# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_rhl19_0m _database_code_depnum_ccdc_archive 'CCDC 892045' #TrackingRef '12599_web_deposit_cif_file_0_RichardHooley_1342215752.M2L2 complex.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39.59 H31.71 Bi Cl3 F9 N7.80 O12.05 S3' _chemical_formula_weight 1391.94 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' 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Bi Bi -4.1077 10.2566 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.5697(3) _cell_length_b 13.7043(4) _cell_length_c 20.0249(6) _cell_angle_alpha 98.057(1) _cell_angle_beta 92.112(1) _cell_angle_gamma 96.452(1) _cell_volume 2849.71(14) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9873 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 30.14 _exptl_crystal_description 'prism frag' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.622 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1366 _exptl_absorpt_coefficient_mu 3.433 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3770 _exptl_absorpt_correction_T_max 0.8001 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _iucr_refine_instructions_details ; TITL rhL19_0m in P-1 CELL 0.71073 10.5697 13.7043 20.0249 98.057 92.112 96.452 ZERR 2.00 0.0003 0.0004 0.0006 0.001 0.001 0.001 LATT 1 SFAC C H N O F S CL BI UNIT 79.19 63.42 15.59 24.09 18 6 6 2 OMIT -1 1 1 OMIT 1 -1 1 OMIT 0 -2 2 OMIT -1 1 0 OMIT 0 2 2 OMIT -2 1 1 OMIT 0 3 0 OMIT 2 -1 1 OMIT 1 -2 1 OMIT 1 0 1 OMIT 0 1 1 OMIT 0 1 2 OMIT 2 -1 2 OMIT 3 0 0 OMIT -3 0 1 OMIT -1 -2 1 OMIT -1 0 1 OMIT 4 -1 3 OMIT 3 -1 2 OMIT 1 0 4 OMIT 0 2 5 L.S. 8 ACTA BOND $H FMAP 2 PLAN 20 DFIX 0.85 0.01 O2W H1W O2W H2W DFIX 1.34 0.01 H1W H2W CONF SIZE 0.068 0.172 0.353 SADI 0.01 F1F F2F F2F F3F F3F F1F SADI 0.01 F1F S1F F2F S1F F3F S1F SADI 0.01 O1F C1F O2F C1F O3F C1F SADI 0.01 O1F O2F O2F O3F O3F O1F SADI 0.01 S1F O1F S1F O2F S1F O3F SADI 0.01 C1F F1F C1F F2F C1F F3F SADI 0.01 F1C F2C F2C F3C F3C F1C SADI 0.01 F1C S1C F2C S1C F3C S1C SADI 0.01 O1C C1C O2C C1C O3C C1C SADI 0.01 O1C O2C O2C O3C O3C O1C SADI 0.01 S1C O1C S1C O2C S1C O3C SADI 0.01 C1C F1C C1C F2C C1C F3C SADI 0.01 S1C C1C S1F C1F SADI 0.01 S2A C2A S2D C2D SADI 0.01 S1A C1A S1D C1D SADI CL1Y CL2Y CL2Y CL3Y CL3Y CL1Y SADI 0.01 C1Y CL1Y C1Y CL2Y C1Y CL3Y SIMU O1W > F6D DELU O1W > F6D EADP S1D S1A EADP C3S C3W SHEL 99 0.77 EQIV $1 -x+1, -y+2, -z+2 HTAB O2W N1S HTAB N3 N1W HTAB N3 O2W HTAB N4 O3C_$1 HTAB N4 O3F_$1 HTAB TEMP -173 WGHT 0.048000 3.874900 FVAR 0.08746 0.58494 0.73043 0.79711 0.79679 0.80910 0.75113 FVAR 0.65973 O1W 4 0.512023 0.456627 0.979791 0.38524 0.14449 0.17716 = 0.18884 0.08352 0.06736 0.06321 PART 1 O2W 4 0.523475 0.947307 0.690802 81.00000 0.04741 0.07778 = 0.09921 0.01620 -0.00220 0.02403 H1W 2 0.462429 0.970158 0.712494 81.00000 -1.20000 H2W 2 0.487118 0.896266 0.665279 81.00000 -1.20000 PART 1 N1S 3 0.300746 0.969593 0.751230 31.00000 0.05453 0.09526 = 0.11744 -0.02896 0.00948 0.04053 C2S 1 0.244431 0.976581 0.798059 31.00000 0.06338 0.05255 = 0.08409 -0.00201 -0.01779 0.02273 C3S 1 0.164998 0.987195 0.857775 31.00000 0.12167 0.07949 = 0.06009 0.01952 -0.00335 0.03514 AFIX 33 H3A 2 0.153010 1.057158 0.870286 31.00000 -1.20000 H3B 2 0.207806 0.963730 0.895690 31.00000 -1.20000 H3C 2 0.081798 0.947696 0.846727 31.00000 -1.20000 AFIX 0 PART 2 SAME N1S > C3S N1W 3 0.527568 0.925555 0.672844 -31.00000 0.01569 0.01527 = 0.04815 0.00440 0.00631 0.00539 C2W 1 0.503260 0.912551 0.725260 -31.00000 0.06811 0.10454 = 0.05659 -0.00271 0.00268 -0.00350 C3W 1 0.452177 0.916510 0.793859 -31.00000 0.12167 0.07949 = 0.06009 0.01952 -0.00335 0.03514 AFIX 33 H3X 2 0.450063 0.851013 0.808413 -31.00000 -1.50000 H3Y 2 0.365681 0.935742 0.792485 -31.00000 -1.50000 H3Z 2 0.507204 0.965378 0.825779 -31.00000 -1.50000 PART 0 AFIX 0 C1Y 1 0.514040 0.207662 0.957172 21.00000 0.10963 0.25324 = 0.03970 0.00841 0.00780 0.10132 AFIX 13 H1Y 2 0.525028 0.205136 1.006691 21.00000 -1.20000 AFIX 0 CL1Y 7 0.514986 0.084987 0.911772 21.00000 0.07487 0.22655 = 0.11391 -0.03605 -0.01121 0.02755 CL2Y 7 0.639470 0.293418 0.933087 21.00000 0.07038 0.22550 = 0.07277 -0.03948 -0.02580 0.07493 CL3Y 7 0.363451 0.253748 0.939913 21.00000 0.06693 0.33075 = 0.06647 0.01237 -0.00416 0.09492 PART 1 C1G 1 0.555015 0.296369 0.708487 -21.00000 0.09677 0.08624 = 0.04009 0.01486 -0.00297 0.00256 AFIX 13 H1G 2 0.523621 0.297291 0.660883 -21.00000 -1.20000 AFIX 0 CL1G 7 0.574986 0.179319 0.717766 -21.00000 0.10666 0.07554 = 0.07633 0.01822 -0.02149 0.01981 CL2G 7 0.701428 0.372850 0.723861 -21.00000 0.12019 0.11798 = 0.14112 -0.01065 0.00801 -0.02369 CL3G 7 0.445340 0.349425 0.763755 -21.00000 0.10335 0.14035 = 0.11920 -0.00101 -0.00867 0.05618 PART 0 N4S 3 0.151498 -0.051842 0.018190 41.00000 0.15957 0.03976 = 0.05611 0.00555 0.01766 -0.01260 C5S 1 0.155740 0.026887 0.042383 41.00000 0.06626 0.04353 = 0.04996 0.00707 -0.00356 -0.00026 C6S 1 0.164793 0.127920 0.075474 41.00000 0.06530 0.04341 = 0.09006 -0.01381 -0.02048 0.01743 AFIX 33 H6A 2 0.218824 0.135359 0.117133 41.00000 -1.20000 H6B 2 0.079462 0.144583 0.086411 41.00000 -1.20000 H6C 2 0.202255 0.172574 0.045399 41.00000 -1.20000 PART 1 AFIX 0 S1C 6 0.470825 0.772511 0.822318 51.00000 0.01962 0.06687 = 0.02456 0.00488 0.00163 -0.00363 O1C 4 0.413377 0.817568 0.880763 51.00000 0.04102 0.10144 = 0.03600 -0.01658 0.00868 -0.00463 O2C 4 0.592103 0.822087 0.807671 51.00000 0.03100 0.08214 = 0.03355 0.00769 0.00421 -0.01820 O3C 4 0.383900 0.740329 0.763901 51.00000 0.02102 0.05817 = 0.02863 0.00314 0.00083 0.00141 C1C 1 0.509448 0.655558 0.844401 51.00000 0.04360 0.08186 = 0.07692 0.04738 0.01295 0.01119 F1C 5 0.567314 0.606541 0.794916 51.00000 0.05333 0.08241 = 0.11673 0.02428 0.00566 0.03022 F2C 5 0.404931 0.599682 0.857033 51.00000 0.05105 0.10908 = 0.14961 0.09054 0.00599 -0.00337 F3C 5 0.587633 0.669671 0.899324 51.00000 0.04987 0.18908 = 0.08836 0.08154 -0.01071 0.02104 SAME S1C O1C O2C O3C C1C F1C F2C F3C PART 2 S1F 6 0.478069 0.707589 0.820029 -51.00000 0.06096 0.23502 = 0.07040 0.01671 0.00998 0.05437 O1F 4 0.430648 0.744880 0.884613 -51.00000 0.12030 0.27259 = 0.05034 0.00364 -0.00730 0.06573 O2F 4 0.601570 0.760287 0.809686 -51.00000 0.06582 0.18362 = 0.11223 0.00674 -0.02131 0.01741 O3F 4 0.386218 0.710361 0.764744 -51.00000 0.04840 0.18214 = 0.04299 -0.00512 0.00686 0.00003 C1F 1 0.499786 0.579960 0.820881 -51.00000 0.06208 0.20512 = 0.13452 0.03843 0.01807 0.00864 F1F 5 0.559091 0.553294 0.766104 -51.00000 0.18250 0.19221 = 0.17691 0.00155 0.05843 0.03289 F2F 5 0.384709 0.532398 0.819945 -51.00000 0.10363 0.31494 = 0.22216 0.06265 -0.02027 -0.07126 F3F 5 0.567654 0.577661 0.876430 -51.00000 0.11454 0.17197 = 0.17793 0.02529 -0.03497 0.01205 PART 1 S1A 6 0.699999 0.842103 0.500291 61.00000 0.02678 0.02541 = 0.03694 0.01157 0.01106 0.00628 O1A 4 0.821737 0.806753 0.514633 61.00000 0.03839 0.06070 = 0.05342 0.03644 0.02340 0.02657 O2A 4 0.601104 0.765189 0.478346 61.00000 0.04663 0.03772 = 0.09432 -0.00067 0.02885 -0.01502 O3A 4 0.668324 0.921014 0.549346 61.00000 0.05161 0.04129 = 0.02904 0.00917 0.01405 0.01459 C1A 1 0.735705 0.899893 0.425609 61.00000 0.03689 0.03402 = 0.02460 0.00482 0.00685 0.00946 F1A 5 0.635809 0.939328 0.404438 61.00000 0.05723 0.07556 = 0.03994 0.02371 -0.00065 0.02830 F2A 5 0.768584 0.833680 0.375536 61.00000 0.06478 0.04781 = 0.03149 -0.00644 0.01436 0.00972 F3A 5 0.833558 0.971312 0.438265 61.00000 0.05246 0.02903 = 0.04377 0.01048 0.02269 -0.00442 SAME S1A O1A O2A O3A C1A F1A F2A F3A PART 2 S1D 6 0.693541 0.831035 0.487030 -61.00000 0.02678 0.02541 = 0.03694 0.01157 0.01106 0.00628 O1D 4 0.788704 0.767888 0.503458 -61.00000 0.01879 0.01756 = 0.02373 -0.00261 0.00451 -0.00157 O2D 4 0.587254 0.773968 0.447977 -61.00000 0.03249 0.04215 = 0.04540 -0.00400 -0.00784 0.01090 O3D 4 0.662334 0.905264 0.539118 -61.00000 0.01966 0.02964 = 0.03346 0.00353 0.01710 0.00396 C1D 1 0.770285 0.899273 0.424848 -61.00000 0.07113 0.04228 = 0.04206 0.01724 0.03622 0.02364 F1D 5 0.695649 0.957691 0.399830 -61.00000 0.14292 0.03489 = 0.05289 0.02679 0.02672 0.03716 F2D 5 0.808013 0.834825 0.374926 -61.00000 0.15342 0.05696 = 0.06623 0.00551 0.06595 0.03618 F3D 5 0.876040 0.952382 0.454146 -61.00000 0.08881 0.04394 = 0.11364 0.01563 0.04026 -0.01084 PART 1 S2A 6 1.094224 0.483707 0.587176 71.00000 0.02663 0.02604 = 0.01617 -0.00033 -0.00117 0.00597 O4A 4 0.985235 0.535844 0.601577 71.00000 0.02473 0.03009 = 0.03709 0.00751 0.00176 0.00853 O5A 4 1.210758 0.548724 0.585757 71.00000 0.02968 0.03995 = 0.04780 -0.00297 0.00673 0.00299 O6A 4 1.071648 0.401237 0.533239 71.00000 0.05071 0.02800 = 0.01635 -0.00073 0.00427 0.00014 C2A 1 1.114667 0.425418 0.662194 71.00000 0.06302 0.03030 = 0.02444 0.00272 -0.00677 0.01534 F4A 5 1.013617 0.362693 0.669662 71.00000 0.09301 0.05131 = 0.02830 0.01740 0.00127 -0.00569 F5A 5 1.213892 0.374230 0.658251 71.00000 0.09525 0.05943 = 0.06799 0.00700 -0.02387 0.04886 F6A 5 1.135191 0.492645 0.716801 71.00000 0.11826 0.03905 = 0.02209 -0.00009 -0.01832 0.01620 SAME S2A O4A O5A O6A C2A F4A F5A F6A PART 2 S2D 6 1.079812 0.457779 0.597769 -71.00000 0.02582 0.02304 = 0.02893 -0.00250 0.00308 0.00877 O4D 4 1.008308 0.532994 0.578534 -71.00000 0.04247 0.02714 = 0.01027 0.00040 0.01328 0.01625 O5D 4 1.196892 0.497474 0.637446 -71.00000 0.03133 0.05392 = 0.05831 -0.01886 -0.00855 0.00986 O6D 4 1.098013 0.380681 0.543202 -71.00000 0.03802 0.02501 = 0.01536 0.00643 -0.00418 0.02111 C2D 1 0.979983 0.395963 0.654951 -71.00000 0.06204 0.03106 = 0.01850 0.00811 0.01096 0.02135 F4D 5 0.863874 0.370131 0.628302 -71.00000 0.04835 0.04779 = 0.06597 0.01496 0.02689 -0.00352 F5D 5 1.029783 0.314961 0.669323 -71.00000 0.10996 0.02826 = 0.02689 0.00833 0.00770 0.02859 F6D 5 0.977400 0.456556 0.713345 -71.00000 0.11917 0.03465 = 0.02089 0.00072 0.02945 0.02339 PART 0 BI1 8 0.915771 0.705569 0.591665 11.00000 0.02033 0.02130 = 0.01593 -0.00075 0.00176 0.00235 N1 3 0.709925 0.578424 0.587888 11.00000 0.02186 0.02662 = 0.03361 -0.00009 -0.00230 0.00157 C1 1 0.700291 0.484667 0.558129 11.00000 0.02625 0.03157 = 0.05628 -0.00623 -0.00386 0.00339 AFIX 43 H1 2 0.773147 0.460863 0.538121 11.00000 -1.20000 AFIX 0 C2 1 0.589300 0.420394 0.554990 11.00000 0.03350 0.03005 = 0.08528 -0.01546 -0.00591 0.00273 AFIX 43 H2 2 0.586094 0.354044 0.532927 11.00000 -1.20000 AFIX 0 C3 1 0.483276 0.453596 0.584221 11.00000 0.02881 0.03572 = 0.09211 -0.01019 -0.00082 -0.00487 AFIX 43 H3 2 0.405513 0.410869 0.582086 11.00000 -1.20000 AFIX 0 C4 1 0.491857 0.550484 0.616849 11.00000 0.02572 0.03368 = 0.06329 -0.00503 0.00135 -0.00051 AFIX 43 H4 2 0.420911 0.574985 0.638483 11.00000 -1.20000 AFIX 0 C5 1 0.606012 0.610492 0.617135 11.00000 0.02243 0.03006 = 0.03151 -0.00019 -0.00252 0.00030 C6 1 0.619599 0.712581 0.651382 11.00000 0.02311 0.03050 = 0.02501 -0.00163 0.00106 0.00203 AFIX 43 H6 2 0.551068 0.739155 0.674165 11.00000 -1.20000 AFIX 0 N2 3 0.726953 0.764963 0.649639 11.00000 0.02542 0.02401 = 0.01953 -0.00202 0.00277 0.00015 N3 3 0.745680 0.858833 0.684249 11.00000 0.02695 0.02605 = 0.02172 -0.00570 0.00706 0.00093 H3N 2 0.681538 0.889041 0.700780 11.00000 -1.20000 C7 1 0.862848 0.906978 0.682895 11.00000 0.02936 0.02562 = 0.02139 -0.00331 0.00754 0.00112 O12 4 0.947863 0.869252 0.649940 11.00000 0.03162 0.02464 = 0.03674 -0.00791 0.01877 -0.00354 C8 1 0.892665 1.005617 0.724794 11.00000 0.02668 0.02550 = 0.02010 -0.00326 0.00586 0.00291 C9 1 1.004077 1.063532 0.714585 11.00000 0.03446 0.02920 = 0.02382 -0.00302 0.01447 -0.00064 AFIX 43 H9 2 1.054116 1.042973 0.677913 11.00000 -1.20000 AFIX 0 C10 1 1.043532 1.151012 0.757111 11.00000 0.03535 0.02783 = 0.02443 -0.00071 0.01068 -0.00260 AFIX 43 H10 2 1.120239 1.190040 0.749369 11.00000 -1.20000 AFIX 0 C11 1 0.971235 1.182475 0.811498 11.00000 0.03079 0.02437 = 0.01779 0.00133 0.00213 0.00320 C12 1 0.856244 1.125558 0.820082 11.00000 0.02435 0.03465 = 0.02180 -0.00715 0.00421 0.00380 AFIX 43 H12 2 0.804287 1.147351 0.855590 11.00000 -1.20000 AFIX 0 C13 1 0.817128 1.037948 0.777565 11.00000 0.02188 0.03071 = 0.02746 -0.00592 0.00558 0.00075 AFIX 43 H13 2 0.739078 0.999740 0.784160 11.00000 -1.20000 AFIX 0 C14 1 1.018982 1.271297 0.861045 11.00000 0.03016 0.02349 = 0.01902 0.00017 0.00356 0.00475 C15 1 1.090694 1.353763 0.841257 11.00000 0.04710 0.02727 = 0.01849 0.00344 0.00598 0.00016 AFIX 43 H15 2 1.107464 1.354411 0.795029 11.00000 -1.20000 AFIX 0 C16 1 1.137501 1.434853 0.889193 11.00000 0.04768 0.02179 = 0.02562 0.00418 0.00885 -0.00218 AFIX 43 H16 2 1.185270 1.490839 0.875401 11.00000 -1.20000 AFIX 0 C17 1 1.114788 1.434241 0.956683 11.00000 0.03665 0.02301 = 0.01956 -0.00115 0.00137 0.00005 AFIX 43 H17 2 1.147674 1.489633 0.989010 11.00000 -1.20000 AFIX 0 C18 1 1.043928 1.352901 0.977723 11.00000 0.02554 0.02412 = 0.01765 0.00180 0.00243 0.00361 C19 1 0.995547 1.272072 0.929286 11.00000 0.02525 0.02145 = 0.01810 0.00111 0.00217 0.00265 AFIX 43 H19 2 0.946004 1.216912 0.943100 11.00000 -1.20000 AFIX 0 C20 1 1.022702 1.348731 1.049881 11.00000 0.02634 0.02032 = 0.01763 0.00063 0.00246 0.00397 C21 1 1.117651 1.389312 1.099714 11.00000 0.02195 0.02915 = 0.02318 0.00286 0.00343 -0.00407 AFIX 43 H21 2 1.193586 1.424854 1.087409 11.00000 -1.20000 AFIX 0 C22 1 1.102423 1.378379 1.166446 11.00000 0.02272 0.03201 = 0.02124 0.00034 -0.00191 -0.00400 AFIX 43 H22 2 1.168384 1.405358 1.199592 11.00000 -1.20000 AFIX 0 C23 1 0.990203 1.327703 1.185567 11.00000 0.02135 0.02733 = 0.01634 0.00012 0.00171 0.00069 C24 1 0.892662 1.290026 1.136756 11.00000 0.01998 0.02654 = 0.02070 0.00086 0.00302 0.00050 AFIX 43 H24 2 0.814973 1.257628 1.149549 11.00000 -1.20000 AFIX 0 C25 1 0.909345 1.299959 1.069653 11.00000 0.02240 0.02622 = 0.01767 -0.00288 -0.00125 0.00191 AFIX 43 H25 2 0.843120 1.273381 1.036566 11.00000 -1.20000 AFIX 0 C26 1 0.983824 1.310994 1.256552 11.00000 0.02137 0.02786 = 0.01897 -0.00194 0.00019 -0.00206 O13 4 1.082794 1.323149 1.293993 11.00000 0.02206 0.04368 = 0.01875 0.00577 -0.00035 -0.00699 N4 3 0.869811 1.279413 1.279176 11.00000 0.02156 0.03547 = 0.01580 0.00140 0.00101 -0.00203 H4N 2 0.793734 1.273980 1.257042 11.00000 -1.20000 N5 3 0.870845 1.259693 1.344460 11.00000 0.02317 0.02761 = 0.01697 0.00033 0.00138 -0.00236 C27 1 0.768406 1.224824 1.368719 11.00000 0.02174 0.02628 = 0.02417 -0.00107 0.00279 -0.00112 AFIX 43 H27 2 0.689894 1.213519 1.342606 11.00000 -1.20000 AFIX 0 C28 1 0.775550 1.202814 1.437888 11.00000 0.02775 0.02056 = 0.02658 0.00183 0.00864 0.00464 C29 1 0.667160 1.168605 1.468287 11.00000 0.02987 0.03234 = 0.04025 0.01290 0.01384 0.00700 AFIX 43 H29 2 0.586005 1.159843 1.444812 11.00000 -1.20000 AFIX 0 C30 1 0.679501 1.147318 1.533925 11.00000 0.03454 0.04525 = 0.04774 0.02323 0.02217 0.01555 AFIX 43 H30 2 0.606560 1.124110 1.556104 11.00000 -1.20000 AFIX 0 C31 1 0.797828 1.160146 1.566251 11.00000 0.04282 0.05551 = 0.03606 0.02405 0.01972 0.02084 AFIX 43 H31 2 0.808456 1.145136 1.610868 11.00000 -1.20000 AFIX 0 C32 1 0.902580 1.195684 1.532454 11.00000 0.03420 0.04355 = 0.02714 0.01106 0.01095 0.01103 AFIX 43 H32 2 0.984542 1.205584 1.555135 11.00000 -1.20000 AFIX 0 N6 3 0.891870 1.216229 1.469582 11.00000 0.02786 0.02763 = 0.02144 0.00223 0.00878 0.00406 HKLF 4 REM rhL19_0m in P-1 REM R1 = 0.0293 for 12130 Fo > 4sig(Fo) and 0.0328 for all 13040 data REM 981 parameters refined using 849 restraints END ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 68323 _diffrn_reflns_av_R_equivalents 0.0256 _diffrn_reflns_av_sigmaI/netI 0.0194 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 27.48 _reflns_number_total 13040 _reflns_number_gt 12130 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0480P)^2^+3.8749P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13040 _refine_ls_number_parameters 981 _refine_ls_number_restraints 849 _refine_ls_R_factor_all 0.0328 _refine_ls_R_factor_gt 0.0293 _refine_ls_wR_factor_ref 0.0795 _refine_ls_wR_factor_gt 0.0774 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1W O 0.512(2) 0.4566(16) 0.9798(12) 0.160(11) Uani 0.385(18) 1 d P . . O2W O 0.5235(12) 0.9473(9) 0.6908(6) 0.073(4) Uani 0.660(16) 1 d PDU A 1 H1W H 0.462(6) 0.970(7) 0.712(5) 0.088 Uiso 0.660(16) 1 d PD A 1 H2W H 0.487(8) 0.896(5) 0.665(5) 0.088 Uiso 0.660(16) 1 d PD A 1 N1S N 0.3007(6) 0.9696(6) 0.7512(5) 0.091(3) Uani 0.730(7) 1 d PDU B 1 C2S C 0.2444(8) 0.9766(5) 0.7981(5) 0.067(2) Uani 0.730(7) 1 d PDU B 1 C3S C 0.1650(10) 0.9872(7) 0.8578(4) 0.085(2) Uani 0.730(7) 1 d PDU B 1 H3A H 0.1530 1.0572 0.8703 0.102 Uiso 0.730(7) 1 calc PR B 1 H3B H 0.2078 0.9637 0.8957 0.102 Uiso 0.730(7) 1 calc PR B 1 H3C H 0.0818 0.9477 0.8467 0.102 Uiso 0.730(7) 1 calc PR B 1 N1W N 0.528(2) 0.9256(15) 0.6728(10) 0.026(3) Uani 0.270(7) 1 d PDU B 2 C2W C 0.503(3) 0.913(3) 0.7253(9) 0.079(7) Uani 0.270(7) 1 d PDU B 2 C3W C 0.452(3) 0.9165(19) 0.7939(10) 0.085(2) Uani 0.270(7) 1 d PDU B 2 H3X H 0.4501 0.8510 0.8084 0.127 Uiso 0.270(7) 1 calc PR B 2 H3Y H 0.3657 0.9357 0.7925 0.127 Uiso 0.270(7) 1 calc PR B 2 H3Z H 0.5072 0.9654 0.8258 0.127 Uiso 0.270(7) 1 calc PR B 2 C1Y C 0.5140(6) 0.2077(5) 0.9572(6) 0.129(4) Uani 0.585(3) 1 d PDU . . H1Y H 0.5250 0.2051 1.0067 0.155 Uiso 0.585(3) 1 calc PR . . Cl1Y Cl 0.5150(3) 0.0850(4) 0.9118(2) 0.1440(19) Uani 0.585(3) 1 d PDU . . Cl2Y Cl 0.6395(3) 0.2934(4) 0.93309(16) 0.1251(16) Uani 0.585(3) 1 d PDU . . Cl3Y Cl 0.3635(3) 0.2537(5) 0.93991(16) 0.151(2) Uani 0.585(3) 1 d PDU . . C1G C 0.5550(16) 0.2964(12) 0.7085(7) 0.075(3) Uani 0.415(3) 1 d PU C 1 H1G H 0.5236 0.2973 0.6609 0.090 Uiso 0.415(3) 1 calc PR C 1 Cl1G Cl 0.5750(4) 0.1793(3) 0.7178(2) 0.0855(13) Uani 0.415(3) 1 d PU C 1 Cl2G Cl 0.7014(6) 0.3728(5) 0.7239(4) 0.132(2) Uani 0.415(3) 1 d PU C 1 Cl3G Cl 0.4453(5) 0.3494(5) 0.7638(3) 0.120(2) Uani 0.415(3) 1 d PU C 1 N4S N 0.1515(8) -0.0518(4) 0.0182(3) 0.087(3) Uani 0.797(9) 1 d PU . . C5S C 0.1557(6) 0.0269(4) 0.0424(3) 0.0539(16) Uani 0.797(9) 1 d PU . . C6S C 0.1648(7) 0.1279(5) 0.0755(4) 0.068(2) Uani 0.797(9) 1 d PU . . H6A H 0.2188 0.1354 0.1171 0.082 Uiso 0.797(9) 1 calc PR . . H6B H 0.0795 0.1446 0.0864 0.082 Uiso 0.797(9) 1 calc PR . . H6C H 0.2023 0.1726 0.0454 0.082 Uiso 0.797(9) 1 calc PR . . S1C S 0.47083(13) 0.77251(14) 0.82232(7) 0.0378(5) Uani 0.797(7) 1 d PDU D 1 O1C O 0.4134(4) 0.8176(4) 0.8808(2) 0.0629(14) Uani 0.797(7) 1 d PDU D 1 O2C O 0.5921(4) 0.8221(3) 0.8077(2) 0.0508(12) Uani 0.797(7) 1 d PDU D 1 O3C O 0.3839(4) 0.7403(4) 0.7639(2) 0.0365(9) Uani 0.797(7) 1 d PDU D 1 C1C C 0.5094(4) 0.6556(5) 0.8444(3) 0.0635(17) Uani 0.797(7) 1 d PDU D 1 F1C F 0.5673(4) 0.6065(3) 0.7949(3) 0.0815(15) Uani 0.797(7) 1 d PDU D 1 F2C F 0.4049(4) 0.5997(4) 0.8570(3) 0.097(2) Uani 0.797(7) 1 d PDU D 1 F3C F 0.5876(4) 0.6697(5) 0.8993(2) 0.103(2) Uani 0.797(7) 1 d PDU D 1 S1F S 0.4781(9) 0.7076(17) 0.8200(5) 0.120(5) Uani 0.203(7) 1 d PDU D 2 O1F O 0.431(2) 0.745(2) 0.8846(8) 0.147(10) Uani 0.203(7) 1 d PDU D 2 O2F O 0.6016(16) 0.760(2) 0.8097(13) 0.122(9) Uani 0.203(7) 1 d PDU D 2 O3F O 0.386(2) 0.710(2) 0.7647(10) 0.094(9) Uani 0.203(7) 1 d PDU D 2 C1F C 0.4998(16) 0.5800(19) 0.8209(10) 0.133(8) Uani 0.203(7) 1 d PDU D 2 F1F F 0.559(3) 0.553(2) 0.7661(14) 0.184(13) Uani 0.203(7) 1 d PDU D 2 F2F F 0.385(2) 0.532(2) 0.8199(17) 0.219(14) Uani 0.203(7) 1 d PDU D 2 F3F F 0.568(2) 0.578(2) 0.8764(13) 0.156(10) Uani 0.203(7) 1 d PDU D 2 S1A S 0.7000(3) 0.8421(3) 0.5003(3) 0.0286(5) Uani 0.81(2) 1 d PDU E 1 O1A O 0.8217(6) 0.8068(7) 0.5146(4) 0.0460(18) Uani 0.81(2) 1 d PDU E 1 O2A O 0.6011(7) 0.7652(4) 0.4783(5) 0.061(2) Uani 0.81(2) 1 d PDU E 1 O3A O 0.6683(10) 0.9210(7) 0.5493(4) 0.0393(17) Uani 0.81(2) 1 d PDU E 1 C1A C 0.7357(6) 0.8999(4) 0.4256(3) 0.0312(12) Uani 0.81(2) 1 d PDU E 1 F1A F 0.6358(5) 0.9393(5) 0.4044(3) 0.0546(14) Uani 0.81(2) 1 d PDU E 1 F2A F 0.7686(6) 0.8337(5) 0.3755(3) 0.0487(13) Uani 0.81(2) 1 d PDU E 1 F3A F 0.8336(5) 0.9713(3) 0.4383(2) 0.0415(11) Uani 0.81(2) 1 d PDU E 1 S1D S 0.6935(14) 0.8310(11) 0.4870(8) 0.0286(5) Uani 0.19(2) 1 d PDU E 2 O1D O 0.7887(17) 0.7679(14) 0.5035(8) 0.021(3) Uani 0.19(2) 1 d PDU E 2 O2D O 0.5873(18) 0.7740(16) 0.4480(14) 0.041(5) Uani 0.19(2) 1 d PDU E 2 O3D O 0.662(3) 0.905(2) 0.5391(16) 0.027(5) Uani 0.19(2) 1 d PDU E 2 C1D C 0.770(3) 0.8993(16) 0.4248(12) 0.049(6) Uani 0.19(2) 1 d PDU E 2 F1D F 0.696(5) 0.9577(16) 0.3998(11) 0.072(8) Uani 0.19(2) 1 d PDU E 2 F2D F 0.808(4) 0.835(2) 0.3749(16) 0.089(10) Uani 0.19(2) 1 d PDU E 2 F3D F 0.876(3) 0.952(2) 0.4541(19) 0.082(7) Uani 0.19(2) 1 d PDU E 2 S2A S 1.0942(2) 0.48371(18) 0.58718(12) 0.0231(4) Uani 0.751(4) 1 d PDU E 1 O4A O 0.9852(4) 0.5358(3) 0.6016(3) 0.0300(10) Uani 0.751(4) 1 d PDU E 1 O5A O 1.2108(3) 0.5487(3) 0.5858(2) 0.0400(9) Uani 0.751(4) 1 d PDU E 1 O6A O 1.0716(6) 0.4012(4) 0.5332(2) 0.0323(12) Uani 0.751(4) 1 d PDU . 1 C2A C 1.1147(6) 0.4254(4) 0.6622(2) 0.0389(11) Uani 0.751(4) 1 d PDU E 1 F4A F 1.0136(5) 0.3627(4) 0.6697(2) 0.0576(13) Uani 0.751(4) 1 d PDU E 1 F5A F 1.2139(4) 0.3742(3) 0.6583(2) 0.0721(13) Uani 0.751(4) 1 d PDU E 1 F6A F 1.1352(4) 0.4926(2) 0.71680(15) 0.0603(12) Uani 0.751(4) 1 d PDU E 1 S2D S 1.0798(7) 0.4578(5) 0.5978(4) 0.0260(13) Uani 0.249(4) 1 d PDU E 2 O4D O 1.0083(15) 0.5330(10) 0.5785(6) 0.026(3) Uani 0.249(4) 1 d PDU E 2 O5D O 1.1969(10) 0.4975(9) 0.6374(6) 0.050(3) Uani 0.249(4) 1 d PDU E 2 O6D O 1.0980(19) 0.3807(11) 0.5432(7) 0.025(3) Uani 0.249(4) 1 d PDU E 2 C2D C 0.9800(13) 0.3960(9) 0.6550(6) 0.035(3) Uani 0.249(4) 1 d PDU E 2 F4D F 0.8639(9) 0.3701(7) 0.6283(5) 0.054(3) Uani 0.249(4) 1 d PDU E 2 F5D F 1.0298(14) 0.3150(8) 0.6693(6) 0.053(3) Uani 0.249(4) 1 d PDU E 2 F6D F 0.9774(13) 0.4566(7) 0.7133(4) 0.057(3) Uani 0.249(4) 1 d PDU E 2 Bi1 Bi 0.915771(10) 0.705569(8) 0.591665(5) 0.01951(4) Uani 1 1 d . . . N1 N 0.7099(3) 0.5784(2) 0.58789(15) 0.0280(6) Uani 1 1 d . E . C1 C 0.7003(3) 0.4847(3) 0.5581(2) 0.0394(9) Uani 1 1 d . . . H1 H 0.7731 0.4609 0.5381 0.047 Uiso 1 1 calc R E . C2 C 0.5893(4) 0.4204(3) 0.5550(3) 0.0522(12) Uani 1 1 d . E . H2 H 0.5861 0.3540 0.5329 0.063 Uiso 1 1 calc R . . C3 C 0.4833(4) 0.4536(3) 0.5842(3) 0.0549(12) Uani 1 1 d . . . H3 H 0.4055 0.4109 0.5821 0.066 Uiso 1 1 calc R E . C4 C 0.4919(4) 0.5505(3) 0.6168(2) 0.0424(9) Uani 1 1 d . E . H4 H 0.4209 0.5750 0.6385 0.051 Uiso 1 1 calc R . . C5 C 0.6060(3) 0.6105(3) 0.61713(17) 0.0288(7) Uani 1 1 d . . . C6 C 0.6196(3) 0.7126(2) 0.65138(16) 0.0268(6) Uani 1 1 d . E . H6 H 0.5511 0.7392 0.6742 0.032 Uiso 1 1 calc R . . N2 N 0.7270(2) 0.76496(19) 0.64964(13) 0.0237(5) Uani 1 1 d . E . N3 N 0.7457(3) 0.8588(2) 0.68425(13) 0.0258(5) Uani 1 1 d . . . H3N H 0.682(4) 0.889(3) 0.701(2) 0.031 Uiso 1 1 d . . . C7 C 0.8628(3) 0.9070(2) 0.68289(16) 0.0261(6) Uani 1 1 d . E . O12 O 0.9479(2) 0.86925(17) 0.64994(13) 0.0323(5) Uani 1 1 d . E . C8 C 0.8927(3) 1.0056(2) 0.72479(15) 0.0246(6) Uani 1 1 d . . . C9 C 1.0041(3) 1.0635(2) 0.71458(17) 0.0298(7) Uani 1 1 d . E . H9 H 1.0541 1.0430 0.6779 0.036 Uiso 1 1 calc R . . C10 C 1.0435(3) 1.1510(2) 0.75711(17) 0.0299(7) Uani 1 1 d . . . H10 H 1.1202 1.1900 0.7494 0.036 Uiso 1 1 calc R E . C11 C 0.9712(3) 1.1825(2) 0.81150(15) 0.0245(6) Uani 1 1 d . E . C12 C 0.8562(3) 1.1256(3) 0.82008(16) 0.0279(7) Uani 1 1 d . . . H12 H 0.8043 1.1474 0.8556 0.034 Uiso 1 1 calc R E . C13 C 0.8171(3) 1.0379(2) 0.77757(17) 0.0277(7) Uani 1 1 d . E . H13 H 0.7391 0.9997 0.7842 0.033 Uiso 1 1 calc R . . C14 C 1.0190(3) 1.2713(2) 0.86105(15) 0.0243(6) Uani 1 1 d . . . C15 C 1.0907(4) 1.3538(2) 0.84126(16) 0.0312(7) Uani 1 1 d . E . H15 H 1.1075 1.3544 0.7950 0.037 Uiso 1 1 calc R . . C16 C 1.1375(4) 1.4349(2) 0.88919(17) 0.0319(7) Uani 1 1 d . . . H16 H 1.1853 1.4908 0.8754 0.038 Uiso 1 1 calc R E . C17 C 1.1148(3) 1.4342(2) 0.95668(16) 0.0271(6) Uani 1 1 d . E . H17 H 1.1477 1.4896 0.9890 0.033 Uiso 1 1 calc R . . C18 C 1.0439(3) 1.3529(2) 0.97772(15) 0.0225(6) Uani 1 1 d . . . C19 C 0.9955(3) 1.2721(2) 0.92929(15) 0.0218(6) Uani 1 1 d . E . H19 H 0.9460 1.2169 0.9431 0.026 Uiso 1 1 calc R . . C20 C 1.0227(3) 1.3487(2) 1.04988(15) 0.0215(6) Uani 1 1 d . E . C21 C 1.1177(3) 1.3893(2) 1.09971(16) 0.0253(6) Uani 1 1 d . . . H21 H 1.1936 1.4249 1.0874 0.030 Uiso 1 1 calc R E . C22 C 1.1024(3) 1.3784(2) 1.16645(16) 0.0263(6) Uani 1 1 d . E . H22 H 1.1684 1.4054 1.1996 0.032 Uiso 1 1 calc R . . C23 C 0.9902(3) 1.3277(2) 1.18557(15) 0.0221(6) Uani 1 1 d . . . C24 C 0.8927(3) 1.2900(2) 1.13676(15) 0.0228(6) Uani 1 1 d . E . H24 H 0.8150 1.2576 1.1495 0.027 Uiso 1 1 calc R . . C25 C 0.9093(3) 1.3000(2) 1.06965(15) 0.0228(6) Uani 1 1 d . . . H25 H 0.8431 1.2734 1.0366 0.027 Uiso 1 1 calc R E . C26 C 0.9838(3) 1.3110(2) 1.25655(15) 0.0237(6) Uani 1 1 d . E . O13 O 1.0828(2) 1.32315(18) 1.29399(11) 0.0289(5) Uani 1 1 d . . . N4 N 0.8698(3) 1.2794(2) 1.27918(13) 0.0249(5) Uani 1 1 d . . . H4N H 0.794(4) 1.274(3) 1.257(2) 0.030 Uiso 1 1 d . . . N5 N 0.8708(2) 1.25969(19) 1.34446(13) 0.0233(5) Uani 1 1 d . . . C27 C 0.7684(3) 1.2248(2) 1.36872(16) 0.0248(6) Uani 1 1 d . . . H27 H 0.6899 1.2135 1.3426 0.030 Uiso 1 1 calc R E . C28 C 0.7755(3) 1.2028(2) 1.43789(16) 0.0248(6) Uani 1 1 d . E . C29 C 0.6672(3) 1.1686(3) 1.46829(19) 0.0329(7) Uani 1 1 d . . . H29 H 0.5860 1.1598 1.4448 0.039 Uiso 1 1 calc R E . C30 C 0.6795(4) 1.1473(3) 1.5339(2) 0.0396(9) Uani 1 1 d . E . H30 H 0.6066 1.1241 1.5561 0.048 Uiso 1 1 calc R . . C31 C 0.7978(4) 1.1601(3) 1.5663(2) 0.0415(9) Uani 1 1 d . . . H31 H 0.8085 1.1451 1.6109 0.050 Uiso 1 1 calc R E . C32 C 0.9026(3) 1.1957(3) 1.53245(18) 0.0337(7) Uani 1 1 d . E . H32 H 0.9845 1.2056 1.5551 0.040 Uiso 1 1 calc R . . N6 N 0.8919(3) 1.2162(2) 1.46958(13) 0.0255(5) Uani 1 1 d . . . 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 O1W 0.144(17) 0.18(2) 0.19(2) 0.084(18) 0.067(15) 0.063(15) O2W 0.047(4) 0.078(9) 0.099(9) 0.016(5) -0.002(5) 0.024(5) N1S 0.055(4) 0.095(5) 0.117(6) -0.029(5) 0.009(4) 0.041(4) C2S 0.063(4) 0.053(4) 0.084(5) -0.002(4) -0.018(3) 0.023(3) C3S 0.122(7) 0.079(5) 0.060(4) 0.020(4) -0.003(4) 0.035(5) N1W 0.016(6) 0.015(6) 0.048(8) 0.004(6) 0.006(6) 0.005(4) C2W 0.068(14) 0.105(18) 0.057(10) -0.003(12) 0.003(10) -0.003(13) C3W 0.122(7) 0.079(5) 0.060(4) 0.020(4) -0.003(4) 0.035(5) C1Y 0.110(8) 0.253(11) 0.040(5) 0.008(7) 0.008(6) 0.101(7) Cl1Y 0.075(2) 0.227(5) 0.114(3) -0.036(3) -0.011(2) 0.028(3) Cl2Y 0.0704(17) 0.225(4) 0.0728(18) -0.039(2) -0.0258(14) 0.075(2) Cl3Y 0.0669(18) 0.331(7) 0.0665(18) 0.012(3) -0.0042(14) 0.095(3) C1G 0.097(9) 0.086(8) 0.040(6) 0.015(6) -0.003(6) 0.003(6) Cl1G 0.107(3) 0.076(2) 0.076(2) 0.0182(19) -0.021(2) 0.020(2) Cl2G 0.120(4) 0.118(4) 0.141(5) -0.011(4) 0.008(4) -0.024(3) Cl3G 0.103(3) 0.140(5) 0.119(4) -0.001(3) -0.009(3) 0.056(3) N4S 0.160(7) 0.040(3) 0.056(4) 0.006(2) 0.018(4) -0.013(3) C5S 0.066(4) 0.044(3) 0.050(3) 0.007(2) -0.004(3) 0.000(3) C6S 0.065(4) 0.043(3) 0.090(5) -0.014(3) -0.020(4) 0.017(3) S1C 0.0196(6) 0.0669(11) 0.0246(6) 0.0049(6) 0.0016(4) -0.0036(5) O1C 0.041(2) 0.101(4) 0.036(2) -0.017(2) 0.0087(17) -0.005(2) O2C 0.0310(18) 0.082(3) 0.0335(19) 0.008(2) 0.0042(15) -0.0182(19) O3C 0.0210(19) 0.058(2) 0.029(2) 0.0031(16) 0.0008(15) 0.0014(15) C1C 0.044(3) 0.082(4) 0.077(4) 0.047(4) 0.013(3) 0.011(3) F1C 0.053(2) 0.082(3) 0.117(4) 0.024(3) 0.006(2) 0.030(2) F2C 0.051(2) 0.109(4) 0.150(5) 0.091(4) 0.006(3) -0.003(2) F3C 0.050(2) 0.189(6) 0.088(3) 0.082(4) -0.011(2) 0.021(3) S1F 0.061(5) 0.235(14) 0.070(5) 0.017(9) 0.010(4) 0.054(8) O1F 0.120(18) 0.27(3) 0.050(9) 0.004(17) -0.007(10) 0.07(2) O2F 0.066(10) 0.18(2) 0.112(19) 0.01(2) -0.021(10) 0.017(14) O3F 0.048(12) 0.18(3) 0.043(10) -0.005(15) 0.007(9) 0.000(16) C1F 0.062(15) 0.205(15) 0.135(18) 0.038(17) 0.018(13) 0.009(14) F1F 0.18(3) 0.19(3) 0.18(2) 0.00(2) 0.06(2) 0.03(2) F2F 0.104(17) 0.31(2) 0.22(3) 0.06(3) -0.020(15) -0.07(2) F3F 0.115(18) 0.17(2) 0.178(19) 0.025(19) -0.035(15) 0.012(18) S1A 0.0268(5) 0.0254(9) 0.0369(14) 0.0116(9) 0.0111(8) 0.0063(6) O1A 0.038(3) 0.061(4) 0.053(3) 0.036(3) 0.023(2) 0.027(3) O2A 0.047(3) 0.038(2) 0.094(6) -0.001(3) 0.029(3) -0.015(2) O3A 0.052(4) 0.041(3) 0.029(3) 0.009(2) 0.014(2) 0.015(3) C1A 0.037(3) 0.034(3) 0.025(2) 0.0048(18) 0.0068(18) 0.0095(19) F1A 0.057(3) 0.076(3) 0.040(2) 0.0237(19) -0.0007(19) 0.028(2) F2A 0.065(3) 0.048(2) 0.031(2) -0.0064(16) 0.0144(17) 0.0097(18) F3A 0.052(2) 0.0290(18) 0.044(2) 0.0105(13) 0.0227(16) -0.0044(15) S1D 0.0268(5) 0.0254(9) 0.0369(14) 0.0116(9) 0.0111(8) 0.0063(6) O1D 0.019(6) 0.018(7) 0.024(6) -0.003(5) 0.005(5) -0.002(5) O2D 0.032(7) 0.042(9) 0.045(12) -0.004(8) -0.008(7) 0.011(6) O3D 0.020(9) 0.030(9) 0.033(10) 0.004(6) 0.017(7) 0.004(6) C1D 0.071(14) 0.042(12) 0.042(11) 0.017(7) 0.036(9) 0.024(8) F1D 0.14(2) 0.035(9) 0.053(9) 0.027(7) 0.027(12) 0.037(12) F2D 0.15(3) 0.057(13) 0.066(13) 0.006(9) 0.066(14) 0.036(14) F3D 0.089(14) 0.044(11) 0.114(19) 0.016(11) 0.040(11) -0.011(10) S2A 0.0266(8) 0.0260(11) 0.0162(7) -0.0003(6) -0.0012(5) 0.0060(7) O4A 0.0247(19) 0.0301(19) 0.037(3) 0.008(2) 0.0018(19) 0.0085(14) O5A 0.0297(17) 0.0400(19) 0.048(2) -0.0030(16) 0.0067(15) 0.0030(14) O6A 0.051(4) 0.028(2) 0.0163(19) -0.0007(17) 0.0043(18) 0.000(2) C2A 0.063(3) 0.030(2) 0.024(2) 0.0027(18) -0.007(2) 0.015(2) F4A 0.093(3) 0.051(3) 0.0283(19) 0.017(2) 0.001(2) -0.006(3) F5A 0.095(3) 0.059(2) 0.068(3) 0.0070(19) -0.024(2) 0.049(2) F6A 0.118(3) 0.0391(17) 0.0221(15) -0.0001(12) -0.0183(17) 0.0162(18) S2D 0.026(2) 0.023(3) 0.029(3) -0.0025(19) 0.0031(18) 0.009(2) O4D 0.042(7) 0.027(5) 0.010(6) 0.000(4) 0.013(4) 0.016(4) O5D 0.031(5) 0.054(7) 0.058(8) -0.019(6) -0.009(5) 0.010(4) O6D 0.038(7) 0.025(6) 0.015(5) 0.006(4) -0.004(4) 0.021(4) C2D 0.062(7) 0.031(8) 0.018(7) 0.008(5) 0.011(5) 0.021(6) F4D 0.048(5) 0.048(6) 0.066(6) 0.015(5) 0.027(4) -0.004(4) F5D 0.110(9) 0.028(5) 0.027(5) 0.008(5) 0.008(5) 0.029(6) F6D 0.119(10) 0.035(5) 0.021(4) 0.001(3) 0.029(5) 0.023(5) Bi1 0.02033(6) 0.02130(6) 0.01593(6) -0.00075(4) 0.00176(4) 0.00235(4) N1 0.0219(12) 0.0266(13) 0.0336(15) -0.0001(11) -0.0023(11) 0.0016(10) C1 0.0262(17) 0.0316(18) 0.056(2) -0.0062(16) -0.0039(16) 0.0034(14) C2 0.033(2) 0.0301(19) 0.085(3) -0.015(2) -0.006(2) 0.0027(15) C3 0.0288(19) 0.036(2) 0.092(4) -0.010(2) -0.001(2) -0.0049(16) C4 0.0257(17) 0.0337(19) 0.063(3) -0.0050(18) 0.0014(17) -0.0005(14) C5 0.0224(15) 0.0301(16) 0.0315(17) -0.0002(13) -0.0025(12) 0.0003(12) C6 0.0231(15) 0.0305(16) 0.0250(16) -0.0016(12) 0.0011(12) 0.0020(12) N2 0.0254(13) 0.0240(12) 0.0195(12) -0.0020(10) 0.0028(10) 0.0002(10) N3 0.0270(13) 0.0260(13) 0.0217(13) -0.0057(10) 0.0071(10) 0.0009(10) C7 0.0294(15) 0.0256(15) 0.0214(15) -0.0033(12) 0.0075(12) 0.0011(12) O12 0.0316(12) 0.0246(11) 0.0367(13) -0.0079(10) 0.0188(10) -0.0035(9) C8 0.0267(15) 0.0255(15) 0.0201(14) -0.0033(12) 0.0059(11) 0.0029(12) C9 0.0345(17) 0.0292(16) 0.0238(16) -0.0030(13) 0.0145(13) -0.0006(13) C10 0.0353(17) 0.0278(16) 0.0244(16) -0.0007(13) 0.0107(13) -0.0026(13) C11 0.0308(16) 0.0244(15) 0.0178(14) 0.0013(11) 0.0021(12) 0.0032(12) C12 0.0244(15) 0.0346(17) 0.0218(15) -0.0072(13) 0.0042(12) 0.0038(13) C13 0.0219(14) 0.0307(16) 0.0275(16) -0.0059(13) 0.0056(12) 0.0008(12) C14 0.0302(15) 0.0235(14) 0.0190(14) 0.0002(11) 0.0036(12) 0.0048(12) C15 0.047(2) 0.0273(16) 0.0185(15) 0.0034(12) 0.0060(13) 0.0002(14) C16 0.048(2) 0.0218(15) 0.0256(16) 0.0042(12) 0.0088(14) -0.0022(14) C17 0.0366(17) 0.0230(15) 0.0196(15) -0.0012(12) 0.0014(12) 0.0001(12) C18 0.0255(14) 0.0241(14) 0.0177(14) 0.0018(11) 0.0024(11) 0.0036(11) C19 0.0252(14) 0.0214(14) 0.0181(14) 0.0011(11) 0.0022(11) 0.0027(11) C20 0.0263(14) 0.0203(13) 0.0176(14) 0.0006(11) 0.0025(11) 0.0040(11) C21 0.0220(14) 0.0291(15) 0.0232(15) 0.0029(12) 0.0034(11) -0.0041(12) C22 0.0227(14) 0.0320(16) 0.0212(15) 0.0003(12) -0.0019(11) -0.0040(12) C23 0.0214(14) 0.0273(15) 0.0163(14) 0.0001(11) 0.0017(11) 0.0007(11) C24 0.0200(14) 0.0265(15) 0.0207(14) 0.0009(11) 0.0030(11) 0.0005(11) C25 0.0224(14) 0.0262(15) 0.0177(14) -0.0029(11) -0.0013(11) 0.0019(11) C26 0.0214(14) 0.0279(15) 0.0190(14) -0.0019(11) 0.0002(11) -0.0021(11) O13 0.0221(11) 0.0437(13) 0.0188(11) 0.0058(9) -0.0004(8) -0.0070(9) N4 0.0216(12) 0.0355(14) 0.0158(12) 0.0014(10) 0.0010(10) -0.0020(10) N5 0.0232(12) 0.0276(13) 0.0170(12) 0.0003(10) 0.0014(9) -0.0024(10) C27 0.0217(14) 0.0263(15) 0.0242(15) -0.0011(12) 0.0028(11) -0.0011(11) C28 0.0278(15) 0.0206(14) 0.0266(16) 0.0018(12) 0.0086(12) 0.0046(11) C29 0.0299(17) 0.0323(17) 0.040(2) 0.0129(15) 0.0138(14) 0.0070(13) C30 0.0345(19) 0.045(2) 0.048(2) 0.0232(18) 0.0222(16) 0.0155(16) C31 0.043(2) 0.056(2) 0.036(2) 0.0240(18) 0.0197(16) 0.0208(18) C32 0.0342(18) 0.044(2) 0.0271(17) 0.0111(15) 0.0109(14) 0.0110(15) N6 0.0279(13) 0.0276(13) 0.0214(13) 0.0022(10) 0.0088(10) 0.0041(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 O1W O1W 1.40(4) 2_667 ? O2W H1W 0.855(10) . ? O2W H2W 0.850(10) . ? N1S C2S 1.128(11) . ? C2S C3S 1.486(12) . ? C3S H3A 0.9800 . ? C3S H3B 0.9800 . ? C3S H3C 0.9800 . ? N1W C2W 1.12(2) . ? N1W H1W 1.22(3) . ? N1W H2W 0.55(5) . ? C2W C3W 1.491(19) . ? C2W H1W 1.00(10) . ? C2W H2W 1.19(9) . ? C3W H3X 0.9800 . ? C3W H3Y 0.9800 . ? C3W H3Z 0.9800 . ? C1Y Cl2Y 1.796(7) . ? C1Y Cl1Y 1.797(7) . ? C1Y Cl3Y 1.816(7) . ? C1Y H1Y 1.0000 . ? C1G Cl1G 1.676(16) . ? C1G Cl2G 1.760(17) . ? C1G Cl3G 1.776(17) . ? C1G H1G 1.0000 . ? N4S C5S 1.114(8) . ? C5S C6S 1.440(8) . ? C6S H6A 0.9800 . ? C6S H6B 0.9800 . ? C6S H6C 0.9800 . ? S1C O1C 1.433(3) . ? S1C O2C 1.442(3) . ? S1C O3C 1.446(4) . ? S1C C1C 1.807(7) . ? C1C F2C 1.325(5) . ? C1C F1C 1.326(6) . ? C1C F3C 1.329(5) . ? S1F O1F 1.451(10) . ? S1F O3F 1.453(10) . ? S1F O2F 1.455(10) . ? S1F C1F 1.792(11) . ? C1F F3F 1.307(10) . ? C1F F1F 1.311(10) . ? C1F F2F 1.312(10) . ? S1A O2A 1.409(5) . ? S1A O3A 1.433(5) . ? S1A O1A 1.458(4) . ? S1A C1A 1.820(5) . ? O1A Bi1 2.467(4) . ? C1A F1A 1.321(6) . ? C1A F3A 1.332(6) . ? C1A F2A 1.338(6) . ? S1D O3D 1.427(15) . ? S1D O2D 1.432(14) . ? S1D O1D 1.456(14) . ? S1D C1D 1.820(9) . ? O1D Bi1 2.482(15) . ? C1D F1D 1.319(17) . ? C1D F3D 1.331(17) . ? C1D F2D 1.341(16) . ? S2A O4A 1.440(4) . ? S2A O5A 1.440(4) . ? S2A O6A 1.442(5) . ? S2A C2A 1.815(5) . ? O4A Bi1 2.548(4) . ? O6A Bi1 2.731(4) 2_766 ? C2A F4A 1.320(7) . ? C2A F6A 1.322(5) . ? C2A F5A 1.324(6) . ? S2D O4D 1.431(12) . ? S2D O6D 1.444(12) . ? S2D O5D 1.454(11) . ? S2D C2D 1.817(9) . ? O4D Bi1 2.643(12) . ? C2D F4D 1.310(15) . ? C2D F6D 1.339(13) . ? C2D F5D 1.342(13) . ? Bi1 O12 2.361(2) . ? Bi1 O13 2.377(2) 2_777 ? Bi1 N2 2.503(3) . ? Bi1 N5 2.515(3) 2_777 ? Bi1 N6 2.617(3) 2_777 ? Bi1 N1 2.622(3) . ? Bi1 O6A 2.731(4) 2_766 ? N1 C1 1.330(5) . ? N1 C5 1.351(4) . ? C1 C2 1.379(5) . ? C1 H1 0.9500 . ? C2 C3 1.376(6) . ? C2 H2 0.9500 . ? C3 C4 1.387(6) . ? C3 H3 0.9500 . ? C4 C5 1.381(5) . ? C4 H4 0.9500 . ? C5 C6 1.458(5) . ? C6 N2 1.277(4) . ? C6 H6 0.9500 . ? N2 N3 1.363(4) . ? N3 C7 1.339(4) . ? N3 H3N 0.88(4) . ? C7 O12 1.250(4) . ? C7 C8 1.482(4) . ? C8 C9 1.383(4) . ? C8 C13 1.400(4) . ? C9 C10 1.383(5) . ? C9 H9 0.9500 . ? C10 C11 1.400(4) . ? C10 H10 0.9500 . ? C11 C12 1.398(4) . ? C11 C14 1.486(4) . ? C12 C13 1.383(4) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C19 1.397(4) . ? C14 C15 1.401(4) . ? C15 C16 1.394(5) . ? C15 H15 0.9500 . ? C16 C17 1.382(5) . ? C16 H16 0.9500 . ? C17 C18 1.396(4) . ? C17 H17 0.9500 . ? C18 C19 1.402(4) . ? C18 C20 1.478(4) . ? C19 H19 0.9500 . ? C20 C21 1.399(4) . ? C20 C25 1.403(4) . ? C21 C22 1.379(4) . ? C21 H21 0.9500 . ? C22 C23 1.400(4) . ? C22 H22 0.9500 . ? C23 C24 1.396(4) . ? C23 C26 1.474(4) . ? C24 C25 1.385(4) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 O13 1.246(4) . ? C26 N4 1.350(4) . ? O13 Bi1 2.377(2) 2_777 ? N4 N5 1.371(4) . ? N4 H4N 0.89(4) . ? N5 C27 1.274(4) . ? N5 Bi1 2.515(3) 2_777 ? C27 C28 1.459(5) . ? C27 H27 0.9500 . ? C28 N6 1.344(4) . ? C28 C29 1.383(4) . ? C29 C30 1.390(5) . ? C29 H29 0.9500 . ? C30 C31 1.369(6) . ? C30 H30 0.9500 . ? C31 C32 1.396(5) . ? C31 H31 0.9500 . ? C32 N6 1.332(4) . ? C32 H32 0.9500 . ? N6 Bi1 2.617(3) 2_777 ? 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 H1W O2W H2W 103.6(17) . . ? N1S C2S C3S 177.2(9) . . ? C2S C3S H3A 109.5 . . ? C2S C3S H3B 109.5 . . ? H3A C3S H3B 109.5 . . ? C2S C3S H3C 109.5 . . ? H3A C3S H3C 109.5 . . ? H3B C3S H3C 109.5 . . ? C2W N1W H1W 50(6) . . ? C2W N1W H2W 83(10) . . ? H1W N1W H2W 91(6) . . ? N1W C2W C3W 166(3) . . ? N1W C2W H1W 70(4) . . ? C3W C2W H1W 96(5) . . ? N1W C2W H2W 27(4) . . ? C3W C2W H2W 150(5) . . ? H1W C2W H2W 75(5) . . ? C2W C3W H3X 109.5 . . ? C2W C3W H3Y 109.5 . . ? H3X C3W H3Y 109.5 . . ? C2W C3W H3Z 109.5 . . ? H3X C3W H3Z 109.5 . . ? H3Y C3W H3Z 109.5 . . ? Cl2Y C1Y Cl1Y 111.7(5) . . ? Cl2Y C1Y Cl3Y 107.8(5) . . ? Cl1Y C1Y Cl3Y 110.1(5) . . ? Cl2Y C1Y H1Y 109.1 . . ? Cl1Y C1Y H1Y 109.1 . . ? Cl3Y C1Y H1Y 109.1 . . ? Cl1G C1G Cl2G 110.1(10) . . ? Cl1G C1G Cl3G 113.8(8) . . ? Cl2G C1G Cl3G 107.2(8) . . ? Cl1G C1G H1G 108.5 . . ? Cl2G C1G H1G 108.5 . . ? Cl3G C1G H1G 108.5 . . ? N4S C5S C6S 177.8(8) . . ? C5S C6S H6A 109.5 . . ? C5S C6S H6B 109.5 . . ? H6A C6S H6B 109.5 . . ? C5S C6S H6C 109.5 . . ? H6A C6S H6C 109.5 . . ? H6B C6S H6C 109.5 . . ? O1C S1C O2C 115.6(2) . . ? O1C S1C O3C 114.6(3) . . ? O2C S1C O3C 114.4(2) . . ? O1C S1C C1C 104.3(3) . . ? O2C S1C C1C 103.8(2) . . ? O3C S1C C1C 101.8(2) . . ? F2C C1C F1C 109.0(5) . . ? F2C C1C F3C 107.8(5) . . ? F1C C1C F3C 107.5(5) . . ? F2C C1C S1C 110.6(4) . . ? F1C C1C S1C 110.9(4) . . ? F3C C1C S1C 111.0(5) . . ? O1F S1F O3F 111.4(9) . . ? O1F S1F O2F 111.4(9) . . ? O3F S1F O2F 111.6(9) . . ? O1F S1F C1F 107.8(9) . . ? O3F S1F C1F 107.0(9) . . ? O2F S1F C1F 107.4(9) . . ? F3F C1F F1F 113.1(11) . . ? F3F C1F F2F 113.1(11) . . ? F1F C1F F2F 112.5(11) . . ? F3F C1F S1F 105.9(11) . . ? F1F C1F S1F 105.8(11) . . ? F2F C1F S1F 105.7(11) . . ? O2A S1A O3A 116.1(5) . . ? O2A S1A O1A 113.5(4) . . ? O3A S1A O1A 114.5(5) . . ? O2A S1A C1A 104.9(3) . . ? O3A S1A C1A 104.9(4) . . ? O1A S1A C1A 100.6(3) . . ? S1A O1A Bi1 139.3(4) . . ? F1A C1A F3A 108.3(4) . . ? F1A C1A F2A 108.9(4) . . ? F3A C1A F2A 106.6(5) . . ? F1A C1A S1A 110.5(4) . . ? F3A C1A S1A 111.4(4) . . ? F2A C1A S1A 111.0(4) . . ? O3D S1D O2D 115.6(16) . . ? O3D S1D O1D 117.9(17) . . ? O2D S1D O1D 111.0(12) . . ? O3D S1D C1D 105.2(15) . . ? O2D S1D C1D 102.0(12) . . ? O1D S1D C1D 102.8(11) . . ? S1D O1D Bi1 148.2(11) . . ? F1D C1D F3D 110.2(18) . . ? F1D C1D F2D 110(2) . . ? F3D C1D F2D 106(2) . . ? F1D C1D S1D 112.7(15) . . ? F3D C1D S1D 108.2(15) . . ? F2D C1D S1D 109.3(17) . . ? O4A S2A O5A 113.3(3) . . ? O4A S2A O6A 114.5(4) . . ? O5A S2A O6A 116.0(3) . . ? O4A S2A C2A 102.5(3) . . ? O5A S2A C2A 104.6(3) . . ? O6A S2A C2A 103.9(3) . . ? S2A O4A Bi1 138.2(3) . . ? S2A O6A Bi1 158.6(4) . 2_766 ? F4A C2A F6A 109.2(5) . . ? F4A C2A F5A 107.1(5) . . ? F6A C2A F5A 107.3(4) . . ? F4A C2A S2A 111.1(4) . . ? F6A C2A S2A 111.0(3) . . ? F5A C2A S2A 111.0(4) . . ? O4D S2D O6D 114.4(8) . . ? O4D S2D O5D 113.3(10) . . ? O6D S2D O5D 113.1(10) . . ? O4D S2D C2D 104.7(8) . . ? O6D S2D C2D 104.9(10) . . ? O5D S2D C2D 105.1(8) . . ? S2D O4D Bi1 156.7(9) . . ? F4D C2D F6D 109.9(11) . . ? F4D C2D F5D 109.4(12) . . ? F6D C2D F5D 107.0(11) . . ? F4D C2D S2D 110.9(9) . . ? F6D C2D S2D 109.5(9) . . ? F5D C2D S2D 110.0(10) . . ? O12 Bi1 O13 78.48(9) . 2_777 ? O12 Bi1 O1A 75.2(3) . . ? O13 Bi1 O1A 141.43(16) 2_777 . ? O12 Bi1 O1D 88.0(4) . . ? O13 Bi1 O1D 143.1(4) 2_777 . ? O1A Bi1 O1D 14.2(3) . . ? O12 Bi1 N2 64.45(8) . . ? O13 Bi1 N2 68.41(8) 2_777 . ? O1A Bi1 N2 74.96(12) . . ? O1D Bi1 N2 74.8(4) . . ? O12 Bi1 N5 68.81(9) . 2_777 ? O13 Bi1 N5 64.20(8) 2_777 2_777 ? O1A Bi1 N5 128.0(2) . 2_777 ? O1D Bi1 N5 141.0(5) . 2_777 ? N2 Bi1 N5 117.99(8) . 2_777 ? O12 Bi1 O4A 139.14(14) . . ? O13 Bi1 O4A 69.58(13) 2_777 . ? O1A Bi1 O4A 144.7(3) . . ? O1D Bi1 O4A 132.7(4) . . ? N2 Bi1 O4A 121.99(12) . . ? N5 Bi1 O4A 74.57(13) 2_777 . ? O12 Bi1 N6 78.36(8) . 2_777 ? O13 Bi1 N6 126.43(8) 2_777 2_777 ? O1A Bi1 N6 74.73(16) . 2_777 ? O1D Bi1 N6 82.9(5) . 2_777 ? N2 Bi1 N6 136.69(8) . 2_777 ? N5 Bi1 N6 62.47(8) 2_777 2_777 ? O4A Bi1 N6 100.47(12) . 2_777 ? O12 Bi1 N1 126.90(8) . . ? O13 Bi1 N1 79.60(8) 2_777 . ? O1A Bi1 N1 94.3(2) . . ? O1D Bi1 N1 81.6(5) . . ? N2 Bi1 N1 62.56(9) . . ? N5 Bi1 N1 137.34(9) 2_777 . ? O4A Bi1 N1 72.06(12) . . ? N6 Bi1 N1 149.61(9) 2_777 . ? O12 Bi1 O4D 143.3(4) . . ? O13 Bi1 O4D 80.3(2) 2_777 . ? O1A Bi1 O4D 135.8(3) . . ? O1D Bi1 O4D 125.7(5) . . ? N2 Bi1 O4D 132.3(3) . . ? N5 Bi1 O4D 75.1(4) 2_777 . ? O4A Bi1 O4D 11.5(2) . . ? N6 Bi1 O4D 90.9(3) 2_777 . ? N1 Bi1 O4D 77.3(4) . . ? O12 Bi1 O6A 142.03(14) . 2_766 ? O13 Bi1 O6A 137.93(13) 2_777 2_766 ? O1A Bi1 O6A 76.3(2) . 2_766 ? O1D Bi1 O6A 67.6(4) . 2_766 ? N2 Bi1 O6A 129.71(15) . 2_766 ? N5 Bi1 O6A 112.26(15) 2_777 2_766 ? O4A Bi1 O6A 69.35(15) . 2_766 ? N6 Bi1 O6A 70.33(15) 2_777 2_766 ? N1 Bi1 O6A 79.61(16) . 2_766 ? O4D Bi1 O6A 59.6(3) . 2_766 ? C1 N1 C5 117.7(3) . . ? C1 N1 Bi1 124.3(2) . . ? C5 N1 Bi1 118.0(2) . . ? N1 C1 C2 123.0(4) . . ? N1 C1 H1 118.5 . . ? C2 C1 H1 118.5 . . ? C3 C2 C1 119.2(4) . . ? C3 C2 H2 120.4 . . ? C1 C2 H2 120.4 . . ? C2 C3 C4 118.9(4) . . ? C2 C3 H3 120.6 . . ? C4 C3 H3 120.6 . . ? C5 C4 C3 118.4(4) . . ? C5 C4 H4 120.8 . . ? C3 C4 H4 120.8 . . ? N1 C5 C4 122.8(3) . . ? N1 C5 C6 116.9(3) . . ? C4 C5 C6 120.2(3) . . ? N2 C6 C5 117.6(3) . . ? N2 C6 H6 121.2 . . ? C5 C6 H6 121.2 . . ? C6 N2 N3 119.3(3) . . ? C6 N2 Bi1 124.9(2) . . ? N3 N2 Bi1 115.74(18) . . ? C7 N3 N2 115.7(3) . . ? C7 N3 H3N 122(3) . . ? N2 N3 H3N 122(3) . . ? O12 C7 N3 121.9(3) . . ? O12 C7 C8 119.8(3) . . ? N3 C7 C8 118.2(3) . . ? C7 O12 Bi1 122.1(2) . . ? C9 C8 C13 119.3(3) . . ? C9 C8 C7 118.5(3) . . ? C13 C8 C7 122.0(3) . . ? C8 C9 C10 120.8(3) . . ? C8 C9 H9 119.6 . . ? C10 C9 H9 119.6 . . ? C9 C10 C11 120.5(3) . . ? C9 C10 H10 119.8 . . ? C11 C10 H10 119.8 . . ? C12 C11 C10 118.5(3) . . ? C12 C11 C14 120.7(3) . . ? C10 C11 C14 120.7(3) . . ? C13 C12 C11 120.9(3) . . ? C13 C12 H12 119.6 . . ? C11 C12 H12 119.6 . . ? C12 C13 C8 119.9(3) . . ? C12 C13 H13 120.0 . . ? C8 C13 H13 120.0 . . ? C19 C14 C15 118.9(3) . . ? C19 C14 C11 119.6(3) . . ? C15 C14 C11 121.5(3) . . ? C16 C15 C14 120.2(3) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C17 C16 C15 120.4(3) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C16 C17 C18 120.5(3) . . ? C16 C17 H17 119.7 . . ? C18 C17 H17 119.7 . . ? C17 C18 C19 118.9(3) . . ? C17 C18 C20 121.6(3) . . ? C19 C18 C20 119.5(3) . . ? C14 C19 C18 121.1(3) . . ? C14 C19 H19 119.5 . . ? C18 C19 H19 119.5 . . ? C21 C20 C25 118.5(3) . . ? C21 C20 C18 120.7(3) . . ? C25 C20 C18 120.7(3) . . ? C22 C21 C20 120.8(3) . . ? C22 C21 H21 119.6 . . ? C20 C21 H21 119.6 . . ? C21 C22 C23 120.3(3) . . ? C21 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? C24 C23 C22 119.5(3) . . ? C24 C23 C26 122.6(3) . . ? C22 C23 C26 117.8(3) . . ? C25 C24 C23 119.9(3) . . ? C25 C24 H24 120.1 . . ? C23 C24 H24 120.1 . . ? C24 C25 C20 120.9(3) . . ? C24 C25 H25 119.5 . . ? C20 C25 H25 119.5 . . ? O13 C26 N4 121.1(3) . . ? O13 C26 C23 120.2(3) . . ? N4 C26 C23 118.7(3) . . ? C26 O13 Bi1 122.99(19) . 2_777 ? C26 N4 N5 116.1(3) . . ? C26 N4 H4N 127(3) . . ? N5 N4 H4N 117(3) . . ? C27 N5 N4 120.2(3) . . ? C27 N5 Bi1 124.3(2) . 2_777 ? N4 N5 Bi1 115.56(18) . 2_777 ? N5 C27 C28 117.9(3) . . ? N5 C27 H27 121.1 . . ? C28 C27 H27 121.1 . . ? N6 C28 C29 122.3(3) . . ? N6 C28 C27 116.8(3) . . ? C29 C28 C27 120.9(3) . . ? C28 C29 C30 118.6(3) . . ? C28 C29 H29 120.7 . . ? C30 C29 H29 120.7 . . ? C31 C30 C29 119.3(3) . . ? C31 C30 H30 120.3 . . ? C29 C30 H30 120.3 . . ? C30 C31 C32 118.8(3) . . ? C30 C31 H31 120.6 . . ? C32 C31 H31 120.6 . . ? N6 C32 C31 122.4(4) . . ? N6 C32 H32 118.8 . . ? C31 C32 H32 118.8 . . ? C32 N6 C28 118.6(3) . . ? C32 N6 Bi1 122.9(2) . 2_777 ? C28 N6 Bi1 118.4(2) . 2_777 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1C S1C C1C F2C 60.8(4) . . . . ? O2C S1C C1C F2C -177.8(4) . . . . ? O3C S1C C1C F2C -58.7(5) . . . . ? O1C S1C C1C F1C -178.2(4) . . . . ? O2C S1C C1C F1C -56.8(4) . . . . ? O3C S1C C1C F1C 62.3(4) . . . . ? O1C S1C C1C F3C -58.9(4) . . . . ? O2C S1C C1C F3C 62.6(4) . . . . ? O3C S1C C1C F3C -178.3(4) . . . . ? O1F S1F C1F F3F -51.1(15) . . . . ? O3F S1F C1F F3F -171.0(15) . . . . ? O2F S1F C1F F3F 69.0(15) . . . . ? O1F S1F C1F F1F -171.3(15) . . . . ? O3F S1F C1F F1F 68.7(16) . . . . ? O2F S1F C1F F1F -51.2(16) . . . . ? O1F S1F C1F F2F 69.2(15) . . . . ? O3F S1F C1F F2F -50.7(15) . . . . ? O2F S1F C1F F2F -170.7(15) . . . . ? O2A S1A O1A Bi1 -62.2(9) . . . . ? O3A S1A O1A Bi1 74.5(10) . . . . ? C1A S1A O1A Bi1 -173.7(8) . . . . ? O2A S1A C1A F1A 63.1(5) . . . . ? O3A S1A C1A F1A -59.8(6) . . . . ? O1A S1A C1A F1A -178.9(5) . . . . ? O2A S1A C1A F3A -176.5(5) . . . . ? O3A S1A C1A F3A 60.6(6) . . . . ? O1A S1A C1A F3A -58.5(5) . . . . ? O2A S1A C1A F2A -57.9(5) . . . . ? O3A S1A C1A F2A 179.3(6) . . . . ? O1A S1A C1A F2A 60.2(5) . . . . ? O3D S1D O1D Bi1 15(3) . . . . ? O2D S1D O1D Bi1 -122(3) . . . . ? C1D S1D O1D Bi1 130(3) . . . . ? O3D S1D C1D F1D -60(2) . . . . ? O2D S1D C1D F1D 61(2) . . . . ? O1D S1D C1D F1D 176.2(18) . . . . ? O3D S1D C1D F3D 62(2) . . . . ? O2D S1D C1D F3D -176.8(18) . . . . ? O1D S1D C1D F3D -61.7(18) . . . . ? O3D S1D C1D F2D 177(2) . . . . ? O2D S1D C1D F2D -62(2) . . . . ? O1D S1D C1D F2D 53(2) . . . . ? O5A S2A O4A Bi1 23.9(6) . . . . ? O6A S2A O4A Bi1 -112.3(5) . . . . ? C2A S2A O4A Bi1 136.0(4) . . . . ? O4A S2A O6A Bi1 107.9(10) . . . 2_766 ? O5A S2A O6A Bi1 -27.1(11) . . . 2_766 ? C2A S2A O6A Bi1 -141.2(9) . . . 2_766 ? O4A S2A C2A F4A 61.8(5) . . . . ? O5A S2A C2A F4A -179.7(4) . . . . ? O6A S2A C2A F4A -57.7(5) . . . . ? O4A S2A C2A F6A -59.9(5) . . . . ? O5A S2A C2A F6A 58.6(5) . . . . ? O6A S2A C2A F6A -179.4(5) . . . . ? O4A S2A C2A F5A -179.1(4) . . . . ? O5A S2A C2A F5A -60.6(4) . . . . ? O6A S2A C2A F5A 61.4(5) . . . . ? O6D S2D O4D Bi1 -166(2) . . . . ? O5D S2D O4D Bi1 -35(3) . . . . ? C2D S2D O4D Bi1 79(2) . . . . ? O4D S2D C2D F4D 50.6(13) . . . . ? O6D S2D C2D F4D -70.2(12) . . . . ? O5D S2D C2D F4D 170.2(10) . . . . ? O4D S2D C2D F6D -70.9(13) . . . . ? O6D S2D C2D F6D 168.3(11) . . . . ? O5D S2D C2D F6D 48.7(12) . . . . ? O4D S2D C2D F5D 171.7(12) . . . . ? O6D S2D C2D F5D 50.9(13) . . . . ? O5D S2D C2D F5D -68.6(12) . . . . ? S1A O1A Bi1 O12 -89.4(7) . . . . ? S1A O1A Bi1 O13 -40.9(10) . . . 2_777 ? S1A O1A Bi1 O1D 65.0(17) . . . . ? S1A O1A Bi1 N2 -22.4(7) . . . . ? S1A O1A Bi1 N5 -136.4(6) . . . 2_777 ? S1A O1A Bi1 O4A 102.3(6) . . . . ? S1A O1A Bi1 N6 -171.1(8) . . . 2_777 ? S1A O1A Bi1 N1 37.7(8) . . . . ? S1A O1A Bi1 O4D 113.9(8) . . . . ? S1A O1A Bi1 O6A 115.9(8) . . . 2_766 ? S1D O1D Bi1 O12 -42(2) . . . . ? S1D O1D Bi1 O13 26(3) . . . 2_777 ? S1D O1D Bi1 O1A -67(2) . . . . ? S1D O1D Bi1 N2 22(2) . . . . ? S1D O1D Bi1 N5 -94(2) . . . 2_777 ? S1D O1D Bi1 O4A 142(2) . . . . ? S1D O1D Bi1 N6 -121(2) . . . 2_777 ? S1D O1D Bi1 N1 86(2) . . . . ? S1D O1D Bi1 O4D 154(2) . . . . ? S1D O1D Bi1 O6A 168(3) . . . 2_766 ? S2A O4A Bi1 O12 -79.6(5) . . . . ? S2A O4A Bi1 O13 -120.5(5) . . . 2_777 ? S2A O4A Bi1 O1A 83.0(6) . . . . ? S2A O4A Bi1 O1D 94.6(8) . . . . ? S2A O4A Bi1 N2 -166.4(4) . . . . ? S2A O4A Bi1 N5 -52.8(5) . . . 2_777 ? S2A O4A Bi1 N6 4.7(5) . . . 2_777 ? S2A O4A Bi1 N1 154.2(5) . . . . ? S2A O4A Bi1 O4D 38(2) . . . . ? S2A O4A Bi1 O6A 68.8(5) . . . 2_766 ? S2D O4D Bi1 O12 21(3) . . . . ? S2D O4D Bi1 O13 -34(2) . . . 2_777 ? S2D O4D Bi1 O1A 162(2) . . . . ? S2D O4D Bi1 O1D 175(2) . . . . ? S2D O4D Bi1 N2 -83(3) . . . . ? S2D O4D Bi1 N5 32(2) . . . 2_777 ? S2D O4D Bi1 O4A -54.0(16) . . . . ? S2D O4D Bi1 N6 93(2) . . . 2_777 ? S2D O4D Bi1 N1 -115(2) . . . . ? S2D O4D Bi1 O6A 159(3) . . . 2_766 ? O12 Bi1 N1 C1 -175.0(3) . . . . ? O13 Bi1 N1 C1 -108.0(3) 2_777 . . . ? O1A Bi1 N1 C1 110.4(3) . . . . ? O1D Bi1 N1 C1 103.8(5) . . . . ? N2 Bi1 N1 C1 -179.0(3) . . . . ? N5 Bi1 N1 C1 -76.5(3) 2_777 . . . ? O4A Bi1 N1 C1 -36.3(3) . . . . ? N6 Bi1 N1 C1 43.6(4) 2_777 . . . ? O4D Bi1 N1 C1 -25.7(4) . . . . ? O6A Bi1 N1 C1 35.2(3) 2_766 . . . ? O12 Bi1 N1 C5 6.1(3) . . . . ? O13 Bi1 N1 C5 73.0(2) 2_777 . . . ? O1A Bi1 N1 C5 -68.5(3) . . . . ? O1D Bi1 N1 C5 -75.1(4) . . . . ? N2 Bi1 N1 C5 2.1(2) . . . . ? N5 Bi1 N1 C5 104.6(3) 2_777 . . . ? O4A Bi1 N1 C5 144.8(3) . . . . ? N6 Bi1 N1 C5 -135.3(2) 2_777 . . . ? O4D Bi1 N1 C5 155.4(4) . . . . ? O6A Bi1 N1 C5 -143.7(3) 2_766 . . . ? C5 N1 C1 C2 1.2(6) . . . . ? Bi1 N1 C1 C2 -177.7(4) . . . . ? N1 C1 C2 C3 -0.5(8) . . . . ? C1 C2 C3 C4 -0.9(8) . . . . ? C2 C3 C4 C5 1.6(8) . . . . ? C1 N1 C5 C4 -0.4(5) . . . . ? Bi1 N1 C5 C4 178.6(3) . . . . ? C1 N1 C5 C6 178.1(3) . . . . ? Bi1 N1 C5 C6 -2.9(4) . . . . ? C3 C4 C5 N1 -1.0(6) . . . . ? C3 C4 C5 C6 -179.4(4) . . . . ? N1 C5 C6 N2 2.0(5) . . . . ? C4 C5 C6 N2 -179.5(4) . . . . ? C5 C6 N2 N3 -176.3(3) . . . . ? C5 C6 N2 Bi1 0.1(4) . . . . ? O12 Bi1 N2 C6 -177.5(3) . . . . ? O13 Bi1 N2 C6 -90.3(3) 2_777 . . . ? O1A Bi1 N2 C6 102.0(4) . . . . ? O1D Bi1 N2 C6 87.3(5) . . . . ? N5 Bi1 N2 C6 -132.6(3) 2_777 . . . ? O4A Bi1 N2 C6 -43.9(3) . . . . ? N6 Bi1 N2 C6 148.9(2) 2_777 . . . ? N1 Bi1 N2 C6 -1.1(2) . . . . ? O4D Bi1 N2 C6 -37.4(5) . . . . ? O6A Bi1 N2 C6 44.8(3) 2_766 . . . ? O12 Bi1 N2 N3 -1.0(2) . . . . ? O13 Bi1 N2 N3 86.2(2) 2_777 . . . ? O1A Bi1 N2 N3 -81.5(3) . . . . ? O1D Bi1 N2 N3 -96.2(5) . . . . ? N5 Bi1 N2 N3 43.9(2) 2_777 . . . ? O4A Bi1 N2 N3 132.6(2) . . . . ? N6 Bi1 N2 N3 -34.6(3) 2_777 . . . ? N1 Bi1 N2 N3 175.4(2) . . . . ? O4D Bi1 N2 N3 139.1(5) . . . . ? O6A Bi1 N2 N3 -138.7(2) 2_766 . . . ? C6 N2 N3 C7 176.5(3) . . . . ? Bi1 N2 N3 C7 -0.2(3) . . . . ? N2 N3 C7 O12 2.5(5) . . . . ? N2 N3 C7 C8 -174.4(3) . . . . ? N3 C7 O12 Bi1 -3.7(5) . . . . ? C8 C7 O12 Bi1 173.1(2) . . . . ? O13 Bi1 O12 C7 -69.0(3) 2_777 . . . ? O1A Bi1 O12 C7 82.6(3) . . . . ? O1D Bi1 O12 C7 76.5(5) . . . . ? N2 Bi1 O12 C7 2.4(3) . . . . ? N5 Bi1 O12 C7 -135.6(3) 2_777 . . . ? O4A Bi1 O12 C7 -107.8(3) . . . . ? N6 Bi1 O12 C7 159.6(3) 2_777 . . . ? N1 Bi1 O12 C7 -1.5(3) . . . . ? O4D Bi1 O12 C7 -124.9(5) . . . . ? O6A Bi1 O12 C7 125.0(3) 2_766 . . . ? O12 C7 C8 C9 14.7(5) . . . . ? N3 C7 C8 C9 -168.4(3) . . . . ? O12 C7 C8 C13 -160.0(3) . . . . ? N3 C7 C8 C13 16.9(5) . . . . ? C13 C8 C9 C10 2.1(5) . . . . ? C7 C8 C9 C10 -172.8(3) . . . . ? C8 C9 C10 C11 0.1(6) . . . . ? C9 C10 C11 C12 -2.5(5) . . . . ? C9 C10 C11 C14 174.3(3) . . . . ? C10 C11 C12 C13 2.6(5) . . . . ? C14 C11 C12 C13 -174.1(3) . . . . ? C11 C12 C13 C8 -0.5(5) . . . . ? C9 C8 C13 C12 -1.9(5) . . . . ? C7 C8 C13 C12 172.8(3) . . . . ? C12 C11 C14 C19 33.8(5) . . . . ? C10 C11 C14 C19 -142.9(3) . . . . ? C12 C11 C14 C15 -148.2(3) . . . . ? C10 C11 C14 C15 35.1(5) . . . . ? C19 C14 C15 C16 0.0(5) . . . . ? C11 C14 C15 C16 -178.1(3) . . . . ? C14 C15 C16 C17 0.7(6) . . . . ? C15 C16 C17 C18 -0.5(6) . . . . ? C16 C17 C18 C19 -0.4(5) . . . . ? C16 C17 C18 C20 177.5(3) . . . . ? C15 C14 C19 C18 -0.9(5) . . . . ? C11 C14 C19 C18 177.2(3) . . . . ? C17 C18 C19 C14 1.1(5) . . . . ? C20 C18 C19 C14 -176.9(3) . . . . ? C17 C18 C20 C21 -35.5(5) . . . . ? C19 C18 C20 C21 142.4(3) . . . . ? C17 C18 C20 C25 147.5(3) . . . . ? C19 C18 C20 C25 -34.6(4) . . . . ? C25 C20 C21 C22 2.5(5) . . . . ? C18 C20 C21 C22 -174.6(3) . . . . ? C20 C21 C22 C23 -1.1(5) . . . . ? C21 C22 C23 C24 -1.3(5) . . . . ? C21 C22 C23 C26 174.9(3) . . . . ? C22 C23 C24 C25 2.3(5) . . . . ? C26 C23 C24 C25 -173.7(3) . . . . ? C23 C24 C25 C20 -0.9(5) . . . . ? C21 C20 C25 C24 -1.5(5) . . . . ? C18 C20 C25 C24 175.6(3) . . . . ? C24 C23 C26 O13 161.7(3) . . . . ? C22 C23 C26 O13 -14.3(5) . . . . ? C24 C23 C26 N4 -16.2(5) . . . . ? C22 C23 C26 N4 167.7(3) . . . . ? N4 C26 O13 Bi1 -0.6(4) . . . 2_777 ? C23 C26 O13 Bi1 -178.4(2) . . . 2_777 ? O13 C26 N4 N5 -1.5(5) . . . . ? C23 C26 N4 N5 176.4(3) . . . . ? C26 N4 N5 C27 -176.5(3) . . . . ? C26 N4 N5 Bi1 2.6(3) . . . 2_777 ? N4 N5 C27 C28 178.5(3) . . . . ? Bi1 N5 C27 C28 -0.5(4) 2_777 . . . ? N5 C27 C28 N6 -3.5(4) . . . . ? N5 C27 C28 C29 177.4(3) . . . . ? N6 C28 C29 C30 -0.1(5) . . . . ? C27 C28 C29 C30 179.0(3) . . . . ? C28 C29 C30 C31 -0.4(6) . . . . ? C29 C30 C31 C32 0.9(6) . . . . ? C30 C31 C32 N6 -1.0(6) . . . . ? C31 C32 N6 C28 0.5(5) . . . . ? C31 C32 N6 Bi1 175.6(3) . . . 2_777 ? C29 C28 N6 C32 0.0(5) . . . . ? C27 C28 N6 C32 -179.1(3) . . . . ? C29 C28 N6 Bi1 -175.3(2) . . . 2_777 ? C27 C28 N6 Bi1 5.5(4) . . . 2_777 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2W H1W N1S 0.855(10) 1.90(4) 2.714(14) 158(9) . N3 H3N N1W 0.88(4) 1.85(5) 2.59(2) 140(4) . N3 H3N O2W 0.88(4) 1.95(4) 2.761(12) 152(4) . N4 H4N O3C 0.89(4) 1.89(4) 2.759(5) 163(4) 2_677 N4 H4N O3F 0.89(4) 1.98(5) 2.839(18) 161(4) 2_677 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.675 _refine_diff_density_min -0.680 _refine_diff_density_rms 0.109