#------------------------------------------------------------------------------ #$Date: 2021-10-20 02:23:35 +0300 (Wed, 20 Oct 2021) $ #$Revision: 270043 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/85/7708595.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_7708595 loop_ _publ_author_name 'Newman, Paul David' 'Kariuki, Benson' 'Lowy, Phoebe' 'Jerwood, Kimberley' 'Deeming, Laura' _publ_section_title ; Remote Control: Stereoselective Coordination of Electron-Deficient 2,2’-bipyridine Ligands to Re(I) and Ir(III) Cores ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D1DT02928B _journal_year 2021 _chemical_absolute_configuration ad _chemical_formula_sum 'C38 H47 Cl2 N4 O9 Re' _chemical_formula_weight 960.89 _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2018/1 _audit_update_record ; 2021-10-02 deposited with the CCDC. 2021-10-07 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 97.194(3) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 9.5272(3) _cell_length_b 11.1664(3) _cell_length_c 19.1835(5) _cell_measurement_reflns_used 15006 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 28.5270 _cell_measurement_theta_min 4.1970 _cell_volume 2024.76(10) _computing_cell_refinement 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_structure_refinement 'SHELXL-2018/1 (Sheldrick, 2018)' _computing_structure_solution SHELXS _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.912 _diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, Atlas' _diffrn_measurement_method '\w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0407 _diffrn_reflns_av_unetI/netI 0.0443 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.912 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 33296 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.876 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 29.643 _diffrn_reflns_theta_min 3.211 _exptl_absorpt_coefficient_mu 3.190 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.384 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.576 _exptl_crystal_description needle _exptl_crystal_F_000 968 _exptl_crystal_size_max 0.460 _exptl_crystal_size_mid 0.092 _exptl_crystal_size_min 0.063 _refine_diff_density_max 1.709 _refine_diff_density_min -0.820 _refine_diff_density_rms 0.115 _refine_ls_abs_structure_details ; Flack x determined using 3802 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.007(5) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 535 _refine_ls_number_reflns 10036 _refine_ls_number_restraints 301 _refine_ls_restrained_S_all 1.121 _refine_ls_R_factor_all 0.0451 _refine_ls_R_factor_gt 0.0381 _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^)+(0.0501P)^2^+1.9918P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0915 _refine_ls_wR_factor_ref 0.0959 _reflns_Friedel_coverage 0.833 _reflns_Friedel_fraction_full 0.999 _reflns_Friedel_fraction_max 0.837 _reflns_number_gt 9072 _reflns_number_total 10036 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt02928b2.cif _cod_data_source_block pdn2004c _cod_original_sg_symbol_H-M 'P 21' _cod_database_code 7708595 _shelx_shelxl_version_number 2018/1 _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 0.322 _shelx_estimated_absorpt_t_max 0.824 _shelx_res_file ; TITL pdn2004c in P2(1) shelx.res created by SHELXL-2018/1 at 17:13:16 on 27-Sep-2021 CELL 0.71073 9.5272 11.1664 19.1835 90.000 97.194 90.000 ZERR 2.00 0.0003 0.0003 0.0005 0.000 0.003 0.000 LATT -1 SYMM - X, 1/2 + Y, - Z SFAC C H CL N O RE UNIT 76 94 4 8 18 2 MERG 2 dfix 1.43 .01 Cl2 O6 Cl2 O7 Cl2 O8 Cl2 O9 dfix 2.4 .02 o6 o7 o6 o8 o6 o9 o7 o8 o7 o9 o8 o9 simu .005 cl2 > o9a isor .005 cl2 > c38, c29 dfix 1.54 .01 c33 c34 c34 c35 dfix 1.23 .01 c34 o4 dfix 2.5 .01 c33 c35 dfix 2.35 .01 c35 o4 o4 c33 flat c33 c34 c35 o4 FMAP 2 PLAN 10 SIZE 0.063 0.092 0.460 ACTA BOND $H LIST 4 BUMP 0.02000 L.S. 24 WGHT 0.050100 1.991800 FVAR 2.32848 0.49102 0.35671 0.34924 C1 1 0.145055 0.485155 0.464471 11.00000 0.03537 0.03926 = 0.05171 -0.00341 -0.00303 -0.00153 AFIX 43 H1 2 0.155465 0.549458 0.434739 11.00000 -1.20000 AFIX 0 C2 1 0.027499 0.412653 0.450673 11.00000 0.03785 0.04915 = 0.06460 -0.01177 -0.00025 -0.00182 AFIX 43 H2 2 -0.041341 0.428437 0.412995 11.00000 -1.20000 AFIX 0 C3 1 0.014973 0.315757 0.494521 11.00000 0.03399 0.07128 = 0.08231 -0.00675 0.00310 -0.01999 AFIX 43 H3 2 -0.063503 0.265791 0.486605 11.00000 -1.20000 AFIX 0 C4 1 0.116334 0.293555 0.548748 11.00000 0.04657 0.05472 = 0.05336 -0.00408 0.01036 -0.01829 AFIX 43 H4 2 0.109186 0.227288 0.577458 11.00000 -1.20000 AFIX 0 C5 1 0.232257 0.371076 0.561407 11.00000 0.03918 0.02866 = 0.04356 -0.00597 0.01176 -0.00649 C6 1 0.347104 0.354091 0.619449 11.00000 0.03860 0.02738 = 0.04323 -0.00577 0.01602 -0.00654 C7 1 0.348747 0.256658 0.663101 11.00000 0.06597 0.03779 = 0.05530 -0.00024 -0.00079 -0.02105 AFIX 43 H7 2 0.276977 0.199724 0.657442 11.00000 -1.20000 AFIX 0 C8 1 0.460184 0.246385 0.715380 11.00000 0.07120 0.04192 = 0.06076 0.01845 -0.00665 -0.00053 AFIX 43 H8 2 0.463888 0.180544 0.745244 11.00000 -1.20000 AFIX 0 C9 1 0.562456 0.326799 0.724781 11.00000 0.06853 0.03935 = 0.04443 0.00533 -0.00508 -0.00512 AFIX 43 H9 2 0.637408 0.318176 0.760444 11.00000 -1.20000 AFIX 0 C10 1 0.554637 0.424366 0.679886 11.00000 0.03758 0.03231 = 0.03302 -0.00303 0.00543 -0.00222 C11 1 0.645879 0.609503 0.726967 11.00000 0.03164 0.03464 = 0.03695 0.00848 0.00127 -0.00153 AFIX 43 H11 2 0.553959 0.631000 0.733181 11.00000 -1.20000 AFIX 0 C12 1 0.813837 0.473377 0.682768 11.00000 0.03598 0.03709 = 0.06081 0.00415 -0.00086 0.01270 AFIX 13 H12 2 0.819438 0.388042 0.671506 11.00000 -1.20000 AFIX 0 C13 1 0.868028 0.551575 0.627816 11.00000 0.02930 0.05961 = 0.06202 0.00241 0.01711 0.01015 AFIX 23 H13A 2 0.793228 0.569030 0.590071 11.00000 -1.20000 H13B 2 0.945263 0.512664 0.608216 11.00000 -1.20000 AFIX 0 C14 1 0.919703 0.667926 0.667248 11.00000 0.03008 0.04704 = 0.07152 0.01291 0.00508 0.00195 AFIX 23 H14A 2 1.017560 0.684071 0.661352 11.00000 -1.20000 H14B 2 0.862439 0.735643 0.649302 11.00000 -1.20000 AFIX 0 C15 1 0.904915 0.646774 0.744333 11.00000 0.02493 0.04385 = 0.07477 0.00331 0.00210 0.00007 C16 1 0.908148 0.505856 0.750469 11.00000 0.05727 0.04336 = 0.06424 0.00180 -0.00509 0.00370 C17 1 1.008799 0.709248 0.794856 11.00000 0.04654 0.06404 = 0.10934 -0.00134 -0.01086 -0.01172 AFIX 33 H17A 2 0.991204 0.690589 0.841836 11.00000 -1.50000 H17B 2 1.102507 0.683818 0.788302 11.00000 -1.50000 H17C 2 1.000460 0.794095 0.787390 11.00000 -1.50000 AFIX 0 C18 1 1.063061 0.462659 0.744217 11.00000 0.03296 0.05997 = 0.12794 0.02126 -0.01079 0.01502 AFIX 33 H18A 2 1.123429 0.482589 0.786507 11.00000 -1.50000 H18B 2 1.063359 0.377496 0.737383 11.00000 -1.50000 H18C 2 1.097029 0.501502 0.704942 11.00000 -1.50000 AFIX 0 C19 1 0.868027 0.451442 0.818622 11.00000 0.06861 0.04832 = 0.06363 0.01225 -0.02154 0.00150 AFIX 33 H19A 2 0.934034 0.477713 0.857551 11.00000 -1.50000 H19B 2 0.774436 0.476866 0.825399 11.00000 -1.50000 H19C 2 0.870486 0.365668 0.815596 11.00000 -1.50000 AFIX 0 C20 1 0.723174 0.799583 0.783135 11.00000 0.05233 0.03566 = 0.07322 -0.01040 0.00759 -0.00853 AFIX 23 H20A 2 0.723969 0.858342 0.745945 11.00000 -1.20000 H20B 2 0.800683 0.818729 0.819165 11.00000 -1.20000 AFIX 0 C21 1 0.585794 0.812393 0.814483 11.00000 0.05394 0.04655 = 0.04924 -0.02158 0.00341 -0.01214 C22 1 0.469563 0.877598 0.780099 11.00000 0.05702 0.03916 = 0.05698 -0.01710 0.00723 -0.00602 C23 1 0.355390 0.903632 0.813746 11.00000 0.07022 0.06281 = 0.06897 -0.03386 0.01305 -0.01038 AFIX 43 H23 2 0.279848 0.947050 0.790990 11.00000 -1.20000 AFIX 0 C24 1 0.353007 0.862986 0.885238 11.00000 0.08236 0.08562 = 0.05914 -0.03504 0.02085 -0.02059 C25 1 0.460678 0.793752 0.916520 11.00000 0.12558 0.09410 = 0.05482 -0.01184 0.03031 -0.03060 AFIX 43 H25 2 0.455717 0.762543 0.961092 11.00000 -1.20000 AFIX 0 C26 1 0.576985 0.769524 0.882682 11.00000 0.08204 0.06887 = 0.04389 -0.00987 -0.00365 -0.01039 C27 1 0.464021 0.925373 0.707434 11.00000 0.09843 0.04552 = 0.06733 0.00134 0.00898 0.01688 AFIX 33 H27A 2 0.548371 0.902654 0.688143 11.00000 -1.50000 H27B 2 0.382907 0.893185 0.678812 11.00000 -1.50000 H27C 2 0.457207 1.011116 0.708446 11.00000 -1.50000 AFIX 0 C28 1 0.701266 0.702702 0.922906 11.00000 0.13877 0.10691 = 0.05439 -0.00832 -0.01038 0.02879 AFIX 33 H28A 2 0.774175 0.692091 0.893154 11.00000 -1.50000 H28B 2 0.737858 0.748120 0.963657 11.00000 -1.50000 H28C 2 0.670006 0.625827 0.937232 11.00000 -1.50000 AFIX 0 C29 1 0.225161 0.891385 0.921462 11.00000 0.09255 0.12502 = 0.09709 -0.04909 0.03324 -0.03568 AFIX 33 H29A 2 0.161158 0.940923 0.891438 11.00000 -1.50000 H29B 2 0.178447 0.818289 0.931372 11.00000 -1.50000 H29C 2 0.254579 0.933001 0.964613 11.00000 -1.50000 AFIX 0 C30 1 0.545850 0.518074 0.487123 11.00000 0.03950 0.04426 = 0.04113 -0.00490 0.01292 -0.00303 C31 1 0.362296 0.699939 0.476411 11.00000 0.05217 0.04010 = 0.04669 0.01461 -0.00183 -0.00931 C32 1 0.563831 0.704208 0.574632 11.00000 0.02743 0.03276 = 0.03304 0.00322 0.00344 -0.00256 N1 4 0.244958 0.466268 0.519245 11.00000 0.03093 0.03377 = 0.04274 -0.00663 0.00527 -0.00272 N2 4 0.450143 0.439311 0.626405 11.00000 0.03038 0.02548 = 0.03739 -0.00382 0.01106 -0.00051 N3 4 0.665925 0.511098 0.691706 11.00000 0.03383 0.03876 = 0.03243 0.00083 0.00147 -0.00275 N4 4 0.750420 0.678289 0.753632 11.00000 0.04338 0.03812 = 0.04604 -0.00376 -0.00149 -0.00392 O1 5 0.625660 0.482266 0.453324 11.00000 0.06300 0.08477 = 0.05782 -0.01844 0.02536 -0.00001 O2 5 0.325366 0.769791 0.433199 11.00000 0.06876 0.05782 = 0.07329 0.03318 -0.02052 -0.01046 O3 5 0.644056 0.779790 0.585923 11.00000 0.03947 0.03483 = 0.06547 0.00549 0.00254 -0.00607 CL1 3 0.274390 0.665987 0.633650 11.00000 0.03697 0.04192 = 0.06284 -0.00917 0.01727 0.00379 RE1 6 0.420839 0.586967 0.547838 11.00000 0.02832 0.02594 = 0.03305 0.00128 0.00482 -0.00047 MOLE 2 PART 1 CL2 3 0.056949 0.593884 0.269094 21.00000 0.05253 0.04161 = 0.05224 -0.00095 0.01317 -0.00708 O6 5 0.083047 0.477270 0.295267 21.00000 0.08763 0.05049 = 0.07442 -0.00298 0.01948 0.01287 O7 5 0.026695 0.661325 0.333180 21.00000 0.08880 0.06484 = 0.07079 -0.01457 0.01728 0.01643 O8 5 0.165311 0.656104 0.243880 21.00000 0.09342 0.08607 = 0.09364 0.00511 0.01207 -0.02107 O9 5 -0.072734 0.618698 0.223361 21.00000 0.08055 0.08066 = 0.08486 0.01171 -0.00565 -0.00969 PART 2 same .01 cl2 > o9 CL2A 3 0.038861 0.585449 0.271898 -21.00000 0.07023 0.04682 = 0.06576 0.00325 0.00402 -0.00860 O6A 5 -0.067926 0.598249 0.319524 -21.00000 0.07260 0.07211 = 0.08037 -0.00376 0.02823 0.01288 O7A 5 0.152797 0.664307 0.303177 -21.00000 0.09148 0.07176 = 0.09269 -0.00514 -0.00047 -0.02452 O8A 5 0.079972 0.476417 0.258192 -21.00000 0.09562 0.05816 = 0.08764 0.00613 0.01749 0.00395 O9A 5 -0.006290 0.652727 0.208241 -21.00000 0.09012 0.07919 = 0.07519 0.01948 0.00306 -0.00807 MOLE 3 O4 5 0.548313 0.332058 0.894771 11.00000 0.13551 0.20149 = 0.11881 0.00448 0.01045 0.00167 C33 1 0.382716 0.491410 0.876809 11.00000 0.19514 0.18907 = 0.22316 0.00276 -0.00153 -0.03684 AFIX 33 H33A 2 0.281330 0.496033 0.871729 11.00000 -1.50000 H33B 2 0.421450 0.537727 0.916811 11.00000 -1.50000 H33C 2 0.416434 0.522469 0.835300 11.00000 -1.50000 AFIX 0 C34 1 0.427464 0.364601 0.886995 11.00000 0.10040 0.11001 = 0.09196 -0.00590 0.00742 -0.00113 C35 1 0.308825 0.275430 0.880919 11.00000 0.09809 0.09384 = 0.10389 0.01635 0.00368 -0.00110 AFIX 33 H35A 2 0.219925 0.316996 0.874972 11.00000 -1.50000 H35B 2 0.315086 0.224559 0.841084 11.00000 -1.50000 H35C 2 0.315528 0.227660 0.922812 11.00000 -1.50000 AFIX 0 MOLE 4 same .005 o4 > c35 O5 5 0.123735 0.527759 -0.015532 11.00000 0.31939 0.30671 = 0.30674 -0.03396 0.03911 -0.01341 C36 1 0.267811 0.566581 0.092791 11.00000 0.12653 0.13202 = 0.17444 0.02256 0.00595 0.04112 AFIX 33 H36A 2 0.255277 0.612126 0.134003 11.00000 -1.50000 H36B 2 0.284545 0.484167 0.105451 11.00000 -1.50000 H36C 2 0.347282 0.597443 0.072272 11.00000 -1.50000 AFIX 0 C37 1 0.137999 0.575901 0.041043 11.00000 0.14614 0.14176 = 0.14465 -0.01100 0.01246 -0.00421 C38 1 0.051548 0.685454 0.051596 11.00000 0.15647 0.17444 = 0.12136 0.00402 0.02084 0.05356 AFIX 33 H38A 2 0.074136 0.713713 0.098934 11.00000 -1.50000 H38B 2 0.072486 0.746857 0.019425 11.00000 -1.50000 H38C 2 -0.047214 0.665788 0.043170 11.00000 -1.50000 AFIX 0 HKLF 4 REM pdn2004c in P2(1) REM R1 = 0.0381 for 9072 Fo > 4sig(Fo) and 0.0451 for all 10036 data REM 535 parameters refined using 301 restraints END WGHT 0.0501 1.9865 REM Highest difference peak 1.709, deepest hole -0.820, 1-sigma level 0.115 Q1 1 0.4950 0.5857 0.5742 11.00000 0.05 1.71 Q2 1 0.3944 0.5867 0.4886 11.00000 0.05 1.68 Q3 1 0.4655 0.5857 0.6077 11.00000 0.05 1.35 Q4 1 -0.1209 0.5834 0.2951 11.00000 0.05 0.88 Q5 1 0.2614 0.0874 0.6439 11.00000 0.05 0.84 Q6 1 0.0691 0.5855 -0.0391 11.00000 0.05 0.77 Q7 1 0.3512 0.5856 0.4524 11.00000 0.05 0.75 Q8 1 0.3264 0.5859 0.5262 11.00000 0.05 0.73 Q9 1 -0.0153 0.5849 0.2055 11.00000 0.05 0.72 Q10 1 0.0942 0.6856 0.3358 11.00000 0.05 0.69 ; _shelx_res_checksum 884 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -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 C1 C 0.1451(9) 0.4852(8) 0.4645(5) 0.0428(19) Uani 1 1 d . . . . . H1 H 0.155465 0.549458 0.434739 0.051 Uiso 1 1 calc R U . . . C2 C 0.0275(11) 0.4127(9) 0.4507(6) 0.051(2) Uani 1 1 d . . . . . H2 H -0.041341 0.428437 0.412995 0.061 Uiso 1 1 calc R U . . . C3 C 0.0150(14) 0.3158(13) 0.4945(9) 0.063(4) Uani 1 1 d . . . . . H3 H -0.063503 0.265791 0.486605 0.075 Uiso 1 1 calc R U . . . C4 C 0.1163(10) 0.2936(10) 0.5487(5) 0.051(2) Uani 1 1 d . . . . . H4 H 0.109186 0.227288 0.577458 0.061 Uiso 1 1 calc R U . . . C5 C 0.2323(9) 0.3711(7) 0.5614(5) 0.0366(18) Uani 1 1 d . . . . . C6 C 0.3471(9) 0.3541(7) 0.6194(4) 0.0355(17) Uani 1 1 d . . . . . C7 C 0.3487(11) 0.2567(8) 0.6631(5) 0.054(2) Uani 1 1 d . . . . . H7 H 0.276977 0.199724 0.657442 0.064 Uiso 1 1 calc R U . . . C8 C 0.4602(15) 0.2464(12) 0.7154(7) 0.059(4) Uani 1 1 d . . . . . H8 H 0.463888 0.180544 0.745244 0.071 Uiso 1 1 calc R U . . . C9 C 0.5625(12) 0.3268(9) 0.7248(5) 0.052(2) Uani 1 1 d . . . . . H9 H 0.637408 0.318176 0.760444 0.062 Uiso 1 1 calc R U . . . C10 C 0.5546(9) 0.4244(7) 0.6799(4) 0.0342(16) Uani 1 1 d . . . . . C11 C 0.6459(8) 0.6095(7) 0.7270(4) 0.035(2) Uani 1 1 d . . . . . H11 H 0.553959 0.631000 0.733181 0.042 Uiso 1 1 calc R U . . . C12 C 0.8138(9) 0.4734(8) 0.6828(5) 0.045(2) Uani 1 1 d . . . . . H12 H 0.819438 0.388042 0.671506 0.054 Uiso 1 1 calc R U . . . C13 C 0.8680(9) 0.5516(8) 0.6278(5) 0.049(2) Uani 1 1 d . . . . . H13A H 0.793228 0.569030 0.590071 0.059 Uiso 1 1 calc R U . . . H13B H 0.945263 0.512664 0.608216 0.059 Uiso 1 1 calc R U . . . C14 C 0.9197(10) 0.6679(9) 0.6672(6) 0.050(2) Uani 1 1 d . . . . . H14A H 1.017560 0.684071 0.661352 0.060 Uiso 1 1 calc R U . . . H14B H 0.862439 0.735643 0.649302 0.060 Uiso 1 1 calc R U . . . C15 C 0.9049(12) 0.6468(12) 0.7443(8) 0.048(3) Uani 1 1 d . . . . . C16 C 0.9081(16) 0.5059(13) 0.7505(8) 0.056(3) Uani 1 1 d . . . . . C17 C 1.0088(11) 0.7092(12) 0.7949(7) 0.075(4) Uani 1 1 d . . . . . H17A H 0.991204 0.690589 0.841836 0.113 Uiso 1 1 calc R U . . . H17B H 1.102507 0.683818 0.788302 0.113 Uiso 1 1 calc R U . . . H17C H 1.000460 0.794095 0.787390 0.113 Uiso 1 1 calc R U . . . C18 C 1.0631(11) 0.4627(11) 0.7442(8) 0.075(4) Uani 1 1 d . . . . . H18A H 1.123429 0.482589 0.786507 0.113 Uiso 1 1 calc R U . . . H18B H 1.063359 0.377496 0.737383 0.113 Uiso 1 1 calc R U . . . H18C H 1.097029 0.501502 0.704942 0.113 Uiso 1 1 calc R U . . . C19 C 0.8680(12) 0.4514(9) 0.8186(6) 0.063(3) Uani 1 1 d . . . . . H19A H 0.934034 0.477713 0.857551 0.094 Uiso 1 1 calc R U . . . H19B H 0.774436 0.476866 0.825399 0.094 Uiso 1 1 calc R U . . . H19C H 0.870486 0.365668 0.815596 0.094 Uiso 1 1 calc R U . . . C20 C 0.7232(10) 0.7996(9) 0.7831(6) 0.054(2) Uani 1 1 d . . . . . H20A H 0.723969 0.858342 0.745945 0.065 Uiso 1 1 calc R U . . . H20B H 0.800683 0.818729 0.819165 0.065 Uiso 1 1 calc R U . . . C21 C 0.5858(11) 0.8124(9) 0.8145(5) 0.050(2) Uani 1 1 d . . . . . C22 C 0.4696(12) 0.8776(8) 0.7801(6) 0.051(2) Uani 1 1 d . . . . . C23 C 0.3554(13) 0.9036(11) 0.8137(7) 0.067(3) Uani 1 1 d . . . . . H23 H 0.279848 0.947050 0.790990 0.080 Uiso 1 1 calc R U . . . C24 C 0.3530(18) 0.8630(15) 0.8852(8) 0.075(4) Uani 1 1 d . . . . . C25 C 0.461(2) 0.7938(16) 0.9165(7) 0.090(5) Uani 1 1 d . . . . . H25 H 0.455717 0.762543 0.961092 0.108 Uiso 1 1 calc R U . . . C26 C 0.5770(14) 0.7695(12) 0.8827(6) 0.066(3) Uani 1 1 d . . . . . C27 C 0.4640(18) 0.9254(13) 0.7074(8) 0.071(4) Uani 1 1 d . . . . . H27A H 0.548371 0.902654 0.688143 0.106 Uiso 1 1 calc R U . . . H27B H 0.382907 0.893185 0.678812 0.106 Uiso 1 1 calc R U . . . H27C H 0.457207 1.011116 0.708446 0.106 Uiso 1 1 calc R U . . . C28 C 0.7013(18) 0.7027(14) 0.9229(6) 0.102(5) Uani 1 1 d . . . . . H28A H 0.774175 0.692091 0.893154 0.153 Uiso 1 1 calc R U . . . H28B H 0.737858 0.748120 0.963657 0.153 Uiso 1 1 calc R U . . . H28C H 0.670006 0.625827 0.937232 0.153 Uiso 1 1 calc R U . . . C29 C 0.2252(18) 0.8914(17) 0.9215(9) 0.103(5) Uani 1 1 d . U . . . H29A H 0.161158 0.940923 0.891438 0.155 Uiso 1 1 calc R U . . . H29B H 0.178447 0.818289 0.931372 0.155 Uiso 1 1 calc R U . . . H29C H 0.254579 0.933001 0.964613 0.155 Uiso 1 1 calc R U . . . C30 C 0.5458(9) 0.5181(8) 0.4871(5) 0.0410(19) Uani 1 1 d . . . . . C31 C 0.3623(10) 0.6999(8) 0.4764(5) 0.047(2) Uani 1 1 d . . . . . C32 C 0.5638(8) 0.7042(7) 0.5746(4) 0.0311(15) Uani 1 1 d . . . . . N1 N 0.2450(7) 0.4663(6) 0.5192(4) 0.0358(14) Uani 1 1 d . . . . . N2 N 0.4501(6) 0.4393(5) 0.6264(3) 0.0305(13) Uani 1 1 d . . . . . N3 N 0.6659(7) 0.5111(6) 0.6917(3) 0.0352(14) Uani 1 1 d . . . . . N4 N 0.7504(8) 0.6783(7) 0.7536(4) 0.0431(16) Uani 1 1 d . . . . . O1 O 0.6257(9) 0.4823(8) 0.4533(4) 0.067(2) Uani 1 1 d . . . . . O2 O 0.3254(8) 0.7698(7) 0.4332(4) 0.069(2) Uani 1 1 d . . . . . O3 O 0.6441(6) 0.7798(6) 0.5859(4) 0.0469(14) Uani 1 1 d . . . . . Cl1 Cl 0.2744(2) 0.6660(2) 0.63365(13) 0.0463(5) Uani 1 1 d . . . . . Re1 Re 0.42084(2) 0.58697(7) 0.54784(2) 0.02902(9) Uani 1 1 d . . . . . Cl2 Cl 0.0569(10) 0.5939(10) 0.2691(5) 0.0482(14) Uani 0.491(10) 1 d D U P A 1 O6 O 0.083(2) 0.4773(11) 0.2953(9) 0.070(3) Uani 0.491(10) 1 d D U P A 1 O7 O 0.0267(19) 0.6613(14) 0.3332(7) 0.074(3) Uani 0.491(10) 1 d D U P A 1 O8 O 0.1653(16) 0.6561(16) 0.2439(10) 0.091(4) Uani 0.491(10) 1 d D U P A 1 O9 O -0.0727(15) 0.6187(16) 0.2234(8) 0.083(4) Uani 0.491(10) 1 d D U P A 1 Cl2A Cl 0.0389(12) 0.5854(12) 0.2719(5) 0.0613(17) Uani 0.509(10) 1 d D U P A 2 O6A O -0.0679(14) 0.598(2) 0.3195(7) 0.073(3) Uani 0.509(10) 1 d D U P A 2 O7A O 0.1528(18) 0.6643(16) 0.3032(10) 0.086(3) Uani 0.509(10) 1 d D U P A 2 O8A O 0.080(2) 0.4764(13) 0.2582(10) 0.080(4) Uani 0.509(10) 1 d D U P A 2 O9A O -0.006(2) 0.6527(15) 0.2082(8) 0.082(3) Uani 0.509(10) 1 d D U P A 2 O4 O 0.5483(14) 0.3321(15) 0.8948(8) 0.152(6) Uani 1 1 d D U . B 2 C33 C 0.383(2) 0.4914(12) 0.8768(14) 0.205(12) Uani 1 1 d D U . B 2 H33A H 0.281330 0.496033 0.871729 0.307 Uiso 1 1 calc R U . B 2 H33B H 0.421450 0.537727 0.916811 0.307 Uiso 1 1 calc R U . B 2 H33C H 0.416434 0.522469 0.835300 0.307 Uiso 1 1 calc R U . B 2 C34 C 0.4275(15) 0.3646(13) 0.8870(9) 0.101(6) Uani 1 1 d D U . B 2 C35 C 0.3088(16) 0.2754(14) 0.8809(10) 0.099(6) Uani 1 1 d D U . B 2 H35A H 0.219925 0.316996 0.874972 0.149 Uiso 1 1 calc R U . B 2 H35B H 0.315086 0.224559 0.841084 0.149 Uiso 1 1 calc R U . B 2 H35C H 0.315528 0.227660 0.922812 0.149 Uiso 1 1 calc R U . B 2 O5 O 0.124(3) 0.528(2) -0.0155(11) 0.311(16) Uani 1 1 d D U . C 2 C36 C 0.2678(17) 0.567(2) 0.0928(10) 0.145(8) Uani 1 1 d D U . C 2 H36A H 0.255277 0.612126 0.134003 0.218 Uiso 1 1 calc R U . C 2 H36B H 0.284545 0.484167 0.105451 0.218 Uiso 1 1 calc R U . C 2 H36C H 0.347282 0.597443 0.072272 0.218 Uiso 1 1 calc R U . C 2 C37 C 0.1380(18) 0.576(2) 0.0410(10) 0.145(7) Uani 1 1 d D U . C 2 C38 C 0.052(2) 0.685(2) 0.0516(10) 0.150(8) Uani 1 1 d D U . C 2 H38A H 0.074136 0.713713 0.098934 0.226 Uiso 1 1 calc R U . C 2 H38B H 0.072486 0.746857 0.019425 0.226 Uiso 1 1 calc R U . C 2 H38C H -0.047214 0.665788 0.043170 0.226 Uiso 1 1 calc R U . C 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 C1 0.035(5) 0.039(5) 0.052(5) -0.003(4) -0.003(4) -0.002(4) C2 0.038(5) 0.049(6) 0.065(6) -0.012(5) 0.000(4) -0.002(4) C3 0.034(6) 0.071(11) 0.082(8) -0.007(7) 0.003(5) -0.020(6) C4 0.047(5) 0.055(6) 0.053(5) -0.004(5) 0.010(4) -0.018(4) C5 0.039(4) 0.029(4) 0.044(4) -0.006(3) 0.012(4) -0.006(3) C6 0.039(4) 0.027(4) 0.043(4) -0.006(3) 0.016(3) -0.007(3) C7 0.066(6) 0.038(5) 0.055(5) 0.000(4) -0.001(5) -0.021(4) C8 0.071(9) 0.042(7) 0.061(8) 0.018(6) -0.007(7) -0.001(6) C9 0.069(7) 0.039(5) 0.044(5) 0.005(4) -0.005(4) -0.005(4) C10 0.038(4) 0.032(4) 0.033(4) -0.003(3) 0.005(3) -0.002(3) C11 0.032(3) 0.035(6) 0.037(3) 0.008(3) 0.001(3) -0.002(3) C12 0.036(5) 0.037(4) 0.061(5) 0.004(4) -0.001(4) 0.013(4) C13 0.029(4) 0.060(7) 0.062(5) 0.002(4) 0.017(4) 0.010(3) C14 0.030(5) 0.047(5) 0.072(6) 0.013(5) 0.005(4) 0.002(4) C15 0.025(5) 0.044(6) 0.075(8) 0.003(5) 0.002(5) 0.000(4) C16 0.057(8) 0.043(7) 0.064(7) 0.002(6) -0.005(6) 0.004(5) C17 0.047(6) 0.064(7) 0.109(10) -0.001(7) -0.011(7) -0.012(5) C18 0.033(5) 0.060(7) 0.128(11) 0.021(7) -0.011(6) 0.015(5) C19 0.069(7) 0.048(6) 0.064(6) 0.012(5) -0.022(5) 0.002(5) C20 0.052(6) 0.036(5) 0.073(6) -0.010(5) 0.008(5) -0.009(4) C21 0.054(6) 0.047(5) 0.049(5) -0.022(4) 0.003(4) -0.012(4) C22 0.057(6) 0.039(5) 0.057(6) -0.017(4) 0.007(5) -0.006(4) C23 0.070(8) 0.063(7) 0.069(7) -0.034(6) 0.013(6) -0.010(6) C24 0.082(10) 0.086(10) 0.059(8) -0.035(7) 0.021(7) -0.021(8) C25 0.126(13) 0.094(11) 0.055(7) -0.012(8) 0.030(8) -0.031(10) C26 0.082(8) 0.069(8) 0.044(5) -0.010(5) -0.004(5) -0.010(6) C27 0.098(12) 0.046(8) 0.067(9) 0.001(7) 0.009(8) 0.017(8) C28 0.139(14) 0.107(12) 0.054(7) -0.008(7) -0.010(8) 0.029(11) C29 0.093(9) 0.125(10) 0.097(9) -0.049(8) 0.033(7) -0.036(8) C30 0.039(5) 0.044(5) 0.041(4) -0.005(4) 0.013(4) -0.003(4) C31 0.052(5) 0.040(5) 0.047(5) 0.015(4) -0.002(4) -0.009(4) C32 0.027(4) 0.033(4) 0.033(4) 0.003(3) 0.003(3) -0.003(3) N1 0.031(3) 0.034(3) 0.043(4) -0.007(3) 0.005(3) -0.003(3) N2 0.030(3) 0.025(3) 0.037(3) -0.004(3) 0.011(3) -0.001(2) N3 0.034(4) 0.039(4) 0.032(3) 0.001(3) 0.001(3) -0.003(3) N4 0.043(4) 0.038(4) 0.046(4) -0.004(3) -0.001(3) -0.004(3) O1 0.063(4) 0.085(6) 0.058(4) -0.018(4) 0.025(4) 0.000(4) O2 0.069(5) 0.058(5) 0.073(5) 0.033(4) -0.021(4) -0.010(4) O3 0.039(3) 0.035(3) 0.065(4) 0.005(3) 0.003(3) -0.006(3) Cl1 0.0370(10) 0.0419(11) 0.0628(13) -0.0092(10) 0.0173(9) 0.0038(8) Re1 0.02832(13) 0.02594(13) 0.03305(13) 0.0013(2) 0.00482(9) -0.00047(19) Cl2 0.053(2) 0.042(3) 0.052(2) -0.001(3) 0.0132(19) -0.007(3) O6 0.088(6) 0.050(6) 0.074(7) -0.003(6) 0.019(6) 0.013(5) O7 0.089(6) 0.065(6) 0.071(6) -0.015(5) 0.017(5) 0.016(5) O8 0.093(6) 0.086(6) 0.094(6) 0.005(6) 0.012(6) -0.021(6) O9 0.081(6) 0.081(6) 0.085(6) 0.012(5) -0.006(5) -0.010(5) Cl2A 0.070(3) 0.047(3) 0.066(3) 0.003(3) 0.004(2) -0.009(3) O6A 0.073(5) 0.072(6) 0.080(5) -0.004(6) 0.028(5) 0.013(6) O7A 0.091(6) 0.072(6) 0.093(6) -0.005(6) 0.000(6) -0.025(5) O8A 0.096(6) 0.058(6) 0.088(7) 0.006(6) 0.017(6) 0.004(6) O9A 0.090(6) 0.079(6) 0.075(6) 0.019(5) 0.003(5) -0.008(6) O4 0.136(10) 0.201(12) 0.119(9) 0.004(9) 0.010(8) 0.002(10) C33 0.195(16) 0.189(16) 0.223(17) 0.003(12) -0.002(12) -0.037(12) C34 0.100(8) 0.110(8) 0.092(8) -0.006(6) 0.007(6) -0.001(6) C35 0.098(10) 0.094(10) 0.104(10) 0.016(8) 0.004(8) -0.001(8) O5 0.319(19) 0.31(2) 0.307(18) -0.034(13) 0.039(13) -0.013(13) C36 0.127(11) 0.132(13) 0.174(12) 0.023(11) 0.006(10) 0.041(10) C37 0.146(9) 0.142(9) 0.145(8) -0.011(7) 0.012(6) -0.004(7) C38 0.156(13) 0.174(13) 0.121(11) 0.004(10) 0.021(10) 0.054(11) 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' Cl Cl 0.1484 0.1585 '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' 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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 122.4(9) . . ? N1 C1 H1 118.8 . . ? C2 C1 H1 118.8 . . ? C1 C2 C3 118.1(11) . . ? C1 C2 H2 120.9 . . ? C3 C2 H2 120.9 . . ? C4 C3 C2 120.2(12) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C3 C4 C5 119.5(11) . . ? C3 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? N1 C5 C4 120.7(8) . . ? N1 C5 C6 116.1(7) . . ? C4 C5 C6 123.1(8) . . ? N2 C6 C7 122.8(8) . . ? N2 C6 C5 116.3(7) . . ? C7 C6 C5 121.0(7) . . ? C8 C7 C6 117.5(9) . . ? C8 C7 H7 121.3 . . ? C6 C7 H7 121.3 . . ? C9 C8 C7 122.2(11) . . ? C9 C8 H8 118.9 . . ? C7 C8 H8 118.9 . . ? C8 C9 C10 117.9(10) . . ? C8 C9 H9 121.0 . . ? C10 C9 H9 121.0 . . ? N2 C10 C9 123.2(8) . . ? N2 C10 N3 119.9(7) . . ? C9 C10 N3 116.9(7) . . ? N4 C11 N3 122.5(7) . . ? N4 C11 H11 118.7 . . ? N3 C11 H11 118.7 . . ? N3 C12 C13 109.0(7) . . ? N3 C12 C16 107.3(9) . . ? C13 C12 C16 103.9(9) . . ? N3 C12 H12 112.1 . . ? C13 C12 H12 112.1 . . ? C16 C12 H12 112.1 . . ? C12 C13 C14 105.0(8) . . ? C12 C13 H13A 110.7 . . ? C14 C13 H13A 110.7 . . ? C12 C13 H13B 110.7 . . ? C14 C13 H13B 110.7 . . ? H13A C13 H13B 108.8 . . ? C15 C14 C13 106.3(9) . . ? C15 C14 H14A 110.5 . . ? C13 C14 H14A 110.5 . . ? C15 C14 H14B 110.5 . . ? C13 C14 H14B 110.5 . . ? H14A C14 H14B 108.7 . . ? C17 C15 C14 115.5(11) . . ? C17 C15 N4 112.8(11) . . ? C14 C15 N4 106.4(9) . . ? C17 C15 C16 114.7(13) . . ? C14 C15 C16 102.9(12) . . ? N4 C15 C16 103.2(11) . . ? C12 C16 C19 116.6(11) . . ? C12 C16 C18 108.7(12) . . ? C19 C16 C18 106.3(11) . . ? C12 C16 C15 99.8(11) . . ? C19 C16 C15 117.0(14) . . ? C18 C16 C15 108.1(12) . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N4 C20 C21 115.7(8) . . ? N4 C20 H20A 108.4 . . ? C21 C20 H20A 108.4 . . ? N4 C20 H20B 108.4 . . ? C21 C20 H20B 108.4 . . ? H20A C20 H20B 107.4 . . ? C26 C21 C22 118.3(10) . . ? C26 C21 C20 119.5(10) . . ? C22 C21 C20 121.8(9) . . ? C23 C22 C21 120.8(11) . . ? C23 C22 C27 115.5(11) . . ? C21 C22 C27 123.7(10) . . ? C22 C23 C24 119.3(13) . . ? C22 C23 H23 120.3 . . ? C24 C23 H23 120.3 . . ? C25 C24 C23 119.7(13) . . ? C25 C24 C29 121.5(15) . . ? C23 C24 C29 118.7(17) . . ? C24 C25 C26 120.6(14) . . ? C24 C25 H25 119.7 . . ? C26 C25 H25 119.7 . . ? C25 C26 C21 121.1(13) . . ? C25 C26 C28 118.5(13) . . ? C21 C26 C28 120.3(12) . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C24 C29 H29A 109.5 . . ? C24 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C24 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? O1 C30 Re1 175.7(8) . . ? O2 C31 Re1 179.2(10) . . ? O3 C32 Re1 174.2(7) . . ? C1 N1 C5 119.0(7) . . ? C1 N1 Re1 123.4(6) . . ? C5 N1 Re1 117.5(5) . . ? C10 N2 C6 116.3(7) . . ? C10 N2 Re1 128.7(5) . . ? C6 N2 Re1 115.0(5) . . ? C11 N3 C10 119.6(7) . . ? C11 N3 C12 119.4(7) . . ? C10 N3 C12 118.6(7) . . ? C11 N4 C20 121.1(7) . . ? C11 N4 C15 120.7(8) . . ? C20 N4 C15 117.4(8) . . ? C31 Re1 C32 82.8(4) . . ? C31 Re1 C30 88.7(4) . . ? C32 Re1 C30 87.8(3) . . ? C31 Re1 N1 94.7(3) . . ? C32 Re1 N1 174.8(3) . . ? C30 Re1 N1 96.6(3) . . ? C31 Re1 N2 169.4(3) . . ? C32 Re1 N2 107.5(3) . . ? C30 Re1 N2 94.5(3) . . ? N1 Re1 N2 74.8(2) . . ? C31 Re1 Cl1 96.0(3) . . ? C32 Re1 Cl1 91.1(2) . . ? C30 Re1 Cl1 175.0(3) . . ? N1 Re1 Cl1 84.65(18) . . ? N2 Re1 Cl1 81.13(16) . . ? O8 Cl2 O6 119.0(11) . . ? O8 Cl2 O9 108.0(10) . . ? O6 Cl2 O9 119.5(12) . . ? O8 Cl2 O7 105.3(11) . . ? O6 Cl2 O7 102.5(10) . . ? O9 Cl2 O7 99.4(9) . . ? O8A Cl2A O9A 112.0(13) . . ? O8A Cl2A O6A 117.7(14) . . ? O9A Cl2A O6A 108.7(13) . . ? O8A Cl2A O7A 114.4(14) . . ? O9A Cl2A O7A 99.2(11) . . ? O6A Cl2A O7A 102.9(12) . . ? C34 C33 H33A 109.5 . . ? C34 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C34 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O4 C34 C33 124.1(11) . . ? O4 C34 C35 120.7(11) . . ? C33 C34 C35 114.9(9) . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C37 C36 H36A 109.5 . . ? C37 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C37 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? O5 C37 C36 124.1(15) . . ? O5 C37 C38 118.9(14) . . ? C36 C37 C38 113.0(12) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.343(11) . ? C1 C2 1.380(14) . ? C1 H1 0.9300 . ? C2 C3 1.38(2) . ? C2 H2 0.9300 . ? C3 C4 1.351(19) . ? C3 H3 0.9300 . ? C4 C5 1.400(12) . ? C4 H4 0.9300 . ? C5 N1 1.350(11) . ? C5 C6 1.472(13) . ? C6 N2 1.362(10) . ? C6 C7 1.372(12) . ? C7 C8 1.371(16) . ? C7 H7 0.9300 . ? C8 C9 1.321(16) . ? C8 H8 0.9300 . ? C9 C10 1.385(12) . ? C9 H9 0.9300 . ? C10 N2 1.347(10) . ? C10 N3 1.433(10) . ? C11 N4 1.310(10) . ? C11 N3 1.317(10) . ? C11 H11 0.9300 . ? C12 N3 1.501(11) . ? C12 C13 1.509(13) . ? C12 C16 1.528(17) . ? C12 H12 0.9800 . ? C13 C14 1.552(14) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.521(18) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C17 1.472(17) . ? C15 N4 1.545(13) . ? C15 C16 1.578(14) . ? C16 C19 1.533(19) . ? C16 C18 1.572(18) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 N4 1.503(12) . ? C20 C21 1.514(14) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C26 1.405(15) . ? C21 C22 1.417(15) . ? C22 C23 1.364(16) . ? C22 C27 1.487(18) . ? C23 C24 1.45(2) . ? C23 H23 0.9300 . ? C24 C25 1.36(2) . ? C24 C29 1.51(2) . ? C25 C26 1.38(2) . ? C25 H25 0.9300 . ? C26 C28 1.525(19) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 O1 1.132(11) . ? C30 Re1 1.927(8) . ? C31 O2 1.160(11) . ? C31 Re1 1.894(9) . ? C32 O3 1.141(9) . ? C32 Re1 1.913(8) . ? N1 Re1 2.167(6) . ? N2 Re1 2.228(6) . ? Cl1 Re1 2.452(2) . ? Cl2 O8 1.381(10) . ? Cl2 O6 1.407(10) . ? Cl2 O9 1.450(9) . ? Cl2 O7 1.500(10) . ? Cl2A O8A 1.316(14) . ? Cl2A O9A 1.452(12) . ? Cl2A O6A 1.457(13) . ? Cl2A O7A 1.466(13) . ? O4 C34 1.199(10) . ? C33 C34 1.485(10) . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 C35 1.500(11) . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? O5 C37 1.203(12) . ? C36 C37 1.489(12) . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 C38 1.503(12) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ?