19646 0.00085 0.000 OSF 2 0.41845 0.00904 0.000 FVAR 2 3 0.53526 0.00620 0.000 FVAR 3 4 0.00110 0.00020 0.000 EXTI Mean shift/su = 0.000 Maximum = -0.001 for y Zn2 Max. shift = 0.000 A for O43_a Max. dU = 0.000 for O53_a Least-squares cycle 17 Maximum vector length = 511 Memory required = 7995 / 915642 wR2 = 0.2976 before cycle 17 for 8912 data and 658 / 658 parameters Disagreeable restraints before cycle 17 Observed Target Error Sigma Restraint 0.0398 0.0100 SAME/SADI O54_a Cl51_a O51_a Cl51_a 0.0875 0.0200 SAME/SADI O56_b O57_b O31 O34 etc. 0.0746 0.0200 SAME/SADI O32 O34 O52_a O54_a etc. 0.0317 0.0100 SIMU U33 C23 C24 0.1138 0.0200 SIMU U22 O33 Cl31 0.1142 0.0200 SIMU U22 O52_a Cl51_a 0.0707 0.0200 SIMU U11 O53_a Cl51_a 0.0609 0.0200 SIMU U22 O56_b Cl56_b 0.0661 0.0200 SIMU U33 O56_b Cl56_b Summary of restraints applied in cycle 17 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 425. 0. 0. 0. 194. 534. 0. 0. rms sigma 0.000 0.000 0.000 0.016 0.000 0.000 0.000 0.010 0.016 0.000 0.000 rms deviation 0.000 0.000 0.000 0.023 0.000 0.000 0.000 0.005 0.018 0.000 0.000 GooF = S = 1.089; Restrained GooF = 1.105 for 1153 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0736 * P )^2 + 181.32 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.19646 0.00085 0.000 OSF 2 0.41845 0.00904 0.000 FVAR 2 3 0.53526 0.00620 0.000 FVAR 3 4 0.00110 0.00020 0.000 EXTI Mean shift/su = 0.000 Maximum = -0.001 for y Zn2 Max. shift = 0.000 A for C9 Max. dU = 0.000 for O103_a Least-squares cycle 18 Maximum vector length = 511 Memory required = 7995 / 915642 wR2 = 0.2976 before cycle 18 for 8912 data and 658 / 658 parameters Disagreeable restraints before cycle 18 Observed Target Error Sigma Restraint 0.0398 0.0100 SAME/SADI O54_a Cl51_a O51_a Cl51_a 0.0875 0.0200 SAME/SADI O56_b O57_b O31 O34 etc. 0.0746 0.0200 SAME/SADI O32 O34 O52_a O54_a etc. 0.0317 0.0100 SIMU U33 C23 C24 0.1138 0.0200 SIMU U22 O33 Cl31 0.1142 0.0200 SIMU U22 O52_a Cl51_a 0.0707 0.0200 SIMU U11 O53_a Cl51_a 0.0609 0.0200 SIMU U22 O56_b Cl56_b 0.0661 0.0200 SIMU U33 O56_b Cl56_b Summary of restraints applied in cycle 18 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 425. 0. 0. 0. 194. 534. 0. 0. rms sigma 0.000 0.000 0.000 0.016 0.000 0.000 0.000 0.010 0.016 0.000 0.000 rms deviation 0.000 0.000 0.000 0.023 0.000 0.000 0.000 0.005 0.018 0.000 0.000 GooF = S = 1.089; Restrained GooF = 1.105 for 1153 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0736 * P )^2 + 181.32 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.19646 0.00085 0.000 OSF 2 0.41844 0.00904 0.000 FVAR 2 3 0.53526 0.00620 0.000 FVAR 3 4 0.00110 0.00020 0.000 EXTI Mean shift/su = 0.000 Maximum = -0.001 for y Zn2 Max. shift = 0.000 A for C14 Max. dU = 0.000 for O52_a Least-squares cycle 19 Maximum vector length = 511 Memory required = 7995 / 915642 wR2 = 0.2976 before cycle 19 for 8912 data and 658 / 658 parameters Disagreeable restraints before cycle 19 Observed Target Error Sigma Restraint 0.0398 0.0100 SAME/SADI O54_a Cl51_a O51_a Cl51_a 0.0875 0.0200 SAME/SADI O56_b O57_b O31 O34 etc. 0.0746 0.0200 SAME/SADI O32 O34 O52_a O54_a etc. 0.0317 0.0100 SIMU U33 C23 C24 0.1138 0.0200 SIMU U22 O33 Cl31 0.1142 0.0200 SIMU U22 O52_a Cl51_a 0.0707 0.0200 SIMU U11 O53_a Cl51_a 0.0609 0.0200 SIMU U22 O56_b Cl56_b 0.0661 0.0200 SIMU U33 O56_b Cl56_b Summary of restraints applied in cycle 19 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 425. 0. 0. 0. 194. 534. 0. 0. rms sigma 0.000 0.000 0.000 0.016 0.000 0.000 0.000 0.010 0.016 0.000 0.000 rms deviation 0.000 0.000 0.000 0.023 0.000 0.000 0.000 0.005 0.018 0.000 0.000 GooF = S = 1.089; Restrained GooF = 1.105 for 1153 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0736 * P )^2 + 181.32 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.19646 0.00085 0.000 OSF 2 0.41844 0.00904 0.000 FVAR 2 3 0.53526 0.00620 0.000 FVAR 3 4 0.00110 0.00020 0.000 EXTI Mean shift/su = 0.000 Maximum = -0.001 for y Zn2 Max. shift = 0.000 A for O46_b Max. dU = 0.000 for O57_b Least-squares cycle 20 Maximum vector length = 511 Memory required = 7995 / 915642 wR2 = 0.2976 before cycle 20 for 8912 data and 658 / 658 parameters Disagreeable restraints before cycle 20 Observed Target Error Sigma Restraint 0.0398 0.0100 SAME/SADI O54_a Cl51_a O51_a Cl51_a 0.0875 0.0200 SAME/SADI O56_b O57_b O31 O34 etc. 0.0746 0.0200 SAME/SADI O32 O34 O52_a O54_a etc. 0.0317 0.0100 SIMU U33 C23 C24 0.1138 0.0200 SIMU U22 O33 Cl31 0.1142 0.0200 SIMU U22 O52_a Cl51_a 0.0707 0.0200 SIMU U11 O53_a Cl51_a 0.0609 0.0200 SIMU U22 O56_b Cl56_b 0.0661 0.0200 SIMU U33 O56_b Cl56_b Summary of restraints applied in cycle 20 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 425. 0. 0. 0. 194. 534. 0. 0. rms sigma 0.000 0.000 0.000 0.016 0.000 0.000 0.000 0.010 0.016 0.000 0.000 rms deviation 0.000 0.000 0.000 0.023 0.000 0.000 0.000 0.005 0.018 0.000 0.000 GooF = S = 1.089; Restrained GooF = 1.105 for 1153 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0736 * P )^2 + 181.32 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.19646 0.00085 0.000 OSF 2 0.41844 0.00904 0.000 FVAR 2 3 0.53526 0.00620 0.000 FVAR 3 4 0.00110 0.00020 0.000 EXTI Mean shift/su = 0.000 Maximum = -0.001 for y Zn2 Max. shift = 0.000 A for H4 Max. dU = 0.000 for O103_a Largest correlation matrix elements 0.764 z O46_b / x O46_b 0.700 U13 Cl31 / U11 Cl31 0.672 z O56_b / x O56_b 0.738 z O33 / x O33 0.700 x Cl41_a / x O44_a 0.672 z O41_a / x O41_a 0.731 z O52_a / x O52_a 0.691 z C5 / x C5 0.669 z N1 / x N1 0.730 z O54_a / x O54_a 0.686 y Cl41_a / y O43_a 0.666 U13 N11 / U33 N11 0.717 U13 Cl31 / U33 Cl31 0.686 U13 O33 / U11 O33 0.663 U13 Zn1 / U33 Zn1 0.716 U13 O57_b / U11 O57_b 0.682 z C4 / x C4 0.662 EXTI / OSF 0.712 z O57_b / x O57_b 0.680 z C2 / x C2 0.656 z C6 / x C6 0.709 z C1 / x C1 0.674 U13 O33 / U33 O33 0.653 U13 O46_b / U11 O46_b Idealized hydrogen atom generation before cycle 21 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1 0.0542 0.8337 0.8909 43 0.950 0.000 C1 N1 C2 H2 0.0175 0.7353 0.9335 43 0.950 0.000 C2 C3 C1 H3 -0.0874 0.6948 0.8635 43 0.950 0.000 C3 C4 C2 H4 -0.1576 0.7526 0.7572 43 0.950 0.000 C4 C3 C5 H7 -0.2222 0.8206 0.6551 43 0.950 0.000 C7 C8 C6 H8 -0.2759 0.8955 0.5563 43 0.950 0.000 C8 C7 C9 H9 -0.2218 0.9979 0.5401 43 0.950 0.000 C9 C10 C8 H14 0.1846 1.1058 0.7068 43 0.950 0.000 C14 C13 C15 H15 0.2561 1.1994 0.7767 43 0.950 0.000 C15 C14 C16 H16 0.2286 1.2787 0.8468 43 0.950 0.000 C16 C17 C15 H21 -0.1098 1.3804 0.8995 43 0.950 0.000 C21 C22 C20 H22 -0.1802 1.4802 0.8587 43 0.950 0.000 C22 C21 C23 H23 -0.1837 1.5549 0.7661 43 0.950 0.000 C23 C22 C24 H26 -0.1848 1.6132 0.6732 43 0.950 0.000 C26 C27 C25 H27 -0.1752 1.6740 0.5810 43 0.950 0.000 C27 C26 C28 H28 -0.0962 1.6356 0.5486 43 0.950 0.000 C28 C27 C29 H29 -0.0294 1.5321 0.6099 43 0.950 0.000 C29 N13 C28 H3A -0.1004 1.1361 0.5892 93 0.880 0.000 N3 C11 N4 H3B -0.1665 1.0996 0.5618 93 0.880 0.000 N3 C11 N4 H6A 0.0484 0.9863 0.6433 93 0.880 0.000 N6 C12 N5 H6B 0.1163 1.0167 0.6680 93 0.880 0.000 N6 C12 N5 H8A 0.1229 1.3899 0.8794 93 0.880 0.000 N8 C18 N9 H8B 0.1800 1.3620 0.8708 93 0.880 0.000 N8 C18 N9 H11A -0.0051 1.2400 0.8992 93 0.880 0.000 N11 C19 N10 H11B -0.0618 1.2781 0.9016 93 0.880 0.000 N11 C19 N10 04src0422 in C2/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq Zn1 0.00000 0.94100 0.75000 0.50000 0.04384 0.03660 0.04961 0.00000 0.02682 0.00000 0.04153 0.00144 0.00000 0.00008 0.00000 0.00000 0.00082 0.00077 0.00091 0.00000 0.00072 0.00000 0.00041 Zn2 0.00000 1.18494 0.75000 0.50000 0.02115 0.03583 0.04385 0.00000 0.01407 0.00000 0.03425 0.00135 0.00000 0.00007 0.00000 0.00000 0.00061 0.00072 0.00080 0.00000 0.00057 0.00000 0.00036 Zn3 0.00000 1.42992 0.75000 0.50000 0.05275 0.03408 0.05313 0.00000 0.01990 0.00000 0.04895 0.00150 0.00000 0.00008 0.00000 0.00000 0.00095 0.00079 0.00100 0.00000 0.00080 0.00000 0.00045 C1 0.01054 0.81759 0.86343 1.00000 0.10395 0.04820 0.07740 0.00125 0.06904 0.00621 0.06591 0.03039 0.00068 0.00058 0.00067 0.00000 0.00563 0.00463 0.00515 0.00398 0.00440 0.00432 0.00222 H1 0.05420 0.83367 0.89088 1.00000 0.07909 0.00000 0.00000 C2 -0.01051 0.75879 0.88883 1.00000 0.11491 0.05889 0.09167 0.01059 0.07388 0.00493 0.07838 0.03405 0.00075 0.00068 0.00079 0.00000 0.00630 0.00527 0.00609 0.00466 0.00514 0.00511 0.00266 H2 0.01753 0.73529 0.93350 1.00000 0.09406 0.00000 0.00000 C3 -0.07257 0.73603 0.84762 1.00000 0.11927 0.06440 0.10981 0.00307 0.07787 -0.01396 0.08830 0.03523 0.00079 0.00077 0.00086 0.00000 0.00681 0.00573 0.00675 0.00494 0.00578 0.00521 0.00301 H3 -0.08737 0.69481 0.86354 1.00000 0.10597 0.00000 0.00000 C4 -0.11422 0.76932 0.78502 1.00000 0.10440 0.05266 0.10527 -0.00890 0.07510 -0.01936 0.07714 0.03195 0.00073 0.00065 0.00080 0.00000 0.00606 0.00508 0.00619 0.00447 0.00501 0.00460 0.00260 H4 -0.15763 0.75257 0.75720 1.00000 0.09257 0.00000 0.00000 C5 -0.09114 0.82913 0.76282 1.00000 0.08607 0.04637 0.08488 -0.02113 0.06613 -0.01978 0.06200 0.02639 0.00061 0.00057 0.00068 0.00000 0.00455 0.00413 0.00468 0.00344 0.00374 0.00364 0.00197 C6 -0.13165 0.87125 0.69761 1.00000 0.06413 0.05980 0.07452 -0.02842 0.05094 -0.03329 0.05880 0.02258 0.00053 0.00060 0.00063 0.00000 0.00398 0.00434 0.00447 0.00341 0.00341 0.00357 0.00194 C7 -0.19975 0.86012 0.64735 1.00000 0.06542 0.08925 0.08665 -0.03586 0.04989 -0.04391 0.07487 0.02493 0.00059 0.00075 0.00073 0.00000 0.00477 0.00608 0.00568 0.00452 0.00418 0.00454 0.00257 H7 -0.22224 0.82057 0.65510 1.00000 0.08985 0.00000 0.00000 C8 -0.23164 0.90476 0.58995 1.00000 0.05510 0.11056 0.07827 -0.03332 0.03300 -0.04302 0.08090 0.02560 0.00060 0.00082 0.00075 0.00000 0.00490 0.00684 0.00579 0.00501 0.00430 0.00464 0.00286 H8 -0.27585 0.89546 0.55635 1.00000 0.09708 0.00000 0.00000 C9 -0.19968 0.96499 0.57968 1.00000 0.04156 0.09951 0.06659 -0.02617 0.02371 -0.02947 0.07015 0.02254 0.00051 0.00076 0.00066 0.00000 0.00407 0.00611 0.00520 0.00458 0.00377 0.00421 0.00252 H9 -0.22180 0.99790 0.54009 1.00000 0.08418 0.00000 0.00000 C10 -0.13459 0.97514 0.62923 1.00000 0.03633 0.06988 0.05487 -0.02081 0.02543 -0.01958 0.05223 0.02034 0.00045 0.00062 0.00057 0.00000 0.00337 0.00442 0.00418 0.00343 0.00312 0.00329 0.00186 C11 -0.09552 1.03825 0.62719 1.00000 0.02882 0.05816 0.04614 -0.00983 0.01530 -0.00602 0.04549 0.01938 0.00041 0.00056 0.00052 0.00000 0.00325 0.00426 0.00415 0.00333 0.00310 0.00300 0.00180 C12 0.06202 1.08235 0.68753 1.00000 0.02830 0.04039 0.04023 0.00132 0.01830 0.00323 0.03553 0.01846 0.00038 0.00046 0.00046 0.00000 0.00312 0.00364 0.00382 0.00300 0.00297 0.00273 0.00157 C13 0.11236 1.13827 0.72841 1.00000 0.02368 0.05380 0.04468 -0.00506 0.01679 -0.00463 0.04056 0.01860 0.00038 0.00052 0.00049 0.00000 0.00297 0.00394 0.00386 0.00318 0.00287 0.00287 0.00165 C14 0.17265 1.14043 0.73231 1.00000 0.02946 0.08297 0.06323 -0.01772 0.02468 -0.00608 0.05754 0.02169 0.00043 0.00066 0.00058 0.00000 0.00362 0.00552 0.00499 0.00430 0.00361 0.00366 0.00221 H14 0.18457 1.10579 0.70684 1.00000 0.06905 0.00000 0.00000 C15 0.21501 1.19498 0.77474 1.00000 0.03293 0.09714 0.07566 -0.01969 0.02598 -0.01265 0.06861 0.02366 0.00048 0.00071 0.00065 0.00000 0.00387 0.00619 0.00555 0.00484 0.00387 0.00405 0.00249 H15 0.25610 1.19944 0.77673 1.00000 0.08234 0.00000 0.00000 C16 0.19840 1.24365 0.81471 1.00000 0.03345 0.08273 0.06452 -0.01831 0.01838 -0.01951 0.06237 0.02222 0.00046 0.00068 0.00061 0.00000 0.00378 0.00560 0.00517 0.00438 0.00375 0.00391 0.00232 H16 0.22863 1.27872 0.84675 1.00000 0.07485 0.00000 0.00000 C17 0.13671 1.23894 0.80599 1.00000 0.02903 0.05565 0.04089 -0.00264 0.01338 -0.01186 0.04327 0.01868 0.00040 0.00054 0.00049 0.00000 0.00315 0.00397 0.00384 0.00318 0.00292 0.00302 0.00168 C18 0.10862 1.29235 0.83624 1.00000 0.03141 0.04522 0.03208 0.00150 0.00745 -0.00810 0.03947 0.01787 0.00040 0.00049 0.00045 0.00000 0.00330 0.00380 0.00364 0.00306 0.00295 0.00288 0.00164 C19 -0.02573 1.33462 0.85205 1.00000 0.04310 0.04535 0.04569 -0.01038 0.01641 -0.00265 0.04676 0.02004 0.00045 0.00053 0.00052 0.00000 0.00395 0.00391 0.00421 0.00322 0.00335 0.00319 0.00177 C20 -0.07082 1.39910 0.83333 1.00000 0.04797 0.04786 0.06695 -0.01377 0.02773 -0.00758 0.05420 0.02194 0.00049 0.00057 0.00061 0.00000 0.00393 0.00394 0.00461 0.00344 0.00351 0.00325 0.00185 C21 -0.11098 1.41189 0.86269 1.00000 0.06169 0.06284 0.09361 -0.01352 0.04758 -0.00530 0.06843 0.02661 0.00056 0.00066 0.00074 0.00000 0.00497 0.00508 0.00596 0.00456 0.00447 0.00401 0.00235 H21 -0.10977 1.38042 0.89948 1.00000 0.08212 0.00000 0.00000 C22 -0.15256 1.47022 0.83846 1.00000 0.07011 0.06835 0.12102 -0.01199 0.05282 0.00438 0.08361 0.03074 0.00063 0.00074 0.00086 0.00000 0.00542 0.00578 0.00688 0.00523 0.00516 0.00457 0.00274 H22 -0.18025 1.48022 0.85868 1.00000 0.10033 0.00000 0.00000 C23 -0.15417 1.51480 0.78415 1.00000 0.06270 0.05911 0.11283 -0.01641 0.03476 0.00941 0.08128 0.02866 0.00061 0.00071 0.00083 0.00000 0.00520 0.00529 0.00664 0.00469 0.00476 0.00450 0.00261 H23 -0.18374 1.55491 0.76607 1.00000 0.09754 0.00000 0.00000 C24 -0.11178 1.50052 0.75570 1.00000 0.05346 0.04394 0.08114 -0.01597 0.02040 0.00164 0.06446 0.02387 0.00053 0.00058 0.00069 0.00000 0.00429 0.00406 0.00499 0.00352 0.00373 0.00350 0.00206 C25 -0.11012 1.54056 0.69817 1.00000 0.06851 0.03706 0.07372 -0.01178 0.00894 0.00753 0.07024 0.02456 0.00060 0.00058 0.00069 0.00000 0.00479 0.00396 0.00493 0.00346 0.00382 0.00365 0.00222 C26 -0.15253 1.59841 0.66076 1.00000 0.08742 0.04476 0.08245 -0.01398 -0.00232 0.01959 0.08946 0.02686 0.00069 0.00064 0.00076 0.00000 0.00598 0.00488 0.00614 0.00422 0.00505 0.00458 0.00319 H26 -0.18476 1.61315 0.67315 1.00000 0.10735 0.00000 0.00000 C27 -0.14720 1.63390 0.60575 1.00000 0.09881 0.04133 0.08562 -0.00154 -0.01078 0.01248 0.09814 0.02858 0.00077 0.00068 0.00081 0.00000 0.00671 0.00508 0.00646 0.00448 0.00561 0.00495 0.00365 H27 -0.17522 1.67396 0.58099 1.00000 0.11777 0.00000 0.00000 C28 -0.10043 1.61108 0.58607 1.00000 0.09933 0.04775 0.08303 0.01245 -0.00172 -0.00145 0.09562 0.02891 0.00075 0.00069 0.00081 0.00000 0.00687 0.00512 0.00628 0.00474 0.00519 0.00502 0.00338 H28 -0.09617 1.63558 0.54859 1.00000 0.11474 0.00000 0.00000 C29 -0.05964 1.55019 0.62393 1.00000 0.08048 0.04821 0.07401 0.01108 0.00926 -0.00122 0.07913 0.02660 0.00067 0.00063 0.00071 0.00000 0.00587 0.00489 0.00574 0.00427 0.00460 0.00438 0.00273 H29 -0.02936 1.53206 0.60991 1.00000 0.09496 0.00000 0.00000 N1 -0.02812 0.85205 0.80228 1.00000 0.08936 0.04027 0.07378 -0.00653 0.06152 -0.00828 0.05850 0.02128 0.00049 0.00045 0.00052 0.00000 0.00464 0.00379 0.00445 0.00315 0.00376 0.00344 0.00181 N2 -0.10198 0.92977 0.68565 1.00000 0.04666 0.05453 0.05726 -0.02452 0.03173 -0.02572 0.05000 0.01624 0.00038 0.00045 0.00046 0.00000 0.00345 0.00390 0.00393 0.00295 0.00301 0.00302 0.00163 N3 -0.12401 1.09800 0.58840 1.00000 0.02803 0.08821 0.05555 0.01344 -0.00237 0.00165 0.06659 0.01907 0.00038 0.00057 0.00047 0.00000 0.00385 0.00596 0.00532 0.00459 0.00370 0.00391 0.00249 H3A -0.10042 1.13607 0.58923 1.00000 0.07990 0.00000 0.00000 H3B -0.16649 1.09956 0.56184 1.00000 0.07990 0.00000 0.00000 N4 -0.03250 1.02892 0.66909 1.00000 0.02511 0.04084 0.04750 -0.00350 0.01660 -0.00087 0.03816 0.01512 0.00031 0.00040 0.00040 0.00000 0.00275 0.00324 0.00364 0.00272 0.00271 0.00244 0.00142 N5 0.00500 1.09411 0.68302 1.00000 0.02150 0.03837 0.03869 -0.00095 0.01093 -0.00116 0.03432 0.01433 0.00030 0.00038 0.00037 0.00000 0.00262 0.00309 0.00337 0.00259 0.00255 0.00235 0.00135 N6 0.07729 1.02158 0.66357 1.00000 0.03167 0.04950 0.05024 -0.00623 0.02448 0.00023 0.04180 0.01622 0.00033 0.00042 0.00040 0.00000 0.00355 0.00407 0.00439 0.00341 0.00338 0.00304 0.00168 H6A 0.04841 0.98627 0.64327 1.00000 0.05016 0.00000 0.00000 H6B 0.11628 1.01667 0.66802 1.00000 0.05016 0.00000 0.00000 N7 0.09489 1.18681 0.76406 1.00000 0.02124 0.05026 0.04144 -0.00123 0.01299 -0.00793 0.03850 0.01454 0.00030 0.00041 0.00038 0.00000 0.00264 0.00353 0.00346 0.00280 0.00254 0.00258 0.00142 N8 0.14091 1.35537 0.86554 1.00000 0.04157 0.04424 0.04941 0.00026 0.01498 -0.01332 0.04792 0.01589 0.00037 0.00042 0.00041 0.00000 0.00400 0.00403 0.00455 0.00345 0.00357 0.00325 0.00184 H8A 0.12290 1.38992 0.87940 1.00000 0.05751 0.00000 0.00000 H8B 0.18003 1.36203 0.87084 1.00000 0.05751 0.00000 0.00000 N9 0.04914 1.27757 0.82617 1.00000 0.03572 0.03823 0.03578 0.00017 0.01445 -0.00581 0.03771 0.01497 0.00033 0.00039 0.00038 0.00000 0.00313 0.00319 0.00335 0.00262 0.00275 0.00253 0.00139 N10 0.01729 1.34212 0.82856 1.00000 0.03450 0.04148 0.04034 -0.00522 0.01285 -0.00461 0.04090 0.01525 0.00034 0.00041 0.00039 0.00000 0.00320 0.00324 0.00353 0.00272 0.00281 0.00262 0.00145 N11 -0.03151 1.27789 0.88837 1.00000 0.06149 0.06016 0.04871 0.00229 0.03507 0.00048 0.05320 0.01836 0.00042 0.00047 0.00043 0.00000 0.00498 0.00473 0.00466 0.00378 0.00411 0.00401 0.00196 H11A -0.00507 1.23997 0.89923 1.00000 0.06384 0.00000 0.00000 H11B -0.06180 1.27815 0.90162 1.00000 0.06384 0.00000 0.00000 N12 -0.07154 1.44247 0.78284 1.00000 0.04808 0.04480 0.05807 -0.01224 0.01913 0.00165 0.05296 0.01765 0.00039 0.00045 0.00047 0.00000 0.00378 0.00371 0.00422 0.00300 0.00331 0.00300 0.00169 N13 -0.06384 1.51849 0.67912 1.00000 0.06831 0.04092 0.07061 0.00543 0.01356 0.00107 0.06818 0.02048 0.00048 0.00048 0.00055 0.00000 0.00477 0.00396 0.00489 0.00340 0.00382 0.00347 0.00208 O31 0.11755 0.15739 0.56307 1.00000 0.10113 0.09481 0.11491 0.00624 0.03393 -0.05360 0.11107 0.01877 0.00043 0.00052 0.00055 0.00000 0.00645 0.00610 0.00748 0.00591 0.00561 0.00563 0.00346 O32 0.22343 0.19785 0.62539 1.00000 0.07901 0.05945 0.10540 -0.01411 0.05851 -0.01602 0.07536 0.01444 0.00031 0.00041 0.00038 0.00000 0.00461 0.00456 0.00540 0.00423 0.00410 0.00374 0.00206 O33 0.17025 0.19513 0.49803 1.00000 0.13281 0.15937 0.10590 -0.03906 0.07894 -0.00285 0.12369 0.02339 0.00055 0.00064 0.00046 0.00000 0.00846 0.00963 0.00619 0.00683 0.00618 0.00727 0.00369 O34 0.14137 0.27928 0.56130 1.00000 0.12393 0.06572 0.11372 -0.00149 0.07171 0.00275 0.09502 0.02153 0.00047 0.00036 0.00053 0.00000 0.00724 0.00462 0.00712 0.00484 0.00597 0.00466 0.00270 Cl31 0.16353 0.20598 0.56035 1.00000 0.07654 0.04553 0.09333 -0.01210 0.05793 -0.01601 0.06466 0.00654 0.00015 0.00014 0.00017 0.00000 0.00179 0.00132 0.00210 0.00136 0.00168 0.00125 0.00077 O41_a 0.22347 0.90989 0.59195 0.41844 0.05004 0.09788 0.12494 -0.02493 0.03198 0.00884 0.09512 0.04230 0.00087 0.00123 0.00096 0.00904 0.00760 0.00958 0.00876 0.00805 0.00683 0.00765 0.00446 O42_a 0.23709 0.88082 0.70506 0.41844 0.11584 0.08880 0.13400 0.01025 0.02515 0.00187 0.12735 0.04534 0.00102 0.00105 0.00094 0.00904 0.01295 0.01132 0.01189 0.01081 0.01035 0.01210 0.00741 O43_a 0.20699 1.00002 0.66181 0.41844 0.05205 0.06955 0.10367 -0.00567 0.04421 -0.00650 0.07225 0.03861 0.00099 0.00067 0.00111 0.00904 0.00772 0.00709 0.00975 0.00720 0.00733 0.00664 0.00471 O44_a 0.13357 0.90463 0.60900 0.41844 0.06422 0.08101 0.13811 -0.03076 0.04105 -0.00812 0.09757 0.03248 0.00058 0.00107 0.00115 0.00904 0.00642 0.00857 0.00974 0.00837 0.00674 0.00666 0.00473 Cl41_a 0.20060 0.92437 0.64222 0.41844 0.06793 0.07521 0.11792 -0.02186 0.03502 -0.00160 0.09100 0.02331 0.00052 0.00061 0.00065 0.00904 0.00432 0.00479 0.00643 0.00460 0.00433 0.00380 0.00313 O46_b 0.24879 0.94801 0.60649 0.58156 0.06266 0.11201 0.11545 -0.03922 0.05035 0.00440 0.09354 0.03166 0.00053 0.00087 0.00086 0.00904 0.00641 0.00926 0.00874 0.00786 0.00629 0.00635 0.00398 O47_b 0.18144 0.86162 0.61726 0.58156 0.07747 0.07764 0.14416 -0.01696 0.02085 0.00326 0.11321 0.03109 0.00072 0.00049 0.00094 0.00904 0.00768 0.00610 0.00938 0.00653 0.00740 0.00610 0.00474 O48_b 0.20225 0.97235 0.67993 0.58156 0.04558 0.10816 0.10109 -0.03604 0.03737 0.00757 0.08404 0.02739 0.00070 0.00087 0.00059 0.00904 0.00623 0.00882 0.00724 0.00765 0.00569 0.00729 0.00428 O49_b 0.13789 0.97066 0.55530 0.58156 0.06332 0.07841 0.09974 -0.02151 0.02958 0.00624 0.08446 0.02575 0.00051 0.00072 0.00060 0.00904 0.00642 0.00784 0.00776 0.00667 0.00607 0.00628 0.00403 Cl46_b 0.19277 0.93849 0.61432 0.58156 0.04204 0.07131 0.10016 -0.04327 0.02980 0.01181 0.07297 0.01368 0.00028 0.00037 0.00039 0.00904 0.00244 0.00343 0.00450 0.00327 0.00276 0.00219 0.00205 O51_a 0.13739 0.57761 0.48882 0.53526 0.10906 0.04498 0.07212 0.00387 0.07390 -0.00889 0.06274 0.02230 0.00072 0.00064 0.00064 0.00620 0.00804 0.00641 0.00731 0.00585 0.00647 0.00596 0.00354 O52_a 0.23552 0.63847 0.54756 0.53526 0.06541 0.20615 0.11021 0.00104 0.04890 -0.00037 0.12445 0.03461 0.00050 0.00116 0.00097 0.00620 0.00701 0.01464 0.01094 0.01102 0.00745 0.00773 0.00538 O53_a 0.14071 0.70176 0.51500 0.53526 0.12544 0.06814 0.08863 -0.01922 0.03376 0.00463 0.10140 0.03897 0.00085 0.00062 0.00093 0.00620 0.01101 0.00715 0.01006 0.00685 0.00952 0.00791 0.00561 O54_a 0.17439 0.61446 0.60734 0.53526 0.10038 0.11384 0.06397 -0.00313 0.05139 0.01757 0.08776 0.03663 0.00086 0.00098 0.00059 0.00620 0.00899 0.00969 0.00613 0.00622 0.00620 0.00842 0.00429 Cl51_a 0.17326 0.63344 0.54204 0.53526 0.05478 0.09197 0.05389 -0.00076 0.02940 -0.00049 0.06550 0.01142 0.00024 0.00032 0.00027 0.00620 0.00274 0.00347 0.00267 0.00246 0.00226 0.00244 0.00149 O56_b 0.05676 0.59679 0.52054 0.46474 0.07586 0.14510 0.13955 0.00227 0.06000 0.01013 0.11672 0.03672 0.00056 0.00111 0.00113 0.00620 0.00772 0.01341 0.01243 0.01109 0.00815 0.00849 0.00550 O57_b 0.15175 0.56184 0.51558 0.46474 0.08677 0.03775 0.06565 0.03284 0.06567 0.01382 0.05130 0.03706 0.00077 0.00062 0.00081 0.00620 0.00773 0.00588 0.00756 0.00573 0.00655 0.00566 0.00334 O58_b 0.11620 0.68313 0.49582 0.46474 0.09304 0.06646 0.07326 -0.00928 0.02325 0.01334 0.08452 0.04166 0.00093 0.00066 0.00093 0.00620 0.00974 0.00730 0.00844 0.00686 0.00806 0.00729 0.00480 O59_b 0.15791 0.63267 0.60944 0.46474 0.09425 0.10875 0.07047 -0.00134 0.03501 0.03430 0.09304 0.02987 0.00086 0.00113 0.00053 0.00620 0.00933 0.01025 0.00626 0.00669 0.00676 0.00865 0.00528 Cl56_b 0.11980 0.61652 0.53430 0.46474 0.07757 0.08422 0.07343 -0.00215 0.04290 0.01087 0.07564 0.01535 0.00033 0.00038 0.00036 0.00620 0.00374 0.00385 0.00352 0.00308 0.00305 0.00317 0.00186 O101 0.06161 0.82566 0.48700 1.00000 0.14351 0.11843 0.07429 -0.00636 0.04531 -0.07233 0.11497 0.02118 0.00059 0.00062 0.00053 0.00000 0.00974 0.00840 0.00632 0.00585 0.00657 0.00744 0.00410 O102 0.01725 0.05946 0.47409 1.00000 0.11879 0.08958 0.05290 -0.00794 0.03000 -0.06836 0.09175 0.01692 0.00049 0.00050 0.00043 0.00000 0.00749 0.00624 0.00475 0.00439 0.00495 0.00571 0.00322 O103_a 0.00292 0.56329 0.51974 0.53526 0.09377 0.19463 0.17179 0.02191 0.03591 0.00851 0.16497 0.06230 0.00123 0.00168 0.00166 0.00620 0.01317 0.01881 0.01757 0.01588 0.01343 0.01395 0.00906 O104_b 0.25760 0.69578 0.51526 0.46474 0.08396 0.18296 0.08958 -0.00302 0.02450 0.02085 0.12597 0.05610 0.00119 0.00162 0.00132 0.00620 0.01260 0.01919 0.01374 0.01383 0.01089 0.01356 0.00772 Final Structure Factor Calculation for 04src0422 in C2/c Total number of l.s. parameters = 658 Maximum vector length = 511 Memory required = 7337 / 25039 wR2 = 0.2976 before cycle 21 for 8912 data and 0 / 658 parameters Disagreeable restraints before cycle 21 Observed Target Error Sigma Restraint 0.0398 0.0100 SAME/SADI O54_a Cl51_a O51_a Cl51_a 0.0875 0.0200 SAME/SADI O56_b O57_b O31 O34 etc. 0.0746 0.0200 SAME/SADI O32 O34 O52_a O54_a etc. 0.0317 0.0100 SIMU U33 C23 C24 0.1138 0.0200 SIMU U22 O33 Cl31 0.1142 0.0200 SIMU U22 O52_a Cl51_a 0.0707 0.0200 SIMU U11 O53_a Cl51_a 0.0609 0.0200 SIMU U22 O56_b Cl56_b 0.0661 0.0200 SIMU U33 O56_b Cl56_b Summary of restraints applied in cycle 21 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 425. 0. 0. 0. 194. 534. 0. 0. rms sigma 0.000 0.000 0.000 0.016 0.000 0.000 0.000 0.010 0.016 0.000 0.000 rms deviation 0.000 0.000 0.000 0.023 0.000 0.000 0.000 0.005 0.018 0.000 0.000 GooF = S = 1.089; Restrained GooF = 1.105 for 1153 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0736 * P )^2 + 181.32 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.1245 for 5898 Fo > 4sig(Fo) and 0.1705 for all 8912 data wR2 = 0.2976, GooF = S = 1.089, Restrained GooF = 1.105 for all data Occupancy sum of asymmetric unit = 61.50 for non-hydrogen and 25.00 for hydrogen atoms Principal mean square atomic displacements U 0.0506 0.0374 0.0366 Zn1 0.0465 0.0358 0.0204 Zn2 0.0636 0.0492 0.0341 Zn3 0.1116 0.0491 0.0370 C1 0.1233 0.0634 0.0485 C2 0.1315 0.0830 0.0505 C3 0.1253 0.0639 0.0421 C4 0.1112 0.0389 0.0359 C5 0.1080 0.0416 0.0267 C6 0.1337 0.0604 0.0305 C7 0.1383 0.0727 0.0316 C8 0.1162 0.0651 0.0292 C9 0.0858 0.0440 0.0269 C10 0.0639 0.0449 0.0276 C11 0.0418 0.0396 0.0253 C12 0.0561 0.0441 0.0215 C13 0.0939 0.0534 0.0253 C14 0.1089 0.0681 0.0288 C15 0.0942 0.0662 0.0266 C16 0.0609 0.0444 0.0245 C17 0.0556 0.0374 0.0254 C18 0.0598 0.0458 0.0346 C19 0.0747 0.0486 0.0393 C20 0.0988 0.0583 0.0482 C21 0.1247 0.0733 0.0528 C22 0.1301 0.0689 0.0448 C23 0.1030 0.0527 0.0377 C24 0.1239 0.0541 0.0328 C25 0.1761 0.0560 0.0362 C26 0.1997 0.0565 0.0382 C27 0.1807 0.0630 0.0432 C28 0.1326 0.0610 0.0438 C29 0.0993 0.0391 0.0371 N1 0.0850 0.0404 0.0245 N2 0.1021 0.0755 0.0222 N3 0.0509 0.0395 0.0240 N4 0.0431 0.0384 0.0214 N5 0.0563 0.0441 0.0250 N6 0.0528 0.0441 0.0186 N7 0.0666 0.0477 0.0295 N8 0.0460 0.0361 0.0310 N9 0.0487 0.0435 0.0305 N10 0.0634 0.0600 0.0362 N11 0.0745 0.0473 0.0371 N12 0.1078 0.0569 0.0398 N13 0.1829 0.1087 0.0415 O31 0.1121 0.0647 0.0493 O32 0.1800 0.1337 0.0574 O33 0.1296 0.0904 0.0650 O34 0.1026 0.0537 0.0377 Cl31 0.1565 0.0834 0.0455 O41_a 0.1938 0.1027 0.0855 O42_a 0.1051 0.0697 0.0420 O43_a 0.1614 0.0704 0.0609 O44_a 0.1391 0.0679 0.0660 Cl41_a 0.1579 0.0810 0.0417 O46_b 0.1917 0.0744 0.0735 O47_b 0.1491 0.0707 0.0323 O48_b 0.1278 0.0678 0.0578 O49_b 0.1468 0.0531 0.0189 Cl46_b 0.1169 0.0501 0.0212 O51_a 0.2062 0.1106 0.0566 O52_a 0.1534 0.0950 0.0558 O53_a 0.1270 0.0908 0.0455 O54_a 0.0920 0.0566 0.0479 Cl51_a 0.1467 0.1402 0.0633 O56_b 0.1068 0.0456 0.0015 O57_b 0.1262 0.0698 0.0576 O58_b 0.1444 0.0710 0.0637 O59_b 0.0926 0.0775 0.0568 Cl56_b 0.2172 0.0734 0.0544 O101 may be split into 0.0661 0.8191 0.4840 and 0.0571 0.8322 0.4900 0.1885 0.0529 0.0339 O102 0.2218 0.1813 0.0918 O103_a 0.1914 0.1130 0.0735 O104_b 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 0.032 0.044 0.058 0.077 0.107 0.166 1.000 Number in group 995. 880. 886. 854. 906. 839. 902. 866. 885. 899. GooF 1.232 1.195 1.208 1.143 1.058 0.982 0.962 0.975 1.000 1.073 K 25.450 5.201 2.700 1.702 1.359 1.173 1.088 1.014 0.999 1.001 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.15 1.32 1.64 inf Number in group 916. 865. 913. 876. 894. 898. 875. 895. 889. 891. GooF 0.845 0.858 0.907 0.928 1.016 1.090 1.173 1.130 1.183 1.572 K 1.247 1.216 1.189 1.101 1.076 1.071 1.034 1.024 0.998 1.020 R1 0.424 0.339 0.308 0.253 0.219 0.173 0.162 0.124 0.094 0.084 Recommended weighting scheme: WGHT 0.0736 181.2994 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) -13 3 4 6306.00 662.12 7.02 0.046 1.71 15 3 0 3563.02 44.33 6.50 0.012 1.34 0 6 2 3965.30 247.79 6.48 0.028 2.87 9 1 2 3812.83 238.07 6.35 0.028 2.00 3 3 0 3400.79 150.95 6.33 0.022 4.54 -3 3 6 4126.63 524.58 5.73 0.041 3.03 5 1 1 2979.50 206.87 5.64 0.026 3.59 11 1 1 2375.72 119.36 5.16 0.020 1.77 1 7 0 2626.22 229.27 5.09 0.027 2.57 -8 4 6 6588.19 2069.44 5.00 0.082 2.33 17 7 1 2329.67 8.72 4.96 0.005 1.07 1 5 1 7069.49 2414.26 4.85 0.089 3.45 -19 5 14 2797.70 328.52 4.72 0.033 1.10 5 1 6 2341.85 246.77 4.65 0.028 2.03 -3 1 2 4144.76 11881.03 4.53 0.197 6.93 9 7 5 1982.53 104.94 4.51 0.019 1.38 -15 11 6 2178.71 198.05 4.43 0.025 1.14 -21 7 5 2532.56 210.66 4.39 0.026 1.00 -19 7 1 3186.83 520.91 4.38 0.041 1.02 -17 7 9 1815.02 34.75 4.22 0.011 1.21 3 1 0 1318.54 20.30 4.20 0.008 6.43 -20 4 10 1595.85 17.88 4.19 0.008 1.13 5 1 5 2530.74 456.71 4.17 0.039 2.24 -15 1 11 1463.57 42.90 4.11 0.012 1.46 8 6 2 1923.51 238.80 4.06 0.028 1.79 -9 1 3 14729.78 7985.21 4.03 0.161 2.57 -17 3 4 1883.00 207.59 3.96 0.026 1.31 -10 2 6 1360.70 73.47 3.96 0.015 2.23 -15 11 2 1746.28 115.42 3.96 0.019 1.10 -6 0 4 4611.16 1601.30 3.92 0.072 3.75 19 5 1 1420.88 5.12 3.92 0.004 1.01 17 3 2 1831.90 98.80 3.92 0.018 1.11 -17 1 5 1371.27 17.92 3.90 0.008 1.36 2 6 12 1372.58 6.96 3.89 0.005 1.29 11 11 0 1392.58 36.97 3.89 0.011 1.24 -23 7 9 1404.48 3.76 3.88 0.004 0.95 5 11 2 1425.72 94.13 3.86 0.018 1.47 -13 7 5 1314.13 45.36 3.86 0.012 1.48 9 11 0 1743.95 93.53 3.83 0.017 1.34 -1 3 10 2181.63 404.91 3.77 0.036 1.83 -5 3 5 1712.50 238.14 3.76 0.028 3.22 -9 7 10 1113.25 5.31 3.75 0.004 1.57 8 0 6 60061.41 94318.96 3.74 0.555 1.63 16 2 3 1260.27 10.55 3.74 0.006 1.15 -21 7 10 1512.95 49.34 3.72 0.013 1.03 -21 5 9 1213.37 10.24 3.70 0.006 1.07 -5 3 4 11799.88 6321.98 3.69 0.144 3.48 -25 3 11 1651.00 141.22 3.68 0.021 0.93 -7 3 3 990.68 11.74 3.68 0.006 2.94 -13 3 2 2347.71 453.80 3.66 0.038 1.64 Bond lengths and angles Zn1 - Distance Angles N2 2.1223 (0.0079) N2_$1 2.1223 (0.0079) 169.00 (0.46) N4_$1 2.1827 (0.0075) 115.60 (0.27) 73.01 (0.29) N4 2.1827 (0.0075) 73.01 (0.29) 115.60 (0.27) 86.24 (0.38) N1_$1 2.2221 (0.0081) 97.39 (0.34) 74.47 (0.36) 146.97 (0.32) 102.75 (0.29) N1 2.2221 (0.0081) 74.47 (0.36) 97.39 (0.34) 102.75 (0.29) 146.97 (0.32) 87.00 (0.41) Zn1 - N2 N2_$1 N4_$1 N4 N1_$1 Zn2 - Distance Angles N7 2.1052 (0.0062) N7_$1 2.1052 (0.0062) 178.16 (0.41) N5 2.2049 (0.0070) 73.98 (0.26) 107.46 (0.26) N5_$1 2.2049 (0.0070) 107.46 (0.26) 73.98 (0.26) 83.43 (0.36) N9 2.2222 (0.0071) 74.77 (0.27) 103.79 (0.27) 148.75 (0.24) 105.84 (0.25) N9_$1 2.2222 (0.0070) 103.79 (0.27) 74.77 (0.27) 105.84 (0.25) 148.75 (0.24) 81.88 (0.37) Zn2 - N7 N7_$1 N5 N5_$1 N9 Zn3 - Distance Angles N12_$1 2.1141 (0.0086) N12 2.1141 (0.0086) 167.65 (0.46) N10_$1 2.1854 (0.0077) 73.78 (0.31) 115.85 (0.29) N10 2.1854 (0.0077) 115.85 (0.29) 73.78 (0.31) 86.56 (0.39) N13_$1 2.2137 (0.0092) 75.69 (0.39) 95.23 (0.37) 148.88 (0.35) 101.52 (0.32) N13 2.2137 (0.0091) 95.23 (0.37) 75.69 (0.38) 101.52 (0.32) 148.88 (0.35) 87.05 (0.48) Zn3 - N12_$1 N12 N10_$1 N10 N13_$1 C1 - Distance Angles N1 1.3211 (0.0148) C2 1.3851 (0.0154) 122.14 (1.33) H1 0.9500 118.93 118.93 C1 - N1 C2 C2 - Distance Angles C3 1.3548 (0.0194) C1 1.3851 (0.0154) 117.54 (1.38) H2 0.9500 121.23 121.23 C2 - C3 C1 C3 - Distance Angles C4 1.3474 (0.0194) C2 1.3548 (0.0195) 122.85 (1.29) H3 0.9500 118.58 118.58 C3 - C4 C2 C4 - Distance Angles C3 1.3474 (0.0195) C5 1.3890 (0.0147) 117.33 (1.37) H4 0.9500 121.33 121.33 C4 - C3 C5 C5 - Distance Angles N1 1.3695 (0.0146) C4 1.3890 (0.0147) 121.12 (1.26) C6 1.4538 (0.0171) 116.11 (0.88) 122.77 (1.17) C5 - N1 C4 C6 - Distance Angles N2 1.3574 (0.0119) C7 1.4474 (0.0160) 117.42 (1.15) C5 1.4538 (0.0171) 114.97 (0.94) 127.52 (1.00) C6 - N2 C7 C7 - Distance Angles C8 1.3426 (0.0188) C6 1.4474 (0.0160) 121.09 (1.09) H7 0.9500 119.45 119.45 C7 - C8 C6 C8 - Distance Angles C7 1.3426 (0.0188) C9 1.3993 (0.0170) 119.92 (1.14) H8 0.9500 120.04 120.04 C8 - C7 C9 C9 - Distance Angles C10 1.3891 (0.0136) C8 1.3993 (0.0170) 117.88 (1.29) H9 0.9500 121.06 121.06 C9 - C10 C8 C10 - Distance Angles N2 1.3401 (0.0137) C9 1.3891 (0.0136) 122.56 (1.00) C11 1.4801 (0.0132) 113.59 (0.80) 123.79 (1.10) C10 - N2 C9 C11 - Distance Angles N4 1.3214 (0.0107) N3 1.3270 (0.0130) 125.97 (0.88) C10 1.4801 (0.0132) 113.24 (0.89) 120.73 (0.84) C11 - N4 N3 C12 - Distance Angles N5 1.3149 (0.0096) N6 1.3298 (0.0105) 123.91 (0.77) C13 1.4794 (0.0117) 115.74 (0.73) 120.07 (0.70) C12 - N5 N6 C13 - Distance Angles N7 1.3409 (0.0110) C14 1.3805 (0.0113) 121.95 (0.83) C12 1.4794 (0.0117) 113.55 (0.67) 124.48 (0.84) C13 - N7 C14 C14 - Distance Angles C13 1.3805 (0.0113) C15 1.3824 (0.0148) 117.37 (0.95) H14 0.9500 121.31 121.31 C14 - C13 C15 C15 - Distance Angles C14 1.3824 (0.0148) C16 1.3966 (0.0155) 121.10 (0.91) H15 0.9500 119.45 119.45 C15 - C14 C16 C16 - Distance Angles C17 1.3742 (0.0122) C15 1.3966 (0.0155) 117.54 (0.94) H16 0.9500 121.23 121.23 C16 - C17 C15 C17 - Distance Angles N7 1.3429 (0.0108) C16 1.3742 (0.0122) 121.63 (0.91) C18 1.4763 (0.0129) 113.93 (0.71) 124.29 (0.87) C17 - N7 C16 C18 - Distance Angles N9 1.3369 (0.0104) N8 1.3455 (0.0109) 124.04 (0.86) C17 1.4763 (0.0130) 116.78 (0.75) 118.86 (0.77) C18 - N9 N8 C19 - Distance Angles N11 1.3256 (0.0125) N10 1.3280 (0.0119) 126.87 (0.89) C20 1.4977 (0.0137) 120.06 (0.89) 113.06 (0.88) C19 - N11 N10 C20 - Distance Angles N12 1.3136 (0.0135) C21 1.3726 (0.0146) 121.11 (1.04) C19 1.4977 (0.0138) 114.33 (0.89) 124.50 (1.07) C20 - N12 C21 C21 - Distance Angles C22 1.3616 (0.0170) C20 1.3726 (0.0146) 119.23 (1.29) H21 0.9500 120.39 120.39 C21 - C22 C20 C22 - Distance Angles C21 1.3616 (0.0171) C23 1.3836 (0.0194) 119.47 (1.26) H22 0.9500 120.26 120.26 C22 - C21 C23 C23 - Distance Angles C22 1.3836 (0.0194) C24 1.4100 (0.0174) 119.81 (1.18) H23 0.9500 120.09 120.09 C23 - C22 C24 C24 - Distance Angles N12 1.3450 (0.0130) C23 1.4100 (0.0174) 117.39 (1.22) C25 1.4261 (0.0180) 117.21 (1.08) 125.33 (1.13) C24 - N12 C23 C25 - Distance Angles N13 1.3861 (0.0163) C26 1.3995 (0.0156) 120.01 (1.37) C24 1.4261 (0.0179) 116.27 (0.98) 123.71 (1.37) C25 - N13 C26 C26 - Distance Angles C27 1.3796 (0.0220) C25 1.3995 (0.0157) 119.53 (1.55) H26 0.9500 120.23 120.23 C26 - C27 C25 C27 - Distance Angles C26 1.3796 (0.0220) C28 1.4097 (0.0231) 120.41 (1.27) H27 0.9500 119.80 119.80 C27 - C26 C28 C28 - Distance Angles C27 1.4097 (0.0231) C29 1.4273 (0.0169) 118.24 (1.52) H28 0.9500 120.88 120.88 C28 - C27 C29 C29 - Distance Angles N13 1.3393 (0.0164) C28 1.4273 (0.0169) 120.33 (1.51) H29 0.9500 119.84 119.84 C29 - N13 C28 N1 - Distance Angles C1 1.3211 (0.0148) C5 1.3695 (0.0146) 118.98 (0.97) Zn1 2.2221 (0.0081) 126.47 (0.82) 114.38 (0.76) N1 - C1 C5 N2 - Distance Angles C10 1.3401 (0.0137) C6 1.3574 (0.0119) 121.09 (0.89) Zn1 2.1223 (0.0078) 119.75 (0.59) 118.73 (0.79) N2 - C10 C6 N3 - Distance Angles C11 1.3270 (0.0130) H3A 0.8800 120.00 H3B 0.8800 120.00 120.00 N3 - C11 H3A N4 - Distance Angles C11 1.3214 (0.0107) N5 1.4180 (0.0094) 114.71 (0.72) Zn1 2.1827 (0.0075) 118.26 (0.61) 119.79 (0.49) N4 - C11 N5 N5 - Distance Angles C12 1.3149 (0.0096) N4 1.4180 (0.0094) 113.03 (0.66) Zn2 2.2049 (0.0070) 116.09 (0.54) 122.36 (0.48) N5 - C12 N4 N6 - Distance Angles C12 1.3298 (0.0105) H6A 0.8800 120.00 H6B 0.8800 120.00 120.00 N6 - C12 H6A N7 - Distance Angles C13 1.3409 (0.0110) C17 1.3429 (0.0109) 120.26 (0.70) Zn2 2.1052 (0.0062) 119.93 (0.53) 119.74 (0.59) N7 - C13 C17 N8 - Distance Angles C18 1.3455 (0.0109) H8A 0.8800 120.00 H8B 0.8800 120.00 120.00 N8 - C18 H8A N9 - Distance Angles C18 1.3369 (0.0104) N10 1.4026 (0.0101) 111.28 (0.69) Zn2 2.2222 (0.0070) 114.07 (0.58) 123.63 (0.50) N9 - C18 N10 N10 - Distance Angles C19 1.3280 (0.0119) N9 1.4026 (0.0101) 116.28 (0.74) Zn3 2.1854 (0.0076) 117.15 (0.62) 119.29 (0.52) N10 - C19 N9 N11 - Distance Angles C19 1.3256 (0.0125) H11A 0.8800 120.00 H11B 0.8800 120.00 120.00 N11 - C19 H11A N12 - Distance Angles C20 1.3136 (0.0135) C24 1.3450 (0.0130) 122.96 (0.99) Zn3 2.1141 (0.0085) 119.68 (0.67) 116.98 (0.81) N12 - C20 C24 N13 - Distance Angles C29 1.3393 (0.0164) C25 1.3861 (0.0163) 121.36 (1.08) Zn3 2.2137 (0.0091) 125.83 (0.92) 112.80 (0.80) N13 - C29 C25 O31 - Distance Angles Cl31 1.4165 (0.0059) O31 - O32 - Distance Angles Cl31 1.4228 (0.0060) O32 - O33 - Distance Angles Cl31 1.4057 (0.0061) O33 - O34 - Distance Angles Cl31 1.4304 (0.0060) O34 - Cl31 - Distance Angles O33 1.4057 (0.0061) O31 1.4165 (0.0059) 112.32 (0.63) O32 1.4228 (0.0061) 112.20 (0.55) 108.64 (0.51) O34 1.4304 (0.0060) 110.32 (0.59) 106.66 (0.57) 106.37 (0.51) Cl31 - O33 O31 O32 O41_a - Distance Angles Cl41_a 1.4204 (0.0075) O41_a - O42_a - Distance Angles Cl41_a 1.4193 (0.0075) O42_a - O43_a - Distance Angles Cl41_a 1.4183 (0.0074) O43_a - O44_a - Distance Angles Cl41_a 1.4291 (0.0075) O44_a - Cl41_a - Distance Angles O43_a 1.4183 (0.0074) O42_a 1.4193 (0.0075) 109.57 (0.94) O41_a 1.4204 (0.0075) 111.67 (0.99) 108.27 (0.93) O44_a 1.4291 (0.0075) 108.78 (0.89) 110.32 (1.00) 108.23 (0.92) Cl41_a - O43_a O42_a O41_a O46_b - Distance Angles Cl46_b 1.4137 (0.0070) O46_b - O47_b - Distance Angles Cl46_b 1.4252 (0.0072) O47_b - O48_b - Distance Angles Cl46_b 1.4251 (0.0070) O48_b - O49_b - Distance Angles Cl46_b 1.4163 (0.0070) O49_b - Cl46_b - Distance Angles O46_b 1.4137 (0.0070) O49_b 1.4163 (0.0070) 110.85 (0.82) O48_b 1.4251 (0.0070) 109.76 (0.81) 108.86 (0.72) O47_b 1.4252 (0.0072) 109.15 (0.76) 109.24 (0.80) 108.95 (0.87) Cl46_b - O46_b O49_b O48_b O51_a - Distance Angles Cl51_a 1.4420 (0.0071) O51_a - O52_a - Distance Angles Cl51_a 1.4146 (0.0070) O52_a - O53_a - Distance Angles Cl51_a 1.4225 (0.0072) O53_a - O54_a - Distance Angles Cl51_a 1.4021 (0.0071) O54_a - Cl51_a - Distance Angles O54_a 1.4021 (0.0071) O52_a 1.4146 (0.0070) 113.74 (0.89) O53_a 1.4225 (0.0072) 110.99 (0.84) 108.28 (0.88) O51_a 1.4420 (0.0071) 108.41 (0.79) 107.80 (0.80) 107.39 (0.80) Cl51_a - O54_a O52_a O53_a O56_b - Distance Angles Cl56_b 1.4129 (0.0072) O56_b - O57_b - Distance Angles Cl56_b 1.4087 (0.0071) O57_b - O58_b - Distance Angles Cl56_b 1.4324 (0.0073) O58_b - O59_b - Distance Angles Cl56_b 1.4220 (0.0073) O59_b - Cl56_b - Distance Angles O57_b 1.4087 (0.0071) O56_b 1.4129 (0.0072) 114.35 (0.88) O59_b 1.4220 (0.0073) 108.57 (0.85) 108.61 (0.88) O58_b 1.4324 (0.0073) 109.29 (0.80) 109.00 (0.91) 106.75 (0.86) Cl56_b - O57_b O56_b O59_b FMAP and GRID set by program FMAP 2 1 -35 GRID -0.781 -1 -1 0.781 1 1 R1 = 0.1652 for 8912 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 1.22 at -0.0019 0.5458 0.2798 [ 0.78 A from ZN3 ] Deepest hole -0.95 at 0.0000 0.3161 0.2500 [ 3.32 A from C1 ] Mean = 0.00, Rms deviation from mean = 0.13 e/A^3, Highest memory used = 7626 /101494 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.0019 1.4542 0.7202 1.00000 0.05 1.22 0.78 ZN3 1.68 N12 1.79 N13 2.22 N10 Q2 1 0.0953 0.7947 0.4800 1.00000 0.05 1.11 1.04 O101 1.94 O53 1.97 H3A 2.07 O58 Q3 1 0.1710 0.4940 0.5469 1.00000 0.05 1.05 1.37 O57 1.87 O51 1.90 H22 2.13 H8 Q4 1 0.2205 0.5877 0.5176 1.00000 0.05 0.97 1.07 O52 1.65 CL51 1.66 O57 1.75 O51 Q5 1 0.1037 0.5726 0.4678 1.00000 0.05 0.94 0.70 O51 1.11 O57 1.49 CL56 1.95 O56 Shortest distances between peaks (including symmetry equivalents) 1 1 1.30 3 5 2.18 3 4 2.30 4 5 2.44 Time profile in seconds ----------------------- 0.05: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.02: 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 0.02: Analyse other restraints etc. 1.69: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.03: Set up l.s. refinement 0.00: Generate idealized H-atoms 16.84: Structure factors and derivatives 96.14: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.36: Apply other restraints 7.95: Solve l.s. equations 0.00: Generate HTAB table 0.09: Other dependent quantities, CIF, tables 0.23: Analysis of variance 0.05: Merge reflections for Fourier and .fcf 0.25: Fourier summations 0.16: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 04src0422 finished at 12:58:04 Total CPU time: 123.7 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++