+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 04src0194 started at 11:49:55 on 16-Oct-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL s93 in Pna2(1) CELL 0.71069 25.8090 11.8990 17.3570 90.000 90.000 90.000 ZERR 4.00 0.0050 0.0050 0.0050 0.000 0.000 0.000 LATT -1 SYMM - X, - Y, 1/2 + Z SYMM 1/2 - X, 1/2 + Y, 1/2 + Z SYMM 1/2 + X, 1/2 - Y, Z SFAC C H N O CL NI UNIT 176 184 64 84 16 8 V = 5330.36 F(000) = 2856.0 Mu = 1.00 mm-1 Cell Wt = 5576.75 Rho = 1.737 MERG 2 OMIT -3.00 55.00 OMIT 8 1 0 OMIT 8 0 2 OMIT 8 0 -2 OMIT 4 3 0 TWIN BASF 0.51652 SHEL 7 0.77 DFIX 21 0.01 O1 CL1 O2 CL1 O3 CL1 O4 CL1 DANG 21.6333 O1 O2 O1 O3 O1 O4 O2 O3 O2 O4 O3 O4 DELU 0.01 SIMU 0.02 FMAP 2 PLAN 10 SIZE 0.03 0.14 0.22 ACTA BOND $H WGHT 0.06230 30.21620 L.S. 6 TEMP -153.00 FVAR 0.07180 1.41794 MOLE 1 C1 1 0.027789 0.087026 0.584658 11.00000 0.03328 0.02840 = 0.01821 0.00115 0.00287 -0.00250 AFIX 43 H1 2 0.045167 0.026741 0.559758 11.00000 -1.20000 AFIX 0 C2 1 -0.013623 0.061322 0.629663 11.00000 0.02631 0.03148 = 0.02077 -0.00807 0.01001 -0.00205 AFIX 43 H2 2 -0.027162 -0.012797 0.632594 11.00000 -1.20000 AFIX 0 C3 1 -0.035229 0.150616 0.671559 11.00000 0.03640 0.04746 = 0.01113 -0.00789 0.00342 -0.00707 AFIX 43 H3 2 -0.063574 0.138037 0.705396 11.00000 -1.20000 AFIX 0 C4 1 -0.014750 0.256807 0.662926 11.00000 0.02268 0.03885 = 0.01317 -0.00354 0.00146 0.00105 AFIX 43 H4 2 -0.028367 0.317826 0.691838 11.00000 -1.20000 AFIX 0 C5 1 0.025607 0.274258 0.612149 11.00000 0.00411 0.03399 = 0.02476 -0.00277 -0.00512 -0.00180 C6 1 0.050750 0.384349 0.603140 11.00000 0.01932 0.02945 = 0.00621 0.00210 0.00009 0.00495 C7 1 0.034047 0.486544 0.631895 11.00000 0.02057 0.03143 = 0.00268 -0.00524 0.00097 -0.00035 AFIX 43 H7 2 0.003392 0.491953 0.661964 11.00000 -1.20000 AFIX 0 C8 1 0.062349 0.576830 0.616013 11.00000 0.03212 0.02574 = 0.01831 -0.00440 0.00050 0.00542 AFIX 43 H8 2 0.050793 0.647499 0.634811 11.00000 -1.20000 AFIX 0 C9 1 0.108016 0.573702 0.573347 11.00000 0.02810 0.01824 = 0.00563 0.00149 0.00210 -0.00019 AFIX 43 H9 2 0.128156 0.638922 0.563356 11.00000 -1.20000 AFIX 0 C10 1 0.121688 0.469265 0.546860 11.00000 0.01615 0.01943 = 0.01076 0.00018 0.00198 0.00469 C11 1 0.167628 0.442882 0.496426 11.00000 0.01849 0.01891 = 0.01437 0.00765 0.00260 0.00486 C12 1 0.205791 0.270910 0.359297 11.00000 0.02593 0.02239 = 0.01077 0.00507 0.00155 0.00554 C13 1 0.249642 0.197714 0.335420 11.00000 0.01365 0.02070 = 0.02004 -0.00057 0.00037 0.00111 C14 1 0.260865 0.161311 0.265080 11.00000 0.02992 0.01800 = 0.01791 0.00161 0.00069 -0.00355 AFIX 43 H14 2 0.239431 0.184049 0.223403 11.00000 -1.20000 AFIX 0 C15 1 0.303231 0.090420 0.249832 11.00000 0.02262 0.02515 = 0.02715 0.00912 0.00744 0.00338 AFIX 43 H15 2 0.312511 0.066557 0.199456 11.00000 -1.20000 AFIX 0 C16 1 0.330140 0.058735 0.315446 11.00000 0.02290 0.03523 = 0.02510 -0.00635 0.00498 -0.00055 AFIX 43 H16 2 0.358483 0.008490 0.309689 11.00000 -1.20000 AFIX 0 C17 1 0.318225 0.095752 0.388389 11.00000 0.02259 0.02135 = 0.01776 0.00101 0.00233 0.00132 C18 1 0.345651 0.072371 0.461750 11.00000 0.01934 0.02302 = 0.01789 -0.00373 -0.00012 0.00377 C19 1 0.386306 0.000652 0.466620 11.00000 0.02084 0.03950 = 0.03210 -0.00218 0.00467 0.01316 AFIX 43 H19 2 0.400066 -0.033701 0.421649 11.00000 -1.20000 AFIX 0 C20 1 0.407053 -0.021252 0.537091 11.00000 0.02289 0.03864 = 0.03559 0.00797 -0.00167 0.00496 AFIX 43 H20 2 0.434922 -0.073044 0.541319 11.00000 -1.20000 AFIX 0 C21 1 0.388859 0.028940 0.600534 11.00000 0.01084 0.03440 = 0.04326 -0.00578 -0.00783 0.00621 AFIX 43 H21 2 0.402449 0.013576 0.650298 11.00000 -1.20000 AFIX 0 C22 1 0.347334 0.107763 0.588431 11.00000 0.01936 0.03105 = 0.02744 -0.00393 0.00136 0.00796 AFIX 43 H22 2 0.334108 0.146978 0.631861 11.00000 -1.20000 AFIX 0 C31 1 0.026777 0.392987 0.406678 11.00000 0.01282 0.02215 = 0.02709 -0.00266 0.00354 -0.00029 AFIX 43 H31 2 0.040220 0.453143 0.436602 11.00000 -1.20000 AFIX 0 C32 1 -0.012725 0.415443 0.354552 11.00000 0.01997 0.02848 = 0.01234 -0.00060 0.00868 0.01190 AFIX 43 H32 2 -0.023903 0.490271 0.345176 11.00000 -1.20000 AFIX 0 C33 1 -0.034554 0.328620 0.317956 11.00000 0.01592 0.03803 = 0.01998 0.00252 -0.00849 0.00136 AFIX 43 H33 2 -0.062508 0.342073 0.283562 11.00000 -1.20000 AFIX 0 C34 1 -0.017770 0.222109 0.328761 11.00000 0.01826 0.03699 = 0.01978 0.00090 -0.00343 -0.00816 AFIX 43 H34 2 -0.034803 0.160161 0.305295 11.00000 -1.20000 AFIX 0 C35 1 0.025222 0.206859 0.375373 11.00000 0.02582 0.02265 = 0.00610 0.00099 -0.00045 -0.00244 C36 1 0.050601 0.098045 0.389136 11.00000 0.01776 0.02024 = 0.02671 -0.00648 0.00041 -0.00065 C37 1 0.032790 -0.005072 0.361698 11.00000 0.01980 0.02754 = 0.04103 -0.00412 -0.00131 -0.00045 AFIX 43 H37 2 0.002427 -0.009183 0.330886 11.00000 -1.20000 AFIX 0 C38 1 0.060410 -0.102101 0.380357 11.00000 0.01507 0.02100 = 0.02430 -0.00307 0.00313 -0.00096 AFIX 43 H38 2 0.048619 -0.173807 0.363871 11.00000 -1.20000 AFIX 0 C39 1 0.105452 -0.091839 0.423477 11.00000 0.01209 0.02809 = 0.03465 0.00166 0.00187 0.00108 AFIX 43 H39 2 0.125463 -0.156303 0.436020 11.00000 -1.20000 AFIX 0 C40 1 0.120534 0.012260 0.447562 11.00000 0.01047 0.02318 = 0.02230 0.00060 0.00763 0.00433 C41 1 0.166159 0.038121 0.493546 11.00000 0.01589 0.02502 = 0.01186 0.00072 0.01043 0.00423 C42 1 0.203622 0.216528 0.631479 11.00000 0.01414 0.02691 = 0.01432 -0.00056 0.00548 0.00781 C43 1 0.245301 0.291425 0.655290 11.00000 0.01792 0.03103 = 0.01324 -0.00184 0.00064 0.00550 C44 1 0.255885 0.328606 0.731356 11.00000 0.02477 0.03168 = 0.01827 0.00156 -0.00190 -0.00045 AFIX 43 H44 2 0.237511 0.301513 0.774995 11.00000 -1.20000 AFIX 0 C45 1 0.294495 0.406249 0.736806 11.00000 0.02599 0.03453 = 0.01303 -0.00968 -0.00649 0.00122 AFIX 43 H45 2 0.301334 0.436529 0.786419 11.00000 -1.20000 AFIX 0 C46 1 0.323416 0.443334 0.678853 11.00000 0.03617 0.03398 = 0.01164 -0.00356 -0.00609 -0.00245 AFIX 43 H46 2 0.350073 0.497455 0.685775 11.00000 -1.20000 AFIX 0 C47 1 0.311627 0.396351 0.606042 11.00000 0.01761 0.03221 = 0.01472 -0.01106 0.00106 0.00211 C48 1 0.340114 0.426020 0.535475 11.00000 0.00685 0.02385 = 0.02111 -0.00221 -0.00117 0.00836 C49 1 0.376375 0.506488 0.530303 11.00000 0.02275 0.02381 = 0.01900 -0.00556 0.00069 0.00192 AFIX 43 H49 2 0.384674 0.549456 0.574753 11.00000 -1.20000 AFIX 0 C50 1 0.401920 0.528452 0.462123 11.00000 0.02773 0.02708 = 0.02305 0.00109 0.00574 -0.00198 AFIX 43 H50 2 0.428212 0.584107 0.458728 11.00000 -1.20000 AFIX 0 C51 1 0.386947 0.463980 0.397833 11.00000 0.03919 0.02918 = 0.00980 0.00696 -0.00003 -0.00057 AFIX 43 H51 2 0.402796 0.476785 0.349220 11.00000 -1.20000 AFIX 0 C52 1 0.350638 0.385105 0.404950 11.00000 0.02217 0.03744 = 0.01779 -0.00150 0.00533 0.00243 AFIX 43 H52 2 0.341112 0.342078 0.361075 11.00000 -1.20000 AFIX 0 N1 3 0.045821 0.190458 0.572867 11.00000 0.01643 0.02035 = 0.01697 0.00485 -0.00122 0.00143 N2 3 0.093948 0.378572 0.561062 11.00000 0.01221 0.02097 = 0.01530 0.00247 0.00043 -0.00022 N3 3 0.207085 0.511160 0.499419 11.00000 0.02182 0.03232 = 0.01480 -0.00707 0.00093 -0.00062 AFIX 93 H3A 2 0.235421 0.495906 0.473230 11.00000 -1.20000 H3B 2 0.205382 0.572500 0.527629 11.00000 -1.20000 AFIX 0 N4 3 0.162752 0.350753 0.459164 11.00000 0.00508 0.02271 = 0.01490 0.00332 0.00368 0.00433 N5 3 0.209879 0.311406 0.427852 11.00000 0.01766 0.02856 = 0.00622 -0.00068 0.00420 0.00485 N6 3 0.167106 0.285503 0.313765 11.00000 0.01437 0.03236 = 0.03394 -0.00483 -0.00279 0.00952 AFIX 93 H6A 2 0.140449 0.326120 0.328735 11.00000 -1.20000 H6B 2 0.167272 0.254878 0.267617 11.00000 -1.20000 AFIX 0 N7 3 0.277993 0.166387 0.399540 11.00000 0.02082 0.02661 = 0.01625 0.00068 0.00392 -0.00105 N8 3 0.327663 0.127557 0.523902 11.00000 0.02178 0.02282 = 0.02294 -0.00315 0.00596 0.00655 N31 3 0.046547 0.290838 0.416428 11.00000 0.01325 0.02029 = 0.01660 -0.00292 0.00699 0.00036 N32 3 0.093611 0.103704 0.430343 11.00000 0.01706 0.02065 = 0.01625 0.00128 0.00594 -0.00436 N33 3 0.208302 -0.025383 0.491555 11.00000 0.01999 0.02232 = 0.03025 0.00430 0.00443 0.00206 AFIX 93 H33A 2 0.235968 -0.005595 0.517901 11.00000 -1.20000 H33B 2 0.208628 -0.087351 0.463887 11.00000 -1.20000 AFIX 0 N34 3 0.162606 0.130614 0.532909 11.00000 0.01834 0.02694 = 0.02339 0.00418 -0.00371 0.00271 N35 3 0.208727 0.172268 0.562603 11.00000 0.01488 0.02075 = 0.01867 -0.00065 0.00215 0.00259 N36 3 0.162852 0.200211 0.678890 11.00000 0.02275 0.03787 = 0.01069 -0.00490 0.00762 -0.00597 AFIX 93 H36A 2 0.136983 0.156990 0.664297 11.00000 -1.20000 H36B 2 0.162142 0.232793 0.724392 11.00000 -1.20000 AFIX 0 N37 3 0.274325 0.325390 0.597903 11.00000 0.01407 0.02264 = 0.01749 -0.00561 0.00558 0.00351 N38 3 0.326629 0.364424 0.474119 11.00000 0.00564 0.03553 = 0.01008 0.00000 0.00494 0.00196 NI1 6 0.102935 0.242136 0.495166 11.00000 0.01621 0.02239 = 0.01481 -0.00082 0.00240 0.00061 NI2 6 0.269057 0.244291 0.497232 11.00000 0.01475 0.02559 = 0.01341 -0.00136 0.00133 0.00193 MOLE 2 O1 4 0.065141 0.170616 0.790498 11.00000 0.03961 0.02816 = 0.03781 -0.00538 -0.01283 -0.00085 O2 4 0.135569 0.257305 0.846459 11.00000 0.02164 0.04685 = 0.03005 -0.01289 -0.00731 0.00001 O3 4 0.074791 0.361852 0.781500 11.00000 0.02875 0.02680 = 0.03143 0.00244 -0.00058 -0.00656 O4 4 0.052655 0.282501 0.899063 11.00000 0.05043 0.03977 = 0.02631 -0.00465 0.01606 0.00943 CL1 5 0.082041 0.267511 0.830475 11.00000 0.01923 0.02439 = 0.03642 -0.00507 0.00381 -0.00097 MOLE 3 SAME O1 > CL1 O11 4 0.136705 0.245045 1.151847 11.00000 0.02253 0.05363 = 0.03720 0.00186 -0.00719 -0.00429 O12 4 0.054641 0.221592 1.099864 11.00000 0.02929 0.04372 = 0.04171 0.00042 -0.02686 0.00293 O13 4 0.063846 0.328898 1.211343 11.00000 0.04052 0.02606 = 0.05312 -0.00710 0.01197 0.00247 O14 4 0.076886 0.136004 1.216688 11.00000 0.03960 0.02907 = 0.02924 -0.00314 -0.01055 -0.00332 CL11 5 0.081388 0.234139 1.169584 11.00000 0.02445 0.03086 = 0.01660 -0.00405 -0.00193 -0.00011 MOLE 4 SAME O1 > CL1 O21 4 0.121532 -0.205948 0.727374 11.00000 0.03869 0.04455 = 0.02771 0.01614 0.00031 -0.00785 O22 4 0.186191 -0.103591 0.665225 11.00000 0.04336 0.05979 = 0.05802 0.00051 0.02362 0.00082 O23 4 0.110590 -0.151114 0.599971 11.00000 0.09826 0.06313 = 0.01885 -0.00550 0.00855 0.00473 O24 4 0.107450 -0.020651 0.696781 11.00000 0.03387 0.02483 = 0.07243 -0.01026 0.00514 0.00356 CL21 5 0.134528 -0.120687 0.672716 11.00000 0.03770 0.02466 = 0.02639 0.00002 0.01416 0.00001 MOLE 5 SAME O1 > CL1 O31 4 -0.061402 0.403643 0.797685 11.00000 0.06760 0.09478 = 0.10948 -0.03928 0.04503 -0.02182 O32 4 -0.131474 0.293756 0.777651 11.00000 0.08505 0.02570 = 0.07126 -0.00493 -0.01946 -0.01631 O33 4 -0.139873 0.485342 0.802512 11.00000 0.09817 0.03863 = 0.08789 -0.00890 -0.03212 0.01884 O34 4 -0.115729 0.363413 0.899133 11.00000 0.11495 0.04976 = 0.04081 0.00725 0.01982 0.01440 CL31 5 -0.114910 0.385645 0.819436 11.00000 0.05900 0.02867 = 0.03293 -0.00178 0.00077 0.00157 MOLE 6 O51 4 0.231398 0.706932 0.581612 11.00000 0.04340 0.03875 = 0.03367 -0.00566 -0.00408 0.00435 O52 4 0.278767 0.595019 0.377644 11.00000 0.03325 0.07619 = 0.07198 0.02962 0.01795 0.01675 O53 4 0.257522 0.039678 0.740443 11.00000 0.07356 0.07169 = 0.08085 0.00114 -0.00096 -0.02352 O54 4 0.215049 -0.219158 0.400314 11.00000 0.06649 0.04303 = 0.03724 0.00300 0.00694 0.01897 O55 4 0.185221 0.292872 1.006116 11.00000 0.05534 0.10710 = 0.09240 -0.00993 -0.00002 0.03564 HKLF 4 Covalent radii and connectivity table for s93 in Pna2(1) C 0.770 H 0.320 N 0.700 O 0.660 CL 0.990 NI 1.250 C1 - N1 C2 C2 - C1 C3 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 - N6 N5 C13 C13 - C14 N7 C12 C14 - C13 C15 C15 - C16 C14 C16 - C17 C15 C17 - N7 C16 C18 C18 - N8 C19 C17 C19 - C18 C20 C20 - C21 C19 C21 - C20 C22 C22 - N8 C21 C31 - N31 C32 C32 - C33 C31 C33 - C32 C34 C34 - C33 C35 C35 - N31 C34 C36 C36 - N32 C37 C35 C37 - C36 C38 C38 - C39 C37 C39 - C40 C38 C40 - N32 C39 C41 C41 - N34 N33 C40 C42 - N35 N36 C43 C43 - N37 C44 C42 C44 - C45 C43 C45 - C46 C44 C46 - C45 C47 C47 - N37 C46 C48 C48 - N38 C49 C47 C49 - C48 C50 C50 - C49 C51 C51 - C52 C50 C52 - C51 N38 N1 - C5 C1 Ni1 N2 - C10 C6 Ni1 N3 - C11 N4 - C11 N5 Ni1 N5 - C12 N4 Ni2 N6 - C12 N7 - C17 C13 Ni2 N8 - C22 C18 Ni2 N31 - C31 C35 Ni1 N32 - C36 C40 Ni1 N33 - C41 N34 - C41 N35 Ni1 N35 - C42 N34 Ni2 N36 - C42 N37 - C47 C43 Ni2 N38 - C48 C52 Ni2 Ni1 - N2 N32 N31 N1 N4 N34 Ni2 - N7 N37 N38 N5 N8 N35 O1 - Cl1 O2 - Cl1 O3 - Cl1 O4 - Cl1 Cl1 - O2 O1 O3 O4 O11 - Cl11 O12 - Cl11 O13 - Cl11 O14 - Cl11 Cl11 - O12 O13 O14 O11 O21 - Cl21 O22 - Cl21 O23 - Cl21 O24 - Cl21 Cl21 - O22 O21 O24 O23 O31 - Cl31 O32 - Cl31 O33 - Cl31 O34 - Cl31 Cl31 - O32 O33 O34 O31 O51 - no bonds found O52 - no bonds found O53 - no bonds found O54 - no bonds found O55 - no bonds found Floating origin restraints generated h k l Fo^2 Sigma Why rejected 0 9 4 5.67 1.13 observed but should be systematically absent 0 8 1 6.93 1.15 observed but should be systematically absent 0 8 1 9.10 1.14 observed but should be systematically absent 0 7 4 16.88 2.25 observed but should be systematically absent 0 7 4 10.23 2.27 observed but should be systematically absent 0 7 -2 9.25 2.31 observed but should be systematically absent 0 7 2 13.62 2.27 observed but should be systematically absent 0 6 7 14.83 2.28 observed but should be systematically absent 0 6 -7 21.23 3.35 observed but should be systematically absent 0 6 7 14.86 2.29 observed but should be systematically absent 0 6 7 14.48 3.34 observed but should be systematically absent 0 6 7 14.52 3.35 observed but should be systematically absent 0 6 -7 15.14 3.49 observed but should be systematically absent 0 6 -7 12.38 2.25 observed but should be systematically absent 0 6 -1 13.59 2.27 observed but should be systematically absent 0 6 1 8.14 1.16 observed but should be systematically absent 0 6 -1 10.36 2.30 observed but should be systematically absent 0 6 1 12.47 1.13 observed but should be systematically absent 0 5 10 6.88 1.15 observed but should be systematically absent 0 5 10 4.60 1.15 observed but should be systematically absent 0 5 -4 16.34 2.33 observed but should be systematically absent 0 5 4 12.65 2.30 observed but should be systematically absent 0 5 -4 17.39 3.48 observed but should be systematically absent 0 5 -4 15.62 2.23 observed but should be systematically absent 0 5 -4 13.49 2.25 observed but should be systematically absent 0 5 4 16.75 2.23 observed but should be systematically absent 0 5 4 13.38 2.23 observed but should be systematically absent 0 5 4 13.78 2.30 observed but should be systematically absent 0 5 -4 23.40 2.23 observed but should be systematically absent 0 4 -11 5.78 1.16 observed but should be systematically absent 0 4 7 8.06 1.15 observed but should be systematically absent 0 4 -7 5.60 1.12 observed but should be systematically absent 0 4 7 6.66 1.11 observed but should be systematically absent 0 4 7 6.97 1.16 observed but should be systematically absent 0 4 7 9.19 1.15 observed but should be systematically absent 0 4 -7 5.63 1.13 observed but should be systematically absent 0 4 -7 5.58 1.12 observed but should be systematically absent 0 4 7 6.67 1.11 observed but should be systematically absent 0 4 -7 5.84 1.17 observed but should be systematically absent 0 4 -5 5.90 1.18 observed but should be systematically absent 0 4 5 4.65 1.16 observed but should be systematically absent 0 4 5 5.81 1.16 observed but should be systematically absent 0 4 -5 4.45 1.11 observed but should be systematically absent 0 4 5 5.56 1.11 observed but should be systematically absent 0 4 -5 4.49 1.12 observed but should be systematically absent 0 4 5 4.61 1.15 observed but should be systematically absent 0 3 14 4.76 1.19 observed but should be systematically absent 0 3 -2 4.61 1.15 observed but should be systematically absent 0 3 -2 4.66 1.16 observed but should be systematically absent 0 3 2 4.45 1.11 observed but should be systematically absent ** etc. ** 92588 Reflections read, of which 4841 rejected -33 =< h =< 33, -15 =< k =< 15, -22 =< l =< 22, Max. 2-theta = 54.96 169 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Su of mean(Fo^2) 2 3 -17 9.09 0.81 6 10.23 3 3 -17 8.83 1.14 6 12.60 1 8 -17 11.36 1.48 4 10.99 4 8 -17 9.37 1.37 5 10.27 9 8 -16 15.65 1.49 5 19.64 16 4 -12 11.50 0.93 8 4.76 14 5 -11 52.71 1.47 9 13.66 21 9 -10 4.91 1.39 5 9.18 18 4 -9 16.89 0.95 9 12.32 11 9 -9 8.66 0.74 8 6.83 17 10 -9 8.43 1.34 5 10.39 20 3 -8 23.02 0.90 9 13.75 19 6 -8 4.01 0.75 8 4.00 9 10 -8 2.55 0.81 6 4.54 22 9 -6 12.32 1.26 6 15.09 6 11 -6 19.05 1.50 5 10.81 23 1 -5 4.75 0.90 8 7.41 9 13 -5 15.04 2.40 3 14.95 5 7 -4 11.72 0.39 14 2.46 19 11 -4 18.51 1.96 4 16.09 5 7 -3 0.33 0.41 11 2.13 19 11 -3 41.18 2.34 4 35.59 7 7 -2 4.55 0.37 13 2.77 20 6 0 4.42 0.73 8 8.05 22 10 0 8.07 1.41 5 8.25 8 15 0 5.59 1.29 4 6.54 19 7 1 6.35 0.82 9 7.79 2 11 1 21.77 1.07 6 11.70 3 11 1 20.39 1.33 5 15.09 0 8 2 38.00 1.02 5 7.86 14 9 2 11.97 0.84 6 25.86 0 9 3 167.75 3.19 5 20.62 16 12 4 18.31 1.02 5 21.85 8 6 5 9.14 0.43 11 4.41 11 9 7 11.89 1.15 5 12.46 12 13 7 15.89 1.42 5 14.26 5 5 8 1.10 0.37 12 1.89 8 9 8 16.82 0.95 9 13.29 1 10 10 15.08 1.12 5 13.45 7 12 10 36.12 1.72 4 30.77 8 12 10 9.65 0.89 5 10.56 17 2 11 12.20 1.02 7 18.26 20 9 11 9.90 1.71 5 9.80 6 8 12 16.55 1.22 5 6.12 0 7 13 21.73 2.11 2 11.51 16 0 14 13.03 1.43 4 10.35 14 0 15 12.44 1.89 3 14.61 19 5 15 11.45 1.73 4 15.78 6 4 16 14.86 1.29 4 20.96 18 4 16 18.69 1.87 6 9.78 ** etc. ** 51 Inconsistent equivalents 12190 Unique reflections, of which 0 suppressed R(int) = 0.1260 R(sigma) = 0.0998 Friedel opposites not merged Maximum memory for data reduction = 7430 / 121561 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 176.00 176.00 H 184.00 144.00 N 64.00 64.00 O 84.00 84.00 CL 16.00 16.00 NI 8.00 8.00 Least-squares cycle 1 Maximum vector length = 511 Memory required = 9464 / 1139194 wR2 = 0.1906 before cycle 1 for 12190 data and 786 / 786 parameters Disagreeable restraints before cycle 1 Observed Target Error Sigma Restraint 0.0700 0.0200 SAME/SADI O33 Cl31 O23 Cl21 Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 6. 60. 0. 0. 0. 260. 492. 0. 0. rms sigma 0.000 0.010 0.040 0.033 0.000 0.000 0.000 0.010 0.026 0.000 0.000 rms deviation 0.000 0.004 0.018 0.037 0.000 0.000 0.000 0.005 0.012 0.000 0.000 GooF = S = 1.070; Restrained GooF = 1.044 for 823 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0623 * P )^2 + 30.22 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.07180 0.00013 0.023 OSF 2 1.41792 0.00535 -0.004 FVAR 2 3 0.51648 0.02909 -0.001 BASF 1 Mean shift/su = 0.004 Maximum = 0.023 for OSF Max. shift = 0.000 A for C19 Max. dU = 0.000 for O34 Least-squares cycle 2 Maximum vector length = 511 Memory required = 9464 / 1139194 wR2 = 0.1905 before cycle 2 for 12190 data and 786 / 786 parameters Disagreeable restraints before cycle 2 Observed Target Error Sigma Restraint 0.0700 0.0200 SAME/SADI O33 Cl31 O23 Cl21 Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 6. 60. 0. 0. 0. 260. 492. 0. 0. rms sigma 0.000 0.010 0.040 0.033 0.000 0.000 0.000 0.010 0.026 0.000 0.000 rms deviation 0.000 0.004 0.018 0.037 0.000 0.000 0.000 0.005 0.012 0.000 0.000 GooF = S = 1.070; Restrained GooF = 1.044 for 823 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0623 * P )^2 + 30.22 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.07180 0.00013 0.011 OSF 2 1.41790 0.00535 -0.003 FVAR 2 3 0.51647 0.02909 0.000 BASF 1 Mean shift/su = 0.003 Maximum = 0.012 for z C35 Max. shift = 0.000 A for C5 Max. dU = 0.000 for O34 Least-squares cycle 3 Maximum vector length = 511 Memory required = 9464 / 1139194 wR2 = 0.1905 before cycle 3 for 12190 data and 786 / 786 parameters Disagreeable restraints before cycle 3 Observed Target Error Sigma Restraint 0.0700 0.0200 SAME/SADI O33 Cl31 O23 Cl21 Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 6. 60. 0. 0. 0. 260. 492. 0. 0. rms sigma 0.000 0.010 0.040 0.033 0.000 0.000 0.000 0.010 0.026 0.000 0.000 rms deviation 0.000 0.004 0.018 0.037 0.000 0.000 0.000 0.005 0.012 0.000 0.000 GooF = S = 1.070; Restrained GooF = 1.044 for 823 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0623 * P )^2 + 30.22 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.07180 0.00013 0.001 OSF 2 1.41789 0.00535 -0.002 FVAR 2 3 0.51647 0.02909 0.000 BASF 1 Mean shift/su = 0.002 Maximum = 0.009 for z C35 Max. shift = 0.000 A for C39 Max. dU = 0.000 for O11 Least-squares cycle 4 Maximum vector length = 511 Memory required = 9464 / 1139194 wR2 = 0.1905 before cycle 4 for 12190 data and 786 / 786 parameters Disagreeable restraints before cycle 4 Observed Target Error Sigma Restraint 0.0700 0.0200 SAME/SADI O33 Cl31 O23 Cl21 Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 6. 60. 0. 0. 0. 260. 492. 0. 0. rms sigma 0.000 0.010 0.040 0.033 0.000 0.000 0.000 0.010 0.026 0.000 0.000 rms deviation 0.000 0.004 0.018 0.037 0.000 0.000 0.000 0.005 0.012 0.000 0.000 GooF = S = 1.069; Restrained GooF = 1.044 for 823 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0623 * P )^2 + 30.22 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.07180 0.00013 0.000 OSF 2 1.41788 0.00535 -0.001 FVAR 2 3 0.51647 0.02909 0.000 BASF 1 Mean shift/su = 0.001 Maximum = 0.006 for z C39 Max. shift = 0.000 A for C39 Max. dU = 0.000 for O11 Least-squares cycle 5 Maximum vector length = 511 Memory required = 9464 / 1139194 wR2 = 0.1905 before cycle 5 for 12190 data and 786 / 786 parameters Disagreeable restraints before cycle 5 Observed Target Error Sigma Restraint 0.0700 0.0200 SAME/SADI O33 Cl31 O23 Cl21 Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 6. 60. 0. 0. 0. 260. 492. 0. 0. rms sigma 0.000 0.010 0.040 0.033 0.000 0.000 0.000 0.010 0.026 0.000 0.000 rms deviation 0.000 0.004 0.018 0.037 0.000 0.000 0.000 0.005 0.012 0.000 0.000 GooF = S = 1.069; Restrained GooF = 1.044 for 823 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0623 * P )^2 + 30.22 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.07180 0.00013 -0.001 OSF 2 1.41788 0.00535 -0.001 FVAR 2 3 0.51648 0.02909 0.000 BASF 1 Mean shift/su = 0.001 Maximum = 0.005 for z C39 Max. shift = 0.000 A for C39 Max. dU = 0.000 for O11 Least-squares cycle 6 Maximum vector length = 511 Memory required = 9464 / 1139194 wR2 = 0.1905 before cycle 6 for 12190 data and 786 / 786 parameters Disagreeable restraints before cycle 6 Observed Target Error Sigma Restraint 0.0700 0.0200 SAME/SADI O33 Cl31 O23 Cl21 Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 6. 60. 0. 0. 0. 260. 492. 0. 0. rms sigma 0.000 0.010 0.040 0.033 0.000 0.000 0.000 0.010 0.026 0.000 0.000 rms deviation 0.000 0.004 0.018 0.037 0.000 0.000 0.000 0.005 0.012 0.000 0.000 GooF = S = 1.069; Restrained GooF = 1.044 for 823 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0623 * P )^2 + 30.22 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.07180 0.00013 0.000 OSF 2 1.41788 0.00535 -0.001 FVAR 2 3 0.51648 0.02909 0.000 BASF 1 Mean shift/su = 0.001 Maximum = 0.004 for z C39 Max. shift = 0.000 A for C39 Max. dU = 0.000 for O11 Largest correlation matrix elements -0.690 U33 O11 / U33 O2 -0.591 x O11 / x O2 -0.555 x C34 / x C4 0.655 z O11 / z O2 0.590 y O12 / y O4 0.554 z C48 / z C18 0.654 U13 O11 / U13 O2 0.586 z C52 / z C22 0.554 U12 O12 / U12 O4 -0.646 U11 Cl11 / U11 Cl1 -0.575 U23 O12 / U23 O4 0.549 z C43 / z C13 0.639 z C34 / z C4 0.574 z C46 / z C16 -0.549 U11 O11 / U11 O2 -0.632 U22 O11 / U22 O2 -0.570 U33 N33 / U33 N3 0.548 U13 O12 / U13 O4 -0.610 x Cl11 / x Cl1 0.561 z N33 / z N3 0.547 z C40 / z C10 0.608 U13 Cl11 / U13 Cl1 -0.556 x C42 / x C12 0.547 z C47 / z C17 Idealized hydrogen atom generation before cycle 7 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1 0.0452 0.0267 0.5598 43 0.950 0.000 C1 N1 C2 H2 -0.0272 -0.0128 0.6326 43 0.950 0.000 C2 C1 C3 H3 -0.0636 0.1380 0.7054 43 0.950 0.000 C3 C4 C2 H4 -0.0284 0.3178 0.6919 43 0.950 0.000 C4 C3 C5 H7 0.0034 0.4919 0.6620 43 0.950 0.000 C7 C8 C6 H8 0.0508 0.6475 0.6348 43 0.950 0.000 C8 C7 C9 H9 0.1282 0.6389 0.5634 43 0.950 0.000 C9 C10 C8 H14 0.2394 0.1841 0.2234 43 0.950 0.000 C14 C13 C15 H15 0.3125 0.0666 0.1994 43 0.950 0.000 C15 C16 C14 H16 0.3585 0.0085 0.3097 43 0.950 0.000 C16 C17 C15 H19 0.4001 -0.0337 0.4217 43 0.950 0.000 C19 C18 C20 H20 0.4349 -0.0731 0.5413 43 0.950 0.000 C20 C21 C19 H21 0.4025 0.0136 0.6503 43 0.950 0.000 C21 C20 C22 H22 0.3341 0.1470 0.6319 43 0.950 0.000 C22 N8 C21 H31 0.0402 0.4531 0.4366 43 0.950 0.000 C31 N31 C32 H32 -0.0239 0.4903 0.3452 43 0.950 0.000 C32 C33 C31 H33 -0.0625 0.3421 0.2835 43 0.950 0.000 C33 C32 C34 H34 -0.0348 0.1602 0.3053 43 0.950 0.000 C34 C33 C35 H37 0.0024 -0.0092 0.3309 43 0.950 0.000 C37 C36 C38 H38 0.0486 -0.1738 0.3639 43 0.950 0.000 C38 C39 C37 H39 0.1255 -0.1563 0.4361 43 0.950 0.000 C39 C40 C38 H44 0.2375 0.3015 0.7750 43 0.950 0.000 C44 C45 C43 H45 0.3013 0.4365 0.7864 43 0.950 0.000 C45 C46 C44 H46 0.3501 0.4974 0.6858 43 0.950 0.000 C46 C45 C47 H49 0.3847 0.5495 0.5748 43 0.950 0.000 C49 C48 C50 H50 0.4282 0.5841 0.4587 43 0.950 0.000 C50 C49 C51 H51 0.4028 0.4768 0.3492 43 0.950 0.000 C51 C52 C50 H52 0.3411 0.3421 0.3611 43 0.950 0.000 C52 C51 N38 H3A 0.2354 0.4959 0.4732 93 0.880 0.000 N3 C11 N4 H3B 0.2054 0.5725 0.5276 93 0.880 0.000 N3 C11 N4 H6A 0.1404 0.3261 0.3287 93 0.880 0.000 N6 C12 N5 H6B 0.1673 0.2548 0.2676 93 0.880 0.000 N6 C12 N5 H33A 0.2360 -0.0056 0.5179 93 0.880 0.000 N33 C41 N34 H33B 0.2086 -0.0873 0.4639 93 0.880 0.000 N33 C41 N34 H36A 0.1370 0.1570 0.6643 93 0.880 0.000 N36 C42 N35 H36B 0.1621 0.2328 0.7244 93 0.880 0.000 N36 C42 N35 s93 in Pna2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.02778 0.08704 0.58466 1.00000 0.03337 0.02844 0.01813 0.00115 0.00286 -0.00253 0.02665 0.01733 0.00039 0.00083 0.00058 0.00000 0.00487 0.00418 0.00469 0.00354 0.00352 0.00367 0.00199 H1 0.04516 0.02675 0.55976 1.00000 0.03197 0.00000 0.00000 C2 -0.01363 0.06131 0.62966 1.00000 0.02632 0.03150 0.02082 -0.00806 0.01001 -0.00207 0.02621 0.01698 0.00037 0.00082 0.00058 0.00000 0.00462 0.00441 0.00467 0.00361 0.00355 0.00354 0.00204 H2 -0.02717 -0.01281 0.63260 1.00000 0.03145 0.00000 0.00000 C3 -0.03523 0.15060 0.67154 1.00000 0.03641 0.04748 0.01115 -0.00791 0.00336 -0.00704 0.03168 0.01654 0.00039 0.00087 0.00058 0.00000 0.00505 0.00515 0.00417 0.00403 0.00392 0.00395 0.00209 H3 -0.06358 0.13803 0.70537 1.00000 0.03802 0.00000 0.00000 C4 -0.01474 0.25680 0.66293 1.00000 0.02269 0.03888 0.01322 -0.00352 0.00145 0.00107 0.02493 0.01760 0.00040 0.00080 0.00060 0.00000 0.00452 0.00470 0.00429 0.00367 0.00322 0.00344 0.00207 H4 -0.02836 0.31781 0.69186 1.00000 0.02991 0.00000 0.00000 C5 0.02560 0.27426 0.61217 1.00000 0.00404 0.03402 0.02487 -0.00274 -0.00518 -0.00181 0.02098 0.01524 0.00032 0.00083 0.00057 0.00000 0.00341 0.00377 0.00439 0.00358 0.00288 0.00303 0.00170 C6 0.05076 0.38435 0.60313 1.00000 0.01930 0.02947 0.00615 0.00209 0.00004 0.00495 0.01831 0.01587 0.00033 0.00078 0.00048 0.00000 0.00383 0.00361 0.00380 0.00318 0.00296 0.00325 0.00161 C7 0.03405 0.48654 0.63190 1.00000 0.02056 0.03143 0.00279 -0.00525 0.00096 -0.00037 0.01826 0.01444 0.00035 0.00073 0.00046 0.00000 0.00425 0.00397 0.00376 0.00320 0.00304 0.00322 0.00172 H7 0.00339 0.49195 0.66197 1.00000 0.02191 0.00000 0.00000 C8 0.06235 0.57683 0.61601 1.00000 0.03215 0.02575 0.01835 -0.00436 0.00046 0.00543 0.02541 0.01695 0.00037 0.00080 0.00057 0.00000 0.00471 0.00414 0.00464 0.00358 0.00352 0.00343 0.00203 H8 0.05079 0.64750 0.63479 1.00000 0.03050 0.00000 0.00000 C9 0.10801 0.57371 0.57337 1.00000 0.02809 0.01820 0.00568 0.00151 0.00206 -0.00018 0.01732 0.01553 0.00037 0.00069 0.00048 0.00000 0.00437 0.00363 0.00371 0.00292 0.00315 0.00321 0.00169 H9 0.12816 0.63893 0.56340 1.00000 0.02079 0.00000 0.00000 C10 0.12169 0.46926 0.54685 1.00000 0.01616 0.01943 0.01076 0.00014 0.00197 0.00468 0.01545 0.01513 0.00033 0.00070 0.00051 0.00000 0.00375 0.00348 0.00388 0.00298 0.00281 0.00286 0.00162 C11 0.16762 0.44289 0.49642 1.00000 0.01850 0.01890 0.01448 0.00765 0.00266 0.00487 0.01729 0.01548 0.00030 0.00060 0.00058 0.00000 0.00353 0.00332 0.00394 0.00351 0.00345 0.00256 0.00151 C12 0.20578 0.27090 0.35931 1.00000 0.02587 0.02239 0.01083 0.00505 0.00158 0.00557 0.01970 0.01690 0.00039 0.00077 0.00051 0.00000 0.00445 0.00410 0.00363 0.00330 0.00304 0.00348 0.00177 C13 0.24965 0.19770 0.33543 1.00000 0.01359 0.02065 0.02008 -0.00054 0.00041 0.00117 0.01811 0.01506 0.00032 0.00069 0.00054 0.00000 0.00367 0.00401 0.00378 0.00334 0.00305 0.00302 0.00167 C14 0.26087 0.16131 0.26509 1.00000 0.02996 0.01799 0.01788 0.00161 0.00068 -0.00354 0.02194 0.01619 0.00037 0.00073 0.00055 0.00000 0.00462 0.00411 0.00399 0.00334 0.00347 0.00335 0.00181 H14 0.23943 0.18406 0.22342 1.00000 0.02633 0.00000 0.00000 C15 0.30323 0.09042 0.24982 1.00000 0.02263 0.02516 0.02712 0.00915 0.00745 0.00338 0.02497 0.01819 0.00036 0.00076 0.00061 0.00000 0.00443 0.00435 0.00432 0.00368 0.00337 0.00333 0.00194 H15 0.31250 0.06656 0.19944 1.00000 0.02996 0.00000 0.00000 C16 0.33015 0.05874 0.31543 1.00000 0.02288 0.03530 0.02508 -0.00639 0.00500 -0.00056 0.02775 0.01638 0.00037 0.00078 0.00059 0.00000 0.00434 0.00486 0.00430 0.00393 0.00363 0.00355 0.00194 H16 0.35849 0.00850 0.30967 1.00000 0.03330 0.00000 0.00000 C17 0.31823 0.09575 0.38839 1.00000 0.02256 0.02138 0.01774 0.00103 0.00232 0.00133 0.02056 0.01619 0.00035 0.00075 0.00053 0.00000 0.00414 0.00406 0.00364 0.00315 0.00319 0.00316 0.00173 C18 0.34566 0.07237 0.46174 1.00000 0.01935 0.02306 0.01790 -0.00375 -0.00016 0.00377 0.02010 0.01594 0.00035 0.00077 0.00055 0.00000 0.00405 0.00426 0.00368 0.00331 0.00321 0.00308 0.00177 C19 0.38631 0.00067 0.46664 1.00000 0.02082 0.03949 0.03216 -0.00220 0.00465 0.01312 0.03083 0.01858 0.00036 0.00088 0.00063 0.00000 0.00444 0.00516 0.00474 0.00403 0.00358 0.00370 0.00216 H19 0.40008 -0.03368 0.42167 1.00000 0.03699 0.00000 0.00000 C20 0.40704 -0.02126 0.53709 1.00000 0.02285 0.03868 0.03576 0.00794 -0.00161 0.00498 0.03243 0.01893 0.00040 0.00093 0.00062 0.00000 0.00494 0.00529 0.00526 0.00416 0.00386 0.00390 0.00220 H20 0.43490 -0.07308 0.54132 1.00000 0.03891 0.00000 0.00000 C21 0.38886 0.02895 0.60053 1.00000 0.01080 0.03439 0.04331 -0.00582 -0.00787 0.00620 0.02950 0.01740 0.00035 0.00082 0.00068 0.00000 0.00420 0.00491 0.00523 0.00426 0.00389 0.00350 0.00208 H21 0.40246 0.01360 0.65029 1.00000 0.03540 0.00000 0.00000 C22 0.34733 0.10777 0.58843 1.00000 0.01929 0.03106 0.02750 -0.00400 0.00134 0.00798 0.02595 0.01747 0.00035 0.00084 0.00064 0.00000 0.00440 0.00486 0.00455 0.00403 0.00363 0.00361 0.00199 H22 0.33410 0.14699 0.63186 1.00000 0.03114 0.00000 0.00000 C31 0.02678 0.39299 0.40667 1.00000 0.01278 0.02215 0.02715 -0.00266 0.00351 -0.00030 0.02069 0.01609 0.00033 0.00077 0.00058 0.00000 0.00390 0.00389 0.00477 0.00356 0.00314 0.00315 0.00180 H31 0.04023 0.45315 0.43660 1.00000 0.02483 0.00000 0.00000 C32 -0.01272 0.41544 0.35456 1.00000 0.02000 0.02845 0.01237 -0.00060 0.00866 0.01192 0.02027 0.01627 0.00034 0.00074 0.00052 0.00000 0.00405 0.00403 0.00411 0.00327 0.00307 0.00326 0.00178 H32 -0.02390 0.49027 0.34519 1.00000 0.02433 0.00000 0.00000 C33 -0.03455 0.32861 0.31794 1.00000 0.01594 0.03801 0.01991 0.00248 -0.00851 0.00137 0.02462 0.01577 0.00033 0.00077 0.00057 0.00000 0.00409 0.00443 0.00458 0.00376 0.00352 0.00337 0.00190 H33 -0.06249 0.34207 0.28352 1.00000 0.02954 0.00000 0.00000 C34 -0.01778 0.22211 0.32877 1.00000 0.01825 0.03701 0.01974 0.00090 -0.00346 -0.00815 0.02500 0.01741 0.00037 0.00087 0.00062 0.00000 0.00427 0.00387 0.00464 0.00401 0.00338 0.00365 0.00187 H34 -0.03482 0.16016 0.30533 1.00000 0.03000 0.00000 0.00000 C35 0.02523 0.20687 0.37539 1.00000 0.02588 0.02267 0.00610 0.00103 -0.00049 -0.00243 0.01822 0.01504 0.00035 0.00075 0.00049 0.00000 0.00427 0.00352 0.00366 0.00316 0.00293 0.00329 0.00166 C36 0.05060 0.09804 0.38913 1.00000 0.01778 0.02023 0.02683 -0.00650 0.00033 -0.00065 0.02161 0.01581 0.00035 0.00077 0.00056 0.00000 0.00389 0.00354 0.00487 0.00341 0.00328 0.00311 0.00180 C37 0.03279 -0.00507 0.36170 1.00000 0.01984 0.02756 0.04091 -0.00411 -0.00134 -0.00045 0.02944 0.01716 0.00038 0.00077 0.00063 0.00000 0.00450 0.00409 0.00585 0.00398 0.00387 0.00346 0.00214 H37 0.00243 -0.00918 0.33089 1.00000 0.03532 0.00000 0.00000 C38 0.06041 -0.10210 0.38036 1.00000 0.01505 0.02100 0.02425 -0.00311 0.00309 -0.00097 0.02010 0.01579 0.00032 0.00077 0.00055 0.00000 0.00387 0.00382 0.00475 0.00345 0.00323 0.00312 0.00183 H38 0.04862 -0.17380 0.36386 1.00000 0.02412 0.00000 0.00000 C39 0.10545 -0.09183 0.42350 1.00000 0.01214 0.02814 0.03449 0.00171 0.00183 0.00111 0.02492 0.01620 0.00035 0.00078 0.00056 0.00000 0.00394 0.00394 0.00539 0.00376 0.00349 0.00330 0.00194 H39 0.12546 -0.15630 0.43606 1.00000 0.02991 0.00000 0.00000 C40 0.12053 0.01226 0.44756 1.00000 0.01044 0.02320 0.02231 0.00061 0.00762 0.00433 0.01865 0.01621 0.00032 0.00073 0.00056 0.00000 0.00348 0.00368 0.00451 0.00323 0.00290 0.00286 0.00169 C41 0.16616 0.03813 0.49354 1.00000 0.01590 0.02506 0.01176 0.00074 0.01047 0.00425 0.01757 0.01530 0.00030 0.00063 0.00055 0.00000 0.00338 0.00352 0.00394 0.00352 0.00330 0.00264 0.00150 C42 0.20363 0.21652 0.63149 1.00000 0.01422 0.02688 0.01431 -0.00052 0.00555 0.00784 0.01847 0.01648 0.00035 0.00081 0.00051 0.00000 0.00395 0.00415 0.00389 0.00345 0.00290 0.00334 0.00166 C43 0.24529 0.29141 0.65530 1.00000 0.01795 0.03106 0.01324 -0.00186 0.00070 0.00551 0.02075 0.01568 0.00034 0.00079 0.00051 0.00000 0.00393 0.00456 0.00369 0.00323 0.00296 0.00312 0.00173 C44 0.25588 0.32861 0.73137 1.00000 0.02476 0.03169 0.01830 0.00162 -0.00190 -0.00046 0.02492 0.01602 0.00037 0.00079 0.00057 0.00000 0.00456 0.00472 0.00404 0.00373 0.00353 0.00347 0.00192 H44 0.23752 0.30152 0.77501 1.00000 0.02990 0.00000 0.00000 C45 0.29450 0.40625 0.73679 1.00000 0.02599 0.03454 0.01304 -0.00970 -0.00655 0.00122 0.02452 0.01528 0.00036 0.00079 0.00055 0.00000 0.00459 0.00476 0.00388 0.00356 0.00336 0.00356 0.00193 H45 0.30134 0.43654 0.78640 1.00000 0.02942 0.00000 0.00000 C46 0.32341 0.44333 0.67885 1.00000 0.03617 0.03397 0.01169 -0.00352 -0.00609 -0.00245 0.02728 0.01668 0.00039 0.00080 0.00057 0.00000 0.00506 0.00489 0.00385 0.00366 0.00360 0.00375 0.00197 H46 0.35007 0.49745 0.68577 1.00000 0.03273 0.00000 0.00000 C47 0.31162 0.39635 0.60604 1.00000 0.01762 0.03221 0.01474 -0.01107 0.00108 0.00208 0.02152 0.01530 0.00034 0.00079 0.00053 0.00000 0.00387 0.00438 0.00360 0.00334 0.00307 0.00322 0.00172 C48 0.34011 0.42602 0.53547 1.00000 0.00677 0.02385 0.02113 -0.00223 -0.00118 0.00838 0.01725 0.01578 0.00033 0.00073 0.00054 0.00000 0.00347 0.00412 0.00375 0.00327 0.00296 0.00274 0.00161 C49 0.37638 0.50649 0.53031 1.00000 0.02274 0.02379 0.01893 -0.00552 0.00068 0.00192 0.02182 0.01605 0.00034 0.00077 0.00054 0.00000 0.00448 0.00426 0.00409 0.00339 0.00327 0.00319 0.00184 H49 0.38467 0.54946 0.57476 1.00000 0.02619 0.00000 0.00000 C50 0.40193 0.52845 0.46212 1.00000 0.02779 0.02707 0.02296 0.00117 0.00574 -0.00194 0.02594 0.01762 0.00039 0.00080 0.00056 0.00000 0.00481 0.00458 0.00450 0.00351 0.00364 0.00363 0.00197 H50 0.42823 0.58408 0.45872 1.00000 0.03113 0.00000 0.00000 C51 0.38695 0.46399 0.39783 1.00000 0.03917 0.02921 0.00982 0.00698 -0.00006 -0.00057 0.02607 0.01728 0.00040 0.00079 0.00055 0.00000 0.00529 0.00459 0.00384 0.00338 0.00371 0.00376 0.00198 H51 0.40279 0.47681 0.34922 1.00000 0.03128 0.00000 0.00000 C52 0.35064 0.38512 0.40495 1.00000 0.02215 0.03748 0.01776 -0.00143 0.00534 0.00249 0.02579 0.01800 0.00035 0.00086 0.00059 0.00000 0.00466 0.00516 0.00427 0.00401 0.00339 0.00352 0.00199 H52 0.34112 0.34209 0.36107 1.00000 0.03095 0.00000 0.00000 N1 0.04582 0.19046 0.57286 1.00000 0.01646 0.02034 0.01688 0.00481 -0.00124 0.00142 0.01790 0.01273 0.00028 0.00059 0.00043 0.00000 0.00330 0.00324 0.00330 0.00262 0.00263 0.00257 0.00139 N2 0.09395 0.37857 0.56106 1.00000 0.01215 0.02098 0.01534 0.00245 0.00042 -0.00021 0.01615 0.01225 0.00027 0.00059 0.00040 0.00000 0.00316 0.00299 0.00351 0.00254 0.00243 0.00244 0.00134 N3 0.20709 0.51116 0.49941 1.00000 0.02191 0.03230 0.01480 -0.00705 0.00093 -0.00064 0.02300 0.01287 0.00027 0.00058 0.00051 0.00000 0.00351 0.00371 0.00377 0.00379 0.00374 0.00274 0.00153 H3A 0.23542 0.49589 0.47322 1.00000 0.02760 0.00000 0.00000 H3B 0.20539 0.57250 0.52761 1.00000 0.02760 0.00000 0.00000 N4 0.16275 0.35075 0.45916 1.00000 0.00507 0.02274 0.01486 0.00331 0.00366 0.00435 0.01422 0.01198 0.00024 0.00057 0.00040 0.00000 0.00271 0.00319 0.00343 0.00249 0.00242 0.00226 0.00132 N5 0.20987 0.31140 0.42785 1.00000 0.01768 0.02858 0.00614 -0.00072 0.00421 0.00482 0.01746 0.01244 0.00027 0.00060 0.00039 0.00000 0.00318 0.00373 0.00301 0.00253 0.00241 0.00268 0.00140 N6 0.16710 0.28549 0.31375 1.00000 0.01431 0.03229 0.03411 -0.00482 -0.00284 0.00952 0.02691 0.01388 0.00028 0.00066 0.00050 0.00000 0.00353 0.00410 0.00477 0.00373 0.00325 0.00316 0.00176 H6A 0.14045 0.32613 0.32870 1.00000 0.03229 0.00000 0.00000 H6B 0.16728 0.25484 0.26761 1.00000 0.03229 0.00000 0.00000 N7 0.27799 0.16639 0.39955 1.00000 0.02084 0.02659 0.01630 0.00069 0.00391 -0.00105 0.02125 0.01326 0.00029 0.00064 0.00044 0.00000 0.00368 0.00375 0.00316 0.00274 0.00265 0.00268 0.00146 N8 0.32767 0.12756 0.52391 1.00000 0.02181 0.02282 0.02300 -0.00314 0.00598 0.00656 0.02255 0.01343 0.00029 0.00062 0.00043 0.00000 0.00353 0.00336 0.00370 0.00279 0.00277 0.00281 0.00155 N31 0.04656 0.29083 0.41641 1.00000 0.01322 0.02028 0.01666 -0.00293 0.00697 0.00038 0.01672 0.01284 0.00028 0.00059 0.00043 0.00000 0.00314 0.00321 0.00320 0.00259 0.00248 0.00254 0.00134 N32 0.09361 0.10371 0.43034 1.00000 0.01715 0.02064 0.01621 0.00131 0.00593 -0.00436 0.01800 0.01225 0.00028 0.00057 0.00041 0.00000 0.00330 0.00299 0.00366 0.00257 0.00250 0.00253 0.00139 N33 0.20830 -0.02538 0.49154 1.00000 0.01994 0.02232 0.03021 0.00424 0.00447 0.00204 0.02416 0.01414 0.00027 0.00056 0.00053 0.00000 0.00350 0.00342 0.00474 0.00392 0.00384 0.00264 0.00166 H33A 0.23597 -0.00560 0.51788 1.00000 0.02899 0.00000 0.00000 H33B 0.20862 -0.08735 0.46387 1.00000 0.02899 0.00000 0.00000 N34 0.16261 0.13062 0.53290 1.00000 0.01837 0.02693 0.02344 0.00419 -0.00372 0.00272 0.02291 0.01326 0.00029 0.00063 0.00044 0.00000 0.00321 0.00351 0.00401 0.00280 0.00275 0.00267 0.00150 N35 0.20873 0.17226 0.56260 1.00000 0.01490 0.02073 0.01873 -0.00062 0.00214 0.00257 0.01812 0.01267 0.00027 0.00059 0.00043 0.00000 0.00310 0.00344 0.00340 0.00255 0.00253 0.00254 0.00138 N36 0.16285 0.20021 0.67889 1.00000 0.02281 0.03788 0.01054 -0.00492 0.00759 -0.00596 0.02375 0.01362 0.00029 0.00066 0.00044 0.00000 0.00380 0.00454 0.00370 0.00357 0.00307 0.00335 0.00169 H36A 0.13698 0.15700 0.66429 1.00000 0.02850 0.00000 0.00000 H36B 0.16214 0.23278 0.72440 1.00000 0.02850 0.00000 0.00000 N37 0.27433 0.32539 0.59791 1.00000 0.01410 0.02264 0.01745 -0.00560 0.00557 0.00350 0.01806 0.01284 0.00027 0.00060 0.00044 0.00000 0.00330 0.00346 0.00315 0.00269 0.00259 0.00248 0.00139 N38 0.32663 0.36443 0.47413 1.00000 0.00563 0.03556 0.01001 0.00002 0.00495 0.00195 0.01707 0.01225 0.00025 0.00063 0.00038 0.00000 0.00286 0.00347 0.00331 0.00258 0.00228 0.00255 0.00140 Ni1 0.10293 0.24214 0.49517 1.00000 0.01621 0.02239 0.01481 -0.00082 0.00242 0.00061 0.01781 0.00221 0.00003 0.00010 0.00010 0.00000 0.00037 0.00045 0.00039 0.00044 0.00064 0.00047 0.00019 Ni2 0.26906 0.24429 0.49723 1.00000 0.01475 0.02560 0.01342 -0.00137 0.00134 0.00193 0.01792 0.00222 0.00003 0.00010 0.00010 0.00000 0.00037 0.00045 0.00037 0.00041 0.00064 0.00048 0.00019 O1 0.06515 0.17061 0.79050 1.00000 0.03969 0.02815 0.03782 -0.00534 -0.01284 -0.00092 0.03522 0.00985 0.00027 0.00054 0.00042 0.00000 0.00428 0.00362 0.00435 0.00325 0.00326 0.00298 0.00181 O2 0.13557 0.25730 0.84646 1.00000 0.02166 0.04677 0.02989 -0.01286 -0.00730 0.00000 0.03277 0.01097 0.00024 0.00055 0.00046 0.00000 0.00334 0.00487 0.00475 0.00320 0.00324 0.00285 0.00194 O3 0.07480 0.36184 0.78150 1.00000 0.02869 0.02685 0.03142 0.00249 -0.00065 -0.00663 0.02898 0.01175 0.00026 0.00051 0.00038 0.00000 0.00366 0.00355 0.00400 0.00300 0.00298 0.00289 0.00159 O4 0.05266 0.28248 0.89906 1.00000 0.05044 0.03985 0.02617 -0.00457 0.01603 0.00945 0.03882 0.01386 0.00030 0.00068 0.00037 0.00000 0.00467 0.00411 0.00399 0.00338 0.00357 0.00394 0.00184 Cl1 0.08204 0.26751 0.83047 1.00000 0.01922 0.02439 0.03643 -0.00505 0.00382 -0.00099 0.02668 0.00429 0.00010 0.00019 0.00015 0.00000 0.00122 0.00107 0.00139 0.00112 0.00108 0.00094 0.00054 O11 0.13671 0.24504 1.15185 1.00000 0.02250 0.05369 0.03740 0.00186 -0.00719 -0.00428 0.03786 0.01311 0.00027 0.00060 0.00049 0.00000 0.00348 0.00553 0.00527 0.00336 0.00340 0.00301 0.00210 O12 0.05464 0.22157 1.09987 1.00000 0.02931 0.04370 0.04186 0.00038 -0.02690 0.00295 0.03829 0.01161 0.00028 0.00068 0.00043 0.00000 0.00395 0.00406 0.00445 0.00363 0.00357 0.00344 0.00187 O13 0.06384 0.32889 1.21134 1.00000 0.04044 0.02610 0.05311 -0.00712 0.01195 0.00241 0.03988 0.01307 0.00029 0.00060 0.00046 0.00000 0.00457 0.00374 0.00509 0.00343 0.00358 0.00319 0.00200 O14 0.07688 0.13599 1.21669 1.00000 0.03967 0.02906 0.02931 -0.00318 -0.01064 -0.00341 0.03268 0.01178 0.00028 0.00056 0.00039 0.00000 0.00414 0.00364 0.00401 0.00298 0.00320 0.00319 0.00168 Cl11 0.08139 0.23413 1.16958 1.00000 0.02447 0.03088 0.01661 -0.00406 -0.00192 -0.00012 0.02398 0.00412 0.00010 0.00020 0.00014 0.00000 0.00128 0.00121 0.00108 0.00103 0.00098 0.00096 0.00051 O21 0.12153 -0.20594 0.72738 1.00000 0.03867 0.04452 0.02772 0.01607 0.00029 -0.00787 0.03697 0.01320 0.00028 0.00063 0.00041 0.00000 0.00402 0.00399 0.00361 0.00317 0.00298 0.00320 0.00172 O22 0.18619 -0.10359 0.66523 1.00000 0.04341 0.05984 0.05795 0.00047 0.02364 0.00081 0.05374 0.01320 0.00025 0.00065 0.00044 0.00000 0.00383 0.00482 0.00475 0.00376 0.00361 0.00351 0.00192 O23 0.11059 -0.15111 0.59998 1.00000 0.09838 0.06316 0.01887 -0.00548 0.00858 0.00476 0.06014 0.01373 0.00037 0.00071 0.00040 0.00000 0.00648 0.00541 0.00365 0.00355 0.00400 0.00499 0.00233 O24 0.10745 -0.02065 0.69678 1.00000 0.03387 0.02482 0.07253 -0.01028 0.00518 0.00356 0.04374 0.01204 0.00025 0.00051 0.00044 0.00000 0.00373 0.00332 0.00534 0.00320 0.00365 0.00290 0.00183 Cl21 0.13453 -0.12069 0.67272 1.00000 0.03772 0.02466 0.02640 0.00002 0.01415 0.00001 0.02959 0.00428 0.00009 0.00019 0.00014 0.00000 0.00122 0.00110 0.00114 0.00095 0.00103 0.00095 0.00051 O31 -0.06140 0.40364 0.79769 1.00000 0.06763 0.09478 0.10952 -0.03923 0.04510 -0.02174 0.09064 0.01598 0.00031 0.00083 0.00059 0.00000 0.00494 0.00700 0.00771 0.00606 0.00535 0.00459 0.00317 O32 -0.13147 0.29375 0.77766 1.00000 0.08507 0.02574 0.07117 -0.00503 -0.01928 -0.01637 0.06066 0.01282 0.00037 0.00063 0.00053 0.00000 0.00628 0.00376 0.00584 0.00390 0.00497 0.00401 0.00250 O33 -0.13987 0.48535 0.80253 1.00000 0.09817 0.03865 0.08789 -0.00895 -0.03209 0.01884 0.07491 0.01481 0.00036 0.00061 0.00055 0.00000 0.00638 0.00408 0.00667 0.00418 0.00574 0.00449 0.00270 O34 -0.11572 0.36340 0.89913 1.00000 0.11473 0.04976 0.04074 0.00726 0.01975 0.01437 0.06841 0.01750 0.00042 0.00073 0.00045 0.00000 0.00798 0.00513 0.00436 0.00383 0.00468 0.00512 0.00274 Cl31 -0.11491 0.38565 0.81944 1.00000 0.05905 0.02868 0.03294 -0.00179 0.00075 0.00156 0.04022 0.00457 0.00011 0.00020 0.00016 0.00000 0.00165 0.00120 0.00140 0.00103 0.00126 0.00117 0.00062 O51 0.23139 0.70694 0.58162 1.00000 0.04333 0.03875 0.03372 -0.00568 -0.00406 0.00428 0.03860 0.01257 0.00028 0.00063 0.00043 0.00000 0.00426 0.00398 0.00406 0.00318 0.00323 0.00334 0.00178 O52 0.27877 0.59504 0.37764 1.00000 0.03325 0.07608 0.07202 0.02953 0.01788 0.01667 0.06045 0.01577 0.00027 0.00071 0.00048 0.00000 0.00404 0.00553 0.00550 0.00448 0.00370 0.00384 0.00227 O53 0.25752 0.03966 0.74043 1.00000 0.07363 0.07165 0.08081 0.00120 -0.00094 -0.02354 0.07536 0.01542 0.00036 0.00072 0.00058 0.00000 0.00616 0.00628 0.00627 0.00553 0.00509 0.00505 0.00262 O54 0.21504 -0.21915 0.40032 1.00000 0.06652 0.04308 0.03728 0.00309 0.00698 0.01898 0.04896 0.01454 0.00033 0.00067 0.00044 0.00000 0.00556 0.00424 0.00450 0.00349 0.00394 0.00407 0.00211 O55 0.18522 0.29286 1.00611 1.00000 0.05528 0.10714 0.09240 -0.00995 0.00009 0.03565 0.08494 0.01679 0.00031 0.00082 0.00069 0.00000 0.00485 0.00748 0.00726 0.00740 0.00579 0.00488 0.00296 Final Structure Factor Calculation for s93 in Pna2(1) Total number of l.s. parameters = 786 Maximum vector length = 511 Memory required = 8680 / 27090 wR2 = 0.1905 before cycle 7 for 12190 data and 2 / 786 parameters Disagreeable restraints before cycle 7 Observed Target Error Sigma Restraint 0.0700 0.0200 SAME/SADI O33 Cl31 O23 Cl21 Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 6. 60. 0. 0. 0. 260. 492. 0. 0. rms sigma 0.000 0.010 0.040 0.033 0.000 0.000 0.000 0.010 0.026 0.000 0.000 rms deviation 0.000 0.004 0.018 0.037 0.000 0.000 0.000 0.005 0.012 0.000 0.000 GooF = S = 1.069; Restrained GooF = 1.044 for 823 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0623 * P )^2 + 30.22 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0810 for 8263 Fo > 4sig(Fo) and 0.1288 for all 12190 data wR2 = 0.1905, GooF = S = 1.069, Restrained GooF = 1.044 for all data Occupancy sum of asymmetric unit = 87.00 for non-hydrogen and 36.00 for hydrogen atoms Principal mean square atomic displacements U 0.0347 0.0278 0.0174 C1 0.0398 0.0271 0.0117 C2 0.0527 0.0330 0.0094 C3 0.0394 0.0229 0.0125 C4 0.0348 0.0255 0.0026 C5 0.0316 0.0173 0.0060 C6 0.0324 0.0206 0.0018 C7 0.0354 0.0250 0.0158 C8 0.0283 0.0184 0.0053 C9 0.0229 0.0136 0.0099 C10 0.0279 0.0154 0.0087 C11 0.0309 0.0193 0.0089 C12 0.0211 0.0199 0.0134 C13 0.0309 0.0192 0.0157 C14 0.0391 0.0203 0.0155 C15 0.0389 0.0264 0.0180 C16 0.0244 0.0205 0.0168 C17 0.0267 0.0186 0.0151 C18 0.0463 0.0335 0.0127 C19 0.0457 0.0313 0.0203 C20 0.0487 0.0317 0.0081 C21 0.0362 0.0272 0.0145 C22 0.0290 0.0211 0.0120 C31 0.0377 0.0188 0.0042 C32 0.0383 0.0266 0.0090 C33 0.0403 0.0210 0.0137 C34 0.0272 0.0214 0.0060 C35 0.0308 0.0178 0.0161 C36 0.0421 0.0265 0.0197 C37 0.0270 0.0192 0.0141 C38 0.0351 0.0277 0.0119 C39 0.0276 0.0224 0.0059 C40 0.0286 0.0211 0.0029 C41 0.0309 0.0178 0.0068 C42 0.0332 0.0164 0.0126 C43 0.0319 0.0252 0.0176 C44 0.0393 0.0268 0.0075 C45 0.0383 0.0340 0.0096 C46 0.0377 0.0179 0.0090 C47 0.0282 0.0202 0.0033 C48 0.0277 0.0228 0.0150 C49 0.0318 0.0274 0.0186 C50 0.0392 0.0314 0.0076 C51 0.0379 0.0256 0.0139 C52 0.0238 0.0173 0.0126 N1 0.0219 0.0145 0.0121 N2 0.0348 0.0219 0.0123 N3 0.0254 0.0140 0.0033 N4 0.0304 0.0174 0.0046 N5 0.0409 0.0296 0.0102 N6 0.0268 0.0230 0.0140 N7 0.0297 0.0260 0.0119 N8 0.0236 0.0192 0.0074 N31 0.0245 0.0201 0.0093 N32 0.0338 0.0205 0.0182 N33 0.0297 0.0242 0.0148 N34 0.0217 0.0196 0.0131 N35 0.0417 0.0228 0.0068 N36 0.0262 0.0206 0.0074 N37 0.0357 0.0132 0.0023 N38 0.0225 0.0180 0.0129 Ni1 0.0260 0.0155 0.0122 Ni2 0.0520 0.0314 0.0222 O1 0.0541 0.0286 0.0157 O2 0.0356 0.0305 0.0209 O3 0.0606 0.0406 0.0153 O4 0.0390 0.0226 0.0184 Cl1 0.0548 0.0395 0.0193 O11 0.0633 0.0438 0.0078 O12 0.0610 0.0362 0.0224 O13 0.0464 0.0313 0.0203 O14 0.0320 0.0248 0.0152 Cl11 0.0567 0.0371 0.0171 O21 0.0755 0.0598 0.0259 O22 0.0998 0.0635 0.0172 O23 0.0751 0.0351 0.0211 O24 0.0473 0.0247 0.0168 Cl21 0.1663 0.0670 0.0386 O31 0.1002 0.0622 0.0195 O32 0.1300 0.0615 0.0332 O33 0.1230 0.0474 0.0348 O34 0.0591 0.0336 0.0279 Cl31 0.0487 0.0371 0.0299 O51 0.1113 0.0446 0.0255 O52 0.0964 0.0807 0.0491 O53 0.0785 0.0360 0.0324 O54 0.1275 0.0906 0.0367 O55 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.018 0.027 0.035 0.044 0.053 0.066 0.081 0.103 0.145 1.000 Number in group 1293. 1223. 1254. 1233. 1111. 1270. 1163. 1218. 1210. 1215. GooF 1.207 1.108 1.087 1.093 1.108 1.017 0.979 0.974 1.019 1.074 K 4.605 1.907 1.429 1.242 1.126 1.060 1.030 1.013 0.995 0.982 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.32 1.64 inf Number in group 1222. 1260. 1190. 1203. 1229. 1225. 1211. 1230. 1191. 1229. GooF 0.979 0.932 0.942 0.909 0.955 0.979 1.010 1.108 1.136 1.577 K 1.107 1.159 1.101 1.075 1.044 1.046 1.026 1.017 0.989 0.987 R1 0.320 0.285 0.215 0.170 0.136 0.113 0.088 0.072 0.061 0.057 Recommended weighting scheme: WGHT 0.0626 30.0686 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) 6 2 -4 10916.45 5767.29 7.30 0.148 2.72 6 2 4 10790.94 5748.78 7.16 0.148 2.72 11 1 -3 824.41 54.36 6.42 0.014 2.14 11 1 3 931.53 54.62 6.39 0.014 2.14 4 4 4 5779.55 2949.86 6.28 0.106 2.29 5 3 -6 1253.45 297.40 6.02 0.034 2.13 4 4 -4 5601.71 2950.84 5.95 0.106 2.29 5 3 6 1224.39 299.06 5.85 0.034 2.13 4 2 -1 1186.51 314.84 5.66 0.035 4.24 4 2 1 1159.02 307.76 5.52 0.034 4.24 14 6 -6 1556.71 433.39 5.46 0.041 1.22 10 2 -1 1656.45 597.42 5.40 0.048 2.35 10 2 0 9208.90 5712.36 5.25 0.148 2.37 12 5 -3 2271.53 703.71 5.09 0.052 1.54 3 4 -13 1127.25 118.67 4.97 0.021 1.21 3 4 13 868.41 118.64 4.96 0.021 1.21 8 5 0 614.69 56.94 4.95 0.015 1.92 9 3 -4 1419.39 526.45 4.92 0.045 2.05 14 6 6 1651.49 437.85 4.82 0.041 1.22 14 2 3 1288.41 403.73 4.76 0.039 1.68 5 2 4 1549.47 624.52 4.75 0.049 2.90 18 2 0 1646.57 594.88 4.64 0.048 1.39 5 2 -4 1470.81 624.42 4.49 0.049 2.90 4 4 0 3964.08 2361.39 4.40 0.095 2.70 10 6 -8 933.83 220.29 4.39 0.029 1.27 10 2 1 1411.31 604.85 4.32 0.048 2.35 8 2 0 1254.96 510.32 4.29 0.044 2.84 10 5 0 455.78 20.03 4.29 0.009 1.75 8 2 7 2634.47 1395.83 4.28 0.073 1.87 10 1 -1 485.23 66.21 4.25 0.016 2.50 9 3 4 1292.92 525.29 4.25 0.045 2.05 3 3 6 422.08 28.68 4.23 0.010 2.26 11 6 0 1281.47 2544.53 4.12 0.099 1.51 12 5 1 534.14 32.02 4.09 0.011 1.59 14 4 0 1696.94 800.16 4.06 0.055 1.57 13 2 -10 637.67 63.93 4.04 0.016 1.28 20 6 -3 996.03 165.85 4.03 0.025 1.06 14 2 -3 1168.55 400.76 3.99 0.039 1.68 1 7 12 1332.86 451.62 3.98 0.042 1.10 7 2 0 3352.71 5312.65 3.97 0.142 3.13 10 6 8 1107.91 222.17 3.90 0.029 1.27 2 3 -3 3277.46 2030.27 3.81 0.088 3.17 12 5 -1 571.49 32.04 3.77 0.011 1.59 18 4 0 651.03 29.41 3.74 0.011 1.29 16 5 -1 479.00 17.24 3.72 0.008 1.33 8 3 0 1664.89 865.70 3.69 0.058 2.50 14 1 0 695.17 81.37 3.63 0.018 1.82 3 2 -1 4442.64 2974.24 3.62 0.107 4.71 3 2 1 4441.68 2976.33 3.61 0.107 4.71 2 3 3 3214.67 2036.47 3.61 0.088 3.17 Bond lengths and angles C1 - Distance Angles N1 1.3316 (0.0117) C2 1.3587 (0.0132) 124.86 (0.93) H1 0.9500 117.57 117.57 C1 - N1 C2 C2 - Distance Angles C1 1.3587 (0.0132) C3 1.4028 (0.0129) 116.09 (0.90) H2 0.9500 121.95 121.95 C2 - C1 C3 C3 - Distance Angles C4 1.3779 (0.0132) C2 1.4028 (0.0129) 119.07 (0.94) H3 0.9500 120.46 120.46 C3 - C4 C2 C4 - Distance Angles C3 1.3779 (0.0132) C5 1.3797 (0.0134) 119.80 (0.92) H4 0.9500 120.10 120.10 C4 - C3 C5 C5 - Distance Angles N1 1.3162 (0.0118) C4 1.3797 (0.0134) 121.07 (0.91) C6 1.4703 (0.0130) 116.40 (0.81) 122.38 (0.87) C5 - N1 C4 C6 - Distance Angles N2 1.3343 (0.0107) C7 1.3835 (0.0121) 120.21 (0.83) C5 1.4703 (0.0130) 112.42 (0.76) 127.36 (0.79) C6 - N2 C7 C7 - Distance Angles C8 1.3281 (0.0128) C6 1.3835 (0.0121) 117.68 (0.84) H7 0.9500 121.16 121.16 C7 - C8 C6 C8 - Distance Angles C7 1.3281 (0.0127) C9 1.3921 (0.0131) 123.68 (0.88) H8 0.9500 118.16 118.16 C8 - C7 C9 C9 - Distance Angles C10 1.3714 (0.0114) C8 1.3921 (0.0130) 114.86 (0.81) H9 0.9500 122.57 122.57 C9 - C10 C8 C10 - Distance Angles N2 1.3184 (0.0110) C9 1.3714 (0.0115) 122.63 (0.80) C11 1.5067 (0.0116) 111.44 (0.70) 125.89 (0.76) C10 - N2 C9 C11 - Distance Angles N4 1.2791 (0.0105) N3 1.3038 (0.0101) 129.12 (0.80) C10 1.5067 (0.0116) 113.27 (0.69) 117.50 (0.78) C11 - N4 N3 C12 - Distance Angles N6 1.2852 (0.0120) N5 1.2880 (0.0112) 125.56 (0.89) C13 1.4874 (0.0124) 119.92 (0.83) 114.46 (0.83) C12 - N6 N5 C13 - Distance Angles C14 1.3273 (0.0132) N7 1.3831 (0.0117) 122.47 (0.79) C12 1.4874 (0.0124) 127.84 (0.85) 109.64 (0.76) C13 - C14 N7 C14 - Distance Angles C13 1.3273 (0.0132) C15 1.4061 (0.0126) 122.60 (0.93) H14 0.9500 118.70 118.70 C14 - C13 C15 C15 - Distance Angles C16 1.3862 (0.0139) C14 1.4061 (0.0126) 113.45 (0.90) H15 0.9500 123.28 123.28 C15 - C16 C14 C16 - Distance Angles C17 1.3756 (0.0131) C15 1.3862 (0.0139) 123.86 (0.89) H16 0.9500 118.07 118.07 C16 - C17 C15 C17 - Distance Angles N7 1.3501 (0.0112) C16 1.3756 (0.0131) 120.23 (0.85) C18 1.4831 (0.0130) 111.14 (0.77) 128.58 (0.84) C17 - N7 C16 C18 - Distance Angles N8 1.3458 (0.0115) C19 1.3550 (0.0128) 121.61 (0.89) C17 1.4831 (0.0130) 115.60 (0.74) 122.79 (0.88) C18 - N8 C19 C19 - Distance Angles C18 1.3550 (0.0128) C20 1.3601 (0.0138) 118.80 (0.94) H19 0.9500 120.60 120.60 C19 - C18 C20 C20 - Distance Angles C21 1.3376 (0.0149) C19 1.3601 (0.0138) 121.09 (0.95) H20 0.9500 119.46 119.46 C20 - C21 C19 C21 - Distance Angles C20 1.3376 (0.0149) C22 1.4397 (0.0128) 115.60 (1.02) H21 0.9500 122.20 122.20 C21 - C20 C22 C22 - Distance Angles N8 1.2518 (0.0125) C21 1.4397 (0.0128) 123.70 (1.01) H22 0.9500 118.15 118.15 C22 - N8 C21 C31 - Distance Angles N31 1.3292 (0.0112) C32 1.3889 (0.0128) 122.72 (0.85) H31 0.9500 118.64 118.64 C31 - N31 C32 C32 - Distance Angles C33 1.3375 (0.0124) C31 1.3889 (0.0128) 118.05 (0.82) H32 0.9500 120.97 120.98 C32 - C33 C31 C33 - Distance Angles C32 1.3375 (0.0124) C34 1.3523 (0.0128) 121.53 (0.88) H33 0.9500 119.24 119.24 C33 - C32 C34 C34 - Distance Angles C33 1.3523 (0.0128) C35 1.3855 (0.0129) 117.41 (0.91) H34 0.9500 121.29 121.30 C34 - C33 C35 C35 - Distance Angles N31 1.3447 (0.0112) C34 1.3855 (0.0129) 122.68 (0.89) C36 1.4706 (0.0126) 112.71 (0.79) 124.52 (0.84) C35 - N31 C34 C36 - Distance Angles N32 1.3223 (0.0114) C37 1.3940 (0.0126) 120.43 (0.84) C35 1.4706 (0.0126) 114.62 (0.77) 124.95 (0.83) C36 - N32 C37 C37 - Distance Angles C36 1.3940 (0.0126) C38 1.3949 (0.0128) 118.73 (0.90) H37 0.9500 120.64 120.64 C37 - C36 C38 C38 - Distance Angles C39 1.3883 (0.0124) C37 1.3949 (0.0128) 118.71 (0.86) H38 0.9500 120.65 120.65 C38 - C39 C37 C39 - Distance Angles C40 1.3638 (0.0125) C38 1.3883 (0.0124) 118.95 (0.85) H39 0.9500 120.53 120.53 C39 - C40 C38 C40 - Distance Angles N32 1.3252 (0.0108) C39 1.3638 (0.0125) 121.81 (0.85) C41 1.4556 (0.0124) 111.98 (0.76) 126.22 (0.78) C40 - N32 C39 C41 - Distance Angles N34 1.2985 (0.0108) N33 1.3248 (0.0098) 123.73 (0.85) C40 1.4556 (0.0124) 114.24 (0.71) 121.95 (0.79) C41 - N34 N33 C42 - Distance Angles N35 1.3132 (0.0112) N36 1.3499 (0.0112) 125.13 (0.88) C43 1.4563 (0.0132) 115.45 (0.78) 119.39 (0.80) C42 - N35 N36 C43 - Distance Angles N37 1.3105 (0.0114) C44 1.4192 (0.0130) 120.05 (0.85) C42 1.4563 (0.0132) 113.29 (0.79) 126.66 (0.83) C43 - N37 C44 C44 - Distance Angles C45 1.3622 (0.0129) C43 1.4192 (0.0130) 114.63 (0.90) H44 0.9500 122.68 122.68 C44 - C45 C43 C45 - Distance Angles C46 1.3279 (0.0141) C44 1.3622 (0.0129) 125.74 (0.92) H45 0.9500 117.13 117.13 C45 - C46 C44 C46 - Distance Angles C45 1.3279 (0.0141) C47 1.4149 (0.0127) 115.11 (0.88) H46 0.9500 122.45 122.45 C46 - C45 C47 C47 - Distance Angles N37 1.2882 (0.0111) C46 1.4149 (0.0127) 121.17 (0.87) C48 1.4717 (0.0128) 116.06 (0.80) 122.77 (0.83) C47 - N37 C46 C48 - Distance Angles N38 1.3385 (0.0110) C49 1.3421 (0.0128) 121.26 (0.85) C47 1.4717 (0.0128) 113.64 (0.74) 125.10 (0.86) C48 - N38 C49 C49 - Distance Angles C48 1.3421 (0.0128) C50 1.3800 (0.0126) 121.71 (0.88) H49 0.9500 119.15 119.15 C49 - C48 C50 C50 - Distance Angles C49 1.3800 (0.0126) C51 1.4081 (0.0137) 116.44 (0.85) H50 0.9500 121.78 121.78 C50 - C49 C51 C51 - Distance Angles C52 1.3319 (0.0134) C50 1.4081 (0.0137) 120.23 (0.94) H51 0.9500 119.88 119.88 C51 - C52 C50 C52 - Distance Angles C51 1.3319 (0.0134) N38 1.3735 (0.0116) 121.65 (0.97) H52 0.9500 119.17 119.17 C52 - C51 N38 N1 - Distance Angles C5 1.3162 (0.0118) C1 1.3316 (0.0117) 118.81 (0.87) Ni1 2.0904 (0.0077) 113.02 (0.61) 128.14 (0.65) N1 - C5 C1 N2 - Distance Angles C10 1.3184 (0.0110) C6 1.3343 (0.0106) 120.92 (0.76) Ni1 1.9993 (0.0073) 119.65 (0.58) 116.86 (0.59) N2 - C10 C6 N3 - Distance Angles C11 1.3038 (0.0101) H3A 0.8800 120.00 H3B 0.8800 120.00 120.00 N3 - C11 H3A N4 - Distance Angles C11 1.2791 (0.0105) N5 1.4119 (0.0091) 113.21 (0.65) Ni1 2.1082 (0.0066) 116.58 (0.55) 122.79 (0.50) N4 - C11 N5 N5 - Distance Angles C12 1.2880 (0.0112) N4 1.4119 (0.0091) 114.13 (0.73) Ni2 2.1026 (0.0072) 116.52 (0.60) 122.10 (0.49) N5 - C12 N4 N6 - Distance Angles C12 1.2852 (0.0121) H6A 0.8800 120.00 H6B 0.8800 120.00 120.00 N6 - C12 H6A N7 - Distance Angles C17 1.3501 (0.0113) C13 1.3831 (0.0117) 117.33 (0.76) Ni2 1.9459 (0.0078) 120.85 (0.63) 120.67 (0.59) N7 - C17 C13 N8 - Distance Angles C22 1.2518 (0.0125) C18 1.3458 (0.0115) 119.05 (0.80) Ni2 2.1052 (0.0074) 127.75 (0.65) 113.17 (0.59) N8 - C22 C18 N31 - Distance Angles C31 1.3292 (0.0112) C35 1.3447 (0.0112) 117.06 (0.83) Ni1 2.0788 (0.0079) 127.39 (0.63) 115.32 (0.60) N31 - C31 C35 N32 - Distance Angles C36 1.3223 (0.0114) C40 1.3252 (0.0108) 121.35 (0.76) Ni1 2.0092 (0.0071) 116.44 (0.58) 118.95 (0.63) N32 - C36 C40 N33 - Distance Angles C41 1.3248 (0.0098) H33A 0.8800 120.00 H33B 0.8800 120.00 120.00 N33 - C41 H33A N34 - Distance Angles C41 1.2985 (0.0108) N35 1.3887 (0.0102) 115.92 (0.71) Ni1 2.1358 (0.0073) 114.60 (0.60) 120.68 (0.53) N34 - C41 N35 N35 - Distance Angles C42 1.3132 (0.0112) N34 1.3887 (0.0102) 113.28 (0.72) Ni2 2.1086 (0.0072) 113.64 (0.61) 125.33 (0.56) N35 - C42 N34 N36 - Distance Angles C42 1.3499 (0.0112) H36A 0.8800 120.00 H36B 0.8800 120.00 120.00 N36 - C42 H36A N37 - Distance Angles C47 1.2882 (0.0111) C43 1.3105 (0.0114) 123.11 (0.83) Ni2 2.0009 (0.0076) 117.56 (0.61) 118.43 (0.61) N37 - C47 C43 N38 - Distance Angles C48 1.3385 (0.0111) C52 1.3735 (0.0117) 118.68 (0.77) Ni2 2.1005 (0.0070) 113.87 (0.54) 127.45 (0.63) N38 - C48 C52 Ni1 - Distance Angles N2 1.9993 (0.0073) N32 2.0092 (0.0071) 166.43 (0.21) N31 2.0788 (0.0079) 93.93 (0.29) 77.08 (0.29) N1 2.0904 (0.0077) 77.76 (0.29) 92.04 (0.29) 90.72 (0.20) N4 2.1082 (0.0066) 75.92 (0.27) 115.10 (0.28) 98.44 (0.27) 152.63 (0.29) N34 2.1358 (0.0073) 114.38 (0.30) 75.45 (0.30) 151.59 (0.30) 97.35 (0.29) 86.78 (0.21) Ni1 - N2 N32 N31 N1 N4 Ni2 - Distance Angles N7 1.9459 (0.0078) N37 2.0009 (0.0076) 169.29 (0.22) N38 2.1005 (0.0070) 94.25 (0.30) 77.90 (0.28) N5 2.1026 (0.0072) 76.59 (0.30) 111.49 (0.28) 98.40 (0.28) N8 2.1052 (0.0074) 78.01 (0.30) 94.43 (0.30) 89.01 (0.21) 153.97 (0.29) N35 2.1086 (0.0073) 111.26 (0.30) 77.07 (0.30) 154.38 (0.29) 85.77 (0.20) 98.27 (0.28) Ni2 - N7 N37 N38 N5 N8 O1 - Distance Angles Cl1 1.4145 (0.0057) O1 - O2 - Distance Angles Cl1 1.4143 (0.0058) O2 - O3 - Distance Angles Cl1 1.4204 (0.0056) O3 - O4 - Distance Angles Cl1 1.4227 (0.0056) O4 - Cl1 - Distance Angles O2 1.4143 (0.0059) O1 1.4145 (0.0057) 109.10 (0.42) O3 1.4204 (0.0056) 108.29 (0.44) 108.06 (0.48) O4 1.4227 (0.0056) 111.55 (0.51) 110.38 (0.49) 109.36 (0.46) Cl1 - O2 O1 O3 O11 - Distance Angles Cl11 1.4663 (0.0070) O11 - O12 - Distance Angles Cl11 1.4010 (0.0065) O12 - O13 - Distance Angles Cl11 1.4148 (0.0066) O13 - O14 - Distance Angles Cl11 1.4303 (0.0065) O14 - Cl11 - Distance Angles O12 1.4010 (0.0065) O13 1.4148 (0.0066) 111.71 (0.50) O14 1.4303 (0.0065) 111.50 (0.47) 109.38 (0.49) O11 1.4663 (0.0071) 107.93 (0.50) 110.40 (0.46) 105.74 (0.44) Cl11 - O12 O13 O14 O21 - Distance Angles Cl21 1.4289 (0.0064) O21 - O22 - Distance Angles Cl21 1.3551 (0.0065) O22 - O23 - Distance Angles Cl21 1.4514 (0.0074) O23 - O24 - Distance Angles Cl21 1.4422 (0.0061) O24 - Cl21 - Distance Angles O22 1.3551 (0.0065) O21 1.4289 (0.0064) 113.66 (0.48) O24 1.4422 (0.0061) 112.38 (0.45) 106.25 (0.45) O23 1.4514 (0.0074) 111.89 (0.51) 107.50 (0.47) 104.57 (0.48) Cl21 - O22 O21 O24 O31 - Distance Angles Cl31 1.4476 (0.0076) O31 - O32 - Distance Angles Cl31 1.3800 (0.0072) O32 - O33 - Distance Angles Cl31 1.3815 (0.0071) O33 - O34 - Distance Angles Cl31 1.4085 (0.0078) O34 - Cl31 - Distance Angles O32 1.3800 (0.0072) O33 1.3815 (0.0071) 115.11 (0.56) O34 1.4085 (0.0078) 111.26 (0.58) 111.30 (0.57) O31 1.4476 (0.0076) 106.00 (0.56) 105.21 (0.62) 107.34 (0.65) Cl31 - O32 O33 O34 FMAP and GRID set by program FMAP 2 3 39 GRID -1.389 -1 -2 1.389 1 2 R1 = 0.1087 for 6313 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 1.01 at 0.2275 0.2165 0.0573 [ 1.15 A from O51 ] Deepest hole -0.82 at 0.2201 0.7995 -0.0045 [ 0.71 A from NI2 ] Mean = 0.00, Rms deviation from mean = 0.13 e/A^3, Highest memory used = 8491 / 71196 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.2725 0.7165 0.5573 1.00000 0.05 1.01 1.15 O51 1.67 O55 2.49 H3B 2.88 O11 Q2 1 -0.1842 0.4280 0.7623 1.00000 0.05 0.94 1.50 O33 1.60 O53 2.11 CL31 2.12 O32 Q3 1 0.2726 -0.2050 0.4303 1.00000 0.05 0.87 1.58 O54 1.71 O55 2.24 H33B 2.55 O52 Q4 1 -0.1529 0.3694 0.8068 1.00000 0.05 0.84 1.02 CL31 1.17 O32 1.42 O33 1.87 O34 Q5 1 0.1601 -0.1564 0.6770 1.00000 0.05 0.81 0.79 CL21 0.94 O22 1.45 O21 1.85 O23 Q6 1 0.2519 0.3134 0.4924 1.00000 0.05 0.72 0.94 NI2 1.56 N5 1.93 N37 2.05 N38 Q7 1 0.1877 -0.0781 0.7301 1.00000 0.05 0.72 1.17 O22 1.77 CL21 2.26 O24 2.29 O21 Q8 1 -0.1712 0.3171 0.8716 1.00000 0.05 0.71 1.61 O34 1.70 O54 1.90 CL31 1.95 O32 Q9 1 0.3675 0.3162 0.4982 1.00000 0.05 0.70 1.27 N38 1.62 C48 1.87 C52 2.34 C49 Q10 1 0.1846 -0.2652 0.3608 1.00000 0.05 0.67 1.18 O54 2.02 O32 2.23 O34 2.39 H39 Shortest distances between peaks (including symmetry equivalents) 8 10 0.73 2 4 1.32 4 8 1.37 5 7 1.49 4 10 1.76 2 8 2.33 1 3 2.39 2 10 2.58 3 10 2.67 6 9 2.99 Time profile in seconds ----------------------- 0.02: Read and process instructions 0.00: Fit rigid groups 0.02: 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 0.02: Analyse other restraints etc. 3.91: 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 32.35: Structure factors and derivatives 57.06: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.19: Apply other restraints 3.81: Solve l.s. equations 0.00: Generate HTAB table 0.05: Other dependent quantities, CIF, tables 0.20: Analysis of variance 0.06: Merge reflections for Fourier and .fcf 0.09: Fourier summations 0.11: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 04src0194 finished at 11:51:39 Total CPU time: 97.8 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++