#------------------------------------------------------------------------------ #$Date: 2014-12-22 15:48:03 +0200 (Mon, 22 Dec 2014) $ #$Revision: 128995 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/11/60/7116062.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_7116062 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 'C37 H33 O3 P3 Re +, C F3 O3 S-' _chemical_formula_sum 'C38 H33 F3 O6 P3 Re S' _chemical_formula_weight 953.81 _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 97.774(4) _cell_angle_beta 96.016(3) _cell_angle_gamma 112.238(4) _cell_formula_units_Z 2 _cell_length_a 10.1353(3) _cell_length_b 11.9377(5) _cell_length_c 16.5611(8) _cell_measurement_reflns_used 6521 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 28.4844 _cell_measurement_theta_min 3.3613 _cell_volume 1810.90(14) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _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 0.996 _diffrn_measured_fraction_theta_max 0.816 _diffrn_measurement_device_type 'Agilent Technologies Gemini A Ultra' _diffrn_measurement_method '\w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0438 _diffrn_reflns_av_unetI/netI 0.0571 _diffrn_reflns_laue_measured_fraction_full 0.996 _diffrn_reflns_laue_measured_fraction_max 0.816 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 15057 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.816 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.547 _diffrn_reflns_theta_min 3.368 _diffrn_source 'sealed tube with Enhance optics' _exptl_absorpt_coefficient_mu 3.608 _exptl_absorpt_correction_T_max 0.715 _exptl_absorpt_correction_T_min 0.310 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.749 _exptl_crystal_density_method 'not measured' _exptl_crystal_description rod _exptl_crystal_F_000 944 _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _refine_diff_density_max 1.787 _refine_diff_density_min -1.878 _refine_diff_density_rms 0.145 _refine_ls_extinction_coef 0.0008(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 525 _refine_ls_number_reflns 7542 _refine_ls_number_restraints 339 _refine_ls_restrained_S_all 1.153 _refine_ls_R_factor_all 0.0428 _refine_ls_R_factor_gt 0.0376 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0341P)^2^+5.7731P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0874 _refine_ls_wR_factor_ref 0.0924 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6893 _reflns_number_total 7542 _reflns_threshold_expression 'I > 2\s(I)' _[local]_cod_data_source_file c4cc06367h2.cif _[local]_cod_data_source_block ljh120152 _cod_database_code 7116062 _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 0.313 _shelx_estimated_absorpt_t_max 0.714 _shelxl_version_number 2014-3 _shelx_res_file ; TITL ljh120152 in P-1 CELL 0.71073 10.1353 11.9377 16.5611 97.774 96.016 112.238 ZERR 2.00 0.0003 0.0005 0.0008 0.004 0.003 0.004 LATT 1 SFAC C H O F P S RE UNIT 76 66 12 6 6 2 2 REM colourless rod SIZE 0.42 0.12 0.10 TEMP -123 L.S. 8 ACTA BOND $H CONF FMAP 2 PLAN 10 WGHT 0.034100 5.773100 EXTI 0.000755 FVAR 0.27558 0.48905 RE 7 0.719652 0.520095 0.315388 11.00000 0.01755 0.01204 = 0.02008 -0.00119 0.00199 0.00585 P1 5 0.506185 0.546801 0.249615 11.00000 0.01956 0.01443 = 0.02449 -0.00027 0.00102 0.00727 P2 5 0.752720 0.482982 0.172399 11.00000 0.02144 0.01616 = 0.02249 0.00120 0.00490 0.00672 P3 5 0.605818 0.292832 0.286108 11.00000 0.02052 0.01282 = 0.01893 -0.00071 0.00313 0.00731 C1 1 0.472963 0.678761 0.297556 11.00000 0.02245 0.01860 = 0.03614 -0.00166 0.00070 0.01031 C2 1 0.432234 0.748711 0.246992 11.00000 0.05936 0.03893 = 0.03643 -0.00548 -0.00635 0.03385 AFIX 43 H2 2 0.428138 0.731103 0.188877 11.00000 -1.20000 AFIX 0 C3 1 0.397761 0.844161 0.282188 11.00000 0.07623 0.04296 = 0.05190 -0.00159 -0.00765 0.04308 AFIX 43 H3 2 0.367558 0.890608 0.247815 11.00000 -1.20000 AFIX 0 C4 1 0.407044 0.872209 0.366988 11.00000 0.04642 0.02737 = 0.04593 -0.00052 0.00564 0.02338 AFIX 43 H4 2 0.381210 0.936317 0.390901 11.00000 -1.20000 AFIX 0 C5 1 0.453539 0.806988 0.415642 11.00000 0.07506 0.04848 = 0.03134 -0.00038 0.01354 0.04293 AFIX 43 H5 2 0.463579 0.827521 0.474051 11.00000 -1.20000 AFIX 0 C6 1 0.486528 0.710321 0.380426 11.00000 0.05465 0.04283 = 0.03259 0.00892 0.01168 0.03656 AFIX 43 H6 2 0.519175 0.665694 0.415252 11.00000 -1.20000 AFIX 0 C7 1 0.325476 0.422326 0.229077 11.00000 0.01895 0.01727 = 0.02867 0.00038 0.00243 0.00873 C8 1 0.263983 0.349781 0.150913 11.00000 0.02291 0.02286 = 0.03565 -0.00024 0.00647 0.00971 AFIX 43 H8 2 0.315758 0.365011 0.106197 11.00000 -1.20000 AFIX 0 C9 1 0.127933 0.255629 0.137922 11.00000 0.02482 0.02619 = 0.03480 -0.00864 -0.00186 0.00721 AFIX 43 H9 2 0.086385 0.206717 0.084285 11.00000 -1.20000 AFIX 0 C10 1 0.051769 0.232287 0.203008 11.00000 0.02200 0.02757 = 0.03884 0.00332 0.00184 0.00942 AFIX 43 H10 2 -0.040602 0.166153 0.194528 11.00000 -1.20000 AFIX 0 C11 1 0.111337 0.305799 0.279801 11.00000 0.02500 0.02793 = 0.04124 0.00637 0.00993 0.01068 AFIX 43 H11 2 0.058250 0.292012 0.324074 11.00000 -1.20000 AFIX 0 C12 1 0.247790 0.399651 0.293289 11.00000 0.02923 0.02742 = 0.02531 -0.00284 0.00085 0.01311 AFIX 43 H12 2 0.288436 0.448834 0.346922 11.00000 -1.20000 AFIX 0 C13 1 0.545562 0.581558 0.148008 11.00000 0.02503 0.01899 = 0.02945 0.00781 0.00297 0.00772 AFIX 23 H13A 2 0.454922 0.571723 0.113133 11.00000 -1.20000 H13B 2 0.613798 0.668758 0.155287 11.00000 -1.20000 AFIX 0 C14 1 0.610153 0.500105 0.103080 11.00000 0.02331 0.02443 = 0.02176 0.00210 0.00210 0.00634 AFIX 23 H14A 2 0.651248 0.536555 0.056458 11.00000 -1.20000 H14B 2 0.532709 0.417761 0.079969 11.00000 -1.20000 AFIX 0 C15 1 0.918049 0.573492 0.138397 11.00000 0.02601 0.02334 = 0.02079 0.00357 0.00586 0.00576 C16 1 0.940214 0.691665 0.127822 11.00000 0.02833 0.02887 = 0.04200 0.00626 0.01595 0.00622 AFIX 43 H16 2 0.871490 0.724621 0.140857 11.00000 -1.20000 AFIX 0 C17 1 1.061866 0.762753 0.098348 11.00000 0.04145 0.03555 = 0.03442 0.00640 0.01351 0.00430 AFIX 43 H17 2 1.075442 0.843505 0.090484 11.00000 -1.20000 AFIX 0 C18 1 1.162568 0.716290 0.080565 11.00000 0.02494 0.05423 = 0.02790 0.00699 0.00589 0.00172 AFIX 43 H18 2 1.246586 0.765275 0.061108 11.00000 -1.20000 AFIX 0 C19 1 1.141751 0.598748 0.090935 11.00000 0.02745 0.06549 = 0.05986 0.01519 0.01104 0.02260 AFIX 43 H19 2 1.211028 0.566454 0.077884 11.00000 -1.20000 AFIX 0 C20 1 1.019540 0.526497 0.120508 11.00000 0.02832 0.03952 = 0.04952 0.01180 0.00892 0.01478 AFIX 43 H20 2 1.006172 0.445750 0.128283 11.00000 -1.20000 AFIX 0 C21 1 0.722298 0.320307 0.142705 11.00000 0.03416 0.02115 = 0.02174 -0.00111 0.00673 0.01446 AFIX 23 H21A 2 0.707940 0.296923 0.081759 11.00000 -1.20000 H21B 2 0.807433 0.306709 0.166671 11.00000 -1.20000 AFIX 0 C22 1 0.589240 0.242341 0.174571 11.00000 0.02721 0.01543 = 0.02323 -0.00265 0.00158 0.00799 AFIX 23 H22A 2 0.576253 0.154907 0.162985 11.00000 -1.20000 H22B 2 0.502752 0.248643 0.145274 11.00000 -1.20000 AFIX 0 C23 1 0.710667 0.218421 0.336853 11.00000 0.02138 0.01659 = 0.02615 0.00446 0.00695 0.00860 C24 1 0.717518 0.111556 0.297269 11.00000 0.02986 0.01961 = 0.03182 0.00083 0.00671 0.01241 AFIX 43 H24 2 0.675053 0.079712 0.240708 11.00000 -1.20000 AFIX 0 C25 1 0.786520 0.050183 0.339985 11.00000 0.04441 0.02806 = 0.04045 0.00542 0.00662 0.02683 AFIX 43 H25 2 0.792721 -0.022238 0.312216 11.00000 -1.20000 AFIX 0 C26 1 0.845553 0.094819 0.422421 11.00000 0.03708 0.04120 = 0.04252 0.01896 0.01309 0.02642 AFIX 43 H26 2 0.890864 0.052248 0.451794 11.00000 -1.20000 AFIX 0 C27 1 0.839029 0.200696 0.462205 11.00000 0.04015 0.04339 = 0.02752 0.00713 0.00279 0.02496 AFIX 43 H27 2 0.879001 0.230926 0.519206 11.00000 -1.20000 AFIX 0 C28 1 0.774011 0.263678 0.419172 11.00000 0.03981 0.02663 = 0.03098 -0.00027 0.00368 0.01859 AFIX 43 H28 2 0.772986 0.338561 0.446489 11.00000 -1.20000 AFIX 0 C29 1 0.427694 0.207894 0.310959 11.00000 0.01947 0.01560 = 0.02923 0.00306 0.00267 0.00829 C30 1 0.402660 0.234282 0.390498 11.00000 0.03002 0.01764 = 0.03369 -0.00072 0.00861 0.00486 AFIX 43 H30 2 0.474161 0.301887 0.428878 11.00000 -1.20000 AFIX 0 C31 1 0.277023 0.164935 0.414900 11.00000 0.03461 0.02486 = 0.03676 0.00052 0.01565 0.00651 AFIX 43 H31 2 0.262131 0.184067 0.469875 11.00000 -1.20000 AFIX 0 C32 1 0.171933 0.067100 0.359469 11.00000 0.02780 0.02089 = 0.05015 0.00755 0.01520 0.00868 AFIX 43 H32 2 0.084873 0.018374 0.376363 11.00000 -1.20000 AFIX 0 C33 1 0.193139 0.040497 0.280594 11.00000 0.02222 0.02334 = 0.04835 -0.00257 0.00050 0.00389 AFIX 43 H33 2 0.119966 -0.026320 0.242486 11.00000 -1.20000 AFIX 0 C34 1 0.320141 0.109680 0.255210 11.00000 0.02757 0.02008 = 0.03169 -0.00204 0.00248 0.00737 AFIX 43 H34 2 0.333919 0.090288 0.200019 11.00000 -1.20000 AFIX 0 C35 1 0.907166 0.516040 0.352939 11.00000 0.02519 0.01615 = 0.03133 -0.00458 0.00533 0.00814 O1 3 1.020597 0.522268 0.375772 11.00000 0.02808 0.03942 = 0.05837 -0.00390 -0.00403 0.01784 C36 1 0.678675 0.531389 0.429245 11.00000 0.01928 0.01418 = 0.03602 0.00517 0.00140 0.00708 O2 3 0.660956 0.538461 0.494884 11.00000 0.05597 0.03627 = 0.02184 0.00233 0.01294 0.02187 C37 1 0.818500 0.699031 0.329698 11.00000 0.02231 0.03018 = 0.03142 0.00454 0.00386 0.01225 O3 3 0.878741 0.801939 0.338761 11.00000 0.03602 0.01246 = 0.07827 0.00106 0.00227 0.00083 C38 1 0.265814 0.023491 -0.023954 11.00000 0.06375 0.05853 = 0.04692 -0.01501 0.00484 0.02100 S 6 0.357467 0.135726 -0.070818 11.00000 0.08544 0.07226 = 0.05675 0.01740 -0.00143 0.00178 PART 1 F1 4 0.295618 0.042450 0.055439 21.00000 0.07799 0.09005 = 0.04360 -0.01517 0.02035 -0.02168 F2 4 0.120403 0.008218 -0.035758 21.00000 0.06932 0.10541 = 0.11735 -0.04977 -0.01508 0.02543 F3 4 0.255654 -0.085647 -0.057579 21.00000 0.11134 0.06633 = 0.04637 -0.01322 -0.01774 0.04574 O4 3 0.498963 0.148041 -0.061545 21.00000 0.05434 0.16096 = 0.08750 0.06056 0.00095 0.01988 O5 3 0.340767 0.245591 -0.016394 21.00000 0.08491 0.03542 = 0.03687 -0.00142 -0.00387 -0.00959 O6 3 0.265112 0.108929 -0.150435 21.00000 0.08047 0.02709 = 0.02707 0.00430 0.00747 0.02236 PART 2 F1' 4 0.347271 0.017808 0.047178 -21.00000 0.09770 0.05398 = 0.04651 0.00934 -0.00250 0.00072 F2' 4 0.152079 0.028819 0.004360 -21.00000 0.12614 0.10796 = 0.09951 0.03972 0.07207 0.07016 F3' 4 0.222580 -0.090211 -0.066785 -21.00000 0.05230 0.04636 = 0.04005 -0.00542 -0.01525 0.01800 O4' 3 0.462421 0.073220 -0.105428 -21.00000 0.04816 0.07414 = 0.06221 0.02031 0.00736 -0.00736 O5' 3 0.446197 0.240384 -0.017071 -21.00000 0.14917 0.04106 = 0.04142 0.01477 -0.03528 -0.02112 O6' 3 0.246891 0.122254 -0.138209 -21.00000 0.15474 0.11419 = 0.08241 -0.03939 -0.04777 0.07643 SADI C38 F1 C38 F2 C38 F3 C38 F1' C38 F2' C38 F3' SADI S O4 S O5 S O6 S O4' S O5' S O6' SADI F1 F2 F2 F3 F3 F1 F1' F2' F2' F3' F3' F1' SADI O4 O5 O5 O6 O6 O4 O4' O5' O5' O6' O6' O4' SADI C38 O4 C38 O5 C38 O6 C38 O4' C38 O5' C38 O6' SADI S F1 S F2 S F3 S F1' S F2' S F3' SIMU C38 > O6' RIGU C38 > O6' HKLF 4 REM ljh120152 in P-1 REM R1 = 0.0376 for 6893 Fo > 4sig(Fo) and 0.0428 for all 7542 data REM 525 parameters refined using 339 restraints END WGHT 0.0321 6.0015 REM Highest difference peak 1.787, deepest hole -1.878, 1-sigma level 0.145 Q1 1 0.2976 0.0742 -0.0459 11.00000 0.05 1.79 Q2 1 0.2075 0.0969 -0.0785 11.00000 0.05 1.50 Q3 1 0.7647 0.4790 0.3299 11.00000 0.05 1.43 Q4 1 0.8367 0.4396 0.0532 11.00000 0.05 1.16 Q5 1 0.6657 0.5558 0.3039 11.00000 0.05 1.12 Q6 1 0.8171 0.5627 0.3160 11.00000 0.05 1.11 Q7 1 0.6983 0.5998 0.3547 11.00000 0.05 1.05 Q8 1 0.7508 0.4490 0.2718 11.00000 0.05 1.02 Q9 1 0.4869 0.2182 -0.0372 11.00000 0.05 1.00 Q10 1 0.2643 0.0979 0.0275 11.00000 0.05 0.95 ; _shelx_res_checksum 15416 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 0.71965(2) 0.52009(2) 0.31539(2) 0.01709(8) Uani 1 1 d . . . . . P1 P 0.50618(13) 0.54680(11) 0.24962(8) 0.0200(3) Uani 1 1 d . . . . . P2 P 0.75272(13) 0.48298(11) 0.17240(8) 0.0204(3) Uani 1 1 d . . . . . P3 P 0.60582(13) 0.29283(11) 0.28611(8) 0.0176(2) Uani 1 1 d . . . . . C1 C 0.4730(5) 0.6788(5) 0.2976(4) 0.0261(11) Uani 1 1 d . . . . . C2 C 0.4322(7) 0.7487(6) 0.2470(4) 0.0430(16) Uani 1 1 d . . . . . H2 H 0.4281 0.7311 0.1889 0.052 Uiso 1 1 calc R U . . . C3 C 0.3978(8) 0.8442(6) 0.2822(5) 0.0537(19) Uani 1 1 d . . . . . H3 H 0.3676 0.8906 0.2478 0.064 Uiso 1 1 calc R U . . . C4 C 0.4070(7) 0.8722(5) 0.3670(4) 0.0382(14) Uani 1 1 d . . . . . H4 H 0.3812 0.9363 0.3909 0.046 Uiso 1 1 calc R U . . . C5 C 0.4535(8) 0.8070(6) 0.4156(4) 0.0465(16) Uani 1 1 d . . . . . H5 H 0.4636 0.8275 0.4741 0.056 Uiso 1 1 calc R U . . . C6 C 0.4865(7) 0.7103(6) 0.3804(4) 0.0376(14) Uani 1 1 d . . . . . H6 H 0.5192 0.6657 0.4153 0.045 Uiso 1 1 calc R U . . . C7 C 0.3255(5) 0.4223(4) 0.2291(3) 0.0217(10) Uani 1 1 d . . . . . C8 C 0.2640(5) 0.3498(5) 0.1509(4) 0.0274(11) Uani 1 1 d . . . . . H8 H 0.3158 0.3650 0.1062 0.033 Uiso 1 1 calc R U . . . C9 C 0.1279(6) 0.2556(5) 0.1379(4) 0.0315(12) Uani 1 1 d . . . . . H9 H 0.0864 0.2067 0.0843 0.038 Uiso 1 1 calc R U . . . C10 C 0.0518(6) 0.2323(5) 0.2030(4) 0.0302(12) Uani 1 1 d . . . . . H10 H -0.0406 0.1662 0.1945 0.036 Uiso 1 1 calc R U . . . C11 C 0.1113(6) 0.3058(5) 0.2798(4) 0.0310(12) Uani 1 1 d . . . . . H11 H 0.0583 0.2920 0.3241 0.037 Uiso 1 1 calc R U . . . C12 C 0.2478(6) 0.3997(5) 0.2933(3) 0.0279(11) Uani 1 1 d . . . . . H12 H 0.2884 0.4488 0.3469 0.033 Uiso 1 1 calc R U . . . C13 C 0.5456(5) 0.5816(5) 0.1480(3) 0.0246(11) Uani 1 1 d . . . . . H13A H 0.4549 0.5717 0.1131 0.030 Uiso 1 1 calc R U . . . H13B H 0.6138 0.6688 0.1553 0.030 Uiso 1 1 calc R U . . . C14 C 0.6102(5) 0.5001(5) 0.1031(3) 0.0245(11) Uani 1 1 d . . . . . H14A H 0.6512 0.5366 0.0565 0.029 Uiso 1 1 calc R U . . . H14B H 0.5327 0.4178 0.0800 0.029 Uiso 1 1 calc R U . . . C15 C 0.9180(5) 0.5735(5) 0.1384(3) 0.0245(11) Uani 1 1 d . . . . . C16 C 0.9402(6) 0.6917(5) 0.1278(4) 0.0339(13) Uani 1 1 d . . . . . H16 H 0.8715 0.7246 0.1409 0.041 Uiso 1 1 calc R U . . . C17 C 1.0619(7) 0.7628(6) 0.0983(4) 0.0400(15) Uani 1 1 d . . . . . H17 H 1.0754 0.8435 0.0905 0.048 Uiso 1 1 calc R U . . . C18 C 1.1626(6) 0.7163(6) 0.0806(4) 0.0399(15) Uani 1 1 d . . . . . H18 H 1.2466 0.7653 0.0611 0.048 Uiso 1 1 calc R U . . . C19 C 1.1418(7) 0.5987(7) 0.0909(5) 0.0491(17) Uani 1 1 d . . . . . H19 H 1.2110 0.5665 0.0779 0.059 Uiso 1 1 calc R U . . . C20 C 1.0195(6) 0.5265(6) 0.1205(4) 0.0382(14) Uani 1 1 d . . . . . H20 H 1.0062 0.4458 0.1283 0.046 Uiso 1 1 calc R U . . . C21 C 0.7223(6) 0.3203(4) 0.1427(3) 0.0250(11) Uani 1 1 d . . . . . H21A H 0.7079 0.2969 0.0818 0.030 Uiso 1 1 calc R U . . . H21B H 0.8074 0.3067 0.1667 0.030 Uiso 1 1 calc R U . . . C22 C 0.5892(5) 0.2423(4) 0.1746(3) 0.0230(10) Uani 1 1 d . . . . . H22A H 0.5763 0.1549 0.1630 0.028 Uiso 1 1 calc R U . . . H22B H 0.5028 0.2486 0.1453 0.028 Uiso 1 1 calc R U . . . C23 C 0.7107(5) 0.2184(4) 0.3369(3) 0.0208(10) Uani 1 1 d . . . . . C24 C 0.7175(5) 0.1116(5) 0.2973(4) 0.0266(11) Uani 1 1 d . . . . . H24 H 0.6751 0.0797 0.2407 0.032 Uiso 1 1 calc R U . . . C25 C 0.7865(6) 0.0502(5) 0.3400(4) 0.0340(13) Uani 1 1 d . . . . . H25 H 0.7927 -0.0222 0.3122 0.041 Uiso 1 1 calc R U . . . C26 C 0.8456(6) 0.0948(6) 0.4224(4) 0.0354(13) Uani 1 1 d . . . . . H26 H 0.8909 0.0522 0.4518 0.042 Uiso 1 1 calc R U . . . C27 C 0.8390(6) 0.2007(6) 0.4622(4) 0.0347(13) Uani 1 1 d . . . . . H27 H 0.8790 0.2309 0.5192 0.042 Uiso 1 1 calc R U . . . C28 C 0.7740(6) 0.2637(5) 0.4192(4) 0.0316(12) Uani 1 1 d . . . . . H28 H 0.7730 0.3386 0.4465 0.038 Uiso 1 1 calc R U . . . C29 C 0.4277(5) 0.2079(4) 0.3110(3) 0.0213(10) Uani 1 1 d . . . . . C30 C 0.4027(6) 0.2343(5) 0.3905(4) 0.0289(12) Uani 1 1 d . . . . . H30 H 0.4742 0.3019 0.4289 0.035 Uiso 1 1 calc R U . . . C31 C 0.2770(6) 0.1649(5) 0.4149(4) 0.0335(13) Uani 1 1 d . . . . . H31 H 0.2621 0.1841 0.4699 0.040 Uiso 1 1 calc R U . . . C32 C 0.1719(6) 0.0671(5) 0.3595(4) 0.0325(13) Uani 1 1 d . . . . . H32 H 0.0849 0.0184 0.3764 0.039 Uiso 1 1 calc R U . . . C33 C 0.1931(6) 0.0405(5) 0.2806(4) 0.0343(13) Uani 1 1 d . . . . . H33 H 0.1200 -0.0263 0.2425 0.041 Uiso 1 1 calc R U . . . C34 C 0.3201(5) 0.1097(5) 0.2552(4) 0.0280(12) Uani 1 1 d . . . . . H34 H 0.3339 0.0903 0.2000 0.034 Uiso 1 1 calc R U . . . C35 C 0.9072(5) 0.5160(4) 0.3529(3) 0.0251(11) Uani 1 1 d . . . . . O1 O 1.0206(4) 0.5223(4) 0.3758(3) 0.0429(11) Uani 1 1 d . . . . . C36 C 0.6787(5) 0.5314(4) 0.4292(4) 0.0233(11) Uani 1 1 d . . . . . O2 O 0.6610(5) 0.5385(4) 0.4949(3) 0.0368(9) Uani 1 1 d . . . . . C37 C 0.8185(5) 0.6990(5) 0.3297(3) 0.0276(12) Uani 1 1 d . . . . . O3 O 0.8787(4) 0.8019(3) 0.3388(3) 0.0463(12) Uani 1 1 d . . . . . C38 C 0.2658(7) 0.0235(7) -0.0240(4) 0.0603(17) Uani 1 1 d D U . . . S S 0.3575(3) 0.1357(2) -0.07082(15) 0.0810(7) Uani 1 1 d D U . . . F1 F 0.2956(15) 0.0424(14) 0.0554(5) 0.089(5) Uani 0.489(14) 1 d D U P A 1 F2 F 0.1204(9) 0.0082(13) -0.0358(10) 0.110(5) Uani 0.489(14) 1 d D U P A 1 F3 F 0.2557(19) -0.0856(9) -0.0576(10) 0.076(5) Uani 0.489(14) 1 d D U P A 1 O4 O 0.4990(10) 0.1480(17) -0.0615(10) 0.105(5) Uani 0.489(14) 1 d D U P A 1 O5 O 0.3408(15) 0.2456(7) -0.0164(6) 0.065(3) Uani 0.489(14) 1 d D U P A 1 O6 O 0.2651(12) 0.1089(10) -0.1504(6) 0.045(3) Uani 0.489(14) 1 d D U P A 1 F1' F 0.3473(14) 0.0178(11) 0.0472(6) 0.076(4) Uani 0.511(14) 1 d D U P A 2 F2' F 0.1521(14) 0.0288(12) 0.0044(10) 0.098(4) Uani 0.511(14) 1 d D U P A 2 F3' F 0.2226(15) -0.0902(7) -0.0668(8) 0.050(3) Uani 0.511(14) 1 d D U P A 2 O4' O 0.4624(10) 0.0732(11) -0.1054(8) 0.071(3) Uani 0.511(14) 1 d D U P A 2 O5' O 0.4462(17) 0.2404(8) -0.0171(6) 0.099(5) Uani 0.511(14) 1 d D U P A 2 O6' O 0.2469(17) 0.1223(16) -0.1382(8) 0.121(7) Uani 0.511(14) 1 d D 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 0.01755(12) 0.01204(11) 0.02008(12) -0.00119(7) 0.00199(7) 0.00585(8) P1 0.0196(6) 0.0144(6) 0.0245(7) -0.0003(5) 0.0010(5) 0.0073(5) P2 0.0214(6) 0.0162(6) 0.0225(7) 0.0012(5) 0.0049(5) 0.0067(5) P3 0.0205(6) 0.0128(6) 0.0189(7) -0.0007(5) 0.0031(5) 0.0073(5) C1 0.022(3) 0.019(3) 0.036(3) -0.002(2) 0.001(2) 0.010(2) C2 0.059(4) 0.039(4) 0.036(4) -0.005(3) -0.006(3) 0.034(3) C3 0.076(5) 0.043(4) 0.052(5) -0.002(3) -0.008(4) 0.043(4) C4 0.046(4) 0.027(3) 0.046(4) -0.001(3) 0.006(3) 0.023(3) C5 0.075(5) 0.048(4) 0.031(4) 0.000(3) 0.014(3) 0.043(4) C6 0.055(4) 0.043(4) 0.033(3) 0.009(3) 0.012(3) 0.037(3) C7 0.019(2) 0.017(2) 0.029(3) 0.000(2) 0.0024(19) 0.0087(19) C8 0.023(3) 0.023(3) 0.036(3) 0.000(2) 0.006(2) 0.010(2) C9 0.025(3) 0.026(3) 0.035(3) -0.009(2) -0.002(2) 0.007(2) C10 0.022(3) 0.028(3) 0.039(3) 0.003(2) 0.002(2) 0.009(2) C11 0.025(3) 0.028(3) 0.041(4) 0.006(2) 0.010(2) 0.011(2) C12 0.029(3) 0.027(3) 0.025(3) -0.003(2) 0.001(2) 0.013(2) C13 0.025(3) 0.019(2) 0.029(3) 0.008(2) 0.003(2) 0.008(2) C14 0.023(3) 0.024(3) 0.022(3) 0.002(2) 0.0021(19) 0.006(2) C15 0.026(3) 0.023(3) 0.021(3) 0.004(2) 0.0059(19) 0.006(2) C16 0.028(3) 0.029(3) 0.042(4) 0.006(3) 0.016(2) 0.006(2) C17 0.041(3) 0.036(3) 0.034(4) 0.006(3) 0.014(3) 0.004(3) C18 0.025(3) 0.054(4) 0.028(3) 0.007(3) 0.006(2) 0.002(3) C19 0.027(3) 0.065(5) 0.060(5) 0.015(4) 0.011(3) 0.023(3) C20 0.028(3) 0.040(3) 0.050(4) 0.012(3) 0.009(3) 0.015(3) C21 0.034(3) 0.021(3) 0.022(3) -0.001(2) 0.007(2) 0.014(2) C22 0.027(3) 0.015(2) 0.023(3) -0.003(2) 0.0016(19) 0.008(2) C23 0.021(2) 0.017(2) 0.026(3) 0.004(2) 0.0070(19) 0.0086(19) C24 0.030(3) 0.020(3) 0.032(3) 0.001(2) 0.007(2) 0.012(2) C25 0.044(3) 0.028(3) 0.040(4) 0.005(3) 0.007(3) 0.027(3) C26 0.037(3) 0.041(3) 0.043(4) 0.019(3) 0.013(3) 0.026(3) C27 0.040(3) 0.043(3) 0.028(3) 0.007(3) 0.003(2) 0.025(3) C28 0.040(3) 0.027(3) 0.031(3) 0.000(2) 0.004(2) 0.019(2) C29 0.019(2) 0.016(2) 0.029(3) 0.003(2) 0.0027(19) 0.0083(19) C30 0.030(3) 0.018(3) 0.034(3) -0.001(2) 0.009(2) 0.005(2) C31 0.035(3) 0.025(3) 0.037(3) 0.001(2) 0.016(2) 0.007(2) C32 0.028(3) 0.021(3) 0.050(4) 0.008(3) 0.015(2) 0.009(2) C33 0.022(3) 0.023(3) 0.048(4) -0.003(3) 0.000(2) 0.004(2) C34 0.028(3) 0.020(3) 0.032(3) -0.002(2) 0.002(2) 0.007(2) C35 0.025(3) 0.016(2) 0.031(3) -0.005(2) 0.005(2) 0.008(2) O1 0.028(2) 0.039(2) 0.058(3) -0.004(2) -0.0040(19) 0.0178(19) C36 0.019(2) 0.014(2) 0.036(3) 0.005(2) 0.001(2) 0.0071(19) O2 0.056(3) 0.036(2) 0.022(2) 0.0023(18) 0.0129(18) 0.022(2) C37 0.022(3) 0.030(3) 0.031(3) 0.005(2) 0.004(2) 0.012(2) O3 0.036(2) 0.012(2) 0.078(4) 0.001(2) 0.002(2) 0.0008(17) C38 0.064(4) 0.059(3) 0.047(3) -0.015(3) 0.005(3) 0.021(3) S 0.0854(16) 0.0723(15) 0.0567(14) 0.0174(11) -0.0014(11) 0.0018(12) F1 0.078(8) 0.090(9) 0.044(4) -0.015(4) 0.020(4) -0.022(6) F2 0.069(5) 0.105(9) 0.117(10) -0.050(8) -0.015(5) 0.025(5) F3 0.111(12) 0.066(6) 0.046(7) -0.013(5) -0.018(7) 0.046(6) O4 0.054(5) 0.161(14) 0.087(11) 0.061(10) 0.001(5) 0.020(6) O5 0.085(8) 0.035(5) 0.037(6) -0.001(4) -0.004(5) -0.010(5) O6 0.080(6) 0.027(5) 0.027(4) 0.004(4) 0.007(4) 0.022(5) F1' 0.098(8) 0.054(6) 0.047(5) 0.009(4) -0.002(5) 0.001(5) F2' 0.126(8) 0.108(9) 0.100(9) 0.040(7) 0.072(7) 0.070(7) F3' 0.052(5) 0.046(4) 0.040(5) -0.005(4) -0.015(4) 0.018(4) O4' 0.048(5) 0.074(7) 0.062(7) 0.020(5) 0.007(5) -0.007(5) O5' 0.149(11) 0.041(5) 0.041(6) 0.015(4) -0.035(7) -0.021(6) O6' 0.155(11) 0.114(12) 0.082(8) -0.039(7) -0.048(8) 0.076(9) 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' 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' P P 0.1023 0.0942 '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' Re Re -1.0185 7.2310 '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 81.88(4) P1 Re P3 95.12(4) P1 Re C35 169.49(16) P1 Re C36 97.48(14) P1 Re C37 85.76(15) P2 Re P3 80.92(4) P2 Re C35 90.22(16) P2 Re C36 173.86(14) P2 Re C37 94.06(17) P3 Re C35 90.43(15) P3 Re C36 93.08(14) P3 Re C37 174.70(16) C35 Re C36 91.1(2) C35 Re C37 87.9(2) C36 Re C37 92.0(2) Re P1 C1 116.81(17) Re P1 C7 121.69(16) Re P1 C13 105.25(17) C1 P1 C7 102.4(2) C1 P1 C13 103.4(2) C7 P1 C13 105.4(2) Re P2 C14 110.32(17) Re P2 C15 121.59(17) Re P2 C21 108.37(17) C14 P2 C15 103.8(2) C14 P2 C21 104.1(2) C15 P2 C21 107.3(2) Re P3 C22 107.24(16) Re P3 C23 114.67(16) Re P3 C29 121.87(16) C22 P3 C23 106.3(2) C22 P3 C29 105.3(2) C23 P3 C29 100.2(2) P1 C1 C2 119.0(4) P1 C1 C6 121.9(4) C2 C1 C6 119.1(5) C1 C2 H2 120.2 C1 C2 C3 119.5(6) H2 C2 C3 120.2 C2 C3 H3 119.8 C2 C3 C4 120.5(6) H3 C3 C4 119.8 C3 C4 H4 120.4 C3 C4 C5 119.2(6) H4 C4 C5 120.4 C4 C5 H5 119.8 C4 C5 C6 120.4(6) H5 C5 C6 119.8 C1 C6 C5 121.2(6) C1 C6 H6 119.4 C5 C6 H6 119.4 P1 C7 C8 122.0(4) P1 C7 C12 119.0(4) C8 C7 C12 119.0(5) C7 C8 H8 119.8 C7 C8 C9 120.4(5) H8 C8 C9 119.8 C8 C9 H9 119.9 C8 C9 C10 120.2(5) H9 C9 C10 119.9 C9 C10 H10 120.3 C9 C10 C11 119.3(5) H10 C10 C11 120.3 C10 C11 H11 119.7 C10 C11 C12 120.7(5) H11 C11 C12 119.7 C7 C12 C11 120.4(5) C7 C12 H12 119.8 C11 C12 H12 119.8 P1 C13 H13A 108.8 P1 C13 H13B 108.8 P1 C13 C14 113.7(3) H13A C13 H13B 107.7 H13A C13 C14 108.8 H13B C13 C14 108.8 P2 C14 C13 111.7(4) P2 C14 H14A 109.3 P2 C14 H14B 109.3 C13 C14 H14A 109.3 C13 C14 H14B 109.3 H14A C14 H14B 107.9 P2 C15 C16 118.4(4) P2 C15 C20 122.1(4) C16 C15 C20 119.5(5) C15 C16 H16 119.7 C15 C16 C17 120.6(6) H16 C16 C17 119.7 C16 C17 H17 120.0 C16 C17 C18 119.9(6) H17 C17 C18 120.0 C17 C18 H18 120.0 C17 C18 C19 119.9(6) H18 C18 C19 120.0 C18 C19 H19 119.7 C18 C19 C20 120.5(6) H19 C19 C20 119.7 C15 C20 C19 119.5(6) C15 C20 H20 120.3 C19 C20 H20 120.3 P2 C21 H21A 110.0 P2 C21 H21B 110.0 P2 C21 C22 108.6(3) H21A C21 H21B 108.3 H21A C21 C22 110.0 H21B C21 C22 110.0 P3 C22 C21 111.0(3) P3 C22 H22A 109.4 P3 C22 H22B 109.4 C21 C22 H22A 109.4 C21 C22 H22B 109.4 H22A C22 H22B 108.0 P3 C23 C24 121.6(4) P3 C23 C28 119.3(4) C24 C23 C28 118.9(5) C23 C24 H24 119.8 C23 C24 C25 120.4(5) H24 C24 C25 119.8 C24 C25 H25 120.1 C24 C25 C26 119.9(5) H25 C25 C26 120.1 C25 C26 H26 119.9 C25 C26 C27 120.1(5) H26 C26 C27 119.9 C26 C27 H27 120.0 C26 C27 C28 120.0(6) H27 C27 C28 120.0 C23 C28 C27 120.7(5) C23 C28 H28 119.7 C27 C28 H28 119.7 P3 C29 C30 118.9(4) P3 C29 C34 122.5(4) C30 C29 C34 118.4(5) C29 C30 H30 119.4 C29 C30 C31 121.3(5) H30 C30 C31 119.4 C30 C31 H31 120.1 C30 C31 C32 119.8(5) H31 C31 C32 120.1 C31 C32 H32 120.0 C31 C32 C33 119.9(5) H32 C32 C33 120.0 C32 C33 H33 119.6 C32 C33 C34 120.8(5) H33 C33 C34 119.6 C29 C34 C33 119.8(5) C29 C34 H34 120.1 C33 C34 H34 120.1 Re C35 O1 175.3(4) Re C36 O2 177.2(4) Re C37 O3 178.2(5) S C38 F1 117.6(7) S C38 F2 108.4(8) S C38 F3 114.2(8) S C38 F1' 113.0(7) S C38 F2' 117.6(7) S C38 F3' 115.7(7) F1 C38 F2 101.1(8) F1 C38 F3 111.6(10) F2 C38 F3 101.7(9) F1' C38 F2' 101.3(8) F1' C38 F3' 101.5(8) F2' C38 F3' 105.6(9) C38 S O4 108.4(6) C38 S O5 98.8(4) C38 S O6 103.7(5) C38 S O4' 96.9(4) C38 S O5' 113.0(5) C38 S O6' 100.5(7) O4 S O5 111.6(7) O4 S O6 124.0(8) O5 S O6 107.1(6) O4' S O5' 105.6(7) O4' S O6' 108.8(7) O5' S O6' 127.8(8) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Re P1 2.4680(12) Re P2 2.4313(13) Re P3 2.4666(12) Re C35 1.957(5) Re C36 1.971(6) Re C37 1.954(6) P1 C1 1.829(5) P1 C7 1.831(5) P1 C13 1.835(5) P2 C14 1.840(5) P2 C15 1.812(5) P2 C21 1.834(5) P3 C22 1.833(5) P3 C23 1.831(5) P3 C29 1.828(5) C1 C2 1.395(8) C1 C6 1.351(8) C2 H2 0.950 C2 C3 1.387(9) C3 H3 0.950 C3 C4 1.384(10) C4 H4 0.950 C4 C5 1.358(9) C5 H5 0.950 C5 C6 1.391(8) C6 H6 0.950 C7 C8 1.390(7) C7 C12 1.384(7) C8 H8 0.950 C8 C9 1.382(7) C9 H9 0.950 C9 C10 1.389(8) C10 H10 0.950 C10 C11 1.374(8) C11 H11 0.950 C11 C12 1.383(7) C12 H12 0.950 C13 H13A 0.990 C13 H13B 0.990 C13 C14 1.522(7) C14 H14A 0.990 C14 H14B 0.990 C15 C16 1.381(8) C15 C20 1.384(8) C16 H16 0.950 C16 C17 1.387(8) C17 H17 0.950 C17 C18 1.372(9) C18 H18 0.950 C18 C19 1.375(10) C19 H19 0.950 C19 C20 1.397(9) C20 H20 0.950 C21 H21A 0.990 C21 H21B 0.990 C21 C22 1.515(7) C22 H22A 0.990 C22 H22B 0.990 C23 C24 1.383(7) C23 C28 1.385(8) C24 H24 0.950 C24 C25 1.397(7) C25 H25 0.950 C25 C26 1.377(9) C26 H26 0.950 C26 C27 1.372(8) C27 H27 0.950 C27 C28 1.389(8) C28 H28 0.950 C29 C30 1.385(8) C29 C34 1.394(7) C30 H30 0.950 C30 C31 1.368(7) C31 H31 0.950 C31 C32 1.380(8) C32 H32 0.950 C32 C33 1.361(9) C33 H33 0.950 C33 C34 1.385(8) C34 H34 0.950 C35 O1 1.143(6) C36 O2 1.117(7) C37 O3 1.126(6) C38 S 1.659(9) C38 F1 1.287(10) C38 F2 1.404(10) C38 F3 1.307(10) C38 F1' 1.391(10) C38 F2' 1.309(10) C38 F3' 1.327(9) S O4 1.375(9) S O5 1.562(9) S O6 1.455(8) S O4' 1.622(9) S O5' 1.358(8) S O6' 1.442(9) 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 Re P1 C1 C2 137.3(4) Re P1 C1 C6 -42.8(5) C7 P1 C1 C2 -87.2(5) C7 P1 C1 C6 92.7(5) C13 P1 C1 C2 22.2(5) C13 P1 C1 C6 -157.9(5) P1 C1 C2 C3 175.9(5) C6 C1 C2 C3 -4.0(9) C1 C2 C3 C4 1.6(11) C2 C3 C4 C5 1.5(11) C3 C4 C5 C6 -2.3(11) P1 C1 C6 C5 -176.6(5) C2 C1 C6 C5 3.3(9) C4 C5 C6 C1 -0.2(10) Re P1 C7 C8 -100.7(4) Re P1 C7 C12 79.3(4) C1 P1 C7 C8 126.6(4) C1 P1 C7 C12 -53.5(5) C13 P1 C7 C8 18.7(5) C13 P1 C7 C12 -161.4(4) P1 C7 C8 C9 179.2(4) C12 C7 C8 C9 -0.7(8) C7 C8 C9 C10 -0.3(8) C8 C9 C10 C11 1.8(8) C9 C10 C11 C12 -2.2(8) C10 C11 C12 C7 1.1(8) P1 C7 C12 C11 -179.6(4) C8 C7 C12 C11 0.3(8) Re P1 C13 C14 43.9(4) C1 P1 C13 C14 167.0(4) C7 P1 C13 C14 -85.9(4) P1 C13 C14 P2 -44.7(4) Re P2 C14 C13 23.6(4) C15 P2 C14 C13 -108.2(4) C21 P2 C14 C13 139.7(4) Re P2 C15 C16 -76.0(5) Re P2 C15 C20 106.0(5) C14 P2 C15 C16 48.8(5) C14 P2 C15 C20 -129.2(5) C21 P2 C15 C16 158.6(5) C21 P2 C15 C20 -19.4(6) P2 C15 C16 C17 -177.1(5) C20 C15 C16 C17 1.0(9) C15 C16 C17 C18 -1.0(9) C16 C17 C18 C19 0.9(10) C17 C18 C19 C20 -0.8(10) P2 C15 C20 C19 177.1(5) C16 C15 C20 C19 -0.9(9) C18 C19 C20 C15 0.8(10) Re P2 C21 C22 43.9(4) C14 P2 C21 C22 -73.6(4) C15 P2 C21 C22 176.8(3) P2 C21 C22 P3 -54.5(4) Re P3 C22 C21 39.8(4) C23 P3 C22 C21 -83.3(4) C29 P3 C22 C21 171.0(3) Re P3 C23 C24 -141.5(4) Re P3 C23 C28 44.3(5) C22 P3 C23 C24 -23.2(5) C22 P3 C23 C28 162.6(4) C29 P3 C23 C24 86.2(4) C29 P3 C23 C28 -88.0(4) P3 C23 C24 C25 -173.8(4) C28 C23 C24 C25 0.4(8) C23 C24 C25 C26 1.3(8) C24 C25 C26 C27 -1.2(9) C25 C26 C27 C28 -0.6(9) P3 C23 C28 C27 172.1(4) C24 C23 C28 C27 -2.2(8) C26 C27 C28 C23 2.3(9) Re P3 C29 C30 -52.6(5) Re P3 C29 C34 133.5(4) C22 P3 C29 C30 -174.7(4) C22 P3 C29 C34 11.4(5) C23 P3 C29 C30 75.1(4) C23 P3 C29 C34 -98.8(4) P3 C29 C30 C31 -173.0(4) C34 C29 C30 C31 1.2(8) C29 C30 C31 C32 -0.5(9) C30 C31 C32 C33 -0.5(9) C31 C32 C33 C34 0.8(9) C32 C33 C34 C29 -0.1(8) P3 C29 C34 C33 173.0(4) C30 C29 C34 C33 -0.9(8) F1 C38 S O4 68.1(11) F1 C38 S O5 -48.3(10) F1 C38 S O6 -158.4(10) F2 C38 S O4 -178.1(10) F2 C38 S O5 65.5(8) F2 C38 S O6 -44.6(9) F3 C38 S O4 -65.5(12) F3 C38 S O5 178.1(10) F3 C38 S O6 68.0(11) F1' C38 S O4' 71.6(8) F1' C38 S O5' -38.7(11) F1' C38 S O6' -177.8(10) F2' C38 S O4' -170.9(9) F2' C38 S O5' 78.8(11) F2' C38 S O6' -60.3(11) F3' C38 S O4' -44.8(9) F3' C38 S O5' -155.1(11) F3' C38 S O6' 65.8(11)