#------------------------------------------------------------------------------ #$Date: 2026-06-16 00:01:12 +0100 (Tue, 16 Jun 2026) $ #$Revision: 306570 $ #$URL: svn://www.crystallography.net/cod/cif/7/72/11/7721133.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7721133 loop_ _publ_author_name 'Hejda, Martin' 'Dost\'al, Libor' 'Mr\'ozek, Ond\ 2\s(I)' _cod_data_source_file d6dt01280a3.cif _cod_data_source_block ld200303B1 _cod_original_sg_symbol_H-M 'C c' _cod_database_code 7721133 _shelx_shelxl_version_number 2016/6 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.773 _shelx_estimated_absorpt_t_max 0.880 _exptl_absorpt_special_details ; The ratio of minimum to maximum apparent transmission was 0.556 ; _shelx_res_file ; TITL ld200303B1.res in Cc ld200303B1.res created by SHELXL-2016/6 at 09:14:57 on 07-Apr-2020 CELL 0.71073 26.4752 11.1673 18.8707 90.000 119.656 90.000 ZERR 4.000 0.0016 0.0007 0.0010 0.000 0.002 0.000 LATT -7 SYMM X, -Y, 1/2+Z SFAC C H B K N O UNIT 180 308 4 4 4 40 SIZE 0.806 1.294 1.669 TEMP -123.130 OMIT 0 52 OMIT -16 2 23 OMIT 3 1 -21 OMIT -11 11 13 OMIT -16 10 15 OMIT -10 10 15 OMIT 11 11 -13 OMIT 19 7 -18 OMIT 8 12 -9 OMIT 29 5 -11 OMIT 5 13 -7 OMIT -18 2 12 OMIT 18 2 -12 OMIT 10 10 -15 OMIT 8 4 -3 OMIT 28 6 -11 OMIT 30 4 -16 OMIT -1 9 -1 OMIT -15 3 22 OMIT -16 2 22 OMIT -19 7 19 OMIT 16 10 -15 OMIT 1 9 -1 OMIT -15 3 21 OMIT 30 4 -15 OMIT -6 2 21 OMIT 7 9 -17 OMIT -4 0 8 OMIT 4 2 -21 OMIT -13 1 20 OMIT 0 10 1 OMIT 29 5 -13 OMIT 5 5 -4 OMIT 1 9 5 OMIT -12 4 21 OMIT 2 2 -20 OMIT -19 5 7 OMIT -28 4 15 OMIT -19 7 18 OMIT 19 5 -5 OMIT 0 10 -1 OMIT -1 5 4 OMIT -9 9 17 OMIT 17 9 5 OMIT -3 5 19 OMIT -2 0 2 OMIT -1 9 1 OMIT -5 5 4 L.S. 45 ACTA LIST 4 BOND $H FMAP 2 PLAN 29 TWIN RIGU EADP c7 c7' REM THF o2s DFIX 1.43 0.01 O7 c30 o7 c33 o8 c34 o8 c37 DFIX 1.54 0.01 c30 c31 c31 c32 c32 c33 c34 c35 c35 c36 c36 c37 DFIX 1.43 0.01 o2s c5s o2s c8s DFIX 1.54 0.01 c5s c6s c6s c7s c7s c8s DFIX 1.43 0.01 o2s' c5s' o2s' c8s' DFIX 1.54 0.01 c5s' c6s' c6s' c7s' c7s' c8s' ISOR 0.01 0.001 o2s o2s' o1s o1s' c34 c34' c5s c5s' c6s c6s' ISOR 0.01 0.001 c32 c32' c15 ISOR 0.005 0.001 c22 EADP O2s O2s' EADP C5s c5s' EADP C6s c6s' EADP C7s c7s' EADP C8s c8s' REM THF o1s DFIX 1.43 0.01 o1s c1s o1s c4s DFIX 1.54 0.01 c1s c2s c2s c3s c3s c4s DFIX 1.43 0.01 o1s' c1s' o1s' c4s' DFIX 1.54 0.01 c1s' c2s' c2s' c3s' c3s' c4s' EADP O1s O1s' EADP C1s c1s' EADP C2s c2s' EADP C3s c3s' EADP C4s c4s' REM THF o7s DFIX 1.43 0.01 o7 c30 o7 c33 DFIX 1.54 0.01 c30 c31 c31 c32 c32 c33 DFIX 1.43 0.01 o7' c30' o7' c33' DFIX 1.54 0.01 c30' c31' c31' c32' c32' c33' DFIX -2.2 0.01 c33' c30' c30 c33 DFIX -2.5 0.01 c30' c32' EADP O7 O7' EADP C30 c30' EADP C31 c31' EADP C32 c32' EADP C33 c33' REM THF o8s DFIX 1.43 0.01 o8 c34 o8 c37 DFIX 1.54 0.01 c34 c35 c35 c36 c36 c37 DFIX 1.43 0.01 o8' c34' o8' c37' DFIX 1.54 0.01 c34' c35' c35' c36' c36' c37' EADP O8 O8' EADP C34 c34' EADP C35 c35' EADP C36 c36' EADP C37 c37' REM t-Bu DFIX 1.54 0.01 c8 c9 c8 c10 c8 c11 c8 c9' c8 c10' c8 c11' EADP c11 c11' DFIX 1.51 0.01 C7 c6 c7' c17 DFIX 1.48 0.01 n1 c7 n1 c7' WGHT 0.195900 3.463400 BASF 0.37445 FVAR 0.14625 K1 4 0.703410 1.001271 0.507377 11.00000 0.02877 0.01863 = 0.04675 -0.00120 0.02121 0.00422 N1 5 0.473253 0.499968 0.365334 11.00000 0.04746 0.17246 = 0.06226 0.00419 0.03509 0.00567 O1 6 0.650045 0.785603 0.504007 11.00000 0.04581 0.02615 = 0.06205 0.00055 0.03089 -0.00121 O2 6 0.607882 1.001522 0.532272 11.00000 0.03580 0.03881 = 0.06321 -0.00642 0.02994 0.00465 O3 6 0.650447 1.217837 0.504360 11.00000 0.03080 0.03182 = 0.07518 -0.00307 0.02512 0.01991 O4 6 0.758412 1.217976 0.511783 11.00000 0.04777 0.02378 = 0.07866 0.00186 0.04205 0.00600 O5 6 0.797726 1.000779 0.480156 11.00000 0.03154 0.02748 = 0.07325 0.00219 0.03413 0.00655 O6 6 0.758716 0.784023 0.513133 11.00000 0.05178 0.01978 = 0.07913 -0.00997 0.04209 0.00037 PART 1 O7 6 0.781430 1.008499 0.659154 10.50000 0.11860 0.11015 = 0.04784 0.02003 0.03636 0.01211 O8 6 0.646140 1.003203 0.344457 10.50000 0.08206 0.06992 = 0.04602 0.00513 0.01835 0.00457 PART 2 O7' 6 0.776294 0.994024 0.672925 10.50000 0.11860 0.11015 = 0.04784 0.02003 0.03636 0.01211 O8' 6 0.616447 1.002460 0.347262 10.50000 0.08206 0.06992 = 0.04602 0.00513 0.01835 0.00457 PART 0 B1 3 0.502496 0.501291 0.460814 11.00000 0.04012 0.02810 = 0.05625 -0.00286 0.03368 0.00376 H1 2 0.550069 0.500755 0.496377 11.00000 0.01035 C1 1 0.480235 0.383069 0.485614 11.00000 0.03911 0.02764 = 0.08171 0.00493 0.04243 0.01315 C2 1 0.494825 0.350207 0.564143 11.00000 0.08161 0.03825 = 0.08629 0.02452 0.04728 0.01932 AFIX 43 H2A 2 0.520539 0.401258 0.607268 11.00000 -1.20000 AFIX 0 C3 1 0.474821 0.248289 0.584977 11.00000 0.12651 0.05824 = 0.11644 0.03838 0.09132 0.03635 AFIX 43 H3A 2 0.487198 0.229776 0.640331 11.00000 -1.20000 AFIX 0 C4 1 0.438172 0.178329 0.525471 11.00000 0.10188 0.03109 = 0.17928 0.02183 0.11351 0.02470 AFIX 43 H4A 2 0.422260 0.110544 0.537856 11.00000 -1.20000 AFIX 0 C5 1 0.422876 0.201422 0.447214 11.00000 0.07147 0.02502 = 0.14982 -0.02636 0.06960 -0.00649 AFIX 43 H5A 2 0.397692 0.147406 0.405859 11.00000 -1.20000 AFIX 0 C6 1 0.443942 0.307022 0.424375 11.00000 0.06975 0.02832 = 0.10555 -0.00500 0.05390 0.00095 AFIX 43 PART 2 H6A 2 0.432934 0.322591 0.369095 10.50000 -1.20000 AFIX 0 PART 1 C7 1 0.450399 0.369858 0.355944 10.50000 0.05814 0.14494 = 0.09421 -0.00769 0.05200 -0.00240 AFIX 23 H7A 2 0.476273 0.318949 0.344758 10.50000 -1.20000 H7B 2 0.411673 0.368007 0.306217 10.50000 -1.20000 AFIX 0 PART 2 C7' 1 0.450399 0.630365 0.355923 10.50000 0.05814 0.14494 = 0.09421 -0.00769 0.05200 -0.00240 AFIX 23 H7'A 2 0.411768 0.631905 0.306016 10.50000 -1.20000 H7'B 2 0.476331 0.680820 0.344580 10.50000 -1.20000 AFIX 0 PART 0 C8 1 0.501802 0.500900 0.318893 11.00000 0.06541 0.05484 = 0.05368 0.00086 0.03676 -0.00051 PART 1 C9 1 0.458896 0.478721 0.227638 10.50000 0.09784 0.15361 = 0.05378 -0.00705 0.04454 -0.02240 AFIX 137 H9A 2 0.474258 0.514684 0.194790 10.50000 -1.50000 H9B 2 0.421267 0.515033 0.212941 10.50000 -1.50000 H9C 2 0.453915 0.392362 0.217230 10.50000 -1.50000 AFIX 0 C10 1 0.554879 0.421462 0.340683 10.50000 0.07393 0.05999 = 0.11945 -0.01268 0.05590 0.00528 AFIX 137 H10A 2 0.579071 0.459158 0.321016 10.50000 -1.50000 H10B 2 0.541827 0.342831 0.314934 10.50000 -1.50000 H10C 2 0.577607 0.411709 0.400001 10.50000 -1.50000 AFIX 0 C11 1 0.522537 0.630550 0.337425 10.50000 0.07633 0.06181 = 0.09452 0.00050 0.06573 -0.00287 AFIX 137 H11A 2 0.529609 0.660958 0.294388 10.50000 -1.50000 H11B 2 0.558615 0.634391 0.389983 10.50000 -1.50000 H11C 2 0.492700 0.679539 0.339801 10.50000 -1.50000 AFIX 0 PART 2 C9' 1 0.458509 0.521145 0.227625 10.50000 0.11139 0.10395 = 0.05739 -0.00346 0.03761 0.00486 AFIX 137 H9'A 2 0.470793 0.474620 0.194743 10.50000 -1.50000 H9'B 2 0.457574 0.606404 0.214726 10.50000 -1.50000 H9'C 2 0.419647 0.495278 0.215399 10.50000 -1.50000 AFIX 0 C10' 1 0.522534 0.370475 0.334624 10.50000 0.10498 0.05851 = 0.05600 -0.01611 0.03927 0.00261 AFIX 137 H10D 2 0.536951 0.348038 0.297603 10.50000 -1.50000 H10E 2 0.490055 0.318159 0.325134 10.50000 -1.50000 H10F 2 0.553851 0.361840 0.391192 10.50000 -1.50000 AFIX 0 C11' 1 0.553267 0.585998 0.338513 10.50000 0.07633 0.06181 = 0.09452 0.00050 0.06573 -0.00287 AFIX 137 H11D 2 0.569869 0.565999 0.303701 10.50000 -1.50000 H11E 2 0.583103 0.576885 0.395894 10.50000 -1.50000 H11F 2 0.539401 0.668969 0.328363 10.50000 -1.50000 AFIX 0 PART 0 C12 1 0.480739 0.619564 0.485453 11.00000 0.03879 0.02626 = 0.08212 -0.00979 0.04288 -0.00869 C13 1 0.494807 0.650628 0.563631 11.00000 0.07280 0.04618 = 0.09152 -0.01806 0.05124 -0.01274 AFIX 43 H13A 2 0.520107 0.598702 0.606465 11.00000 -1.20000 AFIX 0 C14 1 0.474711 0.752901 0.584963 11.00000 0.11482 0.05492 = 0.10699 -0.04138 0.07590 -0.02509 AFIX 43 H14A 2 0.486566 0.770341 0.640298 11.00000 -1.20000 AFIX 0 C15 1 0.438949 0.823798 0.525891 11.00000 0.08008 0.06500 = 0.13146 -0.02951 0.08352 -0.02840 AFIX 43 H15A 2 0.424573 0.893273 0.539080 11.00000 -1.20000 AFIX 0 C16 1 0.421911 0.801036 0.446790 11.00000 0.05964 0.03594 = 0.13185 0.01927 0.05306 0.00758 AFIX 43 H16A 2 0.395614 0.854052 0.405686 11.00000 -1.20000 AFIX 0 C17 1 0.443419 0.695994 0.423736 11.00000 0.06098 0.03722 = 0.09994 0.00527 0.05417 0.00474 AFIX 43 PART 1 H17A 2 0.432221 0.680595 0.368371 10.50000 -1.20000 AFIX 0 PART 0 C18 1 0.612543 0.790232 0.538068 11.00000 0.05242 0.05579 = 0.05805 -0.00204 0.03734 -0.01027 AFIX 23 H18A 2 0.635670 0.797940 0.598127 11.00000 -1.20000 H18B 2 0.589115 0.716048 0.524833 11.00000 -1.20000 AFIX 0 C19 1 0.573306 0.897529 0.501999 11.00000 0.03612 0.06341 = 0.06168 0.00030 0.02957 0.00201 AFIX 23 H19A 2 0.554270 0.895371 0.441752 11.00000 -1.20000 H19B 2 0.542734 0.897196 0.517695 11.00000 -1.20000 AFIX 0 C20 1 0.573412 1.107955 0.501828 11.00000 0.03325 0.05901 = 0.08309 0.00606 0.03548 0.02584 AFIX 23 H20A 2 0.542580 1.108671 0.517018 11.00000 -1.20000 H20B 2 0.554695 1.110675 0.441623 11.00000 -1.20000 AFIX 0 C21 1 0.612108 1.212575 0.537881 11.00000 0.04488 0.04789 = 0.07151 -0.01237 0.03168 0.01963 AFIX 23 H21A 2 0.588821 1.286942 0.524785 11.00000 -1.20000 H21B 2 0.634912 1.204261 0.597927 11.00000 -1.20000 AFIX 0 C22 1 0.688171 1.318241 0.533306 11.00000 0.06460 0.01876 = 0.07894 -0.01294 0.03393 0.01032 AFIX 23 H22A 2 0.715150 1.310770 0.592665 11.00000 -1.20000 H22B 2 0.665406 1.392833 0.523293 11.00000 -1.20000 AFIX 0 C23 1 0.721910 1.321553 0.487853 11.00000 0.05900 0.02262 = 0.13239 0.01739 0.05451 0.01109 AFIX 23 H23A 2 0.694905 1.320678 0.428265 11.00000 -1.20000 H23B 2 0.745743 1.395237 0.501829 11.00000 -1.20000 AFIX 0 C24 1 0.793130 1.212286 0.474764 11.00000 0.05896 0.02019 = 0.10551 0.00817 0.05623 0.00158 AFIX 23 H24A 2 0.816752 1.286059 0.487058 11.00000 -1.20000 H24B 2 0.768135 1.206132 0.414864 11.00000 -1.20000 AFIX 0 C25 1 0.831997 1.105844 0.506182 11.00000 0.04175 0.03379 = 0.07442 -0.01073 0.03990 -0.00517 AFIX 23 H25A 2 0.859718 1.106243 0.485301 11.00000 -1.20000 H25B 2 0.854523 1.108284 0.566495 11.00000 -1.20000 AFIX 0 C26 1 0.832198 0.896092 0.506437 11.00000 0.03995 0.02904 = 0.08870 -0.00428 0.04272 0.00861 AFIX 23 H26A 2 0.854630 0.893810 0.566758 11.00000 -1.20000 H26B 2 0.859995 0.895871 0.485688 11.00000 -1.20000 AFIX 0 C27 1 0.793374 0.789293 0.474926 11.00000 0.05629 0.02589 = 0.10144 -0.00561 0.05451 0.01291 AFIX 23 H27A 2 0.768141 0.795550 0.415076 11.00000 -1.20000 H27B 2 0.816988 0.715540 0.487028 11.00000 -1.20000 AFIX 0 C28 1 0.722256 0.681509 0.489680 11.00000 0.05973 0.02359 = 0.09874 -0.01192 0.04445 0.00469 AFIX 23 H28A 2 0.746057 0.607676 0.505134 11.00000 -1.20000 H28B 2 0.696053 0.681065 0.429877 11.00000 -1.20000 AFIX 0 C29 1 0.687614 0.686536 0.532325 11.00000 0.05876 0.03211 = 0.10858 -0.00085 0.05307 -0.00362 AFIX 23 H29A 2 0.664747 0.611983 0.521792 11.00000 -1.20000 H29B 2 0.714009 0.693593 0.591870 11.00000 -1.20000 AFIX 0 PART 1 C30 1 0.807315 0.906418 0.709667 10.50000 0.13458 0.09242 = 0.08196 0.01742 0.05429 -0.00199 AFIX 23 H30A 2 0.849968 0.910307 0.732732 10.50000 -1.20000 H30B 2 0.793152 0.833225 0.675793 10.50000 -1.20000 AFIX 0 C31 1 0.793853 0.897153 0.779590 10.50000 0.18570 0.13867 = 0.06405 0.01046 0.06490 -0.02907 AFIX 23 H31A 2 0.826397 0.865488 0.830936 10.50000 -1.20000 H31B 2 0.757129 0.854730 0.764924 10.50000 -1.20000 AFIX 0 C32 1 0.788570 1.035266 0.777242 10.50000 0.14802 0.13656 = 0.11737 -0.02101 0.07148 -0.01168 AFIX 23 H32A 2 0.813813 1.066147 0.833121 10.50000 -1.20000 H32B 2 0.748003 1.056170 0.761452 10.50000 -1.20000 AFIX 0 C33 1 0.804652 1.101166 0.719003 10.50000 0.10824 0.09856 = 0.08846 0.00042 0.02242 0.00444 AFIX 23 H33A 2 0.784141 1.178513 0.699126 10.50000 -1.20000 H33B 2 0.847064 1.112126 0.742403 10.50000 -1.20000 AFIX 0 C34 1 0.618013 0.907709 0.288529 10.50000 0.10476 0.08818 = 0.08112 -0.00899 0.03898 -0.02227 AFIX 23 H34A 2 0.583097 0.878233 0.289507 10.50000 -1.20000 H34B 2 0.644583 0.840296 0.296420 10.50000 -1.20000 AFIX 0 C35 1 0.602865 0.982126 0.211669 10.50000 0.11124 0.14417 = 0.04393 0.01331 0.00706 0.05199 AFIX 23 H35A 2 0.625865 0.954249 0.186480 10.50000 -1.20000 H35B 2 0.561074 0.973806 0.171174 10.50000 -1.20000 AFIX 0 C36 1 0.617315 1.112478 0.238515 10.50000 0.08510 0.12904 = 0.06030 0.03573 0.00202 0.01694 AFIX 23 H36A 2 0.590437 1.169379 0.196520 10.50000 -1.20000 H36B 2 0.658060 1.133226 0.255230 10.50000 -1.20000 AFIX 0 C37 1 0.606784 1.102995 0.310955 10.50000 0.16686 0.08761 = 0.05571 0.03196 0.02581 0.03148 AFIX 23 H37A 2 0.619696 1.174641 0.346505 10.50000 -1.20000 H37B 2 0.566145 1.082461 0.294982 10.50000 -1.20000 AFIX 0 PART 2 C30' 1 0.764946 0.902409 0.716221 10.50000 0.13458 0.09242 = 0.08196 0.01742 0.05429 -0.00199 AFIX 23 H30C 2 0.786591 0.827377 0.722065 10.50000 -1.20000 H30D 2 0.723018 0.885709 0.693551 10.50000 -1.20000 AFIX 0 C31' 1 0.791492 0.978673 0.795523 10.50000 0.18570 0.13867 = 0.06405 0.01046 0.06490 -0.02907 AFIX 23 H31C 2 0.766709 0.967858 0.820724 10.50000 -1.20000 H31D 2 0.830119 0.944732 0.833784 10.50000 -1.20000 AFIX 0 C32' 1 0.799177 1.113157 0.789072 10.50000 0.14802 0.13656 = 0.11737 -0.02101 0.07148 -0.01168 AFIX 23 H32C 2 0.784631 1.163987 0.818128 10.50000 -1.20000 H32D 2 0.838680 1.137300 0.801379 10.50000 -1.20000 AFIX 0 C33' 1 0.756834 1.095394 0.700052 10.50000 0.10824 0.09856 = 0.08846 0.00042 0.02242 0.00444 AFIX 23 H33C 2 0.717397 1.080400 0.691693 10.50000 -1.20000 H33D 2 0.755430 1.167776 0.668834 10.50000 -1.20000 AFIX 0 C34' 1 0.600049 0.892915 0.306860 10.50000 0.10476 0.08818 = 0.08112 -0.00899 0.03898 -0.02227 AFIX 23 H34C 2 0.557735 0.880360 0.283461 10.50000 -1.20000 H34D 2 0.620850 0.826677 0.345230 10.50000 -1.20000 AFIX 0 C35' 1 0.615675 0.896044 0.239336 10.50000 0.11124 0.14417 = 0.04393 0.01331 0.00706 0.05199 AFIX 23 H35C 2 0.599971 0.827595 0.201141 10.50000 -1.20000 H35D 2 0.657760 0.906390 0.259486 10.50000 -1.20000 AFIX 0 C36' 1 0.580141 1.012379 0.206014 10.50000 0.08510 0.12904 = 0.06030 0.03573 0.00202 0.01694 AFIX 23 H36C 2 0.586078 1.049149 0.162951 10.50000 -1.20000 H36D 2 0.538124 0.998677 0.184741 10.50000 -1.20000 AFIX 0 C37' 1 0.607235 1.088361 0.284269 10.50000 0.16686 0.08761 = 0.05571 0.03196 0.02581 0.03148 AFIX 23 H37C 2 0.644436 1.124445 0.294626 10.50000 -1.20000 H37D 2 0.580472 1.152898 0.280822 10.50000 -1.20000 AFIX 0 PART 1 O1S 6 0.324097 0.999961 0.663269 10.50000 0.10841 0.09710 = 0.10322 -0.00103 0.03856 0.00063 C1S 1 0.362179 1.098283 0.700815 10.50000 0.13051 0.07125 = 0.06871 0.01923 0.04794 0.01203 AFIX 23 H1SA 2 0.363767 1.118190 0.753003 10.50000 -1.20000 H1SB 2 0.347755 1.169369 0.664853 10.50000 -1.20000 AFIX 0 C2S 1 0.423386 1.064491 0.716529 10.50000 0.11848 0.07914 = 0.06236 -0.00681 0.03915 -0.01897 AFIX 23 H2SA 2 0.429651 1.094149 0.672033 10.50000 -1.20000 H2SB 2 0.453776 1.098400 0.768880 10.50000 -1.20000 AFIX 0 C3S 1 0.424435 0.927305 0.719338 10.50000 0.12113 0.08780 = 0.08125 0.00577 0.04913 0.02288 AFIX 23 H3SA 2 0.452667 0.897299 0.774323 10.50000 -1.20000 H3SB 2 0.433850 0.893120 0.678849 10.50000 -1.20000 AFIX 0 C4S 1 0.361606 0.898682 0.697555 10.50000 0.12867 0.06572 = 0.09545 -0.01449 0.04879 -0.01377 AFIX 23 H4SA 2 0.346868 0.831756 0.657985 10.50000 -1.20000 H4SB 2 0.361066 0.872555 0.747308 10.50000 -1.20000 AFIX 0 PART 2 O1S' 6 0.336654 1.000875 0.632881 10.50000 0.10841 0.09710 = 0.10322 -0.00103 0.03856 0.00063 C1S' 1 0.369999 1.106385 0.667868 10.50000 0.13051 0.07125 = 0.06871 0.01923 0.04794 0.01203 AFIX 23 H1SC 2 0.346342 1.167400 0.676278 10.50000 -1.20000 H1SD 2 0.383340 1.140352 0.631481 10.50000 -1.20000 AFIX 0 C2S' 1 0.422132 1.069980 0.749629 10.50000 0.11848 0.07914 = 0.06236 -0.00681 0.03915 -0.01897 AFIX 23 H2SC 2 0.418153 1.102907 0.795335 10.50000 -1.20000 H2SD 2 0.458635 1.100761 0.753999 10.50000 -1.20000 AFIX 0 C3S' 1 0.422898 0.932384 0.752315 10.50000 0.12113 0.08780 = 0.08125 0.00577 0.04913 0.02288 AFIX 23 H3SC 2 0.459903 0.900486 0.759018 10.50000 -1.20000 H3SD 2 0.417384 0.902516 0.797423 10.50000 -1.20000 AFIX 0 C4S' 1 0.371589 0.897441 0.669319 10.50000 0.12867 0.06572 = 0.09545 -0.01449 0.04879 -0.01377 AFIX 23 H4SC 2 0.386049 0.865512 0.633700 10.50000 -1.20000 H4SD 2 0.348164 0.834419 0.676417 10.50000 -1.20000 AFIX 0 PART 1 O2S 6 0.658620 0.429688 0.240083 10.50000 0.12707 0.11241 = 0.12341 0.00029 0.06016 0.00112 C5S 1 0.706520 0.350260 0.263854 10.50000 0.11294 0.10862 = 0.11497 -0.00381 0.05201 0.00001 AFIX 23 H5SA 2 0.706377 0.312100 0.216402 10.50000 -1.20000 H5SB 2 0.708233 0.288001 0.302332 10.50000 -1.20000 AFIX 0 C8S 1 0.665382 0.537969 0.204190 10.50000 0.10778 0.10180 = 0.14001 0.01722 0.05187 0.00946 AFIX 23 H8SA 2 0.646915 0.607038 0.215343 10.50000 -1.20000 H8SB 2 0.648809 0.529345 0.144540 10.50000 -1.20000 AFIX 0 C7S 1 0.731823 0.551370 0.247851 10.50000 0.11616 0.11942 = 0.11746 0.00291 0.04267 0.00521 AFIX 23 H7SA 2 0.745957 0.550370 0.208114 10.50000 -1.20000 H7SB 2 0.744101 0.627271 0.278973 10.50000 -1.20000 AFIX 0 C6S 1 0.755358 0.443270 0.305439 10.50000 0.11690 0.11089 = 0.12078 0.00300 0.05651 -0.00015 AFIX 23 H6SA 2 0.762095 0.463714 0.360499 10.50000 -1.20000 H6SB 2 0.792094 0.413685 0.309971 10.50000 -1.20000 AFIX 0 PART 2 O2S' 6 0.658407 0.569088 0.239130 10.50000 0.12707 0.11241 = 0.12341 0.00029 0.06016 0.00112 C5S' 1 0.669449 0.458580 0.210605 10.50000 0.11294 0.10862 = 0.11497 -0.00381 0.05201 0.00001 AFIX 23 H5SC 2 0.651114 0.459428 0.150418 10.50000 -1.20000 H5SD 2 0.653362 0.390492 0.226714 10.50000 -1.20000 AFIX 0 C8S' 1 0.705601 0.649322 0.263608 10.50000 0.10778 0.10180 = 0.14001 0.01722 0.05187 0.00946 AFIX 23 H8SC 2 0.706844 0.710245 0.302553 10.50000 -1.20000 H8SD 2 0.705208 0.689303 0.216514 10.50000 -1.20000 AFIX 0 C7S' 1 0.755144 0.558325 0.304442 10.50000 0.11616 0.11942 = 0.11746 0.00291 0.04267 0.00521 AFIX 23 H7SC 2 0.762208 0.538208 0.359708 10.50000 -1.20000 H7SD 2 0.791402 0.591371 0.309222 10.50000 -1.20000 AFIX 0 C6S' 1 0.735904 0.446426 0.249840 10.50000 0.11690 0.11089 = 0.12078 0.00300 0.05651 -0.00015 AFIX 23 H6SC 2 0.750350 0.371909 0.282172 10.50000 -1.20000 H6SD 2 0.748633 0.449353 0.208591 10.50000 -1.20000 PART 0 AFIX 0 HKLF 4 REM ld200303B1.res in Cc REM R1 = 0.1026 for 5329 Fo > 4sig(Fo) and 0.1431 for all 9066 data REM 618 parameters refined using 961 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 0.713, deepest hole -0.826, 1-sigma level 0.080 Q1 1 0.7374 1.0020 0.5510 11.00000 0.05 0.71 Q2 1 0.6671 1.0059 0.4698 11.00000 0.05 0.67 Q3 1 0.7785 1.0998 0.7485 11.00000 0.05 0.52 Q4 1 0.5628 0.9986 0.2614 11.00000 0.05 0.43 Q5 1 0.4279 1.0555 0.6387 11.00000 0.05 0.39 Q6 1 0.6682 0.9552 0.3032 11.00000 0.05 0.35 Q7 1 0.4272 0.9436 0.6393 11.00000 0.05 0.35 Q8 1 0.3643 0.9993 0.6170 11.00000 0.05 0.34 Q9 1 0.4803 0.5545 0.3764 11.00000 0.05 0.34 Q10 1 0.6679 1.0438 0.3018 11.00000 0.05 0.33 Q11 1 0.4621 0.8358 0.6700 11.00000 0.05 0.32 Q12 1 0.4800 0.4469 0.3767 11.00000 0.05 0.32 Q13 1 0.7047 0.6776 0.5073 11.00000 0.05 0.32 Q14 1 0.7734 1.0004 0.6001 11.00000 0.05 0.31 Q15 1 0.4626 1.1641 0.6692 11.00000 0.05 0.31 Q16 1 0.8320 1.0036 0.7339 11.00000 0.05 0.29 Q17 1 0.4070 0.8503 0.4598 11.00000 0.05 0.29 Q18 1 0.7033 1.3236 0.5080 11.00000 0.05 0.28 Q19 1 0.5431 0.5025 0.3972 11.00000 0.05 0.28 Q20 1 0.4076 0.1525 0.4598 11.00000 0.05 0.28 Q21 1 0.6150 0.7949 0.4634 11.00000 0.05 0.26 Q22 1 0.7435 0.9994 0.7515 11.00000 0.05 0.26 Q23 1 0.7340 0.9887 0.6602 11.00000 0.05 0.25 Q24 1 0.4061 0.8017 0.3973 11.00000 0.05 0.25 Q25 1 0.7415 0.9436 0.7155 11.00000 0.05 0.24 Q26 1 0.8184 0.9936 0.9041 11.00000 0.05 0.23 Q27 1 0.7913 1.2071 0.5493 11.00000 0.05 0.23 Q28 1 0.4852 0.5122 0.3317 11.00000 0.05 0.23 Q29 1 0.6309 0.9878 0.4178 11.00000 0.05 0.23 ; _shelx_res_checksum 42065 loop_ _space_group_symop_operation_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group K1 K 0.70341(7) 1.00127(10) 0.50738(10) 0.0303(4) Uani 1 1 d . . . . . N1 N 0.4733(4) 0.5000(8) 0.3653(6) 0.091(3) Uani 1 1 d D . . . . O1 O 0.6500(2) 0.7856(4) 0.5040(3) 0.0428(13) Uani 1 1 d . . . . . O2 O 0.6079(2) 1.0015(4) 0.5323(4) 0.0436(14) Uani 1 1 d . . . . . O3 O 0.6504(2) 1.2178(4) 0.5044(3) 0.0464(14) Uani 1 1 d . . . . . O4 O 0.7584(2) 1.2180(4) 0.5118(3) 0.0454(14) Uani 1 1 d . . . . . O5 O 0.7977(2) 1.0008(3) 0.4802(4) 0.0405(13) Uani 1 1 d . . . . . O6 O 0.7587(2) 0.7840(4) 0.5131(3) 0.0460(14) Uani 1 1 d . . . . . O7 O 0.7814(16) 1.0085(17) 0.6592(12) 0.094(4) Uani 0.5 1 d D . P A 1 O8 O 0.6461(8) 1.0032(13) 0.3445(9) 0.072(3) Uani 0.5 1 d D . P A 1 O7' O 0.7763(15) 0.9940(17) 0.6729(15) 0.094(4) Uani 0.5 1 d D . P A 2 O8' O 0.6164(9) 1.0025(13) 0.3473(9) 0.072(3) Uani 0.5 1 d D . P A 2 B1 B 0.5025(4) 0.5013(5) 0.4608(5) 0.0372(16) Uani 1 1 d . . . . . H1 H 0.550(3) 0.501(3) 0.496(3) 0.010(13) Uiso 1 1 d . . . . . C1 C 0.4802(3) 0.3831(6) 0.4856(5) 0.0440(17) Uani 1 1 d . . . . . C2 C 0.4948(4) 0.3502(7) 0.5641(6) 0.066(2) Uani 1 1 d . . . . . H2A H 0.520539 0.401258 0.607268 0.079 Uiso 1 1 calc R U . . . C3 C 0.4748(6) 0.2483(10) 0.5850(8) 0.087(3) Uani 1 1 d . . . . . H3A H 0.487198 0.229776 0.640331 0.104 Uiso 1 1 calc R U . . . C4 C 0.4382(5) 0.1783(8) 0.5255(9) 0.085(3) Uani 1 1 d . . . . . H4A H 0.422260 0.110544 0.537856 0.102 Uiso 1 1 calc R U . . . C5 C 0.4229(4) 0.2014(7) 0.4472(9) 0.076(3) Uani 1 1 d . . . . . H5A H 0.397692 0.147406 0.405859 0.091 Uiso 1 1 calc R U . . . C6 C 0.4439(4) 0.3070(7) 0.4244(7) 0.063(2) Uani 1 1 d D . . . . H6A H 0.432934 0.322591 0.369095 0.076 Uiso 0.5 1 calc R U P B 2 C7 C 0.4504(9) 0.3699(14) 0.3559(11) 0.093(4) Uani 0.5 1 d D . P C 1 H7A H 0.476273 0.318949 0.344758 0.111 Uiso 0.5 1 calc R U P C 1 H7B H 0.411673 0.368007 0.306217 0.111 Uiso 0.5 1 calc R U P C 1 C7' C 0.4504(9) 0.6304(14) 0.3559(11) 0.093(4) Uani 0.5 1 d D . P C 2 H7'A H 0.411768 0.631905 0.306016 0.111 Uiso 0.5 1 calc R U P C 2 H7'B H 0.476331 0.680820 0.344580 0.111 Uiso 0.5 1 calc R U P C 2 C8 C 0.5018(4) 0.5009(6) 0.3189(5) 0.0548(19) Uani 1 1 d D . . . . C9 C 0.459(2) 0.479(5) 0.2276(12) 0.099(15) Uani 0.5 1 d D . P D 1 H9A H 0.474258 0.514684 0.194790 0.148 Uiso 0.5 1 calc R U P D 1 H9B H 0.421267 0.515033 0.212941 0.148 Uiso 0.5 1 calc R U P D 1 H9C H 0.453915 0.392362 0.217230 0.148 Uiso 0.5 1 calc R U P D 1 C10 C 0.5549(8) 0.4215(19) 0.3407(16) 0.081(6) Uani 0.5 1 d D . P D 1 H10A H 0.579071 0.459158 0.321016 0.121 Uiso 0.5 1 calc R U P D 1 H10B H 0.541827 0.342831 0.314934 0.121 Uiso 0.5 1 calc R U P D 1 H10C H 0.577607 0.411709 0.400001 0.121 Uiso 0.5 1 calc R U P D 1 C11 C 0.5225(9) 0.6305(12) 0.3374(13) 0.067(3) Uani 0.5 1 d D . P D 1 H11A H 0.529609 0.660958 0.294388 0.101 Uiso 0.5 1 calc R U P D 1 H11B H 0.558615 0.634391 0.389983 0.101 Uiso 0.5 1 calc R U P D 1 H11C H 0.492700 0.679539 0.339801 0.101 Uiso 0.5 1 calc R U P D 1 C9' C 0.459(3) 0.521(5) 0.2276(14) 0.093(12) Uani 0.5 1 d D . P D 2 H9'A H 0.470793 0.474620 0.194743 0.139 Uiso 0.5 1 calc R U P D 2 H9'B H 0.457574 0.606404 0.214726 0.139 Uiso 0.5 1 calc R U P D 2 H9'C H 0.419647 0.495278 0.215399 0.139 Uiso 0.5 1 calc R U P D 2 C10' C 0.5225(10) 0.3705(12) 0.3346(12) 0.073(5) Uani 0.5 1 d D . P D 2 H10D H 0.536951 0.348038 0.297603 0.110 Uiso 0.5 1 calc R U P D 2 H10E H 0.490055 0.318159 0.325134 0.110 Uiso 0.5 1 calc R U P D 2 H10F H 0.553851 0.361840 0.391192 0.110 Uiso 0.5 1 calc R U P D 2 C11' C 0.5533(8) 0.5860(16) 0.3385(14) 0.067(3) Uani 0.5 1 d D . P D 2 H11D H 0.569869 0.565999 0.303701 0.101 Uiso 0.5 1 calc R U P D 2 H11E H 0.583103 0.576885 0.395894 0.101 Uiso 0.5 1 calc R U P D 2 H11F H 0.539401 0.668969 0.328363 0.101 Uiso 0.5 1 calc R U P D 2 C12 C 0.4807(3) 0.6196(6) 0.4855(5) 0.0434(17) Uani 1 1 d . . . . . C13 C 0.4948(4) 0.6506(8) 0.5636(6) 0.066(2) Uani 1 1 d . . . . . H13A H 0.520107 0.598702 0.606465 0.079 Uiso 1 1 calc R U . . . C14 C 0.4747(5) 0.7529(9) 0.5850(8) 0.083(3) Uani 1 1 d . . . . . H14A H 0.486566 0.770341 0.640298 0.100 Uiso 1 1 calc R U . . . C15 C 0.4389(5) 0.8238(10) 0.5259(8) 0.079(3) Uani 1 1 d . U . . . H15A H 0.424573 0.893273 0.539080 0.094 Uiso 1 1 calc R U . . . C16 C 0.4219(4) 0.8010(8) 0.4468(8) 0.073(3) Uani 1 1 d . . . . . H16A H 0.395614 0.854052 0.405686 0.088 Uiso 1 1 calc R U . . . C17 C 0.4434(4) 0.6960(7) 0.4237(6) 0.060(2) Uani 1 1 d D . . . . H17A H 0.432221 0.680595 0.368371 0.072 Uiso 0.5 1 calc R U P C 1 C18 C 0.6125(4) 0.7902(7) 0.5381(5) 0.0510(19) Uani 1 1 d . . . . . H18A H 0.635670 0.797940 0.598127 0.061 Uiso 1 1 calc R U . . . H18B H 0.589115 0.716048 0.524833 0.061 Uiso 1 1 calc R U . . . C19 C 0.5733(3) 0.8975(8) 0.5020(5) 0.051(2) Uani 1 1 d . . . . . H19A H 0.554270 0.895371 0.441752 0.062 Uiso 1 1 calc R U . . . H19B H 0.542734 0.897196 0.517695 0.062 Uiso 1 1 calc R U . . . C20 C 0.5734(3) 1.1080(8) 0.5018(6) 0.056(2) Uani 1 1 d . . . . . H20A H 0.542580 1.108671 0.517018 0.067 Uiso 1 1 calc R U . . . H20B H 0.554695 1.110675 0.441623 0.067 Uiso 1 1 calc R U . . . C21 C 0.6121(3) 1.2126(7) 0.5379(6) 0.053(2) Uani 1 1 d . . . . . H21A H 0.588821 1.286942 0.524785 0.064 Uiso 1 1 calc R U . . . H21B H 0.634912 1.204261 0.597927 0.064 Uiso 1 1 calc R U . . . C22 C 0.6882(4) 1.3182(6) 0.5333(6) 0.055(2) Uani 1 1 d . U . . . H22A H 0.715150 1.310770 0.592665 0.066 Uiso 1 1 calc R U . . . H22B H 0.665406 1.392833 0.523293 0.066 Uiso 1 1 calc R U . . . C23 C 0.7219(4) 1.3216(7) 0.4879(7) 0.068(3) Uani 1 1 d . . . . . H23A H 0.694905 1.320678 0.428265 0.082 Uiso 1 1 calc R U . . . H23B H 0.745743 1.395237 0.501829 0.082 Uiso 1 1 calc R U . . . C24 C 0.7931(4) 1.2123(6) 0.4748(6) 0.055(2) Uani 1 1 d . . . . . H24A H 0.816752 1.286059 0.487058 0.066 Uiso 1 1 calc R U . . . H24B H 0.768135 1.206132 0.414864 0.066 Uiso 1 1 calc R U . . . C25 C 0.8320(3) 1.1058(6) 0.5062(6) 0.0451(19) Uani 1 1 d . . . . . H25A H 0.859718 1.106243 0.485301 0.054 Uiso 1 1 calc R U . . . H25B H 0.854523 1.108284 0.566495 0.054 Uiso 1 1 calc R U . . . C26 C 0.8322(3) 0.8961(6) 0.5064(6) 0.048(2) Uani 1 1 d . . . . . H26A H 0.854630 0.893810 0.566758 0.057 Uiso 1 1 calc R U . . . H26B H 0.859995 0.895871 0.485688 0.057 Uiso 1 1 calc R U . . . C27 C 0.7934(4) 0.7893(6) 0.4749(6) 0.054(2) Uani 1 1 d . . . . . H27A H 0.768141 0.795550 0.415076 0.065 Uiso 1 1 calc R U . . . H27B H 0.816988 0.715540 0.487028 0.065 Uiso 1 1 calc R U . . . C28 C 0.7223(4) 0.6815(7) 0.4897(6) 0.058(2) Uani 1 1 d . . . . . H28A H 0.746057 0.607676 0.505134 0.070 Uiso 1 1 calc R U . . . H28B H 0.696053 0.681065 0.429877 0.070 Uiso 1 1 calc R U . . . C29 C 0.6876(4) 0.6865(7) 0.5323(7) 0.061(2) Uani 1 1 d . . . . . H29A H 0.664747 0.611983 0.521792 0.074 Uiso 1 1 calc R U . . . H29B H 0.714009 0.693593 0.591870 0.074 Uiso 1 1 calc R U . . . C30 C 0.8073(13) 0.9064(15) 0.7097(14) 0.103(6) Uani 0.5 1 d D . P A 1 H30A H 0.849968 0.910307 0.732732 0.123 Uiso 0.5 1 calc R U P A 1 H30B H 0.793152 0.833225 0.675793 0.123 Uiso 0.5 1 calc R U P A 1 C31 C 0.7939(18) 0.897(2) 0.7796(17) 0.128(8) Uani 0.5 1 d D . P A 1 H31A H 0.826397 0.865488 0.830936 0.154 Uiso 0.5 1 calc R U P A 1 H31B H 0.757129 0.854730 0.764924 0.154 Uiso 0.5 1 calc R U P A 1 C32 C 0.7886(18) 1.035(2) 0.777(2) 0.131(6) Uani 0.5 1 d D U P A 1 H32A H 0.813813 1.066147 0.833121 0.158 Uiso 0.5 1 calc R U P A 1 H32B H 0.748003 1.056170 0.761452 0.158 Uiso 0.5 1 calc R U P A 1 C33 C 0.8047(14) 1.1012(15) 0.7190(16) 0.110(6) Uani 0.5 1 d D . P A 1 H33A H 0.784141 1.178513 0.699126 0.132 Uiso 0.5 1 calc R U P A 1 H33B H 0.847064 1.112126 0.742403 0.132 Uiso 0.5 1 calc R U P A 1 C34 C 0.6180(13) 0.9077(19) 0.2885(12) 0.094(5) Uani 0.5 1 d D U P A 1 H34A H 0.583097 0.878233 0.289507 0.113 Uiso 0.5 1 calc R U P A 1 H34B H 0.644583 0.840296 0.296420 0.113 Uiso 0.5 1 calc R U P A 1 C35 C 0.6029(16) 0.982(2) 0.2117(13) 0.113(7) Uani 0.5 1 d D . P A 1 H35A H 0.625865 0.954249 0.186480 0.136 Uiso 0.5 1 calc R U P A 1 H35B H 0.561074 0.973806 0.171174 0.136 Uiso 0.5 1 calc R U P A 1 C36 C 0.6173(11) 1.112(2) 0.2385(12) 0.106(6) Uani 0.5 1 d D . P A 1 H36A H 0.590437 1.169379 0.196520 0.128 Uiso 0.5 1 calc R U P A 1 H36B H 0.658060 1.133226 0.255230 0.128 Uiso 0.5 1 calc R U P A 1 C37 C 0.6068(15) 1.103(2) 0.3110(15) 0.116(6) Uani 0.5 1 d D . P A 1 H37A H 0.619696 1.174641 0.346505 0.139 Uiso 0.5 1 calc R U P A 1 H37B H 0.566145 1.082461 0.294982 0.139 Uiso 0.5 1 calc R U P A 1 C30' C 0.7649(13) 0.9024(14) 0.7162(14) 0.103(6) Uani 0.5 1 d D . P A 2 H30C H 0.786591 0.827377 0.722065 0.123 Uiso 0.5 1 calc R U P A 2 H30D H 0.723018 0.885709 0.693551 0.123 Uiso 0.5 1 calc R U P A 2 C31' C 0.791(2) 0.979(3) 0.7955(15) 0.128(8) Uani 0.5 1 d D . P A 2 H31C H 0.766709 0.967858 0.820724 0.154 Uiso 0.5 1 calc R U P A 2 H31D H 0.830119 0.944732 0.833784 0.154 Uiso 0.5 1 calc R U P A 2 C32' C 0.7992(15) 1.113(2) 0.7891(15) 0.131(6) Uani 0.5 1 d D U P A 2 H32C H 0.784631 1.163987 0.818128 0.158 Uiso 0.5 1 calc R U P A 2 H32D H 0.838680 1.137300 0.801379 0.158 Uiso 0.5 1 calc R U P A 2 C33' C 0.7568(12) 1.0954(14) 0.7001(14) 0.110(6) Uani 0.5 1 d D . P A 2 H33C H 0.717397 1.080400 0.691693 0.132 Uiso 0.5 1 calc R U P A 2 H33D H 0.755430 1.167776 0.668834 0.132 Uiso 0.5 1 calc R U P A 2 C34' C 0.6000(14) 0.893(2) 0.3069(15) 0.094(5) Uani 0.5 1 d D U P A 2 H34C H 0.557735 0.880360 0.283461 0.113 Uiso 0.5 1 calc R U P A 2 H34D H 0.620850 0.826677 0.345230 0.113 Uiso 0.5 1 calc R U P A 2 C35' C 0.6157(11) 0.896(2) 0.2393(13) 0.113(7) Uani 0.5 1 d D . P A 2 H35C H 0.599971 0.827595 0.201141 0.136 Uiso 0.5 1 calc R U P A 2 H35D H 0.657760 0.906390 0.259486 0.136 Uiso 0.5 1 calc R U P A 2 C36' C 0.5801(14) 1.012(2) 0.2060(14) 0.106(6) Uani 0.5 1 d D . P A 2 H36C H 0.586078 1.049149 0.162951 0.128 Uiso 0.5 1 calc R U P A 2 H36D H 0.538124 0.998677 0.184741 0.128 Uiso 0.5 1 calc R U P A 2 C37' C 0.6072(17) 1.088(2) 0.2843(12) 0.116(6) Uani 0.5 1 d D . P A 2 H37C H 0.644436 1.124445 0.294626 0.139 Uiso 0.5 1 calc R U P A 2 H37D H 0.580472 1.152898 0.280822 0.139 Uiso 0.5 1 calc R U P A 2 O1S O 0.3241(10) 1.0000(19) 0.6633(15) 0.109(5) Uani 0.5 1 d D U P E 1 C1S C 0.3622(10) 1.098(2) 0.7008(16) 0.091(6) Uani 0.5 1 d D . P E 1 H1SA H 0.363767 1.118190 0.753003 0.109 Uiso 0.5 1 calc R U P E 1 H1SB H 0.347755 1.169369 0.664853 0.109 Uiso 0.5 1 calc R U P E 1 C2S C 0.4234(11) 1.064(3) 0.7165(16) 0.089(6) Uani 0.5 1 d D . P E 1 H2SA H 0.429651 1.094149 0.672033 0.107 Uiso 0.5 1 calc R U P E 1 H2SB H 0.453776 1.098400 0.768880 0.107 Uiso 0.5 1 calc R U P E 1 C3S C 0.4244(12) 0.927(3) 0.7193(19) 0.097(7) Uani 0.5 1 d D . P E 1 H3SA H 0.452667 0.897299 0.774323 0.117 Uiso 0.5 1 calc R U P E 1 H3SB H 0.433850 0.893120 0.678849 0.117 Uiso 0.5 1 calc R U P E 1 C4S C 0.3616(10) 0.899(2) 0.6976(19) 0.100(8) Uani 0.5 1 d D . P E 1 H4SA H 0.346868 0.831756 0.657985 0.119 Uiso 0.5 1 calc R U P E 1 H4SB H 0.361066 0.872555 0.747308 0.119 Uiso 0.5 1 calc R U P E 1 O1S' O 0.3367(11) 1.0009(19) 0.6329(15) 0.109(5) Uani 0.5 1 d D U P F 2 C1S' C 0.3700(11) 1.106(2) 0.6679(13) 0.091(6) Uani 0.5 1 d D . P F 2 H1SC H 0.346342 1.167400 0.676278 0.109 Uiso 0.5 1 calc R U P F 2 H1SD H 0.383340 1.140352 0.631481 0.109 Uiso 0.5 1 calc R U P F 2 C2S' C 0.4221(12) 1.070(3) 0.7496(13) 0.089(6) Uani 0.5 1 d D . P F 2 H2SC H 0.418153 1.102907 0.795335 0.107 Uiso 0.5 1 calc R U P F 2 H2SD H 0.458635 1.100761 0.753999 0.107 Uiso 0.5 1 calc R U P F 2 C3S' C 0.4229(13) 0.932(3) 0.7523(15) 0.097(7) Uani 0.5 1 d D . P F 2 H3SC H 0.459903 0.900486 0.759018 0.117 Uiso 0.5 1 calc R U P F 2 H3SD H 0.417384 0.902516 0.797423 0.117 Uiso 0.5 1 calc R U P F 2 C4S' C 0.3716(12) 0.897(2) 0.6693(15) 0.100(8) Uani 0.5 1 d D . P F 2 H4SC H 0.386049 0.865512 0.633700 0.119 Uiso 0.5 1 calc R U P F 2 H4SD H 0.348164 0.834419 0.676417 0.119 Uiso 0.5 1 calc R U P F 2 O2S O 0.6586(10) 0.4297(19) 0.2401(14) 0.122(5) Uani 0.5 1 d D U P G 1 C5S C 0.7065(11) 0.350(2) 0.264(2) 0.114(5) Uani 0.5 1 d D U P G 1 H5SA H 0.706377 0.312100 0.216402 0.137 Uiso 0.5 1 calc R U P G 1 H5SB H 0.708233 0.288001 0.302332 0.137 Uiso 0.5 1 calc R U P G 1 C8S C 0.6654(12) 0.538(2) 0.204(2) 0.121(6) Uani 0.5 1 d D . P G 1 H8SA H 0.646915 0.607038 0.215343 0.145 Uiso 0.5 1 calc R U P G 1 H8SB H 0.648809 0.529345 0.144540 0.145 Uiso 0.5 1 calc R U P G 1 C7S C 0.7318(12) 0.551(3) 0.248(2) 0.124(7) Uani 0.5 1 d D . P G 1 H7SA H 0.745957 0.550370 0.208114 0.149 Uiso 0.5 1 calc R U P G 1 H7SB H 0.744101 0.627271 0.278973 0.149 Uiso 0.5 1 calc R U P G 1 C6S C 0.7554(13) 0.443(2) 0.305(2) 0.117(6) Uani 0.5 1 d D U P G 1 H6SA H 0.762095 0.463714 0.360499 0.141 Uiso 0.5 1 calc R U P G 1 H6SB H 0.792094 0.413685 0.309971 0.141 Uiso 0.5 1 calc R U P G 1 O2S' O 0.6584(10) 0.5691(19) 0.2391(14) 0.122(5) Uani 0.5 1 d D U P H 2 C5S' C 0.6694(12) 0.459(2) 0.211(2) 0.114(5) Uani 0.5 1 d D U P H 2 H5SC H 0.651114 0.459428 0.150418 0.137 Uiso 0.5 1 calc R U P H 2 H5SD H 0.653362 0.390492 0.226714 0.137 Uiso 0.5 1 calc R U P H 2 C8S' C 0.7056(11) 0.649(2) 0.264(2) 0.121(6) Uani 0.5 1 d D . P H 2 H8SC H 0.706844 0.710245 0.302553 0.145 Uiso 0.5 1 calc R U P H 2 H8SD H 0.705208 0.689303 0.216514 0.145 Uiso 0.5 1 calc R U P H 2 C7S' C 0.7551(14) 0.558(2) 0.304(2) 0.124(7) Uani 0.5 1 d D . P H 2 H7SC H 0.762208 0.538208 0.359708 0.149 Uiso 0.5 1 calc R U P H 2 H7SD H 0.791402 0.591371 0.309222 0.149 Uiso 0.5 1 calc R U P H 2 C6S' C 0.7359(12) 0.446(3) 0.250(2) 0.117(6) Uani 0.5 1 d D U P H 2 H6SC H 0.750350 0.371909 0.282172 0.141 Uiso 0.5 1 calc R U P H 2 H6SD H 0.748633 0.449353 0.208591 0.141 Uiso 0.5 1 calc R U P H 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 K1 0.0288(6) 0.0186(6) 0.0467(6) -0.0012(6) 0.0212(5) 0.0042(5) N1 0.047(4) 0.172(9) 0.062(4) 0.004(5) 0.035(4) 0.006(4) O1 0.046(3) 0.026(2) 0.062(4) 0.001(2) 0.031(3) -0.001(2) O2 0.036(3) 0.039(3) 0.063(4) -0.006(2) 0.030(3) 0.005(2) O3 0.031(3) 0.032(2) 0.075(4) -0.003(2) 0.025(3) 0.020(2) O4 0.048(3) 0.024(2) 0.079(4) 0.002(2) 0.042(3) 0.006(2) O5 0.032(3) 0.027(3) 0.073(4) 0.002(2) 0.034(3) 0.0065(17) O6 0.052(3) 0.020(2) 0.079(4) -0.010(2) 0.042(3) 0.000(2) O7 0.119(9) 0.110(8) 0.048(6) 0.020(4) 0.036(6) 0.012(5) O8 0.082(9) 0.070(5) 0.046(4) 0.005(3) 0.018(6) 0.005(6) O7' 0.119(9) 0.110(8) 0.048(6) 0.020(4) 0.036(6) 0.012(5) O8' 0.082(9) 0.070(5) 0.046(4) 0.005(3) 0.018(6) 0.005(6) B1 0.040(4) 0.028(3) 0.056(4) -0.003(3) 0.034(3) 0.004(3) C1 0.039(4) 0.028(3) 0.082(5) 0.005(3) 0.042(4) 0.013(3) C2 0.082(6) 0.038(4) 0.086(6) 0.025(4) 0.047(5) 0.019(4) C3 0.127(9) 0.058(6) 0.116(8) 0.038(5) 0.091(8) 0.036(5) C4 0.102(8) 0.031(4) 0.179(10) 0.022(5) 0.114(8) 0.025(4) C5 0.071(6) 0.025(4) 0.150(8) -0.026(5) 0.070(7) -0.006(4) C6 0.070(5) 0.028(4) 0.106(6) -0.005(4) 0.054(5) 0.001(3) C7 0.058(8) 0.145(11) 0.094(8) -0.008(7) 0.052(7) -0.002(6) C7' 0.058(8) 0.145(11) 0.094(8) -0.008(7) 0.052(7) -0.002(6) C8 0.065(5) 0.055(5) 0.054(4) 0.001(4) 0.037(4) -0.001(3) C9 0.098(18) 0.15(4) 0.054(9) -0.007(13) 0.045(10) -0.02(3) C10 0.074(12) 0.060(12) 0.119(18) -0.013(12) 0.056(13) 0.005(9) C11 0.076(9) 0.062(7) 0.095(9) 0.001(7) 0.066(8) -0.003(6) C9' 0.11(2) 0.10(3) 0.057(10) -0.003(12) 0.038(11) 0.00(2) C10' 0.105(16) 0.059(9) 0.056(11) -0.016(8) 0.039(12) 0.003(9) C11' 0.076(9) 0.062(7) 0.095(9) 0.001(7) 0.066(8) -0.003(6) C12 0.039(4) 0.026(3) 0.082(5) -0.010(3) 0.043(4) -0.009(2) C13 0.073(6) 0.046(5) 0.092(6) -0.018(4) 0.051(5) -0.013(4) C14 0.115(9) 0.055(6) 0.107(7) -0.041(5) 0.076(7) -0.025(5) C15 0.080(6) 0.065(5) 0.131(7) -0.030(5) 0.084(6) -0.028(4) C16 0.060(5) 0.036(4) 0.132(7) 0.019(5) 0.053(6) 0.008(4) C17 0.061(5) 0.037(4) 0.100(6) 0.005(4) 0.054(5) 0.005(3) C18 0.052(5) 0.056(5) 0.058(5) -0.002(4) 0.037(4) -0.010(4) C19 0.036(4) 0.063(5) 0.062(5) 0.000(4) 0.030(4) 0.002(3) C20 0.033(4) 0.059(5) 0.083(6) 0.006(4) 0.035(4) 0.026(3) C21 0.045(4) 0.048(4) 0.072(6) -0.012(4) 0.032(4) 0.020(3) C22 0.065(4) 0.019(3) 0.079(5) -0.013(3) 0.034(4) 0.010(3) C23 0.059(5) 0.023(4) 0.132(9) 0.017(4) 0.055(6) 0.011(3) C24 0.059(5) 0.020(3) 0.106(7) 0.008(4) 0.056(5) 0.002(3) C25 0.042(4) 0.034(4) 0.074(6) -0.011(3) 0.040(4) -0.005(3) C26 0.040(4) 0.029(3) 0.089(6) -0.004(3) 0.043(4) 0.009(3) C27 0.056(5) 0.026(4) 0.101(7) -0.006(4) 0.055(5) 0.013(3) C28 0.060(5) 0.024(3) 0.099(7) -0.012(4) 0.044(5) 0.005(3) C29 0.059(5) 0.032(4) 0.109(8) -0.001(4) 0.053(5) -0.004(3) C30 0.135(19) 0.092(9) 0.082(9) 0.017(7) 0.054(11) -0.002(10) C31 0.19(2) 0.139(14) 0.064(10) 0.010(11) 0.065(12) -0.029(18) C32 0.148(11) 0.137(11) 0.117(8) -0.021(7) 0.071(8) -0.012(9) C33 0.108(15) 0.099(10) 0.088(8) 0.000(7) 0.022(9) 0.004(10) C34 0.105(10) 0.088(7) 0.081(7) -0.009(5) 0.039(6) -0.022(7) C35 0.111(15) 0.144(14) 0.044(8) 0.013(7) 0.007(9) 0.052(11) C36 0.085(12) 0.129(13) 0.060(8) 0.036(7) 0.002(8) 0.017(9) C37 0.167(13) 0.088(9) 0.056(10) 0.032(7) 0.026(10) 0.031(9) C30' 0.135(19) 0.092(9) 0.082(9) 0.017(7) 0.054(11) -0.002(10) C31' 0.19(2) 0.139(14) 0.064(10) 0.010(11) 0.065(12) -0.029(18) C32' 0.148(11) 0.137(11) 0.117(8) -0.021(7) 0.071(8) -0.012(9) C33' 0.108(15) 0.099(10) 0.088(8) 0.000(7) 0.022(9) 0.004(10) C34' 0.105(10) 0.088(7) 0.081(7) -0.009(5) 0.039(6) -0.022(7) C35' 0.111(15) 0.144(14) 0.044(8) 0.013(7) 0.007(9) 0.052(11) C36' 0.085(12) 0.129(13) 0.060(8) 0.036(7) 0.002(8) 0.017(9) C37' 0.167(13) 0.088(9) 0.056(10) 0.032(7) 0.026(10) 0.031(9) O1S 0.108(8) 0.097(6) 0.103(9) -0.001(7) 0.039(6) 0.001(5) C1S 0.131(11) 0.071(8) 0.069(13) 0.019(9) 0.048(9) 0.012(7) C2S 0.118(10) 0.079(9) 0.062(13) -0.007(12) 0.039(10) -0.019(7) C3S 0.121(10) 0.088(9) 0.081(15) 0.006(13) 0.049(10) 0.023(8) C4S 0.129(12) 0.066(7) 0.095(16) -0.014(10) 0.049(10) -0.014(7) O1S' 0.108(8) 0.097(6) 0.103(9) -0.001(7) 0.039(6) 0.001(5) C1S' 0.131(11) 0.071(8) 0.069(13) 0.019(9) 0.048(9) 0.012(7) C2S' 0.118(10) 0.079(9) 0.062(13) -0.007(12) 0.039(10) -0.019(7) C3S' 0.121(10) 0.088(9) 0.081(15) 0.006(13) 0.049(10) 0.023(8) C4S' 0.129(12) 0.066(7) 0.095(16) -0.014(10) 0.049(10) -0.014(7) O2S 0.127(7) 0.112(8) 0.123(9) 0.000(6) 0.060(7) 0.001(5) C5S 0.113(8) 0.109(8) 0.115(10) -0.004(7) 0.052(7) 0.000(6) C8S 0.108(10) 0.102(11) 0.140(18) 0.017(10) 0.052(12) 0.009(8) C7S 0.116(11) 0.119(13) 0.117(17) 0.003(10) 0.043(12) 0.005(9) C6S 0.117(8) 0.111(9) 0.121(11) 0.003(8) 0.057(7) 0.000(7) O2S' 0.127(7) 0.112(8) 0.123(9) 0.000(6) 0.060(7) 0.001(5) C5S' 0.113(8) 0.109(8) 0.115(10) -0.004(7) 0.052(7) 0.000(6) C8S' 0.108(10) 0.102(11) 0.140(18) 0.017(10) 0.052(12) 0.009(8) C7S' 0.116(11) 0.119(13) 0.117(17) 0.003(10) 0.043(12) 0.005(9) C6S' 0.117(8) 0.111(9) 0.121(11) 0.003(8) 0.057(7) 0.000(7) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 K1 O8 165.1(9) . . ? O7' K1 O8' 170.8(8) . . ? O7 K1 O1 99.9(6) . . ? O8 K1 O1 89.3(4) . . ? O7' K1 O1 93.7(5) . . ? O8' K1 O1 80.7(3) . . ? O7 K1 O3 96.6(5) . . ? O8 K1 O3 88.6(4) . . ? O7' K1 O3 96.5(5) . . ? O8' K1 O3 80.4(4) . . ? O1 K1 O3 120.52(17) . . ? O7 K1 O5 84.6(8) . . ? O8 K1 O5 80.7(4) . . ? O7' K1 O5 91.2(7) . . ? O8' K1 O5 97.9(4) . . ? O1 K1 O5 119.09(13) . . ? O3 K1 O5 119.10(14) . . ? O7 K1 O2 96.2(8) . . ? O8 K1 O2 98.5(4) . . ? O7' K1 O2 89.6(7) . . ? O8' K1 O2 81.3(4) . . ? O1 K1 O2 60.77(13) . . ? O3 K1 O2 60.87(14) . . ? O5 K1 O2 179.2(2) . . ? O7 K1 O4 79.7(6) . . ? O8 K1 O4 91.0(4) . . ? O7' K1 O4 85.9(5) . . ? O8' K1 O4 99.7(4) . . ? O1 K1 O4 179.41(19) . . ? O3 K1 O4 59.97(13) . . ? O5 K1 O4 60.51(12) . . ? O2 K1 O4 119.64(13) . . ? O7 K1 O6 82.4(5) . . ? O8 K1 O6 92.3(4) . . ? O7' K1 O6 82.6(5) . . ? O8' K1 O6 100.6(4) . . ? O1 K1 O6 60.08(13) . . ? O3 K1 O6 178.9(2) . . ? O5 K1 O6 60.52(13) . . ? O2 K1 O6 119.53(14) . . ? O4 K1 O6 119.42(16) . . ? O7' K1 C33' 24.8(4) . . ? O8' K1 C33' 150.0(6) . . ? O1 K1 C33' 103.5(4) . . ? O3 K1 C33' 71.8(4) . . ? O5 K1 C33' 105.4(6) . . ? O2 K1 C33' 75.4(6) . . ? O4 K1 C33' 76.3(4) . . ? O6 K1 C33' 107.3(4) . . ? O7 K1 C37 159.1(7) . . ? O8 K1 C37 22.4(4) . . ? O1 K1 C37 99.2(6) . . ? O3 K1 C37 66.3(4) . . ? O5 K1 C37 93.3(5) . . ? O2 K1 C37 86.0(5) . . ? O4 K1 C37 81.2(6) . . ? O6 K1 C37 114.6(4) . . ? C8 N1 C7 103.6(8) . . ? C8 N1 C7' 102.7(8) . . ? C8 N1 B1 126.9(7) . . ? C7 N1 B1 94.8(9) . . ? C7' N1 B1 93.7(9) . . ? C29 O1 C18 112.1(6) . . ? C29 O1 K1 114.7(4) . . ? C18 O1 K1 114.7(4) . . ? C19 O2 C20 111.3(7) . . ? C19 O2 K1 113.0(4) . . ? C20 O2 K1 112.5(4) . . ? C22 O3 C21 112.2(6) . . ? C22 O3 K1 115.3(4) . . ? C21 O3 K1 114.4(4) . . ? C24 O4 C23 112.7(6) . . ? C24 O4 K1 113.8(4) . . ? C23 O4 K1 115.4(4) . . ? C26 O5 C25 111.9(6) . . ? C26 O5 K1 114.8(4) . . ? C25 O5 K1 114.4(4) . . ? C28 O6 C27 112.7(6) . . ? C28 O6 K1 115.1(4) . . ? C27 O6 K1 113.6(4) . . ? C30 O7 C33 100.0(11) . . ? C30 O7 K1 125.1(14) . . ? C33 O7 K1 134.2(14) . . ? C34 O8 C37 105(2) . . ? C34 O8 K1 129.6(13) . . ? C37 O8 K1 112.7(13) . . ? C30' O7' C33' 98.4(12) . . ? C30' O7' K1 116.3(19) . . ? C33' O7' K1 102.0(17) . . ? C34' O8' C37' 104.6(18) . . ? C34' O8' K1 117.6(15) . . ? C37' O8' K1 127.9(16) . . ? N1 B1 C12 107.3(6) . . ? N1 B1 C1 106.4(6) . . ? C12 B1 C1 110.9(6) . . ? N1 B1 H1 118(3) . . ? C12 B1 H1 107(2) . . ? C1 B1 H1 107(2) . . ? C6 C1 C2 116.5(8) . . ? C6 C1 B1 117.9(7) . . ? C2 C1 B1 125.6(8) . . ? C1 C2 C3 125.2(11) . . ? C1 C2 H2A 117.4 . . ? C3 C2 H2A 117.4 . . ? C4 C3 C2 117.8(11) . . ? C4 C3 H3A 121.1 . . ? C2 C3 H3A 121.1 . . ? C3 C4 C5 121.0(10) . . ? C3 C4 H4A 119.5 . . ? C5 C4 H4A 119.5 . . ? C4 C5 C6 121.8(10) . . ? C4 C5 H5A 119.1 . . ? C6 C5 H5A 119.1 . . ? C1 C6 C5 117.6(10) . . ? C1 C6 C7 95.8(9) . . ? C5 C6 C7 145.9(10) . . ? C1 C6 H6A 121.2 . . ? C5 C6 H6A 121.2 . . ? N1 C7 C6 121.8(12) . . ? N1 C7 H7A 106.9 . . ? C6 C7 H7A 106.9 . . ? N1 C7 H7B 106.9 . . ? C6 C7 H7B 106.9 . . ? H7A C7 H7B 106.7 . . ? N1 C7' C17 122.9(12) . . ? N1 C7' H7'A 106.6 . . ? C17 C7' H7'A 106.6 . . ? N1 C7' H7'B 106.6 . . ? C17 C7' H7'B 106.6 . . ? H7'A C7' H7'B 106.6 . . ? N1 C8 C11 96.1(8) . . ? N1 C8 C10' 97.1(10) . . ? N1 C8 C10 122.0(12) . . ? C11 C8 C10 108.0(13) . . ? N1 C8 C9' 111(3) . . ? C10' C8 C9' 111(2) . . ? N1 C8 C9 112(3) . . ? C11 C8 C9 113(2) . . ? C10 C8 C9 106(3) . . ? N1 C8 C11' 122.3(10) . . ? C10' C8 C11' 110.4(13) . . ? C9' C8 C11' 105(3) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C8 C9' H9'A 109.5 . . ? C8 C9' H9'B 109.5 . . ? H9'A C9' H9'B 109.5 . . ? C8 C9' H9'C 109.5 . . ? H9'A C9' H9'C 109.5 . . ? H9'B C9' H9'C 109.5 . . ? C8 C10' H10D 109.5 . . ? C8 C10' H10E 109.5 . . ? H10D C10' H10E 109.5 . . ? C8 C10' H10F 109.5 . . ? H10D C10' H10F 109.5 . . ? H10E C10' H10F 109.5 . . ? C8 C11' H11D 109.5 . . ? C8 C11' H11E 109.5 . . ? H11D C11' H11E 109.5 . . ? C8 C11' H11F 109.5 . . ? H11D C11' H11F 109.5 . . ? H11E C11' H11F 109.5 . . ? C13 C12 C17 116.6(7) . . ? C13 C12 B1 125.1(8) . . ? C17 C12 B1 118.3(7) . . ? C12 C13 C14 125.0(11) . . ? C12 C13 H13A 117.5 . . ? C14 C13 H13A 117.5 . . ? C15 C14 C13 117.7(11) . . ? C15 C14 H14A 121.1 . . ? C13 C14 H14A 121.1 . . ? C14 C15 C16 122.0(10) . . ? C14 C15 H15A 119.0 . . ? C16 C15 H15A 119.0 . . ? C15 C16 C17 120.9(10) . . ? C15 C16 H16A 119.6 . . ? C17 C16 H16A 119.6 . . ? C12 C17 C16 117.7(9) . . ? C12 C17 C7' 94.3(9) . . ? C16 C17 C7' 147.3(10) . . ? C12 C17 H17A 121.1 . . ? C16 C17 H17A 121.1 . . ? O1 C18 C19 107.6(6) . . ? O1 C18 H18A 110.2 . . ? C19 C18 H18A 110.2 . . ? O1 C18 H18B 110.2 . . ? C19 C18 H18B 110.2 . . ? H18A C18 H18B 108.5 . . ? O2 C19 C18 107.9(6) . . ? O2 C19 H19A 110.1 . . ? C18 C19 H19A 110.1 . . ? O2 C19 H19B 110.1 . . ? C18 C19 H19B 110.1 . . ? H19A C19 H19B 108.4 . . ? O2 C20 C21 108.2(6) . . ? O2 C20 H20A 110.1 . . ? C21 C20 H20A 110.1 . . ? O2 C20 H20B 110.1 . . ? C21 C20 H20B 110.1 . . ? H20A C20 H20B 108.4 . . ? O3 C21 C20 108.0(6) . . ? O3 C21 H21A 110.1 . . ? C20 C21 H21A 110.1 . . ? O3 C21 H21B 110.1 . . ? C20 C21 H21B 110.1 . . ? H21A C21 H21B 108.4 . . ? O3 C22 C23 107.5(6) . . ? O3 C22 H22A 110.2 . . ? C23 C22 H22A 110.2 . . ? O3 C22 H22B 110.2 . . ? C23 C22 H22B 110.2 . . ? H22A C22 H22B 108.5 . . ? O4 C23 C22 107.3(7) . . ? O4 C23 H23A 110.3 . . ? C22 C23 H23A 110.3 . . ? O4 C23 H23B 110.3 . . ? C22 C23 H23B 110.3 . . ? H23A C23 H23B 108.5 . . ? O4 C24 C25 109.3(6) . . ? O4 C24 H24A 109.8 . . ? C25 C24 H24A 109.8 . . ? O4 C24 H24B 109.8 . . ? C25 C24 H24B 109.8 . . ? H24A C24 H24B 108.3 . . ? O5 C25 C24 109.0(6) . . ? O5 C25 H25A 109.9 . . ? C24 C25 H25A 109.9 . . ? O5 C25 H25B 109.9 . . ? C24 C25 H25B 109.9 . . ? H25A C25 H25B 108.3 . . ? O5 C26 C27 108.9(6) . . ? O5 C26 H26A 109.9 . . ? C27 C26 H26A 109.9 . . ? O5 C26 H26B 109.9 . . ? C27 C26 H26B 109.9 . . ? H26A C26 H26B 108.3 . . ? O6 C27 C26 108.7(6) . . ? O6 C27 H27A 109.9 . . ? C26 C27 H27A 109.9 . . ? O6 C27 H27B 109.9 . . ? C26 C27 H27B 109.9 . . ? H27A C27 H27B 108.3 . . ? O6 C28 C29 107.8(7) . . ? O6 C28 H28A 110.1 . . ? C29 C28 H28A 110.1 . . ? O6 C28 H28B 110.1 . . ? C29 C28 H28B 110.1 . . ? H28A C28 H28B 108.5 . . ? O1 C29 C28 109.5(7) . . ? O1 C29 H29A 109.8 . . ? C28 C29 H29A 109.8 . . ? O1 C29 H29B 109.8 . . ? C28 C29 H29B 109.8 . . ? H29A C29 H29B 108.2 . . ? O7 C30 C31 113(2) . . ? O7 C30 H30A 109.0 . . ? C31 C30 H30A 109.0 . . ? O7 C30 H30B 109.0 . . ? C31 C30 H30B 109.0 . . ? H30A C30 H30B 107.8 . . ? C30 C31 C32 88.0(18) . . ? C30 C31 H31A 114.0 . . ? C32 C31 H31A 114.0 . . ? C30 C31 H31B 114.0 . . ? C32 C31 H31B 114.0 . . ? H31A C31 H31B 111.2 . . ? C31 C32 C33 116(2) . . ? C31 C32 H32A 108.2 . . ? C33 C32 H32A 108.2 . . ? C31 C32 H32B 108.2 . . ? C33 C32 H32B 108.2 . . ? H32A C32 H32B 107.4 . . ? O7 C33 C32 93(2) . . ? O7 C33 H33A 113.1 . . ? C32 C33 H33A 113.1 . . ? O7 C33 H33B 113.1 . . ? C32 C33 H33B 113.1 . . ? H33A C33 H33B 110.5 . . ? O8 C34 C35 95.2(16) . . ? O8 C34 H34A 112.7 . . ? C35 C34 H34A 112.7 . . ? O8 C34 H34B 112.7 . . ? C35 C34 H34B 112.7 . . ? H34A C34 H34B 110.2 . . ? C36 C35 C34 107.2(17) . . ? C36 C35 H35A 110.3 . . ? C34 C35 H35A 110.3 . . ? C36 C35 H35B 110.3 . . ? C34 C35 H35B 110.3 . . ? H35A C35 H35B 108.5 . . ? C35 C36 C37 96.0(19) . . ? C35 C36 H36A 112.6 . . ? C37 C36 H36A 112.6 . . ? C35 C36 H36B 112.6 . . ? C37 C36 H36B 112.6 . . ? H36A C36 H36B 110.1 . . ? O8 C37 C36 91.9(15) . . ? O8 C37 K1 44.9(10) . . ? C36 C37 K1 127.6(16) . . ? O8 C37 H37A 113.3 . . ? C36 C37 H37A 113.3 . . ? K1 C37 H37A 73.6 . . ? O8 C37 H37B 113.3 . . ? C36 C37 H37B 113.3 . . ? K1 C37 H37B 111.3 . . ? H37A C37 H37B 110.6 . . ? O7' C30' C31' 92.0(17) . . ? O7' C30' H30C 113.3 . . ? C31' C30' H30C 113.3 . . ? O7' C30' H30D 113.3 . . ? C31' C30' H30D 113.3 . . ? H30C C30' H30D 110.6 . . ? C32' C31' C30' 118.4(19) . . ? C32' C31' H31C 107.7 . . ? C30' C31' H31C 107.7 . . ? C32' C31' H31D 107.7 . . ? C30' C31' H31D 107.7 . . ? H31C C31' H31D 107.1 . . ? C33' C32' C31' 84.5(19) . . ? C33' C32' H32C 114.6 . . ? C31' C32' H32C 114.6 . . ? C33' C32' H32D 114.6 . . ? C31' C32' H32D 114.6 . . ? H32C C32' H32D 111.7 . . ? O7' C33' C32' 108(2) . . ? O7' C33' K1 53.2(14) . . ? C32' C33' K1 159(2) . . ? O7' C33' H33C 110.2 . . ? C32' C33' H33C 110.2 . . ? K1 C33' H33C 85.9 . . ? O7' C33' H33D 110.2 . . ? C32' C33' H33D 110.2 . . ? K1 C33' H33D 74.9 . . ? H33C C33' H33D 108.5 . . ? O8' C34' C35' 107.3(19) . . ? O8' C34' H34C 110.2 . . ? C35' C34' H34C 110.2 . . ? O8' C34' H34D 110.2 . . ? C35' C34' H34D 110.2 . . ? H34C C34' H34D 108.5 . . ? C34' C35' C36' 89.8(19) . . ? C34' C35' H35C 113.7 . . ? C36' C35' H35C 113.7 . . ? C34' C35' H35D 113.7 . . ? C36' C35' H35D 113.7 . . ? H35C C35' H35D 110.9 . . ? C37' C36' C35' 99.9(18) . . ? C37' C36' H36C 111.8 . . ? C35' C36' H36C 111.8 . . ? C37' C36' H36D 111.8 . . ? C35' C36' H36D 111.8 . . ? H36C C36' H36D 109.5 . . ? O8' C37' C36' 103.4(19) . . ? O8' C37' H37C 111.1 . . ? C36' C37' H37C 111.1 . . ? O8' C37' H37D 111.1 . . ? C36' C37' H37D 111.1 . . ? H37C C37' H37D 109.1 . . ? C1S O1S C4S 103(2) . . ? O1S C1S C2S 109(2) . . ? O1S C1S H1SA 109.9 . . ? C2S C1S H1SA 109.9 . . ? O1S C1S H1SB 109.9 . . ? C2S C1S H1SB 109.9 . . ? H1SA C1S H1SB 108.3 . . ? C3S C2S C1S 105(2) . . ? C3S C2S H2SA 110.9 . . ? C1S C2S H2SA 110.9 . . ? C3S C2S H2SB 110.9 . . ? C1S C2S H2SB 110.9 . . ? H2SA C2S H2SB 108.9 . . ? C2S C3S C4S 102(2) . . ? C2S C3S H3SA 111.5 . . ? C4S C3S H3SA 111.5 . . ? C2S C3S H3SB 111.5 . . ? C4S C3S H3SB 111.5 . . ? H3SA C3S H3SB 109.3 . . ? O1S C4S C3S 112(3) . . ? O1S C4S H4SA 109.2 . . ? C3S C4S H4SA 109.2 . . ? O1S C4S H4SB 109.2 . . ? C3S C4S H4SB 109.2 . . ? H4SA C4S H4SB 107.9 . . ? C1S' O1S' C4S' 110(2) . . ? O1S' C1S' C2S' 107(2) . . ? O1S' C1S' H1SC 110.3 . . ? C2S' C1S' H1SC 110.3 . . ? O1S' C1S' H1SD 110.3 . . ? C2S' C1S' H1SD 110.3 . . ? H1SC C1S' H1SD 108.6 . . ? C1S' C2S' C3S' 107(2) . . ? C1S' C2S' H2SC 110.4 . . ? C3S' C2S' H2SC 110.4 . . ? C1S' C2S' H2SD 110.4 . . ? C3S' C2S' H2SD 110.4 . . ? H2SC C2S' H2SD 108.6 . . ? C4S' C3S' C2S' 103(2) . . ? C4S' C3S' H3SC 111.1 . . ? C2S' C3S' H3SC 111.1 . . ? C4S' C3S' H3SD 111.1 . . ? C2S' C3S' H3SD 111.1 . . ? H3SC C3S' H3SD 109.1 . . ? O1S' C4S' C3S' 109(2) . . ? O1S' C4S' H4SC 109.9 . . ? C3S' C4S' H4SC 109.9 . . ? O1S' C4S' H4SD 109.9 . . ? C3S' C4S' H4SD 109.9 . . ? H4SC C4S' H4SD 108.3 . . ? C5S O2S C8S 112(2) . . ? O2S C5S C6S 98(2) . . ? O2S C5S H5SA 112.2 . . ? C6S C5S H5SA 112.2 . . ? O2S C5S H5SB 112.2 . . ? C6S C5S H5SB 112.2 . . ? H5SA C5S H5SB 109.8 . . ? O2S C8S C7S 102(2) . . ? O2S C8S H8SA 111.4 . . ? C7S C8S H8SA 111.4 . . ? O2S C8S H8SB 111.4 . . ? C7S C8S H8SB 111.4 . . ? H8SA C8S H8SB 109.3 . . ? C6S C7S C8S 105(2) . . ? C6S C7S H7SA 110.7 . . ? C8S C7S H7SA 110.7 . . ? C6S C7S H7SB 110.7 . . ? C8S C7S H7SB 110.7 . . ? H7SA C7S H7SB 108.8 . . ? C7S C6S C5S 103(2) . . ? C7S C6S H6SA 111.2 . . ? C5S C6S H6SA 111.2 . . ? C7S C6S H6SB 111.2 . . ? C5S C6S H6SB 111.2 . . ? H6SA C6S H6SB 109.1 . . ? C8S' O2S' C5S' 111(2) . . ? O2S' C5S' C6S' 107(2) . . ? O2S' C5S' H5SC 110.3 . . ? C6S' C5S' H5SC 110.3 . . ? O2S' C5S' H5SD 110.3 . . ? C6S' C5S' H5SD 110.3 . . ? H5SC C5S' H5SD 108.6 . . ? O2S' C8S' C7S' 98(2) . . ? O2S' C8S' H8SC 112.1 . . ? C7S' C8S' H8SC 112.1 . . ? O2S' C8S' H8SD 112.1 . . ? C7S' C8S' H8SD 112.1 . . ? H8SC C8S' H8SD 109.8 . . ? C8S' C7S' C6S' 107(2) . . ? C8S' C7S' H7SC 110.4 . . ? C6S' C7S' H7SC 110.4 . . ? C8S' C7S' H7SD 110.4 . . ? C6S' C7S' H7SD 110.4 . . ? H7SC C7S' H7SD 108.6 . . ? C7S' C6S' C5S' 100(2) . . ? C7S' C6S' H6SC 111.8 . . ? C5S' C6S' H6SC 111.8 . . ? C7S' C6S' H6SD 111.8 . . ? C5S' C6S' H6SD 111.8 . . ? H6SC C6S' H6SD 109.5 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag K1 O7 2.57(2) . ? K1 O8 2.672(15) . ? K1 O7' 2.74(3) . ? K1 O8' 2.747(16) . ? K1 O1 2.777(5) . ? K1 O3 2.782(4) . ? K1 O5 2.787(5) . ? K1 O2 2.792(5) . ? K1 O4 2.804(5) . ? K1 O6 2.808(5) . ? K1 C33' 3.35(2) . ? K1 C37 3.49(2) . ? N1 C8 1.412(12) . ? N1 C7 1.550(13) . ? N1 C7' 1.553(13) . ? N1 B1 1.570(13) . ? O1 C29 1.405(9) . ? O1 C18 1.426(9) . ? O2 C19 1.413(9) . ? O2 C20 1.434(9) . ? O3 C22 1.419(9) . ? O3 C21 1.438(10) . ? O4 C24 1.404(10) . ? O4 C23 1.430(8) . ? O5 C26 1.413(8) . ? O5 C25 1.414(8) . ? O6 C28 1.420(9) . ? O6 C27 1.421(10) . ? O7 C30 1.425(10) . ? O7 C33 1.427(10) . ? O8 C34 1.424(10) . ? O8 C37 1.441(10) . ? O7' C30' 1.431(14) . ? O7' C33' 1.439(14) . ? O8' C34' 1.392(13) . ? O8' C37' 1.451(13) . ? B1 C12 1.599(9) . ? B1 C1 1.607(10) . ? B1 H1 1.10(6) . ? C1 C6 1.372(12) . ? C1 C2 1.383(12) . ? C2 C3 1.392(14) . ? C2 H2A 0.9500 . ? C3 C4 1.317(18) . ? C3 H3A 0.9500 . ? C4 C5 1.349(17) . ? C4 H4A 0.9500 . ? C5 C6 1.458(13) . ? C5 H5A 0.9500 . ? C6 C7 1.552(12) . ? C6 H6A 0.9500 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C7' C17 1.563(12) . ? C7' H7'A 0.9900 . ? C7' H7'B 0.9900 . ? C8 C11 1.526(12) . ? C8 C10' 1.533(12) . ? C8 C10 1.536(12) . ? C8 C9' 1.542(14) . ? C8 C9 1.543(14) . ? C8 C11' 1.548(12) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C9' H9'A 0.9800 . ? C9' H9'B 0.9800 . ? C9' H9'C 0.9800 . ? C10' H10D 0.9800 . ? C10' H10E 0.9800 . ? C10' H10F 0.9800 . ? C11' H11D 0.9800 . ? C11' H11E 0.9800 . ? C11' H11F 0.9800 . ? C12 C13 1.375(12) . ? C12 C17 1.386(12) . ? C13 C14 1.401(13) . ? C13 H13A 0.9500 . ? C14 C15 1.312(17) . ? C14 H14A 0.9500 . ? C15 C16 1.353(16) . ? C15 H15A 0.9500 . ? C16 C17 1.461(13) . ? C16 H16A 0.9500 . ? C17 H17A 0.9500 . ? C18 C19 1.509(12) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.479(12) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.514(11) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.490(10) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.493(10) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.491(11) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.531(10) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.547(10) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.547(10) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.543(10) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.527(10) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.528(10) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C30' C31' 1.555(14) . ? C30' H30C 0.9900 . ? C30' H30D 0.9900 . ? C31' C32' 1.528(14) . ? C31' H31C 0.9900 . ? C31' H31D 0.9900 . ? C32' C33' 1.501(14) . ? C32' H32C 0.9900 . ? C32' H32D 0.9900 . ? C33' H33C 0.9900 . ? C33' H33D 0.9900 . ? C34' C35' 1.522(14) . ? C34' H34C 0.9900 . ? C34' H34D 0.9900 . ? C35' C36' 1.544(14) . ? C35' H35C 0.9900 . ? C35' H35D 0.9900 . ? C36' C37' 1.539(14) . ? C36' H36C 0.9900 . ? C36' H36D 0.9900 . ? C37' H37C 0.9900 . ? C37' H37D 0.9900 . ? O1S C1S 1.420(13) . ? O1S C4S 1.431(13) . ? C1S C2S 1.543(14) . ? C1S H1SA 0.9900 . ? C1S H1SB 0.9900 . ? C2S C3S 1.533(14) . ? C2S H2SA 0.9900 . ? C2S H2SB 0.9900 . ? C3S C4S 1.537(14) . ? C3S H3SA 0.9900 . ? C3S H3SB 0.9900 . ? C4S H4SA 0.9900 . ? C4S H4SB 0.9900 . ? O1S' C1S' 1.424(13) . ? O1S' C4S' 1.426(13) . ? C1S' C2S' 1.531(14) . ? C1S' H1SC 0.9900 . ? C1S' H1SD 0.9900 . ? C2S' C3S' 1.537(14) . ? C2S' H2SC 0.9900 . ? C2S' H2SD 0.9900 . ? C3S' C4S' 1.531(14) . ? C3S' H3SC 0.9900 . ? C3S' H3SD 0.9900 . ? C4S' H4SC 0.9900 . ? C4S' H4SD 0.9900 . ? O2S C5S 1.426(14) . ? O2S C8S 1.440(14) . ? C5S C6S 1.537(14) . ? C5S H5SA 0.9900 . ? C5S H5SB 0.9900 . ? C8S C7S 1.537(14) . ? C8S H8SA 0.9900 . ? C8S H8SB 0.9900 . ? C7S C6S 1.535(14) . ? C7S H7SA 0.9900 . ? C7S H7SB 0.9900 . ? C6S H6SA 0.9900 . ? C6S H6SB 0.9900 . ? O2S' C8S' 1.416(14) . ? O2S' C5S' 1.433(14) . ? C5S' C6S' 1.540(14) . ? C5S' H5SC 0.9900 . ? C5S' H5SD 0.9900 . ? C8S' C7S' 1.532(14) . ? C8S' H8SC 0.9900 . ? C8S' H8SD 0.9900 . ? C7S' C6S' 1.537(14) . ? C7S' H7SC 0.9900 . ? C7S' H7SD 0.9900 . ? C6S' H6SC 0.9900 . ? C6S' H6SD 0.9900 . ?