#------------------------------------------------------------------------------ #$Date: 2014-12-22 15:48:03 +0200 (Mon, 22 Dec 2014) $ #$Revision: 128995 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/11/60/7116063.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_7116063 loop_ _publ_author_name 'Laura H. Davies' 'Benjamin B. Kasten' 'Paul D. Benny' 'Rory L. Arrowsmith' 'Haobo Ge'Sofia I. Pascu' 'Stan W. Botchway' 'William Clegg' 'Ross W. Harrington' 'Lee J. Higham' _publ_section_title ; Re and ^99m^Tc complexes of BodP3 - multi-modality imaging probes ; _journal_name_full Chem.Commun. _journal_page_first 15503 _journal_paper_doi 10.1039/C4cc06367H _journal_volume 50 _journal_year 2014 _chemical_formula_moiety 'C56 H60 B N2 O3 P3 Re +,C F3 O3 S -,C7 H8 N2 O2,C5 H12' _chemical_formula_sum 'C69 H80 B F3 N4 O8 P3 Re S' _chemical_formula_weight 1472.35 _chemical_name_systematic ; ? ; _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2014 _cell_angle_alpha 92.712(2) _cell_angle_beta 97.724(3) _cell_angle_gamma 98.344(3) _cell_formula_units_Z 2 _cell_length_a 11.7574(5) _cell_length_b 16.2273(5) _cell_length_c 18.3187(6) _cell_measurement_reflns_used 15771 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 66.6723 _cell_measurement_theta_min 2.4377 _cell_volume 3418.7(2) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _computing_structure_refinement 'SHELXL-2014 (Sheldrick, 2014)' _computing_structure_solution 'Bruker SHELXTL' _diffrn_ambient_temperature 150(2) _diffrn_detector_area_resol_mean 10.3968 _diffrn_measured_fraction_theta_full 0.955 _diffrn_measured_fraction_theta_max 0.975 _diffrn_measurement_device_type 'Agilent Technologies Gemini A Ultra' _diffrn_measurement_method '\w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0791 _diffrn_reflns_av_unetI/netI 0.0545 _diffrn_reflns_laue_measured_fraction_full 0.955 _diffrn_reflns_laue_measured_fraction_max 0.975 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 23448 _diffrn_reflns_point_group_measured_fraction_full 0.955 _diffrn_reflns_point_group_measured_fraction_max 0.975 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 66.778 _diffrn_reflns_theta_min 2.440 _diffrn_source 'sealed tube with Enhance Ultra optics' _exptl_absorpt_coefficient_mu 4.957 _exptl_absorpt_correction_T_max 1.440 _exptl_absorpt_correction_T_min 0.320 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour red _exptl_crystal_density_diffrn 1.430 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1508 _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _refine_diff_density_max 5.940 _refine_diff_density_min -3.207 _refine_diff_density_rms 0.212 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 839 _refine_ls_number_reflns 11816 _refine_ls_number_restraints 151 _refine_ls_restrained_S_all 1.021 _refine_ls_R_factor_all 0.0748 _refine_ls_R_factor_gt 0.0732 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1725P)^2^+3.1808P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1994 _refine_ls_wR_factor_ref 0.2032 _reflns_Friedel_coverage 0.000 _reflns_number_gt 11250 _reflns_number_total 11816 _reflns_threshold_expression 'I > 2\s(I)' _[local]_cod_data_source_file c4cc06367h2.cif _[local]_cod_data_source_block ljh120041 _cod_database_code 7116063 _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 0.318 _shelx_estimated_absorpt_t_max 0.437 _shelxl_version_number 2014-3 _shelx_res_file ; TITL ljh120041 in P-1 CELL 1.54178 11.7574 16.2273 18.3187 92.712 97.724 98.344 ZERR 2 0.0005 0.0005 0.0006 0.002 0.003 0.003 LATT 1 SFAC C H B F N O P RE S UNIT 138 160 2 6 8 16 6 2 2 TEMP -123 SIZE 0.2 0.2 0.3 L.S. 8 ACTA BOND $H CONF FMAP 2 PLAN 10 EQIV $1 -x, -y+1, -z+1 EQIV $2 -x, -y+1, -z EQIV $3 x+1, y, z HTAB O8 O7_$2 HTAB N4 O5_$3 HTAB N4 O4_$1 SIMU C65 > C68' RIGU C65 > C68' rem EXTI 0.000000 WGHT 0.172500 3.180800 FVAR 0.08315 0.49886 RE 8 0.190198 0.128456 0.351990 11.00000 0.02057 0.01549 = 0.01942 0.00224 0.00150 -0.00142 B 3 0.728546 0.167678 0.876302 11.00000 0.02781 0.02785 = 0.02206 0.00633 -0.00370 0.00427 N1 5 0.768735 0.185624 0.798487 11.00000 0.02887 0.03250 = 0.02042 0.00128 -0.00295 -0.00173 N2 5 0.591116 0.154634 0.861675 11.00000 0.02945 0.02767 = 0.02036 0.00803 -0.00143 0.00176 C1 1 0.878257 0.200154 0.783830 11.00000 0.02952 0.03641 = 0.02695 -0.00035 -0.00170 -0.00184 C2 1 0.880108 0.218595 0.708801 11.00000 0.03030 0.03573 = 0.02861 -0.00132 0.00560 -0.00679 C3 1 0.766377 0.215920 0.677156 11.00000 0.03577 0.03628 = 0.02297 0.00533 0.00328 -0.00768 C4 1 0.695227 0.195158 0.733817 11.00000 0.03238 0.02756 = 0.01698 0.00333 0.00013 -0.00203 C5 1 0.576796 0.187341 0.733325 11.00000 0.03198 0.02058 = 0.02370 0.00327 0.00022 0.00182 C6 1 0.522898 0.167236 0.795011 11.00000 0.02729 0.02639 = 0.02050 0.00153 -0.00016 -0.00003 C7 1 0.404640 0.156388 0.805736 11.00000 0.02887 0.03242 = 0.02693 0.00386 0.00583 0.00520 C8 1 0.402000 0.137586 0.878787 11.00000 0.03549 0.03290 = 0.03520 0.00484 0.01075 0.00076 C9 1 0.517527 0.137225 0.911394 11.00000 0.03745 0.03339 = 0.02335 0.00710 0.00788 0.00505 C10 1 0.984260 0.200365 0.839086 11.00000 0.02973 0.05353 = 0.03255 0.00016 -0.00628 -0.00235 AFIX 33 H10A 2 1.053740 0.212543 0.814949 11.00000 -1.50000 H10B 2 0.986363 0.243181 0.879015 11.00000 -1.50000 H10C 2 0.982131 0.145509 0.859499 11.00000 -1.50000 AFIX 0 C11 1 0.987352 0.236865 0.672978 11.00000 0.03753 0.04611 = 0.03689 0.00496 0.00783 -0.00593 AFIX 23 H11A 2 1.053410 0.260491 0.711088 11.00000 -1.20000 H11B 2 0.976120 0.279458 0.636824 11.00000 -1.20000 AFIX 0 C12 1 1.017502 0.158790 0.633253 11.00000 0.04750 0.06617 = 0.04979 0.00854 0.01623 0.00176 AFIX 33 H12A 2 1.088089 0.174078 0.610837 11.00000 -1.50000 H12B 2 1.030455 0.116825 0.668965 11.00000 -1.50000 H12C 2 0.953145 0.135796 0.594682 11.00000 -1.50000 AFIX 0 C13 1 0.728042 0.230187 0.597885 11.00000 0.03554 0.06700 = 0.02438 0.01277 0.00226 -0.00918 AFIX 33 H13A 2 0.643157 0.224970 0.588833 11.00000 -1.50000 H13B 2 0.762246 0.286297 0.587238 11.00000 -1.50000 H13C 2 0.753688 0.188613 0.565812 11.00000 -1.50000 AFIX 0 C14 1 0.300590 0.165677 0.752387 11.00000 0.02617 0.05461 = 0.03215 0.00570 0.00376 0.00728 AFIX 33 H14A 2 0.324470 0.178925 0.704521 11.00000 -1.50000 H14B 2 0.245873 0.113361 0.746521 11.00000 -1.50000 H14C 2 0.262998 0.210854 0.771034 11.00000 -1.50000 AFIX 0 C15 1 0.295764 0.119721 0.916182 11.00000 0.04020 0.05029 = 0.03731 0.00791 0.01610 0.00385 AFIX 23 H15A 2 0.243301 0.160589 0.901952 11.00000 -1.20000 H15B 2 0.319314 0.127507 0.970313 11.00000 -1.20000 AFIX 0 C16 1 0.229014 0.031222 0.896760 11.00000 0.04145 0.05503 = 0.04816 0.00610 0.01851 -0.00247 AFIX 33 H16A 2 0.160994 0.023421 0.922724 11.00000 -1.50000 H16B 2 0.203673 0.023415 0.843369 11.00000 -1.50000 H16C 2 0.279744 -0.009693 0.911782 11.00000 -1.50000 AFIX 0 C17 1 0.556246 0.120989 0.990057 11.00000 0.05467 0.05165 = 0.02617 0.01233 0.01012 0.00469 AFIX 33 H17A 2 0.488335 0.109800 1.015813 11.00000 -1.50000 H17B 2 0.597271 0.072528 0.991326 11.00000 -1.50000 H17C 2 0.608442 0.170024 1.014453 11.00000 -1.50000 AFIX 0 C18 1 0.772063 0.081747 0.905361 11.00000 0.04167 0.03131 = 0.03529 0.01056 0.00628 0.00777 AFIX 33 H18A 2 0.857131 0.089767 0.914430 11.00000 -1.50000 H18B 2 0.741326 0.068417 0.951255 11.00000 -1.50000 H18C 2 0.743718 0.035747 0.867749 11.00000 -1.50000 AFIX 0 C19 1 0.771506 0.250560 0.931156 11.00000 0.04371 0.03248 = 0.02416 -0.00037 -0.00181 -0.00164 AFIX 33 H19A 2 0.856542 0.260228 0.941226 11.00000 -1.50000 H19B 2 0.744321 0.298675 0.907911 11.00000 -1.50000 H19C 2 0.739705 0.243032 0.977592 11.00000 -1.50000 AFIX 0 C20 1 0.502123 0.198522 0.662547 11.00000 0.02675 0.02913 = 0.01860 0.00435 -0.00220 -0.00086 C21 1 0.457512 0.130259 0.612940 11.00000 0.02570 0.02139 = 0.03234 0.00714 -0.00081 0.00232 AFIX 43 H21 2 0.471957 0.075844 0.624208 11.00000 -1.20000 AFIX 0 C22 1 0.391351 0.142776 0.546497 11.00000 0.03036 0.02412 = 0.02069 0.00077 0.00064 -0.00075 AFIX 43 H22 2 0.359720 0.096235 0.512794 11.00000 -1.20000 AFIX 0 C23 1 0.370824 0.222094 0.528665 11.00000 0.02884 0.02600 = 0.01893 0.00796 0.00142 -0.00285 C24 1 0.415675 0.289880 0.579062 11.00000 0.04205 0.02166 = 0.02536 0.00703 -0.00833 -0.00192 AFIX 43 H24 2 0.402302 0.344383 0.567317 11.00000 -1.20000 AFIX 0 C25 1 0.479925 0.278436 0.646490 11.00000 0.04330 0.02153 = 0.02621 0.00219 -0.00756 -0.00926 AFIX 43 H25 2 0.508364 0.324591 0.681218 11.00000 -1.20000 AFIX 0 P1 7 0.298939 0.214547 0.270223 11.00000 0.02393 0.02043 = 0.02055 0.00225 0.00381 -0.00226 P2 7 0.286424 0.239329 0.442157 11.00000 0.02361 0.01785 = 0.01811 0.00331 0.00015 -0.00178 P3 7 0.036823 0.219264 0.344468 11.00000 0.02024 0.01803 = 0.01816 0.00148 0.00183 -0.00167 C26 1 0.230066 0.229156 0.177331 11.00000 0.02471 0.03740 = 0.02226 0.00082 0.00445 -0.00253 C27 1 0.188119 0.159325 0.129374 11.00000 0.03545 0.04063 = 0.02762 -0.00026 0.00740 0.00328 AFIX 43 H27 2 0.193429 0.105286 0.146068 11.00000 -1.20000 AFIX 0 C28 1 0.138641 0.167234 0.057553 11.00000 0.03962 0.05523 = 0.02741 -0.00857 0.00495 -0.00070 AFIX 43 H28 2 0.109895 0.119017 0.025238 11.00000 -1.20000 AFIX 0 C29 1 0.131353 0.247374 0.032899 11.00000 0.04584 0.06860 = 0.02206 0.00461 0.00084 0.01030 AFIX 43 H29 2 0.098231 0.253829 -0.016338 11.00000 -1.20000 AFIX 0 C30 1 0.172573 0.316069 0.080704 11.00000 0.05485 0.05745 = 0.02961 0.01116 0.00726 0.01093 AFIX 43 H30 2 0.166951 0.370088 0.064052 11.00000 -1.20000 AFIX 0 C31 1 0.222562 0.308687 0.153178 11.00000 0.03817 0.04170 = 0.02286 0.00818 0.00409 0.00505 AFIX 43 H31 2 0.250969 0.356965 0.185479 11.00000 -1.20000 AFIX 0 C32 1 0.434837 0.182331 0.251558 11.00000 0.02635 0.03106 = 0.01853 0.00373 0.00243 -0.00123 C33 1 0.434184 0.099120 0.228969 11.00000 0.02539 0.03448 = 0.03537 -0.00263 0.00341 -0.00562 AFIX 43 H33 2 0.365633 0.059944 0.228450 11.00000 -1.20000 AFIX 0 C34 1 0.532508 0.072533 0.207145 11.00000 0.03569 0.03844 = 0.04159 -0.01028 0.00817 0.00577 AFIX 43 H34 2 0.530388 0.015781 0.190924 11.00000 -1.20000 AFIX 0 C35 1 0.633204 0.128741 0.209091 11.00000 0.03368 0.05235 = 0.03952 0.00668 0.01562 0.00887 AFIX 43 H35 2 0.700883 0.110772 0.194826 11.00000 -1.20000 AFIX 0 C36 1 0.634750 0.211534 0.232008 11.00000 0.02745 0.04930 = 0.03603 0.01045 0.00483 -0.00360 AFIX 43 H36 2 0.704000 0.250259 0.233488 11.00000 -1.20000 AFIX 0 C37 1 0.536335 0.238628 0.252845 11.00000 0.02837 0.03026 = 0.03057 0.00391 0.00499 -0.00649 AFIX 43 H37 2 0.538360 0.295690 0.267996 11.00000 -1.20000 AFIX 0 C38 1 0.340339 0.319618 0.316931 11.00000 0.03491 0.02069 = 0.02023 0.00292 0.00335 -0.00521 AFIX 23 H38A 2 0.401947 0.351618 0.293202 11.00000 -1.20000 H38B 2 0.272326 0.349505 0.311985 11.00000 -1.20000 AFIX 0 C39 1 0.384593 0.314149 0.399188 11.00000 0.03153 0.02077 = 0.02338 0.00481 0.00024 -0.00866 AFIX 23 H39A 2 0.392005 0.369949 0.425228 11.00000 -1.20000 H39B 2 0.462570 0.297006 0.404274 11.00000 -1.20000 AFIX 0 C40 1 0.174415 0.295218 0.472829 11.00000 0.02579 0.02765 = 0.02385 -0.00003 0.00051 -0.00057 AFIX 23 H40A 2 0.131268 0.260889 0.506399 11.00000 -1.20000 H40B 2 0.211854 0.348175 0.500627 11.00000 -1.20000 AFIX 0 C41 1 0.089542 0.314079 0.407058 11.00000 0.02608 0.02280 = 0.02604 -0.00115 -0.00017 0.00290 AFIX 23 H41A 2 0.128732 0.358218 0.379548 11.00000 -1.20000 H41B 2 0.022680 0.335015 0.425147 11.00000 -1.20000 AFIX 0 C42 1 -0.099770 0.173604 0.374207 11.00000 0.02425 0.02610 = 0.01675 0.00498 -0.00023 -0.00180 C43 1 -0.176368 0.224442 0.396628 11.00000 0.02922 0.03198 = 0.02273 0.00527 0.00627 0.00362 AFIX 43 H43 2 -0.155541 0.283428 0.399706 11.00000 -1.20000 AFIX 0 C44 1 -0.282689 0.189185 0.414416 11.00000 0.03123 0.04259 = 0.02661 0.00466 0.00722 0.00581 AFIX 43 H44 2 -0.334302 0.224256 0.429794 11.00000 -1.20000 AFIX 0 C45 1 -0.314478 0.103760 0.410060 11.00000 0.02793 0.05099 = 0.03046 0.00970 0.00753 -0.00420 AFIX 43 H45 2 -0.387451 0.080127 0.422653 11.00000 -1.20000 AFIX 0 C46 1 -0.239750 0.052485 0.387276 11.00000 0.03454 0.03085 = 0.04055 0.00846 0.00638 -0.00816 AFIX 43 H46 2 -0.261392 -0.006442 0.383909 11.00000 -1.20000 AFIX 0 C47 1 -0.133122 0.087561 0.369387 11.00000 0.02420 0.02895 = 0.03266 0.00400 0.00565 -0.00083 AFIX 43 H47 2 -0.082125 0.052231 0.353601 11.00000 -1.20000 AFIX 0 C48 1 -0.017603 0.258688 0.257244 11.00000 0.02086 0.02296 = 0.02252 0.01022 0.00263 0.00337 C49 1 -0.030439 0.342815 0.251486 11.00000 0.03594 0.02252 = 0.02190 0.00198 -0.00159 0.00180 AFIX 43 H49 2 -0.004343 0.381909 0.292700 11.00000 -1.20000 AFIX 0 C50 1 -0.081592 0.368995 0.185137 11.00000 0.03955 0.02700 = 0.02870 0.01020 0.00125 0.00628 AFIX 43 H50 2 -0.090691 0.425941 0.181475 11.00000 -1.20000 AFIX 0 C51 1 -0.119124 0.312778 0.124714 11.00000 0.03764 0.03591 = 0.02533 0.00945 0.00025 0.00204 AFIX 43 H51 2 -0.153181 0.331078 0.079524 11.00000 -1.20000 AFIX 0 C52 1 -0.106947 0.230129 0.130293 11.00000 0.03118 0.03453 = 0.02353 0.00061 0.00026 0.00191 AFIX 43 H52 2 -0.133541 0.191334 0.088920 11.00000 -1.20000 AFIX 0 C53 1 -0.055823 0.202804 0.196262 11.00000 0.03059 0.02798 = 0.02366 0.00053 0.00342 0.00109 AFIX 43 H53 2 -0.047201 0.145712 0.199365 11.00000 -1.20000 AFIX 0 C54 1 0.310919 0.059955 0.367409 11.00000 0.03100 0.01260 = 0.02702 0.00348 0.00124 0.00127 O1 6 0.378759 0.016370 0.379181 11.00000 0.04306 0.03689 = 0.05283 0.00640 0.00310 0.01009 C55 1 0.100254 0.047621 0.273860 11.00000 0.03436 0.01529 = 0.03455 0.00475 0.00829 -0.00093 O2 6 0.048715 0.001417 0.230482 11.00000 0.04615 0.03097 = 0.03725 -0.01077 -0.00281 -0.00247 C56 1 0.127511 0.074211 0.433503 11.00000 0.02378 0.02241 = 0.03725 0.00267 -0.00544 0.00436 O3 6 0.100727 0.044282 0.485628 11.00000 0.03909 0.05600 = 0.04020 0.02658 0.00944 -0.00789 C57 1 -0.190288 0.509840 0.388176 11.00000 0.04710 0.09129 = 0.11191 -0.04597 0.04598 -0.02224 F1 4 -0.100428 0.530459 0.443969 11.00000 0.03597 0.23944 = 0.17200 -0.06475 0.00464 -0.00514 F2 4 -0.204043 0.579198 0.361024 11.00000 0.14619 0.09529 = 0.10152 -0.01172 0.08272 -0.05607 F3 4 -0.157298 0.464236 0.337557 11.00000 0.11646 0.16449 = 0.21582 -0.10355 0.10416 -0.00687 S 9 -0.316344 0.459426 0.424362 11.00000 0.04512 0.02572 = 0.05960 -0.00361 0.00636 -0.00041 O4 6 -0.338224 0.521524 0.475444 11.00000 0.07121 0.03650 = 0.06486 0.00244 0.03199 -0.00547 O5 6 -0.397722 0.440237 0.360583 11.00000 0.06613 0.10716 = 0.07227 -0.01065 0.00405 -0.02779 O6 6 -0.281871 0.387986 0.460488 11.00000 0.18845 0.06095 = 0.13805 0.02603 0.01339 0.05908 C58 1 0.100695 0.532098 0.092763 11.00000 0.06429 0.03125 = 0.04664 0.01352 0.00713 -0.00552 C59 1 0.174521 0.540213 0.165210 11.00000 0.07075 0.02795 = 0.04614 0.01338 0.00330 -0.01347 C60 1 0.129151 0.548580 0.230462 11.00000 0.05024 0.03436 = 0.04916 0.00393 0.00100 -0.01198 AFIX 43 H60 2 0.050560 0.557186 0.228117 11.00000 -1.20000 AFIX 0 C61 1 0.193097 0.544979 0.299048 11.00000 0.06215 0.03135 = 0.04308 0.00074 0.00790 -0.01673 C62 1 0.310846 0.533400 0.302438 11.00000 0.05662 0.02135 = 0.05208 0.00521 -0.00641 -0.01490 C63 1 0.358600 0.528401 0.237011 11.00000 0.05654 0.03146 = 0.04709 0.00852 0.00137 -0.00669 AFIX 43 H63 2 0.438228 0.522882 0.238636 11.00000 -1.20000 AFIX 0 C64 1 0.289988 0.531467 0.169156 11.00000 0.06428 0.03614 = 0.04390 0.01061 0.00499 -0.00563 AFIX 43 H64 2 0.323414 0.527459 0.124948 11.00000 -1.20000 AFIX 0 O7 6 -0.006514 0.540541 0.091322 11.00000 0.06095 0.06509 = 0.05496 0.02295 0.00096 0.00064 O8 6 0.141805 0.515093 0.034787 11.00000 0.07313 0.05802 = 0.04197 0.01581 -0.00290 0.00558 AFIX 83 H8 2 0.089842 0.512618 -0.001858 11.00000 -1.20000 AFIX 0 N3 5 0.146175 0.543181 0.363470 11.00000 0.07329 0.06875 = 0.06420 0.00478 0.00734 -0.00446 AFIX 93 H3A 2 0.071415 0.544319 0.362662 11.00000 -1.20000 H3B 2 0.190751 0.540886 0.405718 11.00000 -1.20000 AFIX 0 N4 5 0.377891 0.528201 0.369398 11.00000 0.06921 0.03853 = 0.04156 0.00740 -0.00275 -0.01275 AFIX 93 H4A 2 0.451174 0.521698 0.370955 11.00000 -1.20000 H4B 2 0.347386 0.531387 0.410564 11.00000 -1.20000 AFIX 0 SAME C65 C66' C67' C68' C69 SAME C69 < C65 C65 1 0.522284 0.345580 1.074501 11.00000 0.21953 0.15005 = 0.27744 0.01038 0.12705 0.08962 PART 1 AFIX 33 H65A 2 0.595076 0.347303 1.108017 21.00000 -1.50000 H65B 2 0.468435 0.374051 1.099162 21.00000 -1.50000 H65C 2 0.487493 0.287347 1.060914 21.00000 -1.50000 AFIX 33 PART 2 H65D 2 0.586687 0.319481 1.097973 -21.00000 -1.50000 H65E 2 0.537284 0.405727 1.088005 -21.00000 -1.50000 H65F 2 0.449911 0.321066 1.091279 -21.00000 -1.50000 AFIX 0 PART 1 C66 1 0.545324 0.386346 1.009670 21.00000 0.19853 0.15709 = 0.28012 0.00971 0.12885 0.08863 AFIX 23 H66A 2 0.598481 0.358270 0.983021 21.00000 -1.20000 H66B 2 0.579260 0.445714 1.021595 21.00000 -1.20000 AFIX 0 C67 1 0.411246 0.376800 0.959888 21.00000 0.19231 0.16143 = 0.28025 0.01433 0.12999 0.07107 AFIX 23 H67A 2 0.364432 0.328202 0.977831 21.00000 -1.20000 H67B 2 0.377842 0.426546 0.974761 21.00000 -1.20000 AFIX 0 C68 1 0.384129 0.365856 0.867564 21.00000 0.19399 0.17880 = 0.27720 0.01919 0.12712 0.03421 AFIX 23 H68A 2 0.445877 0.400240 0.845724 21.00000 -1.20000 H68B 2 0.380475 0.306761 0.849997 21.00000 -1.20000 AFIX 0 PART 0 C69 1 0.275238 0.393077 0.847377 11.00000 0.18851 0.19979 = 0.30475 0.01215 0.11079 0.03644 PART 1 AFIX 33 H69A 2 0.255309 0.387871 0.793498 21.00000 -1.50000 H69B 2 0.215157 0.358556 0.869488 21.00000 -1.50000 H69C 2 0.280227 0.451559 0.865236 21.00000 -1.50000 AFIX 33 PART 2 H69D 2 0.258883 0.416840 0.799583 -21.00000 -1.50000 H69E 2 0.268527 0.332266 0.839924 -21.00000 -1.50000 H69F 2 0.219387 0.407032 0.879385 -21.00000 -1.50000 AFIX 0 PART 2 C66' 1 0.512009 0.331645 0.995940 -21.00000 0.21082 0.17525 = 0.27817 0.00864 0.12480 0.05148 AFIX 23 H66C 2 0.496468 0.271120 0.981253 -21.00000 -1.20000 H66D 2 0.584327 0.356254 0.977960 -21.00000 -1.20000 AFIX 0 C67' 1 0.400165 0.378435 0.961238 -21.00000 0.19858 0.17003 = 0.28513 0.01534 0.12597 0.04492 AFIX 23 H67C 2 0.391219 0.420515 1.000138 -21.00000 -1.20000 H67D 2 0.330245 0.335395 0.956740 -21.00000 -1.20000 AFIX 0 C68' 1 0.390548 0.426820 0.881330 -21.00000 0.18901 0.18819 = 0.28065 0.01480 0.12588 0.04278 AFIX 23 H68C 2 0.399685 0.488191 0.890576 -21.00000 -1.20000 H68D 2 0.449270 0.412746 0.850757 -21.00000 -1.20000 AFIX 0 HKLF 4 REM ljh120041 in P-1 REM R1 = 0.0732 for 11250 Fo > 4sig(Fo) and 0.0748 for all 11816 data REM 839 parameters refined using 151 restraints END WGHT 0.1713 3.1042 REM Highest difference peak 5.940, deepest hole -3.207, 1-sigma level 0.212 Q1 1 0.1950 0.1873 0.3602 11.00000 0.05 5.94 Q2 1 0.1749 0.0694 0.3514 11.00000 0.05 5.71 Q3 1 0.1152 0.1227 0.3356 11.00000 0.05 3.99 Q4 1 0.2633 0.1359 0.3699 11.00000 0.05 3.86 Q5 1 0.1933 0.1573 0.4004 11.00000 0.05 3.19 Q6 1 0.3154 0.2813 0.2770 11.00000 0.05 1.44 Q7 1 0.1365 0.2378 0.3561 11.00000 0.05 1.41 Q8 1 0.1279 0.2338 0.3287 11.00000 0.05 1.40 Q9 1 -0.3238 0.3961 0.4154 11.00000 0.05 1.36 Q10 1 0.2807 0.1423 0.2704 11.00000 0.05 1.36 ; _shelx_res_checksum 28051 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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 Re Re 0.19020(2) 0.12846(2) 0.35199(2) 0.01900(14) Uani 1 1 d . . . . . B B 0.7285(6) 0.1677(4) 0.8763(4) 0.0264(13) Uani 1 1 d . . . . . N1 N 0.7687(4) 0.1856(3) 0.7985(3) 0.0285(10) Uani 1 1 d . . . . . N2 N 0.5911(4) 0.1546(3) 0.8617(2) 0.0263(10) Uani 1 1 d . . . . . C1 C 0.8783(5) 0.2002(4) 0.7838(3) 0.0323(13) Uani 1 1 d . . . . . C2 C 0.8801(5) 0.2186(4) 0.7088(3) 0.0327(13) Uani 1 1 d . . . . . C3 C 0.7664(5) 0.2159(4) 0.6772(3) 0.0330(13) Uani 1 1 d . . . . . C4 C 0.6952(5) 0.1952(4) 0.7338(3) 0.0266(12) Uani 1 1 d . . . . . C5 C 0.5768(5) 0.1873(3) 0.7333(3) 0.0259(11) Uani 1 1 d . . . . . C6 C 0.5229(5) 0.1672(4) 0.7950(3) 0.0255(11) Uani 1 1 d . . . . . C7 C 0.4046(5) 0.1564(4) 0.8057(3) 0.0291(12) Uani 1 1 d . . . . . C8 C 0.4020(6) 0.1376(4) 0.8788(3) 0.0344(13) Uani 1 1 d . . . . . C9 C 0.5175(5) 0.1372(4) 0.9114(3) 0.0309(13) Uani 1 1 d . . . . . C10 C 0.9843(6) 0.2004(5) 0.8391(4) 0.0406(16) Uani 1 1 d . . . . . H10A H 1.0537 0.2125 0.8149 0.061 Uiso 1 1 calc R U . . . H10B H 0.9864 0.2432 0.8790 0.061 Uiso 1 1 calc R U . . . H10C H 0.9821 0.1455 0.8595 0.061 Uiso 1 1 calc R U . . . C11 C 0.9874(6) 0.2369(5) 0.6730(4) 0.0411(16) Uani 1 1 d . . . . . H11A H 1.0534 0.2605 0.7111 0.049 Uiso 1 1 calc R U . . . H11B H 0.9761 0.2795 0.6368 0.049 Uiso 1 1 calc R U . . . C12 C 1.0175(7) 0.1588(6) 0.6333(4) 0.0542(19) Uani 1 1 d . . . . . H12A H 1.0881 0.1741 0.6108 0.081 Uiso 1 1 calc R U . . . H12B H 1.0305 0.1168 0.6690 0.081 Uiso 1 1 calc R U . . . H12C H 0.9531 0.1358 0.5947 0.081 Uiso 1 1 calc R U . . . C13 C 0.7280(6) 0.2302(5) 0.5979(3) 0.0439(17) Uani 1 1 d . . . . . H13A H 0.6432 0.2250 0.5888 0.066 Uiso 1 1 calc R U . . . H13B H 0.7622 0.2863 0.5872 0.066 Uiso 1 1 calc R U . . . H13C H 0.7537 0.1886 0.5658 0.066 Uiso 1 1 calc R U . . . C14 C 0.3006(5) 0.1657(5) 0.7524(4) 0.0375(15) Uani 1 1 d . . . . . H14A H 0.3245 0.1789 0.7045 0.056 Uiso 1 1 calc R U . . . H14B H 0.2459 0.1134 0.7465 0.056 Uiso 1 1 calc R U . . . H14C H 0.2630 0.2109 0.7710 0.056 Uiso 1 1 calc R U . . . C15 C 0.2958(6) 0.1197(5) 0.9162(4) 0.0418(15) Uani 1 1 d . . . . . H15A H 0.2433 0.1606 0.9020 0.050 Uiso 1 1 calc R U . . . H15B H 0.3193 0.1275 0.9703 0.050 Uiso 1 1 calc R U . . . C16 C 0.2290(6) 0.0312(5) 0.8968(4) 0.0480(17) Uani 1 1 d . . . . . H16A H 0.1610 0.0234 0.9227 0.072 Uiso 1 1 calc R U . . . H16B H 0.2037 0.0234 0.8434 0.072 Uiso 1 1 calc R U . . . H16C H 0.2797 -0.0097 0.9118 0.072 Uiso 1 1 calc R U . . . C17 C 0.5562(7) 0.1210(5) 0.9901(3) 0.0438(16) Uani 1 1 d . . . . . H17A H 0.4883 0.1098 1.0158 0.066 Uiso 1 1 calc R U . . . H17B H 0.5973 0.0725 0.9913 0.066 Uiso 1 1 calc R U . . . H17C H 0.6084 0.1700 1.0145 0.066 Uiso 1 1 calc R U . . . C18 C 0.7721(6) 0.0817(4) 0.9054(4) 0.0355(14) Uani 1 1 d . . . . . H18A H 0.8571 0.0898 0.9144 0.053 Uiso 1 1 calc R U . . . H18B H 0.7413 0.0684 0.9513 0.053 Uiso 1 1 calc R U . . . H18C H 0.7437 0.0357 0.8677 0.053 Uiso 1 1 calc R U . . . C19 C 0.7715(6) 0.2506(4) 0.9312(3) 0.0349(14) Uani 1 1 d . . . . . H19A H 0.8565 0.2602 0.9412 0.052 Uiso 1 1 calc R U . . . H19B H 0.7443 0.2987 0.9079 0.052 Uiso 1 1 calc R U . . . H19C H 0.7397 0.2430 0.9776 0.052 Uiso 1 1 calc R U . . . C20 C 0.5021(5) 0.1985(4) 0.6625(3) 0.0258(12) Uani 1 1 d . . . . . C21 C 0.4575(5) 0.1303(3) 0.6129(3) 0.0269(12) Uani 1 1 d . . . . . H21 H 0.4720 0.0758 0.6242 0.032 Uiso 1 1 calc R U . . . C22 C 0.3914(5) 0.1428(4) 0.5465(3) 0.0259(11) Uani 1 1 d . . . . . H22 H 0.3597 0.0962 0.5128 0.031 Uiso 1 1 calc R U . . . C23 C 0.3708(5) 0.2221(4) 0.5287(3) 0.0253(11) Uani 1 1 d . . . . . C24 C 0.4157(5) 0.2899(4) 0.5791(3) 0.0314(13) Uani 1 1 d . . . . . H24 H 0.4023 0.3444 0.5673 0.038 Uiso 1 1 calc R U . . . C25 C 0.4799(6) 0.2784(4) 0.6465(3) 0.0329(13) Uani 1 1 d . . . . . H25 H 0.5084 0.3246 0.6812 0.039 Uiso 1 1 calc R U . . . P1 P 0.29894(12) 0.21455(9) 0.27022(7) 0.0221(3) Uani 1 1 d . . . . . P2 P 0.28642(12) 0.23933(8) 0.44216(7) 0.0205(3) Uani 1 1 d . . . . . P3 P 0.03682(12) 0.21926(8) 0.34447(7) 0.0193(3) Uani 1 1 d . . . . . C26 C 0.2301(5) 0.2292(4) 0.1773(3) 0.0288(12) Uani 1 1 d . . . . . C27 C 0.1881(5) 0.1593(4) 0.1294(3) 0.0346(13) Uani 1 1 d . . . . . H27 H 0.1934 0.1053 0.1461 0.042 Uiso 1 1 calc R U . . . C28 C 0.1386(6) 0.1672(5) 0.0576(4) 0.0419(16) Uani 1 1 d . . . . . H28 H 0.1099 0.1190 0.0252 0.050 Uiso 1 1 calc R U . . . C29 C 0.1314(6) 0.2474(5) 0.0329(4) 0.0457(17) Uani 1 1 d . . . . . H29 H 0.0982 0.2538 -0.0163 0.055 Uiso 1 1 calc R U . . . C30 C 0.1726(7) 0.3161(6) 0.0807(4) 0.0467(18) Uani 1 1 d . . . . . H30 H 0.1670 0.3701 0.0641 0.056 Uiso 1 1 calc R U . . . C31 C 0.2226(6) 0.3087(4) 0.1532(3) 0.0342(13) Uani 1 1 d . . . . . H31 H 0.2510 0.3570 0.1855 0.041 Uiso 1 1 calc R U . . . C32 C 0.4348(5) 0.1823(4) 0.2516(3) 0.0259(11) Uani 1 1 d . . . . . C33 C 0.4342(5) 0.0991(4) 0.2290(3) 0.0330(13) Uani 1 1 d . . . . . H33 H 0.3656 0.0599 0.2284 0.040 Uiso 1 1 calc R U . . . C34 C 0.5325(6) 0.0725(4) 0.2071(4) 0.0387(14) Uani 1 1 d . . . . . H34 H 0.5304 0.0158 0.1909 0.046 Uiso 1 1 calc R U . . . C35 C 0.6332(6) 0.1287(5) 0.2091(4) 0.0405(15) Uani 1 1 d . . . . . H35 H 0.7009 0.1108 0.1948 0.049 Uiso 1 1 calc R U . . . C36 C 0.6348(6) 0.2115(5) 0.2320(4) 0.0383(15) Uani 1 1 d . . . . . H36 H 0.7040 0.2503 0.2335 0.046 Uiso 1 1 calc R U . . . C37 C 0.5363(5) 0.2386(4) 0.2528(3) 0.0307(13) Uani 1 1 d . . . . . H37 H 0.5384 0.2957 0.2680 0.037 Uiso 1 1 calc R U . . . C38 C 0.3403(5) 0.3196(3) 0.3169(3) 0.0262(11) Uani 1 1 d . . . . . H38A H 0.4019 0.3516 0.2932 0.031 Uiso 1 1 calc R U . . . H38B H 0.2723 0.3495 0.3120 0.031 Uiso 1 1 calc R U . . . C39 C 0.3846(5) 0.3141(3) 0.3992(3) 0.0267(12) Uani 1 1 d . . . . . H39A H 0.3920 0.3699 0.4252 0.032 Uiso 1 1 calc R U . . . H39B H 0.4626 0.2970 0.4043 0.032 Uiso 1 1 calc R U . . . C40 C 0.1744(5) 0.2952(4) 0.4728(3) 0.0266(11) Uani 1 1 d . . . . . H40A H 0.1313 0.2609 0.5064 0.032 Uiso 1 1 calc R U . . . H40B H 0.2119 0.3482 0.5006 0.032 Uiso 1 1 calc R U . . . C41 C 0.0895(5) 0.3141(3) 0.4071(3) 0.0255(11) Uani 1 1 d . . . . . H41A H 0.1287 0.3582 0.3795 0.031 Uiso 1 1 calc R U . . . H41B H 0.0227 0.3350 0.4251 0.031 Uiso 1 1 calc R U . . . C42 C -0.0998(5) 0.1736(3) 0.3742(3) 0.0231(11) Uani 1 1 d . . . . . C43 C -0.1764(5) 0.2244(4) 0.3966(3) 0.0277(12) Uani 1 1 d . . . . . H43 H -0.1555 0.2834 0.3997 0.033 Uiso 1 1 calc R U . . . C44 C -0.2827(5) 0.1892(4) 0.4144(3) 0.0331(13) Uani 1 1 d . . . . . H44 H -0.3343 0.2243 0.4298 0.040 Uiso 1 1 calc R U . . . C45 C -0.3145(5) 0.1038(4) 0.4101(3) 0.0370(14) Uani 1 1 d . . . . . H45 H -0.3875 0.0801 0.4227 0.044 Uiso 1 1 calc R U . . . C46 C -0.2398(6) 0.0525(4) 0.3873(4) 0.0363(15) Uani 1 1 d . . . . . H46 H -0.2614 -0.0064 0.3839 0.044 Uiso 1 1 calc R U . . . C47 C -0.1331(5) 0.0876(4) 0.3694(3) 0.0289(12) Uani 1 1 d . . . . . H47 H -0.0821 0.0522 0.3536 0.035 Uiso 1 1 calc R U . . . C48 C -0.0176(4) 0.2587(3) 0.2572(3) 0.0219(10) Uani 1 1 d . . . . . C49 C -0.0304(5) 0.3428(4) 0.2515(3) 0.0276(12) Uani 1 1 d . . . . . H49 H -0.0043 0.3819 0.2927 0.033 Uiso 1 1 calc R U . . . C50 C -0.0816(5) 0.3690(4) 0.1851(3) 0.0317(13) Uani 1 1 d . . . . . H50 H -0.0907 0.4259 0.1815 0.038 Uiso 1 1 calc R U . . . C51 C -0.1191(5) 0.3128(4) 0.1247(3) 0.0335(13) Uani 1 1 d . . . . . H51 H -0.1532 0.3311 0.0795 0.040 Uiso 1 1 calc R U . . . C52 C -0.1069(5) 0.2301(4) 0.1303(3) 0.0304(12) Uani 1 1 d . . . . . H52 H -0.1335 0.1913 0.0889 0.037 Uiso 1 1 calc R U . . . C53 C -0.0558(5) 0.2028(4) 0.1963(3) 0.0278(12) Uani 1 1 d . . . . . H53 H -0.0472 0.1457 0.1994 0.033 Uiso 1 1 calc R U . . . C54 C 0.3109(5) 0.0600(3) 0.3674(3) 0.0239(11) Uani 1 1 d . . . . . O1 O 0.3788(4) 0.0164(3) 0.3792(3) 0.0441(11) Uani 1 1 d . . . . . C55 C 0.1003(5) 0.0476(4) 0.2739(3) 0.0281(13) Uani 1 1 d . . . . . O2 O 0.0487(4) 0.0014(3) 0.2305(3) 0.0402(11) Uani 1 1 d . . . . . C56 C 0.1275(5) 0.0742(4) 0.4335(3) 0.0286(12) Uani 1 1 d . . . . . O3 O 0.1007(4) 0.0443(3) 0.4856(3) 0.0455(12) Uani 1 1 d . . . . . C57 C -0.1903(8) 0.5098(8) 0.3882(7) 0.085(4) Uani 1 1 d . . . . . F1 F -0.1004(5) 0.5305(8) 0.4440(6) 0.155(4) Uani 1 1 d . . . . . F2 F -0.2040(7) 0.5792(5) 0.3610(4) 0.116(3) Uani 1 1 d . . . . . F3 F -0.1573(8) 0.4642(7) 0.3376(6) 0.165(5) Uani 1 1 d . . . . . S S -0.31634(16) 0.45943(10) 0.42436(11) 0.0444(4) Uani 1 1 d . . . . . O4 O -0.3382(5) 0.5215(3) 0.4754(3) 0.0569(15) Uani 1 1 d . . . . . O5 O -0.3977(6) 0.4402(5) 0.3606(4) 0.087(2) Uani 1 1 d . . . . . O6 O -0.2819(11) 0.3880(6) 0.4605(6) 0.125(4) Uani 1 1 d . . . . . C58 C 0.1007(7) 0.5321(5) 0.0928(4) 0.0484(18) Uani 1 1 d . . . . . C59 C 0.1745(8) 0.5402(4) 0.1652(4) 0.0505(19) Uani 1 1 d . . . . . C60 C 0.1292(7) 0.5486(4) 0.2305(4) 0.0470(17) Uani 1 1 d . . . . . H60 H 0.0506 0.5572 0.2281 0.056 Uiso 1 1 calc R U . . . C61 C 0.1931(7) 0.5450(4) 0.2990(4) 0.0479(18) Uani 1 1 d . . . . . C62 C 0.3108(7) 0.5334(4) 0.3024(4) 0.0467(17) Uani 1 1 d . . . . . C63 C 0.3586(7) 0.5284(4) 0.2370(4) 0.0467(17) Uani 1 1 d . . . . . H63 H 0.4382 0.5229 0.2386 0.056 Uiso 1 1 calc R U . . . C64 C 0.2900(7) 0.5315(5) 0.1692(4) 0.0494(18) Uani 1 1 d . . . . . H64 H 0.3234 0.5275 0.1249 0.059 Uiso 1 1 calc R U . . . O7 O -0.0065(6) 0.5405(4) 0.0913(3) 0.0613(16) Uani 1 1 d . . . . . O8 O 0.1418(6) 0.5151(4) 0.0348(3) 0.0588(15) Uani 1 1 d . . . . . H8 H 0.0898 0.5126 -0.0019 0.071 Uiso 1 1 calc R U . . . N3 N 0.1462(8) 0.5432(5) 0.3635(4) 0.071(2) Uani 1 1 d . . . . . H3A H 0.0714 0.5443 0.3627 0.085 Uiso 1 1 calc R U . . . H3B H 0.1908 0.5409 0.4057 0.085 Uiso 1 1 calc R U . . . N4 N 0.3779(7) 0.5282(4) 0.3694(4) 0.0527(17) Uani 1 1 d . . . . . H4A H 0.4512 0.5217 0.3710 0.063 Uiso 1 1 calc R U . . . H4B H 0.3474 0.5314 0.4106 0.063 Uiso 1 1 calc R U . . . C65 C 0.522(2) 0.3456(15) 1.0745(16) 0.201(9) Uani 1 1 d D U . . . H65A H 0.5951 0.3473 1.1080 0.302 Uiso 0.50(3) 1 calc R U P A 1 H65B H 0.4684 0.3741 1.0992 0.302 Uiso 0.50(3) 1 calc R U P A 1 H65C H 0.4875 0.2873 1.0609 0.302 Uiso 0.50(3) 1 calc R U P A 1 H65D H 0.5867 0.3195 1.0980 0.302 Uiso 0.50(3) 1 calc R U P A 2 H65E H 0.5373 0.4057 1.0880 0.302 Uiso 0.50(3) 1 calc R U P A 2 H65F H 0.4499 0.3211 1.0913 0.302 Uiso 0.50(3) 1 calc R U P A 2 C66 C 0.545(3) 0.386(3) 1.010(2) 0.197(10) Uani 0.50(3) 1 d D U P A 1 H66A H 0.5985 0.3583 0.9830 0.237 Uiso 0.50(3) 1 calc R U P A 1 H66B H 0.5793 0.4457 1.0216 0.237 Uiso 0.50(3) 1 calc R U P A 1 C67 C 0.411(3) 0.377(5) 0.9599(17) 0.198(10) Uani 0.50(3) 1 d D U P A 1 H67A H 0.3644 0.3282 0.9778 0.238 Uiso 0.50(3) 1 calc R U P A 1 H67B H 0.3778 0.4265 0.9748 0.238 Uiso 0.50(3) 1 calc R U P A 1 C68 C 0.384(3) 0.366(4) 0.868(2) 0.207(11) Uani 0.50(3) 1 d D U P A 1 H68A H 0.4459 0.4002 0.8457 0.249 Uiso 0.50(3) 1 calc R U P A 1 H68B H 0.3805 0.3068 0.8500 0.249 Uiso 0.50(3) 1 calc R U P A 1 C69 C 0.275(2) 0.3931(18) 0.8474(17) 0.224(10) Uani 1 1 d D U . . . H69A H 0.2553 0.3879 0.7935 0.335 Uiso 0.50(3) 1 calc R U P A 1 H69B H 0.2152 0.3586 0.8695 0.335 Uiso 0.50(3) 1 calc R U P A 1 H69C H 0.2802 0.4516 0.8652 0.335 Uiso 0.50(3) 1 calc R U P A 1 H69D H 0.2589 0.4168 0.7996 0.335 Uiso 0.50(3) 1 calc R U P A 2 H69E H 0.2685 0.3323 0.8399 0.335 Uiso 0.50(3) 1 calc R U P A 2 H69F H 0.2194 0.4070 0.8794 0.335 Uiso 0.50(3) 1 calc R U P A 2 C66' C 0.512(5) 0.332(4) 0.9959(19) 0.211(11) Uani 0.50(3) 1 d D U P A 2 H66C H 0.4965 0.2711 0.9813 0.253 Uiso 0.50(3) 1 calc R U P A 2 H66D H 0.5843 0.3563 0.9780 0.253 Uiso 0.50(3) 1 calc R U P A 2 C67' C 0.400(4) 0.378(5) 0.961(2) 0.208(10) Uani 0.50(3) 1 d D U P A 2 H67C H 0.3912 0.4205 1.0001 0.249 Uiso 0.50(3) 1 calc R U P A 2 H67D H 0.3302 0.3354 0.9567 0.249 Uiso 0.50(3) 1 calc R U P A 2 C68' C 0.391(3) 0.427(3) 0.881(3) 0.209(11) Uani 0.50(3) 1 d D U P A 2 H68C H 0.3997 0.4882 0.8906 0.251 Uiso 0.50(3) 1 calc R U P A 2 H68D H 0.4493 0.4127 0.8508 0.251 Uiso 0.50(3) 1 calc R U P A 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 Re 0.02057(19) 0.01549(19) 0.01942(19) 0.00224(11) 0.00150(12) -0.00142(11) B 0.028(3) 0.028(3) 0.022(3) 0.006(2) -0.004(2) 0.004(2) N1 0.029(3) 0.033(3) 0.020(2) 0.0013(19) -0.0029(19) -0.0017(19) N2 0.029(3) 0.028(3) 0.020(2) 0.0080(18) -0.0014(18) 0.0018(19) C1 0.030(3) 0.036(3) 0.027(3) 0.000(2) -0.002(2) -0.002(2) C2 0.030(3) 0.036(3) 0.029(3) -0.001(2) 0.006(2) -0.007(2) C3 0.036(3) 0.036(3) 0.023(3) 0.005(2) 0.003(2) -0.008(2) C4 0.032(3) 0.028(3) 0.017(2) 0.003(2) 0.000(2) -0.002(2) C5 0.032(3) 0.021(3) 0.024(3) 0.003(2) 0.000(2) 0.002(2) C6 0.027(3) 0.026(3) 0.020(3) 0.002(2) 0.000(2) 0.000(2) C7 0.029(3) 0.032(3) 0.027(3) 0.004(2) 0.006(2) 0.005(2) C8 0.035(3) 0.033(3) 0.035(3) 0.005(3) 0.011(3) 0.001(2) C9 0.037(3) 0.033(3) 0.023(3) 0.007(2) 0.008(2) 0.005(2) C10 0.030(3) 0.054(5) 0.033(3) 0.000(3) -0.006(3) -0.002(3) C11 0.038(4) 0.046(4) 0.037(3) 0.005(3) 0.008(3) -0.006(3) C12 0.048(4) 0.066(5) 0.050(4) 0.009(4) 0.016(3) 0.002(4) C13 0.036(4) 0.067(5) 0.024(3) 0.013(3) 0.002(3) -0.009(3) C14 0.026(3) 0.055(4) 0.032(3) 0.006(3) 0.004(2) 0.007(3) C15 0.040(4) 0.050(4) 0.037(3) 0.008(3) 0.016(3) 0.004(3) C16 0.041(4) 0.055(5) 0.048(4) 0.006(3) 0.019(3) -0.002(3) C17 0.055(4) 0.052(4) 0.026(3) 0.012(3) 0.010(3) 0.005(3) C18 0.042(4) 0.031(3) 0.035(3) 0.011(3) 0.006(3) 0.008(3) C19 0.044(4) 0.032(3) 0.024(3) 0.000(2) -0.002(3) -0.002(3) C20 0.027(3) 0.029(3) 0.019(3) 0.004(2) -0.002(2) -0.001(2) C21 0.026(3) 0.021(3) 0.032(3) 0.007(2) -0.001(2) 0.002(2) C22 0.030(3) 0.024(3) 0.021(3) 0.001(2) 0.001(2) -0.001(2) C23 0.029(3) 0.026(3) 0.019(3) 0.008(2) 0.001(2) -0.003(2) C24 0.042(3) 0.022(3) 0.025(3) 0.007(2) -0.008(2) -0.002(2) C25 0.043(4) 0.022(3) 0.026(3) 0.002(2) -0.008(2) -0.009(2) P1 0.0239(7) 0.0204(7) 0.0206(7) 0.0023(5) 0.0038(5) -0.0023(5) P2 0.0236(7) 0.0179(7) 0.0181(6) 0.0033(5) 0.0002(5) -0.0018(5) P3 0.0202(7) 0.0180(7) 0.0182(6) 0.0015(5) 0.0018(5) -0.0017(5) C26 0.025(3) 0.037(3) 0.022(3) 0.001(2) 0.004(2) -0.003(2) C27 0.035(3) 0.041(4) 0.028(3) 0.000(3) 0.007(2) 0.003(3) C28 0.040(4) 0.055(4) 0.027(3) -0.009(3) 0.005(3) -0.001(3) C29 0.046(4) 0.069(5) 0.022(3) 0.005(3) 0.001(3) 0.010(3) C30 0.055(5) 0.057(5) 0.030(3) 0.011(3) 0.007(3) 0.011(4) C31 0.038(3) 0.042(4) 0.023(3) 0.008(2) 0.004(2) 0.005(3) C32 0.026(3) 0.031(3) 0.019(3) 0.004(2) 0.002(2) -0.001(2) C33 0.025(3) 0.034(3) 0.035(3) -0.003(2) 0.003(2) -0.006(2) C34 0.036(3) 0.038(4) 0.042(4) -0.010(3) 0.008(3) 0.006(3) C35 0.034(3) 0.052(4) 0.040(4) 0.007(3) 0.016(3) 0.009(3) C36 0.027(3) 0.049(4) 0.036(3) 0.010(3) 0.005(3) -0.004(3) C37 0.028(3) 0.030(3) 0.031(3) 0.004(2) 0.005(2) -0.006(2) C38 0.035(3) 0.021(3) 0.020(3) 0.003(2) 0.003(2) -0.005(2) C39 0.032(3) 0.021(3) 0.023(3) 0.005(2) 0.000(2) -0.009(2) C40 0.026(3) 0.028(3) 0.024(3) 0.000(2) 0.001(2) -0.001(2) C41 0.026(3) 0.023(3) 0.026(3) -0.001(2) 0.000(2) 0.003(2) C42 0.024(3) 0.026(3) 0.017(2) 0.005(2) 0.000(2) -0.002(2) C43 0.029(3) 0.032(3) 0.023(3) 0.005(2) 0.006(2) 0.004(2) C44 0.031(3) 0.043(4) 0.027(3) 0.005(2) 0.007(2) 0.006(3) C45 0.028(3) 0.051(4) 0.030(3) 0.010(3) 0.008(2) -0.004(3) C46 0.035(3) 0.031(3) 0.041(4) 0.008(3) 0.006(3) -0.008(3) C47 0.024(3) 0.029(3) 0.033(3) 0.004(2) 0.006(2) -0.001(2) C48 0.021(3) 0.023(3) 0.023(3) 0.010(2) 0.003(2) 0.003(2) C49 0.036(3) 0.023(3) 0.022(3) 0.002(2) -0.002(2) 0.002(2) C50 0.040(3) 0.027(3) 0.029(3) 0.010(2) 0.001(2) 0.006(2) C51 0.038(3) 0.036(3) 0.025(3) 0.009(2) 0.000(2) 0.002(3) C52 0.031(3) 0.035(3) 0.024(3) 0.001(2) 0.000(2) 0.002(2) C53 0.031(3) 0.028(3) 0.024(3) 0.001(2) 0.003(2) 0.001(2) C54 0.031(3) 0.013(2) 0.027(3) 0.003(2) 0.001(2) 0.001(2) O1 0.043(3) 0.037(3) 0.053(3) 0.006(2) 0.003(2) 0.010(2) C55 0.034(3) 0.015(3) 0.035(3) 0.005(2) 0.008(3) -0.001(2) O2 0.046(3) 0.031(2) 0.037(2) -0.011(2) -0.003(2) -0.002(2) C56 0.024(3) 0.022(3) 0.037(3) 0.003(2) -0.005(2) 0.004(2) O3 0.039(3) 0.056(3) 0.040(3) 0.027(2) 0.009(2) -0.008(2) C57 0.047(5) 0.091(8) 0.112(9) -0.046(7) 0.046(6) -0.022(5) F1 0.036(3) 0.239(12) 0.172(9) -0.065(8) 0.005(4) -0.005(5) F2 0.146(7) 0.095(5) 0.102(5) -0.012(4) 0.083(5) -0.056(5) F3 0.116(7) 0.164(9) 0.216(11) -0.104(8) 0.104(7) -0.007(6) S 0.0451(10) 0.0257(8) 0.0596(11) -0.0036(7) 0.0064(8) -0.0004(7) O4 0.071(4) 0.037(3) 0.065(4) 0.002(2) 0.032(3) -0.005(3) O5 0.066(4) 0.107(6) 0.072(4) -0.011(4) 0.004(3) -0.028(4) O6 0.188(11) 0.061(5) 0.138(8) 0.026(5) 0.013(7) 0.059(6) C58 0.064(5) 0.031(4) 0.047(4) 0.014(3) 0.007(4) -0.006(3) C59 0.071(5) 0.028(4) 0.046(4) 0.013(3) 0.003(4) -0.013(3) C60 0.050(4) 0.034(4) 0.049(4) 0.004(3) 0.001(3) -0.012(3) C61 0.062(5) 0.031(4) 0.043(4) 0.001(3) 0.008(3) -0.017(3) C62 0.057(4) 0.021(3) 0.052(4) 0.005(3) -0.006(3) -0.015(3) C63 0.057(4) 0.031(4) 0.047(4) 0.009(3) 0.001(3) -0.007(3) C64 0.064(5) 0.036(4) 0.044(4) 0.011(3) 0.005(3) -0.006(3) O7 0.061(4) 0.065(4) 0.055(3) 0.023(3) 0.001(3) 0.001(3) O8 0.073(4) 0.058(4) 0.042(3) 0.016(3) -0.003(3) 0.006(3) N3 0.073(5) 0.069(5) 0.064(5) 0.005(4) 0.007(4) -0.004(4) N4 0.069(4) 0.039(4) 0.042(3) 0.007(3) -0.003(3) -0.013(3) C65 0.220(17) 0.150(17) 0.28(2) 0.010(14) 0.127(16) 0.090(14) C66 0.199(17) 0.16(2) 0.28(2) 0.010(16) 0.129(17) 0.089(15) C67 0.192(16) 0.161(19) 0.28(2) 0.014(15) 0.130(16) 0.071(15) C68 0.194(17) 0.18(2) 0.28(2) 0.019(16) 0.127(17) 0.034(17) C69 0.189(16) 0.20(2) 0.30(2) 0.012(16) 0.111(16) 0.036(15) C66' 0.211(19) 0.18(2) 0.28(2) 0.009(16) 0.125(17) 0.051(17) C67' 0.199(17) 0.17(2) 0.29(2) 0.015(15) 0.126(17) 0.045(15) C68' 0.189(17) 0.19(2) 0.28(2) 0.015(17) 0.126(17) 0.043(17) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -5.2083 5.8923 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 '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 P1 Re P2 81.44(5) P1 Re P3 91.64(4) P1 Re C54 91.25(17) P1 Re C55 96.49(17) P1 Re C56 167.69(18) P2 Re P3 81.11(4) P2 Re C54 95.05(17) P2 Re C55 173.27(17) P2 Re C56 86.79(18) P3 Re C54 174.80(17) P3 Re C55 92.58(18) P3 Re C56 90.10(17) C54 Re C55 91.4(2) C54 Re C56 86.2(2) C55 Re C56 95.6(2) N1 B N2 105.3(4) N1 B C18 109.9(5) N1 B C19 108.3(5) N2 B C18 109.4(5) N2 B C19 107.6(5) C18 B C19 115.8(5) B N1 C1 126.7(5) B N1 C4 125.5(5) C1 N1 C4 107.7(5) B N2 C6 125.6(5) B N2 C9 127.2(5) C6 N2 C9 106.9(5) N1 C1 C2 110.5(5) N1 C1 C10 125.0(6) C2 C1 C10 124.5(6) C1 C2 C3 107.0(5) C1 C2 C11 125.1(6) C3 C2 C11 127.9(6) C2 C3 C4 106.8(5) C2 C3 C13 124.9(6) C4 C3 C13 128.2(6) N1 C4 C3 108.0(5) N1 C4 C5 120.6(5) C3 C4 C5 131.4(5) C4 C5 C6 123.2(5) C4 C5 C20 118.3(5) C6 C5 C20 118.5(5) N2 C6 C5 119.5(5) N2 C6 C7 108.7(5) C5 C6 C7 131.8(5) C6 C7 C8 106.6(5) C6 C7 C14 128.7(5) C8 C7 C14 124.6(5) C7 C8 C9 107.4(5) C7 C8 C15 126.5(6) C9 C8 C15 126.0(6) N2 C9 C8 110.4(5) N2 C9 C17 123.6(6) C8 C9 C17 126.0(6) C1 C10 H10A 109.5 C1 C10 H10B 109.5 C1 C10 H10C 109.5 H10A C10 H10B 109.5 H10A C10 H10C 109.5 H10B C10 H10C 109.5 C2 C11 H11A 109.0 C2 C11 H11B 109.0 C2 C11 C12 112.7(6) H11A C11 H11B 107.8 H11A C11 C12 109.0 H11B C11 C12 109.0 C11 C12 H12A 109.5 C11 C12 H12B 109.5 C11 C12 H12C 109.5 H12A C12 H12B 109.5 H12A C12 H12C 109.5 H12B C12 H12C 109.5 C3 C13 H13A 109.5 C3 C13 H13B 109.5 C3 C13 H13C 109.5 H13A C13 H13B 109.5 H13A C13 H13C 109.5 H13B C13 H13C 109.5 C7 C14 H14A 109.5 C7 C14 H14B 109.5 C7 C14 H14C 109.5 H14A C14 H14B 109.5 H14A C14 H14C 109.5 H14B C14 H14C 109.5 C8 C15 H15A 108.9 C8 C15 H15B 108.9 C8 C15 C16 113.4(6) H15A C15 H15B 107.7 H15A C15 C16 108.9 H15B C15 C16 108.9 C15 C16 H16A 109.5 C15 C16 H16B 109.5 C15 C16 H16C 109.5 H16A C16 H16B 109.5 H16A C16 H16C 109.5 H16B C16 H16C 109.5 C9 C17 H17A 109.5 C9 C17 H17B 109.5 C9 C17 H17C 109.5 H17A C17 H17B 109.5 H17A C17 H17C 109.5 H17B C17 H17C 109.5 B C18 H18A 109.5 B C18 H18B 109.5 B C18 H18C 109.5 H18A C18 H18B 109.5 H18A C18 H18C 109.5 H18B C18 H18C 109.5 B C19 H19A 109.5 B C19 H19B 109.5 B C19 H19C 109.5 H19A C19 H19B 109.5 H19A C19 H19C 109.5 H19B C19 H19C 109.5 C5 C20 C21 120.3(5) C5 C20 C25 119.2(5) C21 C20 C25 120.6(5) C20 C21 H21 120.4 C20 C21 C22 119.1(5) H21 C21 C22 120.4 C21 C22 H22 119.4 C21 C22 C23 121.2(5) H22 C22 C23 119.4 C22 C23 C24 119.0(5) C22 C23 P2 121.6(4) C24 C23 P2 119.3(4) C23 C24 H24 119.7 C23 C24 C25 120.6(5) H24 C24 C25 119.7 C20 C25 C24 119.4(5) C20 C25 H25 120.3 C24 C25 H25 120.3 Re P1 C26 119.76(19) Re P1 C32 116.06(19) Re P1 C38 107.03(18) C26 P1 C32 101.5(3) C26 P1 C38 106.1(3) C32 P1 C38 105.2(3) Re P2 C23 123.97(19) Re P2 C39 110.10(19) Re P2 C40 107.71(18) C23 P2 C39 104.2(3) C23 P2 C40 102.3(3) C39 P2 C40 107.4(3) Re P3 C41 108.78(18) Re P3 C42 115.23(18) Re P3 C48 121.15(18) C41 P3 C42 105.1(3) C41 P3 C48 104.5(3) C42 P3 C48 100.5(2) P1 C26 C27 118.8(5) P1 C26 C31 121.4(5) C27 C26 C31 119.8(6) C26 C27 H27 119.5 C26 C27 C28 121.0(6) H27 C27 C28 119.5 C27 C28 H28 120.3 C27 C28 C29 119.4(6) H28 C28 C29 120.3 C28 C29 H29 120.3 C28 C29 C30 119.3(6) H29 C29 C30 120.4 C29 C30 H30 119.1 C29 C30 C31 121.7(7) H30 C30 C31 119.1 C26 C31 C30 118.8(7) C26 C31 H31 120.6 C30 C31 H31 120.6 P1 C32 C33 118.4(4) P1 C32 C37 122.6(5) C33 C32 C37 118.8(6) C32 C33 H33 119.5 C32 C33 C34 120.9(6) H33 C33 C34 119.5 C33 C34 H34 120.0 C33 C34 C35 119.9(6) H34 C34 C35 120.0 C34 C35 H35 120.3 C34 C35 C36 119.5(6) H35 C35 C36 120.3 C35 C36 H36 119.6 C35 C36 C37 120.8(6) H36 C36 C37 119.6 C32 C37 C36 120.1(6) C32 C37 H37 120.0 C36 C37 H37 120.0 P1 C38 H38A 109.5 P1 C38 H38B 109.5 P1 C38 C39 110.5(4) H38A C38 H38B 108.1 H38A C38 C39 109.5 H38B C38 C39 109.5 P2 C39 C38 111.6(4) P2 C39 H39A 109.3 P2 C39 H39B 109.3 C38 C39 H39A 109.3 C38 C39 H39B 109.3 H39A C39 H39B 108.0 P2 C40 H40A 109.4 P2 C40 H40B 109.4 P2 C40 C41 111.1(4) H40A C40 H40B 108.0 H40A C40 C41 109.4 H40B C40 C41 109.4 P3 C41 C40 110.8(4) P3 C41 H41A 109.5 P3 C41 H41B 109.5 C40 C41 H41A 109.5 C40 C41 H41B 109.5 H41A C41 H41B 108.1 P3 C42 C43 120.7(4) P3 C42 C47 120.5(4) C43 C42 C47 118.7(5) C42 C43 H43 119.9 C42 C43 C44 120.2(6) H43 C43 C44 119.9 C43 C44 H44 119.6 C43 C44 C45 120.7(6) H44 C44 C45 119.6 C44 C45 H45 120.1 C44 C45 C46 119.8(6) H45 C45 C46 120.1 C45 C46 H46 120.2 C45 C46 C47 119.7(6) H46 C46 C47 120.2 C42 C47 C46 121.0(6) C42 C47 H47 119.5 C46 C47 H47 119.5 P3 C48 C49 121.8(4) P3 C48 C53 119.0(4) C49 C48 C53 119.1(5) C48 C49 H49 120.1 C48 C49 C50 119.9(5) H49 C49 C50 120.1 C49 C50 H50 119.7 C49 C50 C51 120.5(6) H50 C50 C51 119.7 C50 C51 H51 120.2 C50 C51 C52 119.7(5) H51 C51 C52 120.2 C51 C52 H52 119.7 C51 C52 C53 120.6(5) H52 C52 C53 119.7 C48 C53 C52 120.3(5) C48 C53 H53 119.9 C52 C53 H53 119.9 Re C54 O1 175.9(5) Re C55 O2 179.0(6) Re C56 O3 173.5(5) F1 C57 F2 104.1(10) F1 C57 F3 108.6(10) F1 C57 S 109.6(10) F2 C57 F3 106.8(13) F2 C57 S 113.7(8) F3 C57 S 113.4(8) C57 S O4 103.0(4) C57 S O5 102.2(5) C57 S O6 106.5(7) O4 S O5 116.5(5) O4 S O6 111.9(5) O5 S O6 114.8(6) C59 C58 O7 117.9(7) C59 C58 O8 120.4(8) O7 C58 O8 121.7(7) C58 C59 C60 121.8(8) C58 C59 C64 119.7(7) C60 C59 C64 118.2(7) C59 C60 H60 118.5 C59 C60 C61 122.9(8) H60 C60 C61 118.5 C60 C61 C62 118.4(7) C60 C61 N3 123.6(8) C62 C61 N3 117.6(7) C61 C62 C63 119.0(7) C61 C62 N4 120.7(8) C63 C62 N4 120.3(8) C62 C63 H63 119.8 C62 C63 C64 120.3(8) H63 C63 C64 119.9 C59 C64 C63 121.1(8) C59 C64 H64 119.5 C63 C64 H64 119.5 C58 O8 H8 109.5 C61 N3 H3A 120.0 C61 N3 H3B 120.0 H3A N3 H3B 120.0 C62 N4 H4A 120.0 C62 N4 H4B 120.0 H4A N4 H4B 120.0 H65A C65 H65B 109.5 H65A C65 H65C 109.5 H65A C65 C66 109.5 H65B C65 H65C 109.5 H65B C65 C66 109.5 H65C C65 C66 109.5 H65D C65 H65E 109.5 H65D C65 H65F 109.5 H65D C65 C66' 109.5 H65E C65 H65F 109.5 H65E C65 C66' 109.5 H65F C65 C66' 109.5 C65 C66 H66A 111.3 C65 C66 H66B 111.3 C65 C66 C67 102(2) H66A C66 H66B 109.2 H66A C66 C67 111.3 H66B C66 C67 111.3 C66 C67 H67A 106.2 C66 C67 H67B 106.2 C66 C67 C68 125(3) H67A C67 H67B 106.4 H67A C67 C68 106.2 H67B C67 C68 106.2 C67 C68 H68A 110.5 C67 C68 H68B 110.5 C67 C68 C69 106(2) H68A C68 H68B 108.7 H68A C68 C69 110.5 H68B C68 C69 110.5 C68 C69 H69A 109.5 C68 C69 H69B 109.5 C68 C69 H69C 109.5 H69A C69 H69B 109.5 H69A C69 H69C 109.5 H69B C69 H69C 109.5 H69D C69 H69E 109.5 H69D C69 H69F 109.5 H69D C69 C68' 109.5 H69E C69 H69F 109.5 H69E C69 C68' 109.5 H69F C69 C68' 109.5 C65 C66' H66C 110.6 C65 C66' H66D 110.6 C65 C66' C67' 106(2) H66C C66' H66D 108.7 H66C C66' C67' 110.6 H66D C66' C67' 110.6 C66' C67' H67C 106.0 C66' C67' H67D 106.0 C66' C67' C68' 125(3) H67C C67' H67D 106.3 H67C C67' C68' 106.0 H67D C67' C68' 106.0 C69 C68' C67' 102(2) C69 C68' H68C 111.4 C69 C68' H68D 111.4 C67' C68' H68C 111.4 C67' C68' H68D 111.4 H68C C68' H68D 109.3 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Re P1 2.4544(13) Re P2 2.4230(14) Re P3 2.4831(14) Re C54 1.926(6) Re C55 1.975(6) Re C56 1.944(6) B N1 1.588(8) B N2 1.583(8) B C18 1.641(8) B C19 1.616(9) N1 C1 1.340(8) N1 C4 1.398(7) N2 C6 1.409(7) N2 C9 1.350(8) C1 C2 1.423(9) C1 C10 1.496(8) C2 C3 1.378(9) C2 C11 1.497(9) C3 C4 1.441(8) C3 C13 1.501(8) C4 C5 1.379(8) C5 C6 1.397(8) C5 C20 1.499(7) C6 C7 1.417(8) C7 C8 1.390(9) C7 C14 1.490(8) C8 C9 1.409(9) C8 C15 1.502(9) C9 C17 1.499(8) C10 H10A 0.980 C10 H10B 0.980 C10 H10C 0.980 C11 H11A 0.990 C11 H11B 0.990 C11 C12 1.540(11) C12 H12A 0.980 C12 H12B 0.980 C12 H12C 0.980 C13 H13A 0.980 C13 H13B 0.980 C13 H13C 0.980 C14 H14A 0.980 C14 H14B 0.980 C14 H14C 0.980 C15 H15A 0.990 C15 H15B 0.990 C15 C16 1.534(10) C16 H16A 0.980 C16 H16B 0.980 C16 H16C 0.980 C17 H17A 0.980 C17 H17B 0.980 C17 H17C 0.980 C18 H18A 0.980 C18 H18B 0.980 C18 H18C 0.980 C19 H19A 0.980 C19 H19B 0.980 C19 H19C 0.980 C20 C21 1.391(8) C20 C25 1.396(9) C21 H21 0.950 C21 C22 1.394(8) C22 H22 0.950 C22 C23 1.389(8) C23 C24 1.395(8) C23 P2 1.809(5) C24 H24 0.950 C24 C25 1.394(8) C25 H25 0.950 P1 C26 1.825(6) P1 C32 1.821(6) P1 C38 1.840(6) P2 C39 1.831(5) P2 C40 1.836(6) P3 C41 1.852(6) P3 C42 1.831(5) P3 C48 1.820(5) C26 C27 1.388(9) C26 C31 1.395(9) C27 H27 0.950 C27 C28 1.385(9) C28 H28 0.950 C28 C29 1.407(11) C29 H29 0.950 C29 C30 1.372(12) C30 H30 0.950 C30 C31 1.396(9) C31 H31 0.950 C32 C33 1.392(9) C32 C37 1.390(8) C33 H33 0.950 C33 C34 1.391(9) C34 H34 0.950 C34 C35 1.381(10) C35 H35 0.950 C35 C36 1.385(11) C36 H36 0.950 C36 C37 1.389(10) C37 H37 0.950 C38 H38A 0.990 C38 H38B 0.990 C38 C39 1.538(7) C39 H39A 0.990 C39 H39B 0.990 C40 H40A 0.990 C40 H40B 0.990 C40 C41 1.530(7) C41 H41A 0.990 C41 H41B 0.990 C42 C43 1.394(8) C42 C47 1.390(8) C43 H43 0.950 C43 C44 1.384(8) C44 H44 0.950 C44 C45 1.378(10) C45 H45 0.950 C45 C46 1.384(10) C46 H46 0.950 C46 C47 1.387(9) C47 H47 0.950 C48 C49 1.402(8) C48 C53 1.387(8) C49 H49 0.950 C49 C50 1.395(8) C50 H50 0.950 C50 C51 1.381(9) C51 H51 0.950 C51 C52 1.376(9) C52 H52 0.950 C52 C53 1.397(8) C53 H53 0.950 C54 O1 1.147(7) C55 O2 1.115(7) C56 O3 1.152(8) C57 F1 1.359(15) C57 F2 1.275(16) C57 F3 1.293(11) C57 S 1.808(10) S O4 1.417(6) S O5 1.399(7) S O6 1.443(8) C58 C59 1.474(11) C58 O7 1.284(10) C58 O8 1.260(10) C59 C60 1.382(11) C59 C64 1.378(12) C60 H60 0.950 C60 C61 1.383(11) C61 C62 1.417(12) C61 N3 1.368(11) C62 C63 1.394(11) C62 N4 1.379(10) C63 H63 0.950 C63 C64 1.395(11) C64 H64 0.950 O8 H8 0.840 N3 H3A 0.880 N3 H3B 0.880 N4 H4A 0.880 N4 H4B 0.880 C65 H65A 0.980 C65 H65B 0.980 C65 H65C 0.980 C65 H65D 0.980 C65 H65E 0.980 C65 H65F 0.980 C65 C66 1.42(3) C65 C66' 1.43(3) C66 H66A 0.990 C66 H66B 0.990 C66 C67 1.69(3) C67 H67A 0.990 C67 H67B 0.990 C67 C68 1.67(3) C68 H68A 0.990 C68 H68B 0.990 C68 C69 1.42(3) C69 H69A 0.980 C69 H69B 0.980 C69 H69C 0.980 C69 H69D 0.980 C69 H69E 0.980 C69 H69F 0.980 C69 C68' 1.43(3) C66' H66C 0.990 C66' H66D 0.990 C66' C67' 1.68(3) C67' H67C 0.990 C67' H67D 0.990 C67' C68' 1.69(3) C68' H68C 0.990 C68' H68D 0.990 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 O8 H8 O7 0.84 1.89 2.661(8) 151.6 2_565 N4 H4A O5 0.88 2.39 3.195(12) 153.2 1_655 N4 H4B O4 0.88 2.30 3.068(9) 145.0 2_566 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 N2 B N1 C1 -179.7(5) N2 B N1 C4 5.4(8) C18 B N1 C1 -61.9(8) C18 B N1 C4 123.1(6) C19 B N1 C1 65.4(8) C19 B N1 C4 -109.5(6) N1 B N2 C6 -7.1(7) N1 B N2 C9 179.6(5) C18 B N2 C6 -125.1(6) C18 B N2 C9 61.5(8) C19 B N2 C6 108.3(6) C19 B N2 C9 -65.1(7) B N1 C1 C2 -176.5(6) B N1 C1 C10 1.3(10) C4 N1 C1 C2 -0.8(7) C4 N1 C1 C10 177.0(6) N1 C1 C2 C3 0.7(8) N1 C1 C2 C11 -179.1(6) C10 C1 C2 C3 -177.1(6) C10 C1 C2 C11 3.1(11) C1 C2 C3 C4 -0.3(7) C1 C2 C3 C13 -178.9(7) C11 C2 C3 C4 179.5(6) C11 C2 C3 C13 0.9(11) B N1 C4 C3 176.3(5) B N1 C4 C5 -1.5(9) C1 N1 C4 C3 0.6(7) C1 N1 C4 C5 -177.2(5) C2 C3 C4 N1 -0.2(7) C2 C3 C4 C5 177.3(6) C13 C3 C4 N1 178.4(7) C13 C3 C4 C5 -4.2(12) N1 C4 C5 C6 -2.1(9) N1 C4 C5 C20 179.8(5) C3 C4 C5 C6 -179.3(6) C3 C4 C5 C20 2.5(10) C4 C5 C6 N2 0.5(9) C4 C5 C6 C7 -180.0(6) C20 C5 C6 N2 178.6(5) C20 C5 C6 C7 -1.8(10) B N2 C6 C5 4.8(8) B N2 C6 C7 -174.8(5) C9 N2 C6 C5 179.3(5) C9 N2 C6 C7 -0.3(6) N2 C6 C7 C8 0.2(7) N2 C6 C7 C14 178.0(6) C5 C6 C7 C8 -179.4(6) C5 C6 C7 C14 -1.6(11) C6 C7 C8 C9 0.0(7) C6 C7 C8 C15 -179.2(6) C14 C7 C8 C9 -177.9(6) C14 C7 C8 C15 2.8(11) B N2 C9 C8 174.7(5) B N2 C9 C17 -4.7(10) C6 N2 C9 C8 0.3(7) C6 N2 C9 C17 -179.1(6) C7 C8 C9 N2 -0.2(7) C7 C8 C9 C17 179.2(6) C15 C8 C9 N2 179.0(6) C15 C8 C9 C17 -1.6(11) C1 C2 C11 C12 94.4(8) C3 C2 C11 C12 -85.4(9) C7 C8 C15 C16 77.8(9) C9 C8 C15 C16 -101.3(8) C4 C5 C20 C21 90.4(7) C4 C5 C20 C25 -88.4(7) C6 C5 C20 C21 -87.8(7) C6 C5 C20 C25 93.4(7) C5 C20 C21 C22 -178.0(5) C25 C20 C21 C22 0.7(9) C20 C21 C22 C23 1.0(9) C21 C22 C23 C24 -1.2(9) C21 C22 C23 P2 179.3(4) C22 C23 C24 C25 -0.2(9) P2 C23 C24 C25 179.3(5) C23 C24 C25 C20 1.8(10) C5 C20 C25 C24 176.6(6) C21 C20 C25 C24 -2.1(10) C22 C23 P2 Re 4.1(6) C22 C23 P2 C39 -122.6(5) C22 C23 P2 C40 125.6(5) C24 C23 P2 Re -175.4(4) C24 C23 P2 C39 57.9(5) C24 C23 P2 C40 -53.9(5) Re P1 C26 C27 -58.0(5) Re P1 C26 C31 124.2(5) C32 P1 C26 C27 71.2(5) C32 P1 C26 C31 -106.6(5) C38 P1 C26 C27 -179.1(5) C38 P1 C26 C31 3.1(6) P1 C26 C27 C28 -177.8(5) C31 C26 C27 C28 0.0(9) C26 C27 C28 C29 0.3(10) C27 C28 C29 C30 -0.5(11) C28 C29 C30 C31 0.5(11) P1 C26 C31 C30 177.8(5) C27 C26 C31 C30 0.0(9) C29 C30 C31 C26 -0.3(11) Re P1 C32 C33 50.0(5) Re P1 C32 C37 -135.6(4) C26 P1 C32 C33 -81.6(5) C26 P1 C32 C37 92.8(5) C38 P1 C32 C33 168.1(4) C38 P1 C32 C37 -17.6(5) P1 C32 C33 C34 173.8(5) C37 C32 C33 C34 -0.8(9) C32 C33 C34 C35 1.3(10) C33 C34 C35 C36 -0.8(10) C34 C35 C36 C37 -0.1(10) C35 C36 C37 C32 0.6(10) P1 C32 C37 C36 -174.5(5) C33 C32 C37 C36 -0.1(9) Re P1 C38 C39 43.5(4) C26 P1 C38 C39 172.4(4) C32 P1 C38 C39 -80.5(4) P1 C38 C39 P2 -48.2(5) Re P2 C39 C38 30.5(5) C23 P2 C39 C38 165.4(4) C40 P2 C39 C38 -86.5(5) Re P2 C40 C41 -46.2(4) C23 P2 C40 C41 -178.3(4) C39 P2 C40 C41 72.4(4) P2 C40 C41 P3 49.2(5) Re P3 C41 C40 -29.7(4) C42 P3 C41 C40 94.2(4) C48 P3 C41 C40 -160.4(4) Re P3 C42 C43 158.1(4) Re P3 C42 C47 -27.0(5) C41 P3 C42 C43 38.4(5) C41 P3 C42 C47 -146.7(4) C48 P3 C42 C43 -70.0(5) C48 P3 C42 C47 105.0(5) P3 C42 C43 C44 175.8(4) C47 C42 C43 C44 0.7(8) C42 C43 C44 C45 -0.2(9) C43 C44 C45 C46 -0.4(9) C44 C45 C46 C47 0.3(10) C45 C46 C47 C42 0.2(9) P3 C42 C47 C46 -175.8(5) C43 C42 C47 C46 -0.8(8) Re P3 C48 C49 -133.0(4) Re P3 C48 C53 52.1(5) C41 P3 C48 C49 -9.9(5) C41 P3 C48 C53 175.2(4) C42 P3 C48 C49 98.8(5) C42 P3 C48 C53 -76.1(5) P3 C48 C49 C50 -174.6(5) C53 C48 C49 C50 0.3(9) C48 C49 C50 C51 -0.4(9) C49 C50 C51 C52 0.6(10) C50 C51 C52 C53 -0.7(9) P3 C48 C53 C52 174.7(4) C49 C48 C53 C52 -0.4(8) C51 C52 C53 C48 0.6(9) F1 C57 S O4 60.7(10) F1 C57 S O5 -178.1(9) F1 C57 S O6 -57.2(10) F2 C57 S O4 -55.3(9) F2 C57 S O5 65.9(9) F2 C57 S O6 -173.3(9) F3 C57 S O4 -177.7(12) F3 C57 S O5 -56.5(14) F3 C57 S O6 64.4(14) O7 C58 C59 C60 6.2(10) O7 C58 C59 C64 179.9(7) O8 C58 C59 C60 -171.9(7) O8 C58 C59 C64 1.9(10) C58 C59 C60 C61 171.0(7) C64 C59 C60 C61 -2.8(11) C59 C60 C61 C62 0.9(11) C59 C60 C61 N3 -171.9(7) C60 C61 C62 C63 1.7(10) C60 C61 C62 N4 -179.1(6) N3 C61 C62 C63 175.1(7) N3 C61 C62 N4 -5.8(10) C61 C62 C63 C64 -2.5(10) N4 C62 C63 C64 178.3(6) C58 C59 C64 C63 -171.9(7) C60 C59 C64 C63 2.0(11) C62 C63 C64 C59 0.6(11) C66' C65 C66 C67 60(4) C65 C66 C67 C68 -147(5) C66 C67 C68 C69 -157(5) C67 C68 C69 C68' 65(4) C66 C65 C66' C67' -75(4) C65 C66' C67' C68' 145(5) C68 C69 C68' C67' -67(4) C66' C67' C68' C69 133(6)