+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 04skc0014p21c started at 11:33:42 on 13-Aug-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 04skc0014p21c in P2(1)/c CELL 0.71073 8.8190 13.0997 8.3959 90.000 97.523 90.000 ZERR 4.00 0.0019 0.0051 0.0019 0.000 0.026 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O UNIT 28 64 8 24 V = 961.60 F(000) = 480.0 Mu = 0.14 mm-1 Cell Wt = 896.87 Rho = 1.549 MERG 2 OMIT -3.00 55.00 OMIT 2 1 1 SHEL 7 0.77 EADP N25A N21A EADP N25B N21B EADP C23A C22A EADP C23B C22B DELU C22A > C24A DELU C22B > C24B FMAP 2 PLAN 10 SIZE 0.02 0.04 0.14 ACTA EQIV_$1 -x+2, -y+1, -z HTAB O2 O4B_$1 EQIV_$2 x, -y+3/2, z+1/2 HTAB O3 O1B_$2 EQIV_$3 x-1, -y+1/2, z-1/2 HTAB N21A O4B_$3 HTAB N21B O4B_$3 EQIV_$4 -x+1, y-1/2, -z+1/2 HTAB N21A O4A_$4 HTAB N21B O4A_$4 EQIV_$5 -x+1, -y+1, -z HTAB N21A O2_$5 HTAB N21B O2_$5 HTAB N21B O1B_$5 EQIV_$6 -x, -y+1, -z HTAB N25A O3_$6 HTAB N25A O1B_$6 EQIV_$7 -x, y-1/2, -z+1/2 HTAB N25A O3_$7 HTAB N25A O4A_$7 HTAB N25B O4A_$7 HTAB N25B O3_$7 EQIV_$8 -x, y-1/2, -z-1/2 HTAB N25A O1A_$8 HTAB N25B O1A_$8 EQIV_$9 x-1, -y+1/2, z+1/2 HTAB N25B O1A_$9 BOND $H WGHT 0.05870 1.38890 L.S. 4 TEMP -153.00 FVAR 0.92103 0.50620 MOLE 1 C1 1 0.734121 0.633506 -0.205305 11.00000 0.01437 0.01536 = 0.01220 0.00061 0.00194 0.00026 C2 1 0.813246 0.572414 -0.061816 11.00000 0.01119 0.01193 = 0.01235 -0.00085 -0.00025 -0.00079 AFIX 13 H2 2 0.845203 0.505068 -0.102564 11.00000 -1.20000 AFIX 0 C3 1 0.702959 0.552328 0.060324 11.00000 0.01135 0.01085 = 0.01326 -0.00026 -0.00004 0.00028 AFIX 13 H3 2 0.624484 0.503055 0.009561 11.00000 -1.20000 AFIX 0 C4 1 0.784728 0.500481 0.212034 11.00000 0.00905 0.01345 = 0.01403 0.00208 0.00051 -0.00220 O1A 4 0.614224 0.595015 -0.277129 11.00000 0.03533 0.03947 = 0.03160 0.01948 -0.02130 -0.02139 O1B 4 0.794473 0.714254 -0.241091 11.00000 0.02032 0.01654 = 0.02402 0.00720 -0.00172 -0.00176 O2 4 0.946042 0.622455 0.015636 11.00000 0.00965 0.01670 = 0.01449 -0.00068 0.00123 -0.00118 AFIX 147 H2A 2 1.018852 0.613815 -0.038221 11.00000 -1.50000 AFIX 0 O3 4 0.623843 0.641786 0.095779 11.00000 0.01331 0.01235 = 0.01873 -0.00175 0.00137 0.00239 AFIX 147 H3A 2 0.685639 0.683181 0.145474 11.00000 -1.50000 AFIX 0 O4A 4 0.768995 0.538168 0.345834 11.00000 0.01508 0.01632 = 0.01317 -0.00126 0.00240 0.00030 O4B 4 0.861108 0.421037 0.192354 11.00000 0.01720 0.01467 = 0.01563 0.00207 0.00368 0.00434 MOLE 2 PART 1 C22A 1 -0.124058 0.143485 0.097115 21.00000 0.01157 0.02134 = 0.00937 -0.00034 0.00083 -0.00443 AFIX 23 H22A 2 -0.150853 0.070110 0.097775 21.00000 -1.20000 H22B 2 -0.087509 0.164876 0.208637 21.00000 -1.20000 AFIX 0 C23A 1 -0.262348 0.206137 0.029599 21.00000 0.01157 0.02134 = 0.00937 -0.00034 0.00083 -0.00443 AFIX 23 H23A 2 -0.231887 0.278747 0.025861 21.00000 -1.20000 H23B 2 -0.296462 0.183785 -0.081984 21.00000 -1.20000 AFIX 0 C24A 1 -0.395424 0.197184 0.126372 21.00000 0.02095 0.02010 = 0.01574 -0.00414 0.00715 -0.00269 AFIX 23 H24A 2 -0.362209 0.146068 0.210606 21.00000 -1.20000 H24B 2 -0.398046 0.263342 0.182946 21.00000 -1.20000 AFIX 0 N21A 3 0.006040 0.162816 -0.016134 21.00000 0.01102 0.01494 = 0.01241 0.00263 0.00109 0.00174 AFIX 137 H21A 2 -0.022573 0.133745 -0.113889 21.00000 -1.50000 H21B 2 0.095501 0.134533 0.029655 21.00000 -1.50000 H21C 2 0.019039 0.231145 -0.028449 21.00000 -1.50000 AFIX 0 N25A 3 -0.533554 0.176186 0.079803 21.00000 0.01102 0.01494 = 0.01241 0.00263 0.00109 0.00174 AFIX 137 H25A 2 -0.587266 0.235015 0.058491 21.00000 -1.50000 H25B 2 -0.573128 0.140893 0.158129 21.00000 -1.50000 H25C 2 -0.540024 0.137484 -0.010841 21.00000 -1.50000 AFIX 0 PART 2 C22B 1 -0.102219 0.144864 0.100771 -21.00000 0.01245 0.01338 = 0.01776 0.00043 0.00099 -0.00133 AFIX 23 H22C 2 -0.064311 0.182714 0.200101 -21.00000 -1.20000 H22D 2 -0.108355 0.071796 0.129355 -21.00000 -1.20000 AFIX 0 C23B 1 -0.262679 0.182937 0.038261 -21.00000 0.01245 0.01338 = 0.01776 0.00043 0.00099 -0.00133 AFIX 23 H23C 2 -0.263911 0.258506 0.038427 -21.00000 -1.20000 H23D 2 -0.291541 0.159385 -0.073645 -21.00000 -1.20000 AFIX 0 C24B 1 -0.376484 0.143190 0.142684 -21.00000 0.01253 0.01577 = 0.01197 0.00370 -0.00100 0.00075 AFIX 23 H24C 2 -0.321520 0.095013 0.220794 -21.00000 -1.20000 H24D 2 -0.408693 0.201614 0.205110 -21.00000 -1.20000 AFIX 0 N21B 3 0.000357 0.155592 -0.005635 -21.00000 0.01638 0.01443 = 0.01285 0.00073 0.00060 -0.00159 AFIX 137 H21D 2 -0.045264 0.139510 -0.106041 -21.00000 -1.50000 H21E 2 0.081128 0.113124 0.022285 -21.00000 -1.50000 H21F 2 0.033877 0.221323 -0.004380 -21.00000 -1.50000 AFIX 0 N25B 3 -0.485218 0.102963 0.084355 -21.00000 0.01638 0.01443 = 0.01285 0.00073 0.00060 -0.00159 AFIX 137 H25D 2 -0.501433 0.118332 -0.022218 -21.00000 -1.50000 H25E 2 -0.566494 0.124365 0.132076 -21.00000 -1.50000 H25F 2 -0.474043 0.034259 0.096902 -21.00000 -1.50000 AFIX 0 HKLF 4 Covalent radii and connectivity table for 04skc0014p21c in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1B O1A C2 C2 - O2 C3 C1 C3 - O3 C2 C4 C4 - O4A O4B C3 O1A - C1 O1B - C1 O2 - C2 O3 - C3 O4A - C4 O4B - C4 C22A_a - C23A_a N21A_a C23A_a - C24A_a C22A_a C24A_a - N25A_a C23A_a N21A_a - C22A_a N25A_a - C24A_a C22B_b - N21B_b C23B_b C23B_b - C24B_b C22B_b C24B_b - N25B_b C23B_b N21B_b - C22B_b N25B_b - C24B_b Operators for generating equivalent atoms: $1 -x+2, -y+1, -z $2 x, -y+3/2, z+1/2 $3 x-1, -y+1/2, z-1/2 $4 -x+1, y-1/2, -z+1/2 $5 -x+1, -y+1, -z $6 -x, -y+1, -z $7 -x, y-1/2, -z+1/2 $8 -x, y-1/2, -z-1/2 $9 x-1, -y+1/2, z+1/2 15796 Reflections read, of which 439 rejected -11 =< h =< 11, -16 =< k =< 17, -10 =< l =< 10, Max. 2-theta = 54.97 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 1 3 7 8.58 0.42 9 2.65 1 Inconsistent equivalents 2201 Unique reflections, of which 0 suppressed R(int) = 0.0483 R(sigma) = 0.0328 Friedel opposites merged Maximum memory for data reduction = 3053 / 21668 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 = 3622 / 204461 wR2 = 0.1367 before cycle 1 for 2201 data and 164 / 164 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 6. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.010 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.002 0.000 0.000 0.000 GooF = S = 1.035; Restrained GooF = 1.034 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0587 * P )^2 + 1.39 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.92101 0.00280 -0.007 OSF 2 0.50613 0.00545 -0.013 FVAR 2 Mean shift/esd = 0.012 Maximum = 0.081 for x C23A_a Max. shift = 0.002 A for C22A_a Max. dU = 0.000 for C22A_a Least-squares cycle 2 Maximum vector length = 511 Memory required = 3622 / 204461 wR2 = 0.1367 before cycle 2 for 2201 data and 164 / 164 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 6. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.010 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.002 0.000 0.000 0.000 GooF = S = 1.035; Restrained GooF = 1.034 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0587 * P )^2 + 1.39 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.92100 0.00280 -0.006 OSF 2 0.50612 0.00544 0.000 FVAR 2 Mean shift/esd = 0.007 Maximum = -0.063 for x C23B_b Max. shift = 0.002 A for C22A_a Max. dU = 0.000 for C22A_a Least-squares cycle 3 Maximum vector length = 511 Memory required = 3622 / 204461 wR2 = 0.1366 before cycle 3 for 2201 data and 164 / 164 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 6. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.010 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.002 0.000 0.000 0.000 GooF = S = 1.035; Restrained GooF = 1.034 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0587 * P )^2 + 1.39 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.92100 0.00280 0.002 OSF 2 0.50615 0.00544 0.004 FVAR 2 Mean shift/esd = 0.004 Maximum = -0.040 for x C23B_b Max. shift = 0.001 A for H22B_a Max. dU = 0.000 for C22A_a Least-squares cycle 4 Maximum vector length = 511 Memory required = 3622 / 204461 wR2 = 0.1366 before cycle 4 for 2201 data and 164 / 164 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 6. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.010 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.002 0.000 0.000 0.000 GooF = S = 1.035; Restrained GooF = 1.034 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0587 * P )^2 + 1.39 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.92101 0.00280 0.002 OSF 2 0.50618 0.00544 0.006 FVAR 2 Mean shift/esd = 0.003 Maximum = -0.025 for x C23B_b Max. shift = 0.001 A for H25E_b Max. dU = 0.000 for C22A_a Largest correlation matrix elements -0.981 y C22B_b / y C22A_a 0.864 y C22B_b / x C23A_a 0.802 U12 C22A_a / y C22A_a -0.964 x N21B_b / x N21A_a 0.861 x C23B_b / y C22A_a 0.794 x C23B_b / U12 C22B_b -0.957 z N21B_b / z N21A_a 0.861 U12 C22B_b / y C22A_a -0.769 x C23A_a / U12 C22A_a -0.951 y N21B_b / y N21A_a -0.856 U12 C22B_b / x C23A_a -0.743 z C23B_b / z C23A_a -0.946 x C23B_b / x C23A_a -0.834 y C22B_b / U12 C22A_a 0.651 y C24B_b / y C24A_a -0.904 z C22B_b / z C22A_a 0.832 x C23B_b / U12 C22A_a -0.629 U11 C22B_b / U11 C22A_a -0.869 x C23A_a / y C22A_a -0.830 U12 C22B_b / y C22B_b 0.617 y C23B_b / U22 C22A_a -0.866 x C23B_b / y C22B_b -0.816 U33 C22B_b / U33 C22A_a -0.612 tors H21D_b / tors H21A_a Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.8452 0.5051 -0.1026 13 1.000 0.000 C2 O2 C3 C1 H3 0.6245 0.5031 0.0096 13 1.000 0.000 C3 O3 C2 C4 H2A 1.0189 0.6138 -0.0382 147 0.840 0.000 O2 C2 H2A H3A 0.6856 0.6832 0.1454 147 0.840 0.000 O3 C3 H3A H22A -0.1510 0.0698 0.0975 23 0.990 0.000 C22A_a C23A_a N21A_a H22B -0.0875 0.1643 0.2089 23 0.990 0.000 C22A_a C23A_a N21A_a H23A -0.2313 0.2787 0.0263 23 0.990 0.000 C23A_a C24A_a C22A_a H23B -0.2961 0.1840 -0.0820 23 0.990 0.000 C23A_a C24A_a C22A_a H24A -0.3623 0.1461 0.2107 23 0.990 0.000 C24A_a N25A_a C23A_a H24B -0.3981 0.2634 0.1829 23 0.990 0.000 C24A_a N25A_a C23A_a H21A -0.0226 0.1339 -0.1140 137 0.910 0.000 N21A_a C22A_a H21A_a H21B 0.0956 0.1345 0.0294 137 0.910 0.000 N21A_a C22A_a H21A_a H21C 0.0188 0.2312 -0.0282 137 0.910 0.000 N21A_a C22A_a H21A_a H25A -0.5873 0.2350 0.0585 137 0.910 0.000 N25A_a C24A_a H25A_a H25B -0.5731 0.1409 0.1581 137 0.910 0.000 N25A_a C24A_a H25A_a H25C -0.5400 0.1375 -0.0108 137 0.910 0.000 N25A_a C24A_a H25A_a H22C -0.0644 0.1834 0.1996 23 0.990 0.001 C22B_b N21B_b C23B_b H22D -0.1081 0.0722 0.1298 23 0.990 0.001 C22B_b N21B_b C23B_b H23C -0.2646 0.2585 0.0382 23 0.990 0.000 C23B_b C24B_b C22B_b H23D -0.2919 0.1592 -0.0736 23 0.990 0.000 C23B_b C24B_b C22B_b H24C -0.3214 0.0950 0.2207 23 0.990 0.000 C24B_b N25B_b C23B_b H24D -0.4087 0.2016 0.2052 23 0.990 0.000 C24B_b N25B_b C23B_b H21D -0.0452 0.1394 -0.1060 137 0.910 0.000 N21B_b C22B_b H21D_b H21E 0.0810 0.1131 0.0226 137 0.910 0.000 N21B_b C22B_b H21D_b H21F 0.0341 0.2213 -0.0046 137 0.910 0.000 N21B_b C22B_b H21D_b H25D -0.5016 0.1185 -0.0221 137 0.910 0.000 N25B_b C24B_b H25D_b H25E -0.5664 0.1242 0.1323 137 0.910 0.000 N25B_b C24B_b H25D_b H25F -0.4739 0.0342 0.0966 137 0.910 0.000 N25B_b C24B_b H25D_b 04skc0014p21c in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.73412 0.63350 -0.20530 1.00000 0.01438 0.01537 0.01219 0.00061 0.00194 0.00027 0.01396 0.00350 0.00022 0.00015 0.00023 0.00000 0.00088 0.00091 0.00091 0.00070 0.00070 0.00070 0.00039 C2 0.81324 0.57241 -0.06182 1.00000 0.01119 0.01191 0.01236 -0.00084 -0.00025 -0.00077 0.01198 0.00323 0.00020 0.00014 0.00022 0.00000 0.00085 0.00085 0.00090 0.00068 0.00066 0.00067 0.00038 H2 0.84520 0.50507 -0.10257 1.00000 0.01437 0.00000 0.00000 C3 0.70296 0.55233 0.06032 1.00000 0.01135 0.01084 0.01325 -0.00027 -0.00004 0.00028 0.01196 0.00332 0.00021 0.00014 0.00023 0.00000 0.00083 0.00083 0.00092 0.00069 0.00066 0.00066 0.00038 H3 0.62448 0.50305 0.00956 1.00000 0.01435 0.00000 0.00000 C4 0.78472 0.50048 0.21203 1.00000 0.00903 0.01344 0.01405 0.00208 0.00051 -0.00221 0.01226 0.00337 0.00020 0.00014 0.00023 0.00000 0.00081 0.00089 0.00093 0.00069 0.00067 0.00066 0.00038 O1A 0.61422 0.59502 -0.27713 1.00000 0.03531 0.03949 0.03160 0.01948 -0.02129 -0.02139 0.03774 0.00296 0.00020 0.00014 0.00021 0.00000 0.00098 0.00103 0.00098 0.00081 0.00077 0.00081 0.00050 O1B 0.79447 0.71426 -0.24109 1.00000 0.02030 0.01653 0.02401 0.00721 -0.00172 -0.00175 0.02069 0.00271 0.00017 0.00011 0.00019 0.00000 0.00074 0.00072 0.00080 0.00059 0.00058 0.00056 0.00034 O2 0.94604 0.62246 0.01563 1.00000 0.00965 0.01669 0.01448 -0.00068 0.00122 -0.00118 0.01364 0.00239 0.00015 0.00010 0.00016 0.00000 0.00062 0.00069 0.00068 0.00052 0.00050 0.00050 0.00031 H2A 1.01886 0.61380 -0.03820 1.00000 0.02046 0.00000 0.00000 O3 0.62384 0.64179 0.09578 1.00000 0.01330 0.01234 0.01872 -0.00175 0.00137 0.00240 0.01485 0.00251 0.00015 0.00010 0.00017 0.00000 0.00065 0.00065 0.00072 0.00053 0.00053 0.00050 0.00031 H3A 0.68564 0.68319 0.14545 1.00000 0.02228 0.00000 0.00000 O4A 0.76899 0.53817 0.34583 1.00000 0.01508 0.01631 0.01317 -0.00126 0.00241 0.00030 0.01480 0.00245 0.00015 0.00010 0.00016 0.00000 0.00066 0.00069 0.00069 0.00052 0.00051 0.00052 0.00031 O4B 0.86111 0.42104 0.19235 1.00000 0.01720 0.01466 0.01563 0.00207 0.00368 0.00434 0.01569 0.00257 0.00016 0.00010 0.00017 0.00000 0.00068 0.00068 0.00071 0.00052 0.00052 0.00053 0.00032 C22A_a -0.12402 0.14312 0.09728 0.50618 0.01152 0.02140 0.00914 -0.00038 0.00108 -0.00492 0.01404 0.02285 0.00073 0.00176 0.00121 0.00544 0.00205 0.00210 0.00224 0.00150 0.00157 0.00248 0.00130 H22A_a -0.15098 0.06976 0.09749 0.50618 0.01685 0.00544 0.00000 H22B_a -0.08747 0.16427 0.20891 0.50618 0.01685 0.00544 0.00000 C23A_a -0.26203 0.20614 0.02965 0.50618 0.01152 0.02140 0.00914 -0.00038 0.00108 -0.00492 0.01404 0.01886 0.00153 0.00049 0.00081 0.00544 0.00205 0.00210 0.00224 0.00150 0.00157 0.00248 0.00130 H23A_a -0.23128 0.27871 0.02625 0.50618 0.01685 0.00544 0.00000 H23B_a -0.29607 0.18398 -0.08205 0.50618 0.01685 0.00544 0.00000 C24A_a -0.39543 0.19719 0.12638 0.50618 0.02091 0.02012 0.01574 -0.00416 0.00717 -0.00271 0.01850 0.00821 0.00052 0.00049 0.00055 0.00544 0.00219 0.00262 0.00214 0.00199 0.00161 0.00204 0.00098 H24A_a -0.36226 0.14610 0.21067 0.50618 0.02220 0.00544 0.00000 H24B_a -0.39809 0.26336 0.18290 0.50618 0.02220 0.00544 0.00000 N21A_a 0.00600 0.16280 -0.01615 0.50618 0.01104 0.01493 0.01240 0.00261 0.00109 0.00175 0.01283 0.02364 0.00141 0.00086 0.00141 0.00544 0.00132 0.00178 0.00150 0.00101 0.00098 0.00109 0.00086 H21A_a -0.02265 0.13386 -0.11399 0.50618 0.01924 0.00544 0.00000 H21B_a 0.09556 0.13455 0.02944 0.50618 0.01924 0.00544 0.00000 H21C_a 0.01884 0.23117 -0.02822 0.50618 0.01924 0.00544 0.00000 N25A_a -0.53356 0.17618 0.07980 0.50618 0.01104 0.01493 0.01240 0.00261 0.00109 0.00175 0.01283 0.00583 0.00035 0.00026 0.00039 0.00544 0.00132 0.00178 0.00150 0.00101 0.00098 0.00109 0.00086 H25A_a -0.58727 0.23501 0.05847 0.50618 0.01924 0.00544 0.00000 H25B_a -0.57313 0.14089 0.15813 0.50618 0.01924 0.00544 0.00000 H25C_a -0.54001 0.13747 -0.01084 0.50618 0.01924 0.00544 0.00000 C22B_b -0.10222 0.14522 0.10058 0.49382 0.01250 0.01314 0.01809 0.00042 0.00098 -0.00176 0.01467 0.02294 0.00077 0.00172 0.00133 0.00544 0.00218 0.00188 0.00271 0.00152 0.00175 0.00263 0.00139 H22C_b -0.06435 0.18337 0.19963 0.49382 0.01760 0.00544 0.00000 H22D_b -0.10813 0.07223 0.12976 0.49382 0.01760 0.00544 0.00000 C23B_b -0.26301 0.18292 0.03824 0.49382 0.01250 0.01314 0.01809 0.00042 0.00098 -0.00176 0.01467 0.01972 0.00157 0.00048 0.00089 0.00544 0.00218 0.00188 0.00271 0.00152 0.00175 0.00263 0.00139 H23C_b -0.26455 0.25849 0.03819 0.49382 0.01760 0.00544 0.00000 H23D_b -0.29189 0.15923 -0.07358 0.49382 0.01760 0.00544 0.00000 C24B_b -0.37648 0.14318 0.14268 0.49382 0.01253 0.01579 0.01197 0.00366 -0.00102 0.00077 0.01366 0.00831 0.00048 0.00046 0.00050 0.00544 0.00194 0.00252 0.00199 0.00181 0.00142 0.00179 0.00092 H24C_b -0.32143 0.09499 0.22070 0.49382 0.01640 0.00544 0.00000 H24D_b -0.40865 0.20158 0.20519 0.49382 0.01640 0.00544 0.00000 N21B_b 0.00039 0.15560 -0.00563 0.49382 0.01638 0.01445 0.01284 0.00075 0.00062 -0.00159 0.01467 0.02445 0.00154 0.00091 0.00146 0.00544 0.00149 0.00181 0.00158 0.00108 0.00108 0.00118 0.00091 H21D_b -0.04518 0.13940 -0.10600 0.49382 0.02201 0.00544 0.00000 H21E_b 0.08104 0.11308 0.02255 0.49382 0.02201 0.00544 0.00000 H21F_b 0.03407 0.22129 -0.00460 0.49382 0.02201 0.00544 0.00000 N25B_b -0.48521 0.10296 0.08436 0.49382 0.01638 0.01445 0.01284 0.00075 0.00062 -0.00159 0.01467 0.00594 0.00038 0.00026 0.00040 0.00544 0.00149 0.00181 0.00158 0.00108 0.00108 0.00118 0.00091 H25D_b -0.50163 0.11852 -0.02214 0.49382 0.02201 0.00544 0.00000 H25E_b -0.56643 0.12419 0.13234 0.49382 0.02201 0.00544 0.00000 H25F_b -0.47390 0.03424 0.09658 0.49382 0.02201 0.00544 0.00000 Final Structure Factor Calculation for 04skc0014p21c in P2(1)/c Total number of l.s. parameters = 164 Maximum vector length = 511 Memory required = 3458 / 22995 wR2 = 0.1366 before cycle 5 for 2201 data and 0 / 164 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 6. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.010 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.002 0.000 0.000 0.000 GooF = S = 1.035; Restrained GooF = 1.034 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0587 * P )^2 + 1.39 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0514 for 1889 Fo > 4sig(Fo) and 0.0626 for all 2201 data wR2 = 0.1366, GooF = S = 1.035, Restrained GooF = 1.034 for all data Occupancy sum of asymmetric unit = 15.00 for non-hydrogen and 16.00 for hydrogen atoms Principal mean square atomic displacements U 0.0155 0.0143 0.0120 C1 0.0139 0.0124 0.0096 C2 0.0145 0.0108 0.0105 C3 0.0168 0.0119 0.0081 C4 0.0845 0.0181 0.0107 O1A 0.0315 0.0184 0.0121 O1B 0.0170 0.0145 0.0095 O2 0.0197 0.0147 0.0101 O3 0.0168 0.0152 0.0125 O4A 0.0212 0.0145 0.0114 O4B 0.0234 0.0097 0.0090 C22A_a 0.0234 0.0097 0.0090 C23A_a 0.0262 0.0178 0.0115 C24A_a 0.0167 0.0121 0.0097 N21A_a 0.0167 0.0121 0.0097 N25A_a 0.0186 0.0144 0.0110 C22B_b 0.0186 0.0144 0.0110 C23B_b 0.0183 0.0142 0.0085 C24B_b 0.0180 0.0136 0.0125 N21B_b 0.0180 0.0136 0.0125 N25B_b Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.015 0.028 0.041 0.055 0.072 0.091 0.117 0.150 0.211 1.000 Number in group 228. 214. 218. 221. 225. 218. 218. 219. 223. 217. GooF 1.189 0.989 0.989 0.952 1.100 1.011 1.057 1.020 0.990 1.026 K 3.850 1.268 1.096 0.997 1.003 1.001 1.000 0.999 1.012 0.995 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.31 1.64 inf Number in group 225. 222. 221. 220. 217. 215. 220. 223. 217. 221. GooF 0.827 0.814 0.880 0.823 0.850 0.832 0.838 0.969 1.335 1.757 K 0.997 1.021 1.025 1.031 1.016 0.993 0.993 1.006 1.016 0.991 R1 0.112 0.098 0.089 0.074 0.066 0.054 0.043 0.051 0.053 0.049 Recommended weighting scheme: WGHT 0.0599 1.3327 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) 2 2 2 96.55 36.00 6.30 0.057 2.60 3 1 1 213.17 125.44 4.98 0.106 2.59 3 2 2 14.12 0.15 4.91 0.004 2.13 3 3 0 160.72 93.94 4.54 0.092 2.42 4 3 2 40.47 87.49 4.30 0.089 1.69 0 6 1 15.40 1.75 4.29 0.013 2.11 4 2 0 87.66 45.23 4.27 0.064 2.07 -4 7 2 63.32 119.85 4.24 0.104 1.38 1 6 1 16.39 2.16 4.04 0.014 2.04 5 3 2 8.37 33.67 4.02 0.055 1.45 5 2 0 2.14 19.59 3.80 0.042 1.69 1 1 6 188.86 278.77 3.75 0.159 1.34 3 4 3 183.82 125.39 3.48 0.106 1.64 2 7 0 115.95 73.11 3.47 0.081 1.72 -9 3 6 44.53 13.46 3.43 0.035 0.83 -1 2 3 164.58 237.05 3.38 0.146 2.54 0 2 1 93.03 56.92 3.38 0.072 5.15 3 7 2 13.56 2.65 3.33 0.015 1.44 -3 0 2 272.64 195.60 3.31 0.133 2.55 2 5 2 20.89 45.94 3.28 0.064 1.92 0 6 9 29.82 9.79 3.24 0.030 0.85 0 4 5 20.13 6.60 3.20 0.024 1.48 1 5 1 411.19 314.48 3.18 0.168 2.38 1 5 2 114.18 168.06 3.17 0.123 2.11 0 1 4 163.53 231.69 3.16 0.145 2.06 -2 6 1 633.05 500.10 3.11 0.212 1.93 3 6 0 842.75 680.84 2.98 0.248 1.75 3 2 4 39.80 67.94 2.88 0.078 1.55 0 5 4 15.29 4.95 2.83 0.021 1.63 0 9 3 9.24 0.02 2.83 0.001 1.29 0 7 3 23.09 9.70 2.82 0.030 1.55 1 3 4 136.11 187.92 2.81 0.130 1.79 1 7 0 5.84 18.74 2.76 0.041 1.83 3 4 2 519.59 417.89 2.74 0.194 1.86 -1 3 10 46.34 11.13 2.73 0.032 0.82 0 6 4 101.10 143.58 2.70 0.114 1.51 4 5 1 127.31 90.05 2.69 0.090 1.61 4 8 5 9.73 1.22 2.69 0.010 0.99 8 2 4 12.13 1.46 2.68 0.011 0.91 0 8 0 16.96 35.00 2.64 0.056 1.64 1 2 1 6838.50 8090.67 2.64 0.854 4.29 3 0 4 71.99 107.13 2.61 0.098 1.60 4 1 1 729.85 887.35 2.61 0.283 2.02 4 2 4 142.13 191.29 2.61 0.131 1.39 0 0 2 256.08 330.21 2.60 0.173 4.16 -5 1 10 -0.19 24.51 2.59 0.047 0.79 0 2 6 147.66 108.08 2.58 0.099 1.36 7 0 0 239.68 183.90 2.54 0.129 1.25 0 3 1 2269.90 2676.76 2.50 0.491 3.87 2 3 4 113.44 154.30 2.50 0.118 1.66 Bond lengths and angles C1 - Distance Angles O1B 1.2387 (0.0024) O1A 1.2526 (0.0025) 126.11 (0.19) C2 1.5357 (0.0026) 118.02 (0.17) 115.86 (0.17) C1 - O1B O1A C2 - Distance Angles O2 1.4229 (0.0022) C3 1.5258 (0.0026) 109.34 (0.15) C1 1.5357 (0.0026) 112.37 (0.15) 110.67 (0.15) H2 1.0000 108.11 108.11 108.11 C2 - O2 C3 C1 C3 - Distance Angles O3 1.4153 (0.0022) C2 1.5258 (0.0026) 111.95 (0.15) C4 1.5372 (0.0026) 112.47 (0.15) 111.22 (0.15) H3 1.0000 106.94 106.94 106.94 C3 - O3 C2 C4 C4 - Distance Angles O4A 1.2513 (0.0024) O4B 1.2623 (0.0024) 124.51 (0.18) C3 1.5372 (0.0026) 118.33 (0.16) 117.15 (0.17) C4 - O4A O4B O1A - Distance Angles C1 1.2526 (0.0025) O1A - O1B - Distance Angles C1 1.2387 (0.0024) O1B - O2 - Distance Angles C2 1.4229 (0.0022) H2A 0.8400 109.47 O2 - C2 O3 - Distance Angles C3 1.4153 (0.0022) H3A 0.8400 109.47 O3 - C3 O4A - Distance Angles C4 1.2513 (0.0024) O4A - O4B - Distance Angles C4 1.2623 (0.0024) O4B - C22A_a - Distance Angles C23A_a 1.5180 (0.0091) N21A_a 1.6044 (0.0147) 106.91 (1.40) H22A_a 0.9900 110.35 110.35 H22B_a 0.9900 110.33 110.33 108.57 C22A_a - C23A_a N21A_a H22A_a C23A_a - Distance Angles C24A_a 1.5190 (0.0119) C22A_a 1.5180 (0.0091) 113.40 (0.73) H23A_a 0.9900 108.89 108.91 H23B_a 0.9900 108.88 108.88 107.72 C23A_a - C24A_a C22A_a H23A_a C24A_a - Distance Angles N25A_a 1.2601 (0.0055) C23A_a 1.5190 (0.0119) 129.48 (0.53) H24A_a 0.9900 104.91 104.91 H24B_a 0.9900 104.91 104.91 105.82 C24A_a - N25A_a C23A_a H24A_a N21A_a - Distance Angles C22A_a 1.6044 (0.0147) H21A_a 0.9100 109.47 H21B_a 0.9100 109.46 109.47 H21C_a 0.9100 109.49 109.47 109.47 N21A_a - C22A_a H21A_a H21B_a N25A_a - Distance Angles C24A_a 1.2601 (0.0055) H25A_a 0.9100 109.47 H25B_a 0.9100 109.47 109.47 H25C_a 0.9100 109.47 109.47 109.47 N25A_a - C24A_a H25A_a H25B_a C22B_b - Distance Angles N21B_b 1.3579 (0.0157) C23B_b 1.5278 (0.0092) 114.27 (1.32) H22C_b 0.9900 108.70 108.70 H22D_b 0.9900 108.68 108.67 107.62 C22B_b - N21B_b C23B_b H22C_b C23B_b - Distance Angles C24B_b 1.5070 (0.0115) C22B_b 1.5278 (0.0092) 110.26 (0.70) H23C_b 0.9900 109.61 109.58 H23D_b 0.9900 109.61 109.61 108.13 C23B_b - C24B_b C22B_b H23C_b C24B_b - Distance Angles N25B_b 1.1463 (0.0055) C23B_b 1.5070 (0.0115) 119.50 (0.53) H24C_b 0.9900 107.44 107.45 H24D_b 0.9900 107.44 107.44 106.96 C24B_b - N25B_b C23B_b H24C_b N21B_b - Distance Angles C22B_b 1.3579 (0.0157) H21D_b 0.9100 109.47 H21E_b 0.9100 109.49 109.47 H21F_b 0.9100 109.45 109.47 109.47 N21B_b - C22B_b H21D_b H21E_b N25B_b - Distance Angles C24B_b 1.1463 (0.0055) H25D_b 0.9100 109.47 H25E_b 0.9100 109.47 109.47 H25F_b 0.9100 109.47 109.47 109.47 N25B_b - C24B_b H25D_b H25E_b Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.84 1.83 2.654(2) 165.0 O2-H2A...O4B_$1 0.84 1.84 2.675(2) 171.0 O3-H3A...O1B_$2 0.91 1.94 2.830(13) 164.4 N21A_a-H21A_a...O4B_$3 0.91 1.95 2.852(14) 169.5 N21B_b-H21D_b...O4B_$3 0.91 1.95 2.812(12) 158.1 N21A_a-H21B_a...O4A_$4 0.91 1.88 2.755(14) 159.4 N21B_b-H21E_b...O4A_$4 0.91 1.94 2.845(11) 170.5 N21A_a-H21C_a...O2_$5 0.91 2.06 2.948(11) 165.9 N21B_b-H21F_b...O2_$5 0.91 2.54 3.080(14) 118.8 N21B_b-H21F_b...O1B_$5 0.91 2.07 2.861(4) 144.9 N25A_a-H25A_a...O3_$6 0.91 2.62 3.163(4) 119.0 N25A_a-H25A_a...O1B_$6 0.91 2.17 2.971(4) 146.3 N25A_a-H25B_a...O3_$7 0.91 2.19 2.883(4) 132.7 N25A_a-H25B_a...O4A_$7 0.91 2.14 2.777(4) 126.2 N25B_b-H25E_b...O4A_$7 0.91 2.41 3.134(4) 136.3 N25B_b-H25E_b...O3_$7 0.91 1.90 2.761(4) 157.5 N25A_a-H25C_a...O1A_$8 0.91 1.87 2.681(4) 148.0 N25B_b-H25D_b...O1A_$8 0.91 2.09 2.929(4) 152.3 N25B_b-H25F_b...O1A_$9 FMAP and GRID set by program FMAP 2 3 13 GRID -2.500 -2 -2 2.500 2 2 R1 = 0.0625 for 2201 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.57 at 0.3490 0.6894 0.2405 [ 0.67 A from H24D ] Deepest hole -0.54 at 0.6808 0.1078 0.2218 [ 0.17 A from H24C ] Mean = 0.00, Rms deviation from mean = 0.07 e/A^3, Highest memory used = 3464 / 16527 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.3490 0.1894 0.2595 1.00000 0.05 0.57 0.67 H24D 0.70 H24A 1.14 C24A 1.15 C24B Q2 1 -0.3908 0.0595 0.1264 1.00000 0.05 0.56 0.81 H25F 1.03 N25B 1.04 H24C 1.11 C24B Q3 1 -0.4857 0.2587 0.0797 1.00000 0.05 0.49 0.94 H25A 1.08 H24B 1.16 N25A 1.16 C24A Q4 1 0.7487 0.5310 0.1400 1.00000 0.05 0.35 0.76 C4 0.79 C3 1.49 H3 1.72 O4A Q5 1 0.7716 0.6003 -0.1313 1.00000 0.05 0.32 0.74 C2 0.79 C1 1.41 H2 1.73 O1A Q6 1 0.7582 0.5591 0.0015 1.00000 0.05 0.24 0.74 C3 0.78 C2 1.40 H3 1.42 H2 Q7 1 0.6165 0.5790 -0.3291 1.00000 0.05 0.21 0.49 O1A 1.54 C1 1.59 H25D 1.62 H25C Q8 1 0.8483 0.5178 0.3886 1.00000 0.05 0.19 0.79 O4A 1.53 C4 1.54 H21E 1.72 H21B Q9 1 -0.1907 0.1629 0.0777 1.00000 0.05 0.18 0.64 C22A 0.73 C23B 0.81 C22B 0.90 C23A Q10 1 0.7597 0.6877 -0.3105 1.00000 0.05 0.18 0.71 O1B 1.18 C1 1.81 O1A 1.83 H3A Shortest distances between peaks (including symmetry equivalents) 4 6 1.23 5 6 1.26 2 7 1.85 5 10 1.88 7 10 1.90 1 3 2.02 5 7 2.03 1 2 2.04 4 8 2.16 1 9 2.23 2 9 2.30 4 5 2.48 2 3 2.75 3 9 2.89 8 9 2.89 6 7 2.90 2 7 2.99 Time profile in seconds ----------------------- 0.06: 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 0.00: Analyse other restraints etc. 0.72: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.55: Structure factors and derivatives 0.41: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.05: Apply other restraints 0.08: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.03: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.00: Fourier summations 0.03: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 04skc0014p21c finished at 11:33:44 Total CPU time: 2.0 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++