+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2006slh0986 started at 15:28:26 on 27-Nov-2006 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2006slh0986 in P2(1)2(1)2(1) CELL 0.69050 12.1130 16.3070 19.2570 90.000 90.000 90.000 ZERR 4.00 0.0050 0.0060 0.0080 0.000 0.000 0.000 LATT -1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM 1/2 + X, 1/2 - Y, - Z SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N S NI UNIT 160 208 4 16 4 V = 3803.77 F(000) = 1564.0 Mu = 0.76 mm-1 Cell Wt = 2935.10 Rho = 1.281 MERG 2 OMIT -3.00 55.00 OMIT 0 16 1 OMIT 1 1 7 EXTI 0.01013 FMAP 2 PLAN 10 SIZE 0.02 0.02 0.15 ACTA BOND $H WGHT 0.05900 L.S. 6 TEMP -153.00 FVAR 0.15891 MOLE 1 C1 1 0.222600 -0.208720 0.660500 11.00000 0.03420 0.03250 = 0.02580 0.00210 0.00010 -0.00300 AFIX 43 H1 2 0.227770 -0.265020 0.672770 11.00000 -1.20000 AFIX 0 C2 1 0.313220 -0.160020 0.667360 11.00000 0.03180 0.03190 = 0.02510 -0.00270 0.00130 -0.00290 C3 1 0.420870 -0.191070 0.692020 11.00000 0.03730 0.02960 = 0.02570 -0.00080 0.00220 0.00150 C4 1 0.427320 -0.261710 0.736660 11.00000 0.03510 0.04020 = 0.02420 0.00490 -0.00160 -0.00580 AFIX 43 H4 2 0.361680 -0.290500 0.748230 11.00000 -1.20000 AFIX 0 C5 1 0.524900 -0.287860 0.762420 11.00000 0.04420 0.02840 = 0.03090 0.00590 -0.00280 0.00110 AFIX 43 H5 2 0.526600 -0.334600 0.791850 11.00000 -1.20000 AFIX 0 C6 1 0.625190 -0.246610 0.746230 11.00000 0.03950 0.03000 = 0.02490 -0.00310 -0.00020 0.00380 C7 1 0.727810 -0.270480 0.775480 11.00000 0.04600 0.03450 = 0.02880 -0.00280 -0.00630 0.01040 AFIX 43 H7 2 0.731300 -0.316710 0.805420 11.00000 -1.20000 AFIX 0 C8 1 0.822090 -0.227080 0.760740 11.00000 0.03830 0.04190 = 0.02870 -0.00380 0.00020 0.00810 AFIX 43 H8 2 0.890050 -0.242280 0.781740 11.00000 -1.20000 AFIX 0 C9 1 0.818390 -0.159600 0.714230 11.00000 0.03300 0.03840 = 0.03080 0.00240 0.00060 0.00360 AFIX 43 H9 2 0.884310 -0.131060 0.702830 11.00000 -1.20000 AFIX 0 C10 1 0.720540 -0.135710 0.685950 11.00000 0.03240 0.03510 = 0.03110 0.00250 0.00170 0.00430 AFIX 43 H10 2 0.719000 -0.090070 0.655310 11.00000 -1.20000 AFIX 0 C11 1 0.621190 -0.177450 0.701250 11.00000 0.03590 0.03000 = 0.02070 -0.00170 0.00070 0.00310 C12 1 0.518140 -0.152300 0.675300 11.00000 0.03160 0.03160 = 0.02300 0.00220 -0.00320 0.00260 AFIX 43 H12 2 0.515580 -0.106490 0.644850 11.00000 -1.20000 AFIX 0 C13 1 -0.040830 0.071540 0.552440 11.00000 0.02950 0.03610 = 0.02800 0.00140 -0.00080 0.00460 AFIX 43 H13 2 -0.109550 0.092830 0.536950 11.00000 -1.20000 AFIX 0 C14 1 0.048090 0.121340 0.551910 11.00000 0.03220 0.03880 = 0.02170 -0.00320 -0.00300 0.00280 C15 1 0.046660 0.207330 0.528800 11.00000 0.03040 0.03120 = 0.02360 -0.00060 0.00120 0.00580 C16 1 0.119560 0.264680 0.554470 11.00000 0.03210 0.03660 = 0.02090 -0.00130 0.00260 0.00770 AFIX 43 H16 2 0.173430 0.247610 0.587290 11.00000 -1.20000 AFIX 0 C17 1 0.117420 0.347670 0.533990 11.00000 0.03180 0.03260 = 0.02550 -0.00010 0.00250 0.00490 C18 1 0.192030 0.406800 0.561260 11.00000 0.03360 0.03440 = 0.02930 0.00150 0.00070 0.00700 AFIX 43 H18 2 0.244940 0.390750 0.595040 11.00000 -1.20000 AFIX 0 C19 1 0.188440 0.486400 0.539390 11.00000 0.03620 0.03880 = 0.04200 -0.00060 0.00430 -0.00080 AFIX 43 H19 2 0.238450 0.525260 0.558410 11.00000 -1.20000 AFIX 0 C20 1 0.111150 0.511550 0.488800 11.00000 0.04430 0.03390 = 0.04880 0.01210 0.00560 0.00470 AFIX 43 H20 2 0.110300 0.566830 0.473230 11.00000 -1.20000 AFIX 0 C21 1 0.037560 0.456300 0.462240 11.00000 0.03720 0.04270 = 0.03640 0.01170 0.00180 0.00660 AFIX 43 H21 2 -0.015090 0.473790 0.428810 11.00000 -1.20000 AFIX 0 C22 1 0.038760 0.373460 0.483870 11.00000 0.03100 0.03730 = 0.02530 0.00400 0.00310 0.00510 C23 1 -0.036360 0.314260 0.458050 11.00000 0.03380 0.04400 = 0.02990 0.00710 -0.00500 0.00520 AFIX 43 H23 2 -0.090630 0.330550 0.425220 11.00000 -1.20000 AFIX 0 C24 1 -0.032720 0.234440 0.479160 11.00000 0.03820 0.04210 = 0.02640 -0.00130 -0.00320 0.00090 AFIX 43 H24 2 -0.083960 0.196260 0.460460 11.00000 -1.20000 AFIX 0 S1 4 0.099210 -0.171180 0.630270 11.00000 0.03180 0.03290 = 0.03810 0.00080 -0.00070 -0.00320 S2 4 0.300420 -0.057210 0.646180 11.00000 0.03090 0.03000 = 0.02860 0.00090 -0.00030 -0.00080 S3 4 -0.035450 -0.027990 0.579660 11.00000 0.03170 0.03570 = 0.03490 0.00050 -0.00150 -0.00350 S4 4 0.171870 0.080280 0.582890 11.00000 0.03020 0.03090 = 0.02890 -0.00050 -0.00340 0.00040 NI1 5 0.133280 -0.044130 0.610350 11.00000 0.03030 0.02990 = 0.02480 -0.00140 -0.00030 -0.00120 MOLE 2 C25 1 0.664350 0.418490 0.068020 11.00000 0.03990 0.03630 = 0.02460 -0.00230 0.00110 0.00080 AFIX 23 H25A 2 0.698420 0.446200 0.027610 11.00000 -1.20000 H25B 2 0.583390 0.419580 0.061020 11.00000 -1.20000 AFIX 0 C26 1 0.701580 0.329630 0.067960 11.00000 0.05460 0.03530 = 0.02780 -0.00190 -0.00480 0.00430 AFIX 23 H26A 2 0.782660 0.326910 0.061940 11.00000 -1.20000 H26B 2 0.682700 0.303760 0.112930 11.00000 -1.20000 AFIX 0 C27 1 0.645170 0.283820 0.009280 11.00000 0.06510 0.04300 = 0.02810 -0.00760 0.00290 -0.00920 AFIX 23 H27A 2 0.649680 0.317250 -0.033540 11.00000 -1.20000 H27B 2 0.566110 0.276820 0.020880 11.00000 -1.20000 AFIX 0 C28 1 0.695580 0.199950 -0.004770 11.00000 0.08860 0.03350 = 0.03600 0.00050 0.00300 -0.01020 AFIX 137 H28A 2 0.773480 0.206440 -0.017360 11.00000 -1.50000 H28B 2 0.655940 0.173460 -0.043040 11.00000 -1.50000 H28C 2 0.689770 0.165970 0.037040 11.00000 -1.50000 AFIX 0 C29 1 0.624050 0.437230 0.194200 11.00000 0.03600 0.03070 = 0.02530 0.00090 -0.00140 0.00260 AFIX 23 H29A 2 0.636700 0.377500 0.198840 11.00000 -1.20000 H29B 2 0.653100 0.463660 0.236720 11.00000 -1.20000 AFIX 0 C30 1 0.500810 0.452050 0.191140 11.00000 0.03360 0.03890 = 0.03170 0.00060 0.00330 0.00090 AFIX 23 H30A 2 0.472090 0.435580 0.145070 11.00000 -1.20000 H30B 2 0.485250 0.511130 0.197780 11.00000 -1.20000 AFIX 0 C31 1 0.443680 0.402310 0.247900 11.00000 0.03560 0.03020 = 0.04040 0.00160 0.00410 -0.00110 AFIX 23 H31A 2 0.452610 0.343150 0.237830 11.00000 -1.20000 H31B 2 0.479790 0.413730 0.293000 11.00000 -1.20000 AFIX 0 C32 1 0.321760 0.422100 0.253510 11.00000 0.03930 0.03390 = 0.05270 -0.00660 0.00890 -0.00340 AFIX 137 H32A 2 0.312600 0.479210 0.268260 11.00000 -1.50000 H32B 2 0.287340 0.385660 0.287690 11.00000 -1.50000 H32C 2 0.286510 0.414230 0.208190 11.00000 -1.50000 AFIX 0 C33 1 0.664250 0.556930 0.117130 11.00000 0.03270 0.03090 = 0.02860 0.00600 0.00030 -0.00050 AFIX 23 H33A 2 0.708860 0.574640 0.076750 11.00000 -1.20000 H33B 2 0.585580 0.560730 0.103580 11.00000 -1.20000 AFIX 0 C34 1 0.684460 0.615490 0.175640 11.00000 0.04010 0.03630 = 0.03250 0.00550 -0.00180 0.00190 AFIX 23 H34A 2 0.762760 0.612110 0.190100 11.00000 -1.20000 H34B 2 0.638060 0.599960 0.215860 11.00000 -1.20000 AFIX 0 C35 1 0.657350 0.704330 0.153760 11.00000 0.04260 0.03050 = 0.03320 -0.00010 -0.00480 0.00280 AFIX 23 H35A 2 0.583430 0.705350 0.131850 11.00000 -1.20000 H35B 2 0.654300 0.739240 0.195770 11.00000 -1.20000 AFIX 0 C36 1 0.740960 0.740290 0.103410 11.00000 0.05090 0.03750 = 0.03810 0.00360 0.00190 -0.00320 AFIX 137 H36A 2 0.815080 0.736460 0.123560 11.00000 -1.50000 H36B 2 0.723020 0.797950 0.094560 11.00000 -1.50000 H36C 2 0.738710 0.709660 0.059650 11.00000 -1.50000 AFIX 0 C37 1 0.812280 0.458020 0.152760 11.00000 0.03090 0.03710 = 0.02300 -0.00190 -0.00420 0.00550 AFIX 23 H37A 2 0.826060 0.489800 0.195690 11.00000 -1.20000 H37B 2 0.826130 0.399530 0.163450 11.00000 -1.20000 AFIX 0 C38 1 0.893930 0.485510 0.097630 11.00000 0.03880 0.04540 = 0.03070 0.00710 0.00000 -0.00100 AFIX 23 H38A 2 0.883340 0.544600 0.087900 11.00000 -1.20000 H38B 2 0.880480 0.454780 0.054110 11.00000 -1.20000 AFIX 0 C39 1 1.013020 0.470470 0.122320 11.00000 0.03380 0.04830 = 0.03600 -0.00570 0.00480 0.00430 AFIX 23 H39A 2 1.020230 0.412690 0.137450 11.00000 -1.20000 H39B 2 1.064040 0.479030 0.082820 11.00000 -1.20000 AFIX 0 C40 1 1.046650 0.525970 0.181310 11.00000 0.03910 0.07910 = 0.05160 -0.01430 -0.00160 -0.00340 AFIX 137 H40A 2 1.034470 0.583240 0.167940 11.00000 -1.50000 H40B 2 1.125000 0.517570 0.191830 11.00000 -1.50000 H40C 2 1.002340 0.513150 0.222480 11.00000 -1.50000 AFIX 0 N1 3 0.690810 0.468110 0.132400 11.00000 0.03330 0.02920 = 0.02290 0.00440 -0.00020 0.00030 HKLF 4 1.0 1.00 0.00 0.00 0.00 1.00 0.00 0.00 0.00 1.00 Covalent radii and connectivity table for 2006slh0986 in P2(1)2(1)2(1) C 0.770 H 0.320 N 0.700 S 1.030 NI 1.250 C1 - C2 S1 C2 - C1 C3 S2 C3 - C12 C4 C2 C4 - C5 C3 C5 - C4 C6 C6 - C7 C11 C5 C7 - C8 C6 C8 - C7 C9 C9 - C10 C8 C10 - C9 C11 C11 - C12 C10 C6 C12 - C3 C11 C13 - C14 S3 C14 - C13 C15 S4 C15 - C16 C24 C14 C16 - C15 C17 C17 - C16 C22 C18 C18 - C19 C17 C19 - C18 C20 C20 - C21 C19 C21 - C20 C22 C22 - C21 C23 C17 C23 - C24 C22 C24 - C23 C15 S1 - C1 Ni1 S2 - C2 Ni1 S3 - C13 Ni1 S4 - C14 Ni1 Ni1 - S3 S1 S4 S2 C25 - N1 C26 C26 - C27 C25 C27 - C26 C28 C28 - C27 C29 - C30 N1 C30 - C29 C31 C31 - C32 C30 C32 - C31 C33 - C34 N1 C34 - C33 C35 C35 - C36 C34 C36 - C35 C37 - C38 N1 C38 - C37 C39 C39 - C40 C38 C40 - C39 N1 - C33 C25 C29 C37 21917 Reflections read, of which 37 rejected -15 =< h =< 15, -18 =< k =< 20, -22 =< l =< 24, Max. 2-theta = 51.12 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) -2 15 6 29.90 2.59 2 13.57 -2 13 8 10.90 1.53 2 7.69 2 Inconsistent equivalents 7715 Unique reflections, of which 0 suppressed R(int) = 0.0821 R(sigma) = 0.0976 Friedel opposites not merged Maximum memory for data reduction = 4611 / 77391 Default effective X-H distances for T = -153.0 C AFIX m = 1 2 3 4 4[N] 3[N] 15[B] 8[O] 9 9[N] 16 d(X-H) = 1.00 0.99 0.98 0.95 0.88 0.91 1.12 0.84 0.95 0.88 0.95 Note that these distances are chosen to give the best fit to the X-ray data and so avoid the introduction of systematic error. The true internuclear distances are longer and do not vary with temperature ! The apparent variation with temperature is caused by libration. Least-squares cycle 1 Maximum vector length = 511 Memory required = 5889 / 542507 wR2 = 0.1318 before cycle 1 for 7715 data and 420 / 420 parameters GooF = S = 0.986; Restrained GooF = 0.986 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0590 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.15891 0.00033 0.011 OSF 2 0.01013 0.00106 0.002 EXTI Mean shift/esd = 0.012 Maximum = 0.119 for U33 Ni1 Max. shift = 0.000 A for H36B Max. dU = 0.000 for C22 Least-squares cycle 2 Maximum vector length = 511 Memory required = 5889 / 542507 wR2 = 0.1318 before cycle 2 for 7715 data and 420 / 420 parameters GooF = S = 0.986; Restrained GooF = 0.986 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0590 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.15891 0.00033 0.004 OSF 2 0.01013 0.00106 0.000 EXTI Mean shift/esd = 0.004 Maximum = 0.039 for U33 Ni1 Max. shift = 0.000 A for H36B Max. dU = 0.000 for C27 Least-squares cycle 3 Maximum vector length = 511 Memory required = 5889 / 542507 wR2 = 0.1318 before cycle 3 for 7715 data and 420 / 420 parameters GooF = S = 0.986; Restrained GooF = 0.986 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0590 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.15892 0.00033 0.002 OSF 2 0.01013 0.00106 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.002 for U23 C16 Max. shift = 0.000 A for H36B Max. dU = 0.000 for C10 Least-squares cycle 4 Maximum vector length = 511 Memory required = 5889 / 542507 wR2 = 0.1317 before cycle 4 for 7715 data and 420 / 420 parameters GooF = S = 0.986; Restrained GooF = 0.986 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0590 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.15891 0.00033 -0.001 OSF 2 0.01013 0.00106 -0.001 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for OSF Max. shift = 0.000 A for H36A Max. dU = 0.000 for C19 Least-squares cycle 5 Maximum vector length = 511 Memory required = 5889 / 542507 wR2 = 0.1318 before cycle 5 for 7715 data and 420 / 420 parameters GooF = S = 0.986; Restrained GooF = 0.986 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0590 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.15891 0.00033 -0.002 OSF 2 0.01013 0.00106 -0.001 EXTI Mean shift/esd = 0.000 Maximum = -0.002 for OSF Max. shift = 0.000 A for H32B Max. dU = 0.000 for C19 Least-squares cycle 6 Maximum vector length = 511 Memory required = 5889 / 542507 wR2 = 0.1318 before cycle 6 for 7715 data and 420 / 420 parameters GooF = S = 0.986; Restrained GooF = 0.986 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0590 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.15891 0.00033 0.001 OSF 2 0.01013 0.00106 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.001 for OSF Max. shift = 0.000 A for H19 Max. dU = 0.000 for C9 Largest correlation matrix elements 0.652 EXTI / OSF Idealized hydrogen atom generation before cycle 7 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1 0.2278 -0.2650 0.6728 43 0.950 0.000 C1 C2 S1 H4 0.3617 -0.2905 0.7482 43 0.950 0.000 C4 C5 C3 H5 0.5266 -0.3346 0.7919 43 0.950 0.000 C5 C4 C6 H7 0.7313 -0.3167 0.8054 43 0.950 0.000 C7 C8 C6 H8 0.8900 -0.2423 0.7817 43 0.950 0.000 C8 C7 C9 H9 0.8843 -0.1311 0.7028 43 0.950 0.000 C9 C10 C8 H10 0.7190 -0.0901 0.6553 43 0.950 0.000 C10 C9 C11 H12 0.5156 -0.1065 0.6449 43 0.950 0.000 C12 C3 C11 H13 -0.1096 0.0928 0.5370 43 0.950 0.000 C13 C14 S3 H16 0.1734 0.2476 0.5873 43 0.950 0.000 C16 C15 C17 H18 0.2449 0.3907 0.5950 43 0.950 0.000 C18 C19 C17 H19 0.2384 0.5253 0.5584 43 0.950 0.000 C19 C18 C20 H20 0.1103 0.5668 0.4732 43 0.950 0.000 C20 C21 C19 H21 -0.0151 0.4738 0.4288 43 0.950 0.000 C21 C20 C22 H23 -0.0906 0.3305 0.4252 43 0.950 0.000 C23 C24 C22 H24 -0.0840 0.1963 0.4605 43 0.950 0.000 C24 C23 C15 H25A 0.6984 0.4462 0.0276 23 0.990 0.000 C25 N1 C26 H25B 0.5834 0.4196 0.0610 23 0.990 0.000 C25 N1 C26 H26A 0.7827 0.3269 0.0619 23 0.990 0.000 C26 C27 C25 H26B 0.6827 0.3038 0.1129 23 0.990 0.000 C26 C27 C25 H27A 0.6497 0.3172 -0.0335 23 0.990 0.000 C27 C26 C28 H27B 0.5661 0.2768 0.0209 23 0.990 0.000 C27 C26 C28 H28A 0.7735 0.2064 -0.0174 137 0.980 0.000 C28 C27 H28A H28B 0.6559 0.1735 -0.0430 137 0.980 0.000 C28 C27 H28A H28C 0.6898 0.1660 0.0370 137 0.980 0.000 C28 C27 H28A H29A 0.6367 0.3775 0.1988 23 0.990 0.000 C29 C30 N1 H29B 0.6531 0.4637 0.2367 23 0.990 0.000 C29 C30 N1 H30A 0.4721 0.4356 0.1451 23 0.990 0.000 C30 C29 C31 H30B 0.4852 0.5111 0.1978 23 0.990 0.000 C30 C29 C31 H31A 0.4526 0.3431 0.2378 23 0.990 0.000 C31 C32 C30 H31B 0.4798 0.4137 0.2930 23 0.990 0.000 C31 C32 C30 H32A 0.3126 0.4792 0.2683 137 0.980 0.000 C32 C31 H32A H32B 0.2873 0.3857 0.2877 137 0.980 0.000 C32 C31 H32A H32C 0.2865 0.4142 0.2082 137 0.980 0.000 C32 C31 H32A H33A 0.7089 0.5746 0.0767 23 0.990 0.000 C33 C34 N1 H33B 0.5856 0.5607 0.1036 23 0.990 0.000 C33 C34 N1 H34A 0.7628 0.6121 0.1901 23 0.990 0.000 C34 C33 C35 H34B 0.6381 0.6000 0.2159 23 0.990 0.000 C34 C33 C35 H35A 0.5834 0.7054 0.1318 23 0.990 0.000 C35 C36 C34 H35B 0.6543 0.7392 0.1958 23 0.990 0.000 C35 C36 C34 H36A 0.8151 0.7365 0.1236 137 0.980 0.000 C36 C35 H36A H36B 0.7230 0.7980 0.0946 137 0.980 0.000 C36 C35 H36A H36C 0.7387 0.7097 0.0597 137 0.980 0.000 C36 C35 H36A H37A 0.8261 0.4898 0.1957 23 0.990 0.000 C37 C38 N1 H37B 0.8261 0.3995 0.1634 23 0.990 0.000 C37 C38 N1 H38A 0.8833 0.5446 0.0879 23 0.990 0.000 C38 C37 C39 H38B 0.8805 0.4548 0.0541 23 0.990 0.000 C38 C37 C39 H39A 1.0202 0.4127 0.1375 23 0.990 0.000 C39 C40 C38 H39B 1.0640 0.4790 0.0828 23 0.990 0.000 C39 C40 C38 H40A 1.0345 0.5832 0.1679 137 0.980 0.000 C40 C39 H40A H40B 1.1250 0.5176 0.1918 137 0.980 0.000 C40 C39 H40A H40C 1.0023 0.5131 0.2225 137 0.980 0.000 C40 C39 H40A 2006slh0986 in P2(1)2(1)2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.22260 -0.20872 0.66050 1.00000 0.03416 0.03252 0.02582 0.00205 0.00009 -0.00297 0.03083 0.00733 0.00034 0.00027 0.00023 0.00000 0.00233 0.00232 0.00234 0.00185 0.00176 0.00181 0.00096 H1 0.22777 -0.26502 0.67277 1.00000 0.03700 0.00000 0.00000 C2 0.31322 -0.16002 0.66736 1.00000 0.03175 0.03190 0.02507 -0.00273 0.00129 -0.00294 0.02957 0.00711 0.00034 0.00026 0.00022 0.00000 0.00218 0.00225 0.00225 0.00184 0.00174 0.00183 0.00091 C3 0.42086 -0.19107 0.69202 1.00000 0.03732 0.02956 0.02567 -0.00080 0.00218 0.00149 0.03085 0.00761 0.00036 0.00026 0.00023 0.00000 0.00235 0.00220 0.00227 0.00177 0.00184 0.00180 0.00095 C4 0.42732 -0.26171 0.73666 1.00000 0.03514 0.04024 0.02415 0.00491 -0.00159 -0.00578 0.03317 0.00767 0.00036 0.00028 0.00023 0.00000 0.00236 0.00250 0.00236 0.00195 0.00180 0.00191 0.00099 H4 0.36168 -0.29050 0.74823 1.00000 0.03981 0.00000 0.00000 C5 0.52490 -0.28786 0.76242 1.00000 0.04419 0.02843 0.03092 0.00586 -0.00281 0.00113 0.03451 0.00773 0.00037 0.00026 0.00024 0.00000 0.00268 0.00232 0.00261 0.00195 0.00201 0.00192 0.00104 H5 0.52660 -0.33460 0.79185 1.00000 0.04142 0.00000 0.00000 C6 0.62519 -0.24661 0.74623 1.00000 0.03953 0.02995 0.02491 -0.00311 -0.00023 0.00377 0.03146 0.00739 0.00036 0.00025 0.00022 0.00000 0.00237 0.00213 0.00219 0.00177 0.00192 0.00186 0.00092 C7 0.72781 -0.27048 0.77548 1.00000 0.04598 0.03449 0.02881 -0.00284 -0.00632 0.01036 0.03643 0.00782 0.00038 0.00028 0.00025 0.00000 0.00273 0.00248 0.00248 0.00199 0.00202 0.00203 0.00107 H7 0.73130 -0.31671 0.80542 1.00000 0.04371 0.00000 0.00000 C8 0.82209 -0.22708 0.76074 1.00000 0.03833 0.04189 0.02871 -0.00376 0.00017 0.00810 0.03631 0.00809 0.00038 0.00028 0.00025 0.00000 0.00248 0.00256 0.00251 0.00202 0.00193 0.00202 0.00103 H8 0.89005 -0.24228 0.78174 1.00000 0.04357 0.00000 0.00000 C9 0.81839 -0.15960 0.71423 1.00000 0.03302 0.03843 0.03084 0.00242 0.00056 0.00363 0.03410 0.00802 0.00036 0.00029 0.00023 0.00000 0.00233 0.00246 0.00245 0.00196 0.00188 0.00194 0.00100 H9 0.88431 -0.13106 0.70283 1.00000 0.04092 0.00000 0.00000 C10 0.72054 -0.13571 0.68595 1.00000 0.03241 0.03510 0.03105 0.00247 0.00174 0.00431 0.03286 0.00768 0.00035 0.00027 0.00024 0.00000 0.00223 0.00239 0.00251 0.00195 0.00183 0.00184 0.00099 H10 0.71900 -0.09007 0.65531 1.00000 0.03943 0.00000 0.00000 C11 0.62119 -0.17745 0.70125 1.00000 0.03590 0.03001 0.02074 -0.00169 0.00071 0.00313 0.02888 0.00721 0.00035 0.00025 0.00021 0.00000 0.00227 0.00218 0.00205 0.00166 0.00173 0.00184 0.00090 C12 0.51814 -0.15230 0.67530 1.00000 0.03165 0.03157 0.02298 0.00215 -0.00315 0.00259 0.02873 0.00724 0.00032 0.00026 0.00022 0.00000 0.00215 0.00223 0.00219 0.00179 0.00170 0.00174 0.00091 H12 0.51558 -0.10649 0.64485 1.00000 0.03448 0.00000 0.00000 C13 -0.04083 0.07154 0.55244 1.00000 0.02953 0.03614 0.02797 0.00136 -0.00077 0.00460 0.03121 0.00760 0.00035 0.00026 0.00023 0.00000 0.00210 0.00242 0.00231 0.00190 0.00176 0.00183 0.00095 H13 -0.10955 0.09283 0.53695 1.00000 0.03746 0.00000 0.00000 C14 0.04809 0.12134 0.55191 1.00000 0.03217 0.03876 0.02167 -0.00318 -0.00299 0.00276 0.03087 0.00735 0.00035 0.00026 0.00023 0.00000 0.00220 0.00252 0.00218 0.00185 0.00172 0.00186 0.00096 C15 0.04666 0.20733 0.52880 1.00000 0.03037 0.03124 0.02359 -0.00060 0.00122 0.00580 0.02840 0.00738 0.00034 0.00026 0.00022 0.00000 0.00218 0.00224 0.00225 0.00176 0.00172 0.00178 0.00092 C16 0.11956 0.26468 0.55447 1.00000 0.03212 0.03665 0.02086 -0.00130 0.00256 0.00770 0.02988 0.00739 0.00034 0.00026 0.00021 0.00000 0.00226 0.00233 0.00209 0.00174 0.00174 0.00186 0.00092 H16 0.17343 0.24761 0.58729 1.00000 0.03585 0.00000 0.00000 C17 0.11742 0.34767 0.53399 1.00000 0.03179 0.03256 0.02552 -0.00006 0.00246 0.00491 0.02996 0.00736 0.00034 0.00026 0.00022 0.00000 0.00224 0.00223 0.00221 0.00173 0.00174 0.00180 0.00091 C18 0.19203 0.40680 0.56126 1.00000 0.03357 0.03437 0.02932 0.00147 0.00070 0.00700 0.03242 0.00768 0.00035 0.00026 0.00023 0.00000 0.00228 0.00247 0.00233 0.00188 0.00183 0.00185 0.00097 H18 0.24494 0.39075 0.59504 1.00000 0.03890 0.00000 0.00000 C19 0.18844 0.48640 0.53939 1.00000 0.03623 0.03882 0.04204 -0.00063 0.00432 -0.00075 0.03903 0.00867 0.00038 0.00028 0.00026 0.00000 0.00254 0.00263 0.00287 0.00215 0.00214 0.00197 0.00111 H19 0.23845 0.52526 0.55841 1.00000 0.04684 0.00000 0.00000 C20 0.11115 0.51155 0.48880 1.00000 0.04429 0.03386 0.04884 0.01214 0.00556 0.00473 0.04233 0.00926 0.00040 0.00030 0.00027 0.00000 0.00290 0.00249 0.00311 0.00220 0.00227 0.00211 0.00119 H20 0.11030 0.56683 0.47323 1.00000 0.05080 0.00000 0.00000 C21 0.03756 0.45630 0.46224 1.00000 0.03719 0.04267 0.03636 0.01173 0.00181 0.00662 0.03874 0.00883 0.00037 0.00030 0.00025 0.00000 0.00233 0.00259 0.00262 0.00229 0.00195 0.00225 0.00105 H21 -0.01509 0.47379 0.42881 1.00000 0.04649 0.00000 0.00000 C22 0.03876 0.37346 0.48387 1.00000 0.03104 0.03732 0.02535 0.00396 0.00309 0.00510 0.03124 0.00789 0.00035 0.00026 0.00023 0.00000 0.00220 0.00252 0.00228 0.00185 0.00180 0.00186 0.00097 C23 -0.03636 0.31426 0.45805 1.00000 0.03383 0.04402 0.02986 0.00705 -0.00499 0.00521 0.03590 0.00811 0.00037 0.00028 0.00024 0.00000 0.00233 0.00269 0.00246 0.00208 0.00193 0.00200 0.00104 H23 -0.09063 0.33055 0.42522 1.00000 0.04308 0.00000 0.00000 C24 -0.03272 0.23444 0.47916 1.00000 0.03818 0.04211 0.02637 -0.00134 -0.00316 0.00089 0.03555 0.00802 0.00037 0.00029 0.00024 0.00000 0.00245 0.00270 0.00244 0.00206 0.00191 0.00210 0.00104 H24 -0.08396 0.19626 0.46046 1.00000 0.04266 0.00000 0.00000 S1 0.09921 -0.17118 0.63027 1.00000 0.03178 0.03286 0.03812 0.00075 -0.00073 -0.00317 0.03425 0.00193 0.00009 0.00007 0.00006 0.00000 0.00055 0.00058 0.00065 0.00049 0.00045 0.00043 0.00027 S2 0.30042 -0.05721 0.64618 1.00000 0.03087 0.02997 0.02861 0.00086 -0.00029 -0.00082 0.02982 0.00182 0.00008 0.00006 0.00006 0.00000 0.00052 0.00057 0.00057 0.00044 0.00041 0.00042 0.00025 S3 -0.03545 -0.02799 0.57966 1.00000 0.03166 0.03569 0.03495 0.00054 -0.00147 -0.00348 0.03410 0.00193 0.00009 0.00007 0.00006 0.00000 0.00054 0.00063 0.00062 0.00049 0.00046 0.00045 0.00027 S4 0.17187 0.08028 0.58289 1.00000 0.03021 0.03090 0.02887 -0.00054 -0.00338 0.00040 0.02999 0.00182 0.00008 0.00007 0.00006 0.00000 0.00051 0.00054 0.00056 0.00045 0.00043 0.00042 0.00024 Ni1 0.13328 -0.04413 0.61035 1.00000 0.03029 0.02991 0.02484 -0.00138 -0.00029 -0.00118 0.02835 0.00090 0.00004 0.00003 0.00003 0.00000 0.00027 0.00028 0.00028 0.00023 0.00021 0.00022 0.00015 C25 0.66435 0.41849 0.06802 1.00000 0.03994 0.03634 0.02456 -0.00226 0.00106 0.00081 0.03361 0.00739 0.00036 0.00027 0.00023 0.00000 0.00241 0.00237 0.00226 0.00190 0.00178 0.00189 0.00098 H25A 0.69842 0.44620 0.02761 1.00000 0.04034 0.00000 0.00000 H25B 0.58339 0.41958 0.06102 1.00000 0.04034 0.00000 0.00000 C26 0.70158 0.32963 0.06796 1.00000 0.05463 0.03525 0.02777 -0.00191 -0.00481 0.00433 0.03922 0.00795 0.00041 0.00027 0.00024 0.00000 0.00289 0.00255 0.00254 0.00204 0.00208 0.00215 0.00110 H26A 0.78266 0.32691 0.06194 1.00000 0.04706 0.00000 0.00000 H26B 0.68270 0.30376 0.11293 1.00000 0.04706 0.00000 0.00000 C27 0.64517 0.28382 0.00928 1.00000 0.06509 0.04295 0.02807 -0.00762 0.00294 -0.00923 0.04537 0.00826 0.00046 0.00029 0.00026 0.00000 0.00340 0.00277 0.00254 0.00210 0.00239 0.00250 0.00124 H27A 0.64968 0.31725 -0.03354 1.00000 0.05444 0.00000 0.00000 H27B 0.56611 0.27682 0.02088 1.00000 0.05444 0.00000 0.00000 C28 0.69558 0.19995 -0.00477 1.00000 0.08864 0.03348 0.03603 0.00052 0.00302 -0.01018 0.05271 0.00949 0.00051 0.00030 0.00028 0.00000 0.00430 0.00268 0.00298 0.00224 0.00285 0.00263 0.00143 H28A 0.77348 0.20644 -0.01736 1.00000 0.07907 0.00000 0.00000 H28B 0.65594 0.17346 -0.04304 1.00000 0.07907 0.00000 0.00000 H28C 0.68977 0.16597 0.03704 1.00000 0.07907 0.00000 0.00000 C29 0.62405 0.43723 0.19420 1.00000 0.03599 0.03070 0.02535 0.00089 -0.00137 0.00265 0.03068 0.00741 0.00034 0.00025 0.00022 0.00000 0.00221 0.00227 0.00217 0.00166 0.00178 0.00184 0.00092 H29A 0.63670 0.37750 0.19884 1.00000 0.03682 0.00000 0.00000 H29B 0.65310 0.46366 0.23672 1.00000 0.03682 0.00000 0.00000 C30 0.50081 0.45205 0.19114 1.00000 0.03361 0.03886 0.03170 0.00057 0.00327 0.00085 0.03472 0.00806 0.00033 0.00030 0.00024 0.00000 0.00219 0.00245 0.00243 0.00212 0.00177 0.00202 0.00098 H30A 0.47209 0.43558 0.14507 1.00000 0.04167 0.00000 0.00000 H30B 0.48525 0.51113 0.19778 1.00000 0.04167 0.00000 0.00000 C31 0.44368 0.40231 0.24790 1.00000 0.03556 0.03022 0.04043 0.00157 0.00405 -0.00109 0.03540 0.00811 0.00035 0.00026 0.00026 0.00000 0.00239 0.00229 0.00268 0.00208 0.00203 0.00183 0.00102 H31A 0.45261 0.34315 0.23783 1.00000 0.04248 0.00000 0.00000 H31B 0.47979 0.41373 0.29300 1.00000 0.04248 0.00000 0.00000 C32 0.32176 0.42210 0.25351 1.00000 0.03935 0.03390 0.05273 -0.00662 0.00895 -0.00336 0.04200 0.00845 0.00036 0.00028 0.00029 0.00000 0.00254 0.00241 0.00314 0.00230 0.00232 0.00199 0.00114 H32A 0.31260 0.47921 0.26826 1.00000 0.06299 0.00000 0.00000 H32B 0.28734 0.38566 0.28769 1.00000 0.06299 0.00000 0.00000 H32C 0.28651 0.41423 0.20819 1.00000 0.06299 0.00000 0.00000 C33 0.66425 0.55693 0.11713 1.00000 0.03269 0.03086 0.02855 0.00604 0.00025 -0.00051 0.03070 0.00715 0.00033 0.00024 0.00022 0.00000 0.00204 0.00222 0.00228 0.00185 0.00171 0.00168 0.00091 H33A 0.70886 0.57464 0.07675 1.00000 0.03684 0.00000 0.00000 H33B 0.58558 0.56073 0.10358 1.00000 0.03684 0.00000 0.00000 C34 0.68446 0.61549 0.17564 1.00000 0.04009 0.03633 0.03252 0.00552 -0.00178 0.00191 0.03631 0.00805 0.00038 0.00027 0.00025 0.00000 0.00251 0.00249 0.00253 0.00202 0.00206 0.00199 0.00103 H34A 0.76276 0.61211 0.19010 1.00000 0.04357 0.00000 0.00000 H34B 0.63806 0.59996 0.21586 1.00000 0.04357 0.00000 0.00000 C35 0.65735 0.70433 0.15376 1.00000 0.04257 0.03050 0.03324 -0.00006 -0.00478 0.00284 0.03544 0.00789 0.00037 0.00026 0.00025 0.00000 0.00267 0.00227 0.00255 0.00189 0.00198 0.00190 0.00105 H35A 0.58343 0.70535 0.13185 1.00000 0.04253 0.00000 0.00000 H35B 0.65430 0.73924 0.19577 1.00000 0.04253 0.00000 0.00000 C36 0.74096 0.74029 0.10341 1.00000 0.05090 0.03748 0.03813 0.00355 0.00193 -0.00316 0.04217 0.00856 0.00039 0.00028 0.00027 0.00000 0.00278 0.00255 0.00284 0.00224 0.00236 0.00211 0.00113 H36A 0.81508 0.73646 0.12356 1.00000 0.06325 0.00000 0.00000 H36B 0.72302 0.79795 0.09456 1.00000 0.06325 0.00000 0.00000 H36C 0.73871 0.70966 0.05965 1.00000 0.06325 0.00000 0.00000 C37 0.81228 0.45802 0.15276 1.00000 0.03086 0.03714 0.02299 -0.00189 -0.00417 0.00550 0.03033 0.00732 0.00032 0.00028 0.00021 0.00000 0.00211 0.00232 0.00214 0.00188 0.00162 0.00193 0.00091 H37A 0.82606 0.48980 0.19569 1.00000 0.03640 0.00000 0.00000 H37B 0.82613 0.39953 0.16345 1.00000 0.03640 0.00000 0.00000 C38 0.89393 0.48551 0.09763 1.00000 0.03876 0.04543 0.03072 0.00710 -0.00002 -0.00095 0.03830 0.00826 0.00036 0.00029 0.00025 0.00000 0.00245 0.00267 0.00257 0.00202 0.00188 0.00197 0.00109 H38A 0.88334 0.54460 0.08790 1.00000 0.04596 0.00000 0.00000 H38B 0.88048 0.45478 0.05411 1.00000 0.04596 0.00000 0.00000 C39 1.01302 0.47047 0.12232 1.00000 0.03377 0.04830 0.03599 -0.00569 0.00478 0.00431 0.03935 0.00811 0.00035 0.00030 0.00026 0.00000 0.00227 0.00285 0.00274 0.00228 0.00192 0.00194 0.00111 H39A 1.02023 0.41269 0.13745 1.00000 0.04722 0.00000 0.00000 H39B 1.06404 0.47903 0.08282 1.00000 0.04722 0.00000 0.00000 C40 1.04665 0.52597 0.18131 1.00000 0.03905 0.07913 0.05160 -0.01427 -0.00158 -0.00341 0.05659 0.00895 0.00042 0.00037 0.00031 0.00000 0.00273 0.00421 0.00345 0.00309 0.00241 0.00271 0.00152 H40A 1.03447 0.58324 0.16794 1.00000 0.08489 0.00000 0.00000 H40B 1.12500 0.51757 0.19183 1.00000 0.08489 0.00000 0.00000 H40C 1.00234 0.51315 0.22248 1.00000 0.08489 0.00000 0.00000 N1 0.69081 0.46811 0.13240 1.00000 0.03332 0.02924 0.02288 0.00441 -0.00017 0.00035 0.02848 0.00586 0.00027 0.00021 0.00018 0.00000 0.00184 0.00189 0.00179 0.00148 0.00143 0.00144 0.00076 Final Structure Factor Calculation for 2006slh0986 in P2(1)2(1)2(1) Total number of l.s. parameters = 420 Maximum vector length = 511 Memory required = 5471 / 26068 wR2 = 0.1317 before cycle 7 for 7715 data and 2 / 420 parameters GooF = S = 0.986; Restrained GooF = 0.986 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0590 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0529 for 6360 Fo > 4sig(Fo) and 0.0679 for all 7715 data wR2 = 0.1317, GooF = S = 0.986, Restrained GooF = 0.986 for all data Flack x parameter = 0.0091 with esd 0.0160 Expected values are 0 (within 3 esd's) for correct and +1 for inverted absolute structure. Note that this rough estimate ignores correlation with other parameters; if the above value differs significantly from zero, it is ESSENTIAL to test the inverted structure or refine x as a full-matrix parameter using TWIN and BASF Occupancy sum of asymmetric unit = 46.00 for non-hydrogen and 52.00 for hydrogen atoms Principal mean square atomic displacements U 0.0366 0.0308 0.0251 C1 0.0355 0.0291 0.0241 C2 0.0379 0.0296 0.0250 C3 0.0452 0.0316 0.0228 C4 0.0448 0.0354 0.0233 C5 0.0409 0.0302 0.0233 C6 0.0540 0.0287 0.0266 C7 0.0488 0.0331 0.0270 C8 0.0408 0.0315 0.0300 C9 0.0394 0.0300 0.0292 C10 0.0373 0.0291 0.0203 C11 0.0343 0.0308 0.0212 C12 0.0386 0.0289 0.0262 C13 0.0406 0.0314 0.0206 C14 0.0366 0.0258 0.0228 C15 0.0424 0.0276 0.0197 C16 0.0373 0.0283 0.0242 C17 0.0412 0.0292 0.0268 C18 0.0445 0.0387 0.0339 C19 0.0591 0.0409 0.0270 C20 0.0541 0.0355 0.0266 C21 0.0417 0.0283 0.0237 C22 0.0477 0.0372 0.0228 C23 0.0426 0.0386 0.0255 C24 0.0385 0.0352 0.0291 S1 0.0315 0.0297 0.0282 S2 0.0382 0.0347 0.0295 S3 0.0332 0.0307 0.0261 S4 0.0314 0.0292 0.0244 Ni1 0.0401 0.0367 0.0241 C25 0.0565 0.0344 0.0268 C26 0.0692 0.0421 0.0248 C27 0.0906 0.0361 0.0314 C28 0.0372 0.0300 0.0249 C29 0.0392 0.0357 0.0293 C30 0.0428 0.0340 0.0294 C31 0.0594 0.0349 0.0317 C32 0.0359 0.0327 0.0235 C33 0.0410 0.0399 0.0280 C34 0.0451 0.0318 0.0294 C35 0.0517 0.0413 0.0335 C36 0.0411 0.0287 0.0212 C37 0.0484 0.0387 0.0278 C38 0.0509 0.0396 0.0276 C39 0.0853 0.0466 0.0379 C40 0.0334 0.0315 0.0206 N1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.033 0.048 0.063 0.077 0.092 0.112 0.132 0.166 0.229 1.000 Number in group 804. 755. 782. 760. 754. 804. 737. 771. 776. 772. GooF 0.861 0.868 0.956 0.959 1.003 1.027 1.008 1.022 1.082 1.052 K 0.969 1.012 1.033 1.029 1.025 1.031 1.028 1.007 0.991 1.007 Resolution(A) 0.80 0.83 0.86 0.90 0.95 1.01 1.09 1.20 1.37 1.71 inf Number in group 780. 798. 752. 762. 767. 775. 789. 751. 772. 769. GooF 0.876 0.938 1.045 0.954 1.011 0.943 1.006 0.961 0.991 1.121 K 1.022 1.000 1.004 1.010 1.008 1.021 1.024 1.004 0.994 1.011 R1 0.146 0.135 0.108 0.088 0.074 0.065 0.058 0.043 0.038 0.039 Recommended weighting scheme: WGHT 0.0589 0.0000 Note that in most cases convergence will be faster if fixed weights (e.g. the default WGHT 0.1) are retained until the refinement is virtually complete, and only then should the above recommended values be used. Most Disagreeable Reflections (* if suppressed or used for Rfree) h k l Fo^2 Fc^2 Delta(F^2)/esd Fc/Fc(max) Resolution(A) -5 4 20 290.15 1031.37 7.99 0.144 0.87 -4 8 11 2572.83 5427.32 7.28 0.331 1.22 -2 3 19 267.53 942.12 7.25 0.138 0.98 -10 10 1 635.65 1565.73 6.31 0.178 0.97 -3 11 10 776.77 1729.79 6.02 0.187 1.13 -1 11 18 221.76 802.18 5.91 0.127 0.87 9 0 16 1104.56 2223.34 5.85 0.212 0.90 -2 4 18 157.42 528.83 5.74 0.103 1.02 -4 4 13 851.65 1471.70 5.43 0.172 1.26 -2 8 6 3173.09 5023.40 5.30 0.318 1.66 0 1 2 8450.25 13893.31 5.15 0.529 8.29 -5 11 16 87.60 436.56 4.88 0.094 0.87 3 2 14 1523.09 2673.94 4.64 0.232 1.29 -6 5 20 0.79 220.99 4.46 0.067 0.84 -4 11 8 1047.93 1864.96 4.45 0.194 1.17 -3 10 17 -7.13 234.30 4.42 0.069 0.91 -1 6 14 942.91 1682.36 4.34 0.184 1.22 -2 13 15 714.62 1361.59 4.18 0.166 0.89 0 11 3 1450.39 2603.14 4.11 0.229 1.44 -2 1 4 22363.86 32353.03 4.10 0.807 3.67 0 7 1 34286.48 49676.88 4.05 1.000 2.31 5 2 6 308.62 174.40 4.05 0.059 1.88 -1 6 15 316.62 681.47 4.00 0.117 1.16 3 3 15 1338.74 1975.18 3.99 0.199 1.19 -5 11 8 299.34 556.38 3.96 0.106 1.12 -2 17 4 890.89 1640.40 3.96 0.182 0.93 2 6 9 2594.17 3620.53 3.83 0.270 1.62 1 5 0 612.15 421.05 3.77 0.092 3.15 -11 8 4 -8.96 148.59 3.76 0.055 0.95 -2 10 15 393.60 787.13 3.65 0.126 1.00 -4 5 19 332.35 655.42 3.58 0.115 0.92 -5 7 13 821.23 1362.04 3.54 0.166 1.11 -2 6 1 471.71 335.61 3.54 0.082 2.46 1 16 2 -40.02 122.60 3.50 0.050 1.01 5 0 2 2254.25 2977.21 3.38 0.245 2.35 2 1 19 1193.78 1787.77 3.37 0.190 1.00 11 12 1 695.23 1195.48 3.35 0.155 0.85 -2 9 12 1207.56 613.25 3.26 0.111 1.18 -2 1 3 34878.84 25588.94 3.26 0.718 4.25 13 5 3 1097.23 1586.34 3.25 0.179 0.89 0 3 1 7428.11 5476.14 3.21 0.332 5.23 0 6 8 520.05 369.01 3.20 0.086 1.80 -11 10 2 52.30 201.33 3.20 0.064 0.91 -1 9 10 381.31 592.09 3.18 0.109 1.31 12 8 4 37.50 160.02 3.16 0.057 0.89 3 0 9 302.65 164.23 3.12 0.057 1.89 -1 9 19 33.28 238.18 3.12 0.069 0.88 -6 1 6 507.72 343.91 3.09 0.083 1.70 9 5 15 2772.85 2113.39 3.08 0.206 0.89 1 17 0 139.36 342.86 3.08 0.083 0.96 Bond lengths and angles C1 - Distance Angles C2 1.3612 (0.0057) S1 1.7168 (0.0044) 121.80 (0.35) H1 0.9500 119.10 119.10 C1 - C2 S1 C2 - Distance Angles C1 1.3612 (0.0057) C3 1.4772 (0.0059) 122.90 (0.39) S2 1.7325 (0.0044) 118.01 (0.34) 119.10 (0.30) C2 - C1 C3 C3 - Distance Angles C12 1.3755 (0.0059) C4 1.4395 (0.0059) 117.46 (0.39) C2 1.4772 (0.0059) 121.56 (0.38) 120.94 (0.38) C3 - C12 C4 C4 - Distance Angles C5 1.3509 (0.0060) C3 1.4395 (0.0059) 121.30 (0.40) H4 0.9500 119.35 119.35 C4 - C5 C3 C5 - Distance Angles C4 1.3509 (0.0060) C6 1.4232 (0.0060) 121.14 (0.41) H5 0.9500 119.43 119.43 C5 - C4 C6 C6 - Distance Angles C7 1.4191 (0.0061) C11 1.4228 (0.0057) 119.27 (0.41) C5 1.4232 (0.0060) 122.08 (0.41) 118.61 (0.38) C6 - C7 C11 C7 - Distance Angles C8 1.3732 (0.0064) C6 1.4191 (0.0061) 120.33 (0.43) H7 0.9500 119.83 119.83 C7 - C8 C6 C8 - Distance Angles C7 1.3732 (0.0064) C9 1.4195 (0.0062) 120.24 (0.42) H8 0.9500 119.88 119.88 C8 - C7 C9 C9 - Distance Angles C10 1.3613 (0.0060) C8 1.4195 (0.0062) 120.12 (0.42) H9 0.9500 119.94 119.94 C9 - C10 C8 C10 - Distance Angles C9 1.3613 (0.0060) C11 1.4137 (0.0060) 121.33 (0.43) H10 0.9500 119.34 119.34 C10 - C9 C11 C11 - Distance Angles C12 1.4058 (0.0057) C10 1.4137 (0.0060) 122.77 (0.39) C6 1.4228 (0.0057) 118.56 (0.39) 118.66 (0.39) C11 - C12 C10 C12 - Distance Angles C3 1.3755 (0.0059) C11 1.4058 (0.0057) 122.90 (0.41) H12 0.9500 118.55 118.55 C12 - C3 C11 C13 - Distance Angles C14 1.3489 (0.0060) S3 1.7069 (0.0044) 122.98 (0.34) H13 0.9500 118.51 118.51 C13 - C14 S3 C14 - Distance Angles C13 1.3489 (0.0060) C15 1.4713 (0.0060) 124.51 (0.40) S4 1.7470 (0.0044) 116.87 (0.34) 118.60 (0.32) C14 - C13 C15 C15 - Distance Angles C16 1.3781 (0.0059) C24 1.4261 (0.0060) 117.53 (0.40) C14 1.4713 (0.0060) 122.05 (0.39) 120.42 (0.40) C15 - C16 C24 C16 - Distance Angles C15 1.3781 (0.0059) C17 1.4098 (0.0059) 122.63 (0.39) H16 0.9500 118.68 118.68 C16 - C15 C17 C17 - Distance Angles C16 1.4098 (0.0059) C22 1.4201 (0.0060) 119.13 (0.39) C18 1.4221 (0.0060) 122.41 (0.39) 118.46 (0.39) C17 - C16 C22 C18 - Distance Angles C19 1.3653 (0.0061) C17 1.4221 (0.0060) 120.70 (0.42) H18 0.9500 119.65 119.65 C18 - C19 C17 C19 - Distance Angles C18 1.3653 (0.0061) C20 1.4121 (0.0068) 120.67 (0.45) H19 0.9500 119.67 119.67 C19 - C18 C20 C20 - Distance Angles C21 1.3667 (0.0069) C19 1.4121 (0.0068) 119.94 (0.44) H20 0.9500 120.03 120.03 C20 - C21 C19 C21 - Distance Angles C20 1.3667 (0.0069) C22 1.4137 (0.0063) 120.87 (0.44) H21 0.9500 119.57 119.57 C21 - C20 C22 C22 - Distance Angles C21 1.4137 (0.0063) C23 1.4167 (0.0065) 122.77 (0.41) C17 1.4201 (0.0060) 119.35 (0.42) 117.88 (0.40) C22 - C21 C23 C23 - Distance Angles C24 1.3642 (0.0064) C22 1.4167 (0.0065) 121.66 (0.41) H23 0.9500 119.17 119.17 C23 - C24 C22 C24 - Distance Angles C23 1.3642 (0.0064) C15 1.4261 (0.0060) 121.15 (0.42) H24 0.9500 119.43 119.43 C24 - C23 C15 S1 - Distance Angles C1 1.7168 (0.0044) Ni1 2.1470 (0.0014) 103.73 (0.15) S1 - C1 S2 - Distance Angles C2 1.7325 (0.0044) Ni1 2.1494 (0.0014) 104.82 (0.14) S2 - C2 S3 - Distance Angles C13 1.7069 (0.0044) Ni1 2.1438 (0.0014) 103.76 (0.15) S3 - C13 S4 - Distance Angles C14 1.7470 (0.0044) Ni1 2.1481 (0.0014) 105.03 (0.16) S4 - C14 Ni1 - Distance Angles S3 2.1438 (0.0014) S1 2.1470 (0.0014) 89.11 (0.05) S4 2.1481 (0.0014) 91.35 (0.05) 175.70 (0.05) S2 2.1494 (0.0014) 177.00 (0.05) 91.60 (0.05) 88.15 (0.05) Ni1 - S3 S1 S4 C25 - Distance Angles N1 1.5147 (0.0053) C26 1.5176 (0.0062) 116.60 (0.36) H25A 0.9900 108.14 108.14 H25B 0.9900 108.14 108.14 107.32 C25 - N1 C26 H25A C26 - Distance Angles C27 1.5171 (0.0064) C25 1.5176 (0.0062) 109.68 (0.39) H26A 0.9900 109.73 109.73 H26B 0.9900 109.73 109.73 108.21 C26 - C27 C25 H26A C27 - Distance Angles C26 1.5171 (0.0064) C28 1.5220 (0.0067) 113.21 (0.45) H27A 0.9900 108.93 108.93 H27B 0.9900 108.93 108.93 107.75 C27 - C26 C28 H27A C28 - Distance Angles C27 1.5220 (0.0067) H28A 0.9800 109.47 H28B 0.9800 109.47 109.47 H28C 0.9800 109.47 109.47 109.47 C28 - C27 H28A H28B C29 - Distance Angles C30 1.5134 (0.0055) N1 1.5244 (0.0053) 116.11 (0.34) H29A 0.9900 108.26 108.26 H29B 0.9900 108.26 108.26 107.38 C29 - C30 N1 H29A C30 - Distance Angles C29 1.5134 (0.0055) C31 1.5269 (0.0061) 109.53 (0.36) H30A 0.9900 109.77 109.77 H30B 0.9900 109.77 109.77 108.23 C30 - C29 C31 H30A C31 - Distance Angles C32 1.5155 (0.0060) C30 1.5269 (0.0061) 112.30 (0.38) H31A 0.9900 109.14 109.14 H31B 0.9900 109.14 109.14 107.87 C31 - C32 C30 H31A C32 - Distance Angles C31 1.5155 (0.0060) H32A 0.9800 109.47 H32B 0.9800 109.47 109.47 H32C 0.9800 109.47 109.47 109.47 C32 - C31 H32A H32B C33 - Distance Angles C34 1.4971 (0.0061) N1 1.5126 (0.0051) 115.45 (0.35) H33A 0.9900 108.41 108.41 H33B 0.9900 108.41 108.41 107.46 C33 - C34 N1 H33A C34 - Distance Angles C33 1.4971 (0.0061) C35 1.5441 (0.0058) 111.00 (0.38) H34A 0.9900 109.44 109.44 H34B 0.9900 109.44 109.44 108.04 C34 - C33 C35 H34A C35 - Distance Angles C36 1.5197 (0.0064) C34 1.5441 (0.0058) 113.23 (0.38) H35A 0.9900 108.93 108.93 H35B 0.9900 108.93 108.93 107.75 C35 - C36 C34 H35A C36 - Distance Angles C35 1.5197 (0.0064) H36A 0.9800 109.47 H36B 0.9800 109.47 109.47 H36C 0.9800 109.47 109.47 109.47 C36 - C35 H36A H36B C37 - Distance Angles C38 1.5185 (0.0060) N1 1.5317 (0.0049) 114.52 (0.34) H37A 0.9900 108.63 108.63 H37B 0.9900 108.63 108.63 107.58 C37 - C38 N1 H37A C38 - Distance Angles C37 1.5185 (0.0059) C39 1.5385 (0.0060) 110.34 (0.37) H38A 0.9900 109.59 109.59 H38B 0.9900 109.59 109.59 108.12 C38 - C37 C39 H38A C39 - Distance Angles C40 1.5085 (0.0068) C38 1.5385 (0.0060) 112.97 (0.39) H39A 0.9900 108.99 108.99 H39B 0.9900 108.99 108.99 107.78 C39 - C40 C38 H39A C40 - Distance Angles C39 1.5085 (0.0068) H40A 0.9800 109.47 H40B 0.9800 109.47 109.47 H40C 0.9800 109.47 109.47 109.47 C40 - C39 H40A H40B N1 - Distance Angles C33 1.5126 (0.0051) C25 1.5147 (0.0053) 107.90 (0.31) C29 1.5244 (0.0053) 110.81 (0.31) 110.50 (0.31) C37 1.5317 (0.0049) 110.91 (0.32) 110.81 (0.31) 105.92 (0.30) N1 - C33 C25 C29 FMAP and GRID set by program FMAP 2 3 23 GRID -1.250 -2 -2 1.250 2 2 R1 = 0.0540 for 4309 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.36 at 0.2861 -0.0043 0.0923 [ 1.30 A from NI1 ] Deepest hole -0.42 at 0.3010 0.0456 0.1124 [ 0.80 A from NI1 ] Mean = 0.00, Rms deviation from mean = 0.07 e/A^3, Highest memory used = 5275 / 31077 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.2139 0.0043 0.5923 1.00000 0.05 0.36 1.30 NI1 1.35 S4 1.78 S2 2.71 H25A Q2 1 0.0951 0.0425 0.6153 1.00000 0.05 0.30 1.28 S4 1.49 NI1 1.86 C14 2.07 S3 Q3 1 -0.0262 0.1435 0.4257 1.00000 0.05 0.29 1.30 H24 1.81 C24 2.05 H40A 2.38 H38A Q4 1 0.0380 -0.0135 0.6149 1.00000 0.05 0.29 1.14 S3 1.26 NI1 2.07 C13 2.31 S4 Q5 1 0.1568 0.1641 0.5858 1.00000 0.05 0.28 1.38 H16 1.38 S4 1.63 C14 1.81 C16 Q6 1 0.1958 -0.0820 0.6449 1.00000 0.05 0.27 1.18 NI1 1.33 S2 1.89 S1 1.96 C2 Q7 1 0.0745 -0.0386 0.6525 1.00000 0.05 0.26 1.08 NI1 1.94 S3 2.23 S1 2.56 H31B Q8 1 1.0962 0.4068 0.0816 1.00000 0.05 0.26 1.24 H39B 1.42 H39A 1.65 C39 1.67 H28B Q9 1 0.8671 0.2433 0.0014 1.00000 0.05 0.26 1.33 H28A 2.07 H26A 2.20 C28 2.47 H27B Q10 1 0.4664 -0.1803 0.6571 1.00000 0.05 0.25 0.85 C12 0.89 C3 1.36 H12 1.90 C2 Shortest distances between peaks (including symmetry equivalents) 4 7 0.94 2 4 1.14 2 7 1.52 1 2 1.63 6 7 1.64 1 6 1.75 1 7 2.16 1 4 2.19 2 5 2.19 4 6 2.29 2 6 2.44 1 5 2.70 Time profile in seconds ----------------------- 0.03: Read and process instructions 0.00: Fit rigid groups 0.01: Interpret restraints etc. 0.00: Generate connectivity array 0.01: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 1.14: 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 13.37: Structure factors and derivatives 17.86: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 1.08: Solve l.s. equations 0.00: Generate HTAB table 0.04: Other dependent quantities, CIF, tables 0.21: Analysis of variance 0.09: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.18: Peaksearch 0.01: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2006slh0986 finished at 15:29:03 Total CPU time: 34.1 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++