#------------------------------------------------------------------------------ #$Date: 2026-06-30 01:17:23 +0100 (Tue, 30 Jun 2026) $ #$Revision: 306684 $ #$URL: svn://www.crystallography.net/cod/cif/7/72/11/7721186.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_7721186 loop_ _publ_author_name 'Jacobs, Frederick J. F.' 'Fourie, Eleanor' 'Brink, Alice' _publ_section_title ; Engineering the rhenium metalation of phenanthroline imino complexes for variable structure activity relationships. ; _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_paper_doi 10.1039/d6dt00636a _journal_year 2026 _chemical_formula_sum 'C27 H23.04 Br N3 O10.52 Re2' _chemical_formula_weight 1010.12 _chemical_name_common fac-[Re(CO)3Br(Phen5MeSal)Re(CO)3(MeOH)] _chemical_name_systematic fac-{2-([1,10-Phenanthrolin-5-ylimino]methyl)phenolato-N,N'}-(methanol)(bromido)-hexacarbonyl-di-rhenium(I) _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2026-06-02 deposited with the CCDC. 2026-06-15 downloaded from the CCDC. ; _cell_angle_alpha 76.475(6) _cell_angle_beta 84.564(8) _cell_angle_gamma 81.830(7) _cell_formula_units_Z 2 _cell_length_a 7.8174(14) _cell_length_b 10.9256(17) _cell_length_c 18.312(3) _cell_measurement_reflns_used 7935 _cell_measurement_temperature 109(2) _cell_measurement_theta_max 64.191 _cell_measurement_theta_min 2.487 _cell_volume 1502.1(4) _computing_data_collection 'APEX5 (Bruker, 2016)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _diffrn_ambient_temperature 109(2) _diffrn_measured_fraction_theta_full 0.980 _diffrn_measured_fraction_theta_max 0.980 _diffrn_measurement_device_type 'Bruker D8 Venture 4K Kappa Photon III C28 diffractometer' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0617 _diffrn_reflns_av_unetI/netI 0.0312 _diffrn_reflns_Laue_measured_fraction_full 0.980 _diffrn_reflns_Laue_measured_fraction_max 0.980 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 42707 _diffrn_reflns_point_group_measured_fraction_full 0.980 _diffrn_reflns_point_group_measured_fraction_max 0.980 _diffrn_reflns_theta_full 64.787 _diffrn_reflns_theta_max 64.787 _diffrn_reflns_theta_min 2.487 _exptl_absorpt_coefficient_mu 17.623 _exptl_absorpt_correction_T_max 0.7525 _exptl_absorpt_correction_T_min 0.4360 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1509 before and 0.0926 after correction. The Ratio of minimum to maximum transmission is 0.5794. The \l/2 correction factor is Not present. ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 2.233 _exptl_crystal_description Plate _exptl_crystal_F_000 950 _exptl_crystal_size_max 0.090 _exptl_crystal_size_mid 0.023 _exptl_crystal_size_min 0.011 _refine_diff_density_max 1.510 _refine_diff_density_min -3.014 _refine_diff_density_rms 0.194 _refine_ls_extinction_coef 0.00038(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2018/3 (Sheldrick 2018)' _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 430 _refine_ls_number_reflns 4983 _refine_ls_number_restraints 6 _refine_ls_restrained_S_all 1.071 _refine_ls_R_factor_all 0.0609 _refine_ls_R_factor_gt 0.0484 _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^)+(0.0190P)^2^+28.4529P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1024 _refine_ls_wR_factor_ref 0.1143 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4294 _reflns_number_total 4983 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d6dt00636a2.cif _cod_data_source_block cu_v1_22ffj2_0m _cod_database_code 7721186 _shelx_shelxl_version_number 2018/3 _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 0.300 _shelx_estimated_absorpt_t_max 0.830 _shelx_res_file ; TITL shelxt_a.res in P-1 cu_v1_22ffj2_0m.res created by SHELXL-2018/3 at 15:41:16 on 25-May-2026 CELL 1.54178 7.8174 10.9256 18.3119 76.475 84.564 81.83 ZERR 2 0.0014 0.0017 0.0029 0.006 0.008 0.007 LATT 1 SFAC C H Br N O Re UNIT 54 46.072 2 6 21.036 4 EQIV $1 -X,1-Y,-Z DFIX 0.87 0.01 O4B H4B DANG 1.914358 0.02 C4B H4B DANG 2.773034 0.02 Re1B H4B EADP C18A C19A C17A EADP C21A C22A C20A EADP C21B C22B C17B EADP C17B C18B C20B EADP O1A C1A EADP O4A O4B EADP O3 C3 EADP C3B O3B EADP O3A C3A EADP O2A C2A EADP O1B C1B EADP O3 O2 EADP C2A C2B EADP C23A C23B DFIX 0.87 0.01 O4A H4A DANG 1.94466 0.02 C4A H4A DANG 2.812194 0.02 Re1A H4A EADP O5 O6 L.S. 20 PLAN 10 SIZE 0.011 0.023 0.09 TEMP -164.15 CONF HTAB C23A O2B_$1 HTAB C21A O2B_$1 BOND $H LIST 4 MORE -1 ABIN fmap 2 acta MERG 2 OMIT -4 180 REM REM REM WGHT 0.019000 28.452900 EXTI 0.000384 FVAR 0.09290 0.49109 C1 1 0.282661 0.229895 0.712805 11.00000 0.09589 0.02331 = 0.03239 -0.00378 -0.01604 0.00513 C2 1 0.016514 0.133078 0.675187 11.00000 0.13296 0.02999 = 0.02585 -0.00575 -0.00657 -0.02156 C3 1 0.054738 0.381457 0.610976 11.00000 0.09187 0.04869 = 0.03700 -0.01090 -0.00750 -0.03338 C4 1 -0.005584 0.156130 0.495085 11.00000 0.04737 0.01127 = 0.02948 -0.00274 0.00339 0.00607 AFIX 43 H4 2 -0.083189 0.123910 0.535909 11.00000 -1.20000 AFIX 0 C17 1 -0.042052 0.152332 0.422256 11.00000 0.03893 0.01826 = 0.02580 -0.00448 -0.00473 0.00339 AFIX 43 H17 2 -0.142612 0.118961 0.414090 11.00000 -1.20000 AFIX 0 C6 1 0.069477 0.197445 0.363142 11.00000 0.02568 0.01960 = 0.02668 -0.00862 -0.01086 0.00606 AFIX 43 H6 2 0.046065 0.196814 0.313271 11.00000 -1.20000 AFIX 0 C7 1 0.220093 0.245140 0.376525 11.00000 0.03095 0.02172 = 0.02498 -0.00833 -0.00582 0.00396 C8 1 0.244487 0.247158 0.451417 11.00000 0.04163 0.01682 = 0.02379 -0.00748 -0.01644 0.01310 C9 1 0.392796 0.295146 0.468558 11.00000 0.04125 0.02076 = 0.04429 -0.01754 -0.02236 0.01122 C10 1 0.546642 0.335144 0.560722 11.00000 0.06757 0.03867 = 0.06318 -0.02994 -0.04440 0.01931 AFIX 43 H10 2 0.561361 0.332001 0.612061 11.00000 -1.20000 AFIX 0 C11 1 0.673578 0.382405 0.506016 11.00000 0.05030 0.03652 = 0.09844 -0.04459 -0.04385 0.02093 AFIX 43 H11 2 0.771021 0.411226 0.520973 11.00000 -1.20000 AFIX 0 C12 1 0.658969 0.387564 0.431386 11.00000 0.02127 0.03938 = 0.07204 -0.03758 -0.01458 0.00664 AFIX 43 H12 2 0.744252 0.420456 0.394324 11.00000 -1.20000 AFIX 0 C13 1 0.512133 0.342177 0.410817 11.00000 0.03133 0.02087 = 0.04789 -0.01809 -0.01297 0.01038 C14 1 0.486096 0.341021 0.334960 11.00000 0.02341 0.03491 = 0.04606 -0.02369 -0.00109 -0.00557 AFIX 43 H14 2 0.567109 0.373003 0.295542 11.00000 -1.20000 AFIX 0 C15 1 0.345769 0.294294 0.319092 11.00000 0.02780 0.02346 = 0.03282 -0.01507 -0.00762 0.00291 C16 1 0.334460 0.184847 0.224654 11.00000 0.02617 0.05858 = 0.04434 -0.03446 0.00139 -0.01015 PART 1 AFIX 43 H16 2 0.363027 0.118963 0.267309 21.00000 -1.20000 AFIX 43 PART 2 H16A 2 0.375704 0.110450 0.259996 -21.00000 -1.20000 AFIX 0 PART 0 BR1 3 0.397952 0.003569 0.622139 11.00000 0.11744 0.02399 = 0.05013 -0.01223 -0.04720 0.01985 N1 4 0.405097 0.294200 0.543099 11.00000 0.06212 0.02041 = 0.04031 -0.01601 -0.03224 0.01835 N2 4 0.132777 0.202771 0.509943 11.00000 0.05566 0.01377 = 0.02313 -0.00442 -0.01524 0.00550 N3 4 0.317686 0.295706 0.242329 11.00000 0.03513 0.04222 = 0.02686 -0.01702 0.00536 -0.01329 O1 5 0.330623 0.236399 0.769914 11.00000 0.11289 0.04617 = 0.02879 -0.00491 -0.03098 -0.00335 O2 5 -0.103139 0.080762 0.705778 11.00000 0.09187 0.04869 = 0.03700 -0.01090 -0.00750 -0.03338 O3 5 -0.017322 0.470889 0.604461 11.00000 0.09187 0.04869 = 0.03700 -0.01090 -0.00750 -0.03338 RE2 6 0.199515 0.217466 0.619527 11.00000 0.08859 0.01874 = 0.02375 -0.00592 -0.02232 0.00534 PART 1 C22B 1 0.284656 0.223403 0.098038 21.00000 0.02603 0.02686 = 0.02077 -0.00407 -0.00593 -0.00213 C17B 1 0.323748 0.136680 0.165521 21.00000 0.02603 0.02686 = 0.02077 -0.00407 -0.00593 -0.00213 C18B 1 0.347575 0.003634 0.166301 21.00000 0.02603 0.02686 = 0.02077 -0.00407 -0.00593 -0.00213 AFIX 43 H18B 2 0.378706 -0.055638 0.211351 21.00000 -1.20000 AFIX 0 C19B 1 0.326447 -0.040596 0.103264 21.00000 0.02123 0.02577 = 0.02894 -0.01168 -0.00051 0.00322 AFIX 43 H19B 2 0.342575 -0.128986 0.104823 21.00000 -1.20000 AFIX 0 C20B 1 0.279503 0.050040 0.035208 21.00000 0.02603 0.02686 = 0.02077 -0.00407 -0.00593 -0.00213 C21B 1 0.265229 0.174328 0.034426 21.00000 0.02603 0.02686 = 0.02077 -0.00407 -0.00593 -0.00213 AFIX 43 H21B 2 0.240575 0.233112 -0.011604 21.00000 -1.20000 AFIX 0 C23B 1 0.253399 -0.001113 -0.032965 21.00000 0.05555 0.04441 = 0.03341 -0.02135 0.00296 -0.01921 AFIX 33 H23A 2 0.270066 -0.094063 -0.019545 21.00000 -1.50000 H23B 2 0.135786 0.028650 -0.049141 21.00000 -1.50000 H23C 2 0.337546 0.029157 -0.074077 21.00000 -1.50000 AFIX 0 O9 5 0.256840 0.347733 0.089962 21.00000 0.04568 0.01883 = 0.01496 -0.00831 0.00219 0.00053 O2A 5 0.237804 0.703267 0.041428 21.00000 0.05421 0.02857 = 0.03816 0.00126 -0.01367 -0.00788 C2A 1 0.254919 0.612044 0.088861 21.00000 0.05421 0.02857 = 0.03816 0.00126 -0.01367 -0.00788 RE1A 6 0.280829 0.460704 0.166732 21.00000 0.03326 0.01618 = 0.01869 -0.00215 -0.00573 -0.00284 O1A 5 -0.100950 0.497377 0.220540 21.00000 0.01561 0.05714 = 0.07307 -0.03578 0.00505 0.00686 C1A 1 0.030371 0.485525 0.197811 21.00000 0.01561 0.05714 = 0.07307 -0.03578 0.00505 0.00686 O3A 5 0.339719 0.636947 0.267407 21.00000 0.04324 0.03883 = 0.01579 -0.00017 0.01027 -0.01679 C3A 1 0.314202 0.567368 0.229054 21.00000 0.04324 0.03883 = 0.01579 -0.00017 0.01027 -0.01679 O4A 5 0.555843 0.407952 0.137929 21.00000 0.03008 0.02726 = 0.03851 0.00235 0.01398 -0.01264 H4A 2 0.621005 0.341142 0.161463 21.00000 -1.50000 C4A 1 0.671903 0.499527 0.095602 21.00000 0.04003 0.04331 = 0.03827 0.00201 -0.00518 -0.00949 AFIX 137 H4AA 2 0.628168 0.538445 0.045974 21.00000 -1.50000 H4AB 2 0.788652 0.455224 0.089455 21.00000 -1.50000 H4AC 2 0.675799 0.565597 0.123329 21.00000 -1.50000 AFIX 0 PART 2 C23A 1 0.183473 0.074966 -0.056456 -21.00000 0.05555 0.04441 = 0.03341 -0.02135 0.00296 -0.01921 AFIX 33 H23D 2 0.124446 0.149293 -0.089815 -21.00000 -1.50000 H23E 2 0.294423 0.047709 -0.081131 -21.00000 -1.50000 H23F 2 0.110974 0.005878 -0.045478 -21.00000 -1.50000 AFIX 66 C22A 1 0.204619 0.265704 0.089763 -21.00000 0.03630 0.03632 = 0.01805 -0.00661 0.00301 -0.01507 C17A 1 0.287124 0.175257 0.146328 -21.00000 0.02741 0.02606 = 0.02815 -0.00978 -0.00160 -0.00167 C18A 1 0.333626 0.051597 0.137686 -21.00000 0.02741 0.02606 = 0.02815 -0.00978 -0.00160 -0.00167 AFIX 43 H18A 2 0.390015 -0.010219 0.176346 -21.00000 -1.20000 AFIX 65 C19A 1 0.297622 0.018382 0.072479 -21.00000 0.02741 0.02606 = 0.02815 -0.00978 -0.00160 -0.00167 AFIX 43 H19A 2 0.329404 -0.066135 0.066573 -21.00000 -1.20000 AFIX 65 C20A 1 0.215117 0.108827 0.015913 -21.00000 0.03630 0.03632 = 0.01805 -0.00661 0.00301 -0.01507 C21A 1 0.168615 0.232488 0.024554 -21.00000 0.03630 0.03632 = 0.01805 -0.00661 0.00301 -0.01507 AFIX 43 H21A 2 0.112226 0.294304 -0.014106 -21.00000 -1.20000 AFIX 0 O4 5 0.149016 0.388145 0.095276 -21.00000 0.05253 0.02696 = 0.02600 -0.01258 -0.00286 0.00129 O2B 5 0.047909 0.752046 0.085251 -21.00000 0.07676 0.02364 = 0.05124 0.00565 -0.03667 -0.00216 C2B 1 0.099133 0.651958 0.117049 -21.00000 0.05421 0.02857 = 0.03816 0.00126 -0.01367 -0.00788 RE1B 6 0.192756 0.489659 0.175197 -21.00000 0.03295 0.01901 = 0.01795 -0.00351 -0.00382 -0.00382 O1B 5 -0.162365 0.477026 0.262064 -21.00000 0.03041 0.03489 = 0.04631 -0.02265 -0.00133 0.00362 C1B 1 -0.017972 0.484139 0.224747 -21.00000 0.03041 0.03489 = 0.04631 -0.02265 -0.00133 0.00362 C3B 1 0.255591 0.582039 0.243857 -21.00000 0.01843 0.03159 = 0.01693 -0.01146 0.00654 -0.01027 O3B 5 0.287409 0.637563 0.285026 -21.00000 0.01843 0.03159 = 0.01693 -0.01146 0.00654 -0.01027 O4B 5 0.446171 0.486025 0.113312 -21.00000 0.03008 0.02726 = 0.03851 0.00235 0.01398 -0.01264 H4B 2 0.527540 0.421784 0.122562 -21.00000 -1.50000 C4B 1 0.524620 0.597246 0.076584 -21.00000 0.06718 0.03740 = 0.04632 -0.00452 0.03141 -0.00874 AFIX 33 H4BA 2 0.637558 0.572162 0.052674 -21.00000 -1.50000 H4BB 2 0.449765 0.649927 0.038215 -21.00000 -1.50000 H4BC 2 0.540150 0.645657 0.113765 -21.00000 -1.50000 AFIX 6 O5 5 0.935198 0.437709 0.035379 -21.00000 0.03619 0.06150 = 0.06962 0.01710 0.00804 0.00730 H5A 2 0.922879 0.507304 0.000621 -21.00000 -1.50000 H5B 2 1.045106 0.410413 0.031725 -21.00000 -1.50000 AFIX 6 O6 5 0.695340 0.308990 0.119638 -21.00000 0.03619 0.06150 = 0.06962 0.01710 0.00804 0.00730 H6A 2 0.717051 0.349440 0.152682 -21.00000 -1.50000 H6B 2 0.761423 0.336974 0.079998 -21.00000 -1.50000 AFIX 0 HKLF 4 REM shelxt_a.res in P-1 REM wR2 = 0.1143, GooF = S = 1.071, Restrained GooF = 1.071 for all data REM R1 = 0.0484 for 4294 Fo > 4sig(Fo) and 0.0609 for all 4983 data REM 430 parameters refined using 6 restraints END WGHT 0.0190 28.4561 REM Highest difference peak 1.510, deepest hole -3.014, 1-sigma level 0.194 Q1 1 -0.0056 0.0735 0.7162 11.00000 0.05 1.51 Q2 1 0.2066 0.2770 0.5821 11.00000 0.05 1.30 Q3 1 0.2822 0.1874 0.6174 11.00000 0.05 1.29 Q4 1 0.1544 0.2001 0.6241 11.00000 0.05 1.17 Q5 1 -0.1683 0.0637 0.6887 11.00000 0.05 0.87 Q6 1 0.3499 0.1053 0.5929 11.00000 0.05 0.86 Q7 1 0.3087 0.5435 0.1012 11.00000 0.05 0.83 Q8 1 0.3013 0.3816 0.1822 11.00000 0.05 0.82 Q9 1 0.3560 0.0001 0.6298 11.00000 0.05 0.79 Q10 1 0.1565 0.3803 0.2234 11.00000 0.05 0.78 ; _shelx_res_checksum 14693 _shelx_fab_file ; -9 -3 1 -1.4534 -0.0629 -9 -2 1 -1.4666 -0.0185 -9 -1 1 0.7902 -0.1107 -9 -1 2 1.8639 -0.0282 -9 0 1 1.2548 -0.0827 -8 -7 1 -0.5232 0.0934 -8 -6 1 0.6655 0.1038 -8 -6 2 1.1341 0.0735 -8 -6 3 0.0498 -0.0951 -8 -5 1 1.5301 0.1872 -8 -5 2 0.7333 0.1063 -8 -5 3 -1.1094 -0.1282 -8 -5 4 -1.7388 -0.1616 -8 -5 5 -0.1971 -0.0201 -8 -4 1 1.2999 0.2067 -8 -4 2 -0.9486 0.0105 -8 -4 3 -3.1071 -0.2194 -8 -4 4 -1.5698 -0.1959 -8 -4 5 2.4223 0.0308 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1 0 -2.0531 0.2408 7 1 1 1.3862 0.0866 7 1 2 3.3368 -0.1243 7 1 3 0.6864 -0.1629 7 1 4 -2.7118 0.0021 7 1 5 -1.7485 0.1575 7 1 6 1.5158 0.0909 7 1 7 2.3449 -0.1005 7 1 8 0.7356 -0.1422 7 1 9 -0.6916 0.0032 7 1 10 -1.1882 0.0980 7 1 11 -1.2798 0.0213 7 1 12 -0.8223 -0.0737 7 1 13 0.4417 -0.0469 7 1 14 1.4684 0.0699 7 2 0 1.6312 0.1637 7 2 1 3.3821 -0.1276 7 2 2 1.3146 -0.1646 7 2 3 -2.3414 0.0487 7 2 4 -2.2320 0.1202 7 2 5 1.1953 -0.0211 7 2 6 2.5522 -0.0921 7 2 7 0.5665 -0.0192 7 2 8 -1.4593 0.0038 7 2 9 -1.6253 -0.0465 7 2 10 -0.6745 0.0068 7 2 11 0.1735 0.1442 7 2 12 0.4517 0.1269 7 2 13 0.5953 -0.0493 7 2 14 0.7974 -0.0838 7 2 15 0.4564 0.0519 7 3 0 2.7211 -0.0292 7 3 1 0.8707 -0.0592 7 3 2 -1.9238 0.0556 7 3 3 -1.9312 0.0735 7 3 4 0.9075 -0.0840 7 3 5 2.1541 -0.1329 7 3 6 0.2992 0.0292 7 3 7 -1.5955 0.1152 7 3 8 -1.5674 -0.0134 7 3 9 -0.3061 -0.0822 7 3 10 0.9273 0.0919 7 3 11 1.0117 0.2212 7 3 12 0.1270 0.0177 7 3 13 -0.1602 -0.2534 7 3 14 0.3419 -0.1940 7 3 15 0.2837 0.0252 7 4 0 0.0668 0.1094 7 4 1 -2.1264 0.1171 7 4 2 -1.4755 -0.0152 7 4 3 1.2651 -0.1157 7 4 4 2.0129 -0.0825 7 4 5 -0.0681 0.0208 7 4 6 -1.5445 0.0862 7 4 7 -0.9760 0.0644 7 4 8 0.0578 -0.0149 7 4 9 0.7822 -0.0353 7 4 10 1.0086 0.0454 7 4 11 0.2536 0.0456 7 4 12 -0.5863 -0.1285 7 4 13 -0.3639 -0.2119 7 4 14 0.1634 -0.0304 7 4 15 0.1265 0.1646 7 5 0 -2.3074 0.2182 7 5 1 -1.4839 -0.0127 7 5 2 1.5654 -0.1895 7 5 3 2.4548 -0.0531 7 5 4 0.1154 0.0869 7 5 5 -1.5978 0.0304 7 5 6 -0.7867 -0.0049 7 5 7 0.2625 0.0404 7 5 8 0.3399 -0.0144 7 5 9 0.3873 -0.0969 7 5 10 0.3355 -0.0434 7 5 11 -0.2066 0.0194 7 5 12 -0.5054 0.0046 7 5 13 -0.2625 0.0519 7 5 14 0.1254 0.1242 7 5 15 0.4950 0.0663 7 6 0 -1.4414 0.0995 7 6 1 1.2935 -0.1578 7 6 2 2.5180 -0.1228 7 6 3 0.6801 0.0994 7 6 4 -1.3041 0.0844 7 6 5 -1.1039 -0.0561 7 6 6 -0.1512 -0.0428 7 6 7 0.0091 -0.0036 7 6 8 0.0445 -0.0351 7 6 9 0.3492 0.0118 7 6 10 0.2835 0.0833 7 6 11 -0.1188 0.0638 7 6 12 -0.3241 0.0926 7 6 13 -0.1152 0.1211 7 6 14 0.4404 -0.0988 7 7 0 1.0389 0.0194 7 7 1 1.8347 -0.1155 7 7 2 0.5750 -0.0158 7 7 3 -0.8135 0.0638 7 7 4 -1.0496 -0.0125 7 7 5 -0.6405 -0.0493 7 7 6 -0.2406 -0.0171 7 7 7 0.1617 0.0290 7 7 8 0.5032 0.1504 7 7 9 0.5126 0.1795 7 7 10 0.2087 -0.0499 7 7 11 -0.1662 -0.1634 7 7 12 -0.2690 0.0411 7 7 13 0.1021 0.0165 7 8 0 1.2253 0.0052 7 8 1 -0.2081 -0.1030 7 8 2 -0.8072 -0.1091 7 8 3 -0.4956 -0.0699 7 8 4 -0.3422 0.0641 7 8 5 -0.1104 0.1733 7 8 6 0.3504 0.1050 7 8 7 0.4346 0.0597 7 8 8 0.2790 0.1009 7 8 9 0.3152 -0.0997 7 8 10 0.1060 -0.3824 7 8 11 -0.3916 -0.1807 7 8 12 -0.3222 0.2000 7 9 0 -0.6442 -0.1249 7 9 1 -1.0789 -0.2456 7 9 2 -0.0553 -0.2115 7 9 3 0.4192 0.0933 7 9 4 0.4359 0.4554 7 9 5 0.5469 0.3527 7 9 6 0.0445 -0.1327 7 9 7 -0.5302 -0.3384 7 9 8 0.0341 -0.2128 7 9 9 0.5888 -0.1995 8 -4 0 2.3870 0.3004 8 -4 1 1.4044 0.0821 8 -4 2 -1.0247 -0.4946 8 -4 3 -2.1464 -0.2664 8 -4 4 -0.2860 0.3792 8 -3 0 -0.1619 -0.0070 8 -3 1 -0.8858 -0.1632 8 -3 2 -1.2166 -0.1100 8 -3 3 -0.6000 0.2135 8 -3 4 0.5315 0.1469 8 -3 5 0.3021 -0.2754 8 -3 6 -0.6225 -0.1318 8 -2 0 -0.8832 0.0081 8 -2 1 -0.0682 0.1783 8 -2 2 -0.3943 0.1040 8 -2 3 -0.3109 -0.0257 8 -2 4 0.4864 -0.1092 8 -2 5 0.5257 -0.0296 8 -2 6 0.0834 0.2127 8 -2 7 0.1394 0.2154 8 -2 8 0.3049 -0.1344 8 -1 0 0.5956 0.2497 8 -1 1 -0.5413 0.1164 8 -1 2 -1.4377 -0.1452 8 -1 3 0.3317 -0.0450 8 -1 4 1.9710 0.1298 8 -1 5 0.7616 0.0572 8 -1 6 -1.0254 -0.0691 8 -1 7 -0.8543 -0.0820 8 -1 8 0.2051 -0.0570 8 -1 9 0.3679 -0.0341 8 -1 10 -0.1967 0.0097 8 0 0 -1.2792 0.0488 8 0 1 -2.7533 -0.0906 8 0 2 -0.4991 0.0199 8 0 3 3.0451 0.1906 8 0 4 2.2484 0.0046 8 0 5 -1.6295 -0.2447 8 0 6 -2.5897 -0.1213 8 0 7 -0.1627 0.1307 8 0 8 1.3116 0.1260 8 0 9 0.5697 -0.0167 8 0 10 -0.1637 -0.0281 8 0 11 0.0038 0.0548 8 1 0 -3.5388 -0.0439 8 1 1 -1.4381 0.1191 8 1 2 2.8321 0.1886 8 1 3 3.6337 -0.0241 8 1 4 -0.7106 -0.2396 8 1 5 -3.6733 -0.1090 8 1 6 -1.2742 0.1465 8 1 7 1.9417 0.1583 8 1 8 1.7853 0.0158 8 1 9 0.1191 -0.0562 8 1 10 -0.4674 -0.0762 8 1 11 -0.4141 -0.0821 8 2 0 -1.4795 0.0831 8 2 1 1.8641 0.1346 8 2 2 3.5416 -0.0134 8 2 3 0.7872 -0.1322 8 2 4 -2.9783 -0.0340 8 2 5 -2.2313 0.0837 8 2 6 1.3765 0.0324 8 2 7 2.4851 -0.0234 8 2 8 0.6626 0.0119 8 2 9 -1.0062 -0.0463 8 2 10 -1.2307 -0.1636 8 2 11 -0.6324 -0.0479 8 2 12 0.0103 0.2105 8 3 0 1.4068 -0.0485 8 3 1 2.4248 -0.0108 8 3 2 1.1769 0.0293 8 3 3 -1.4989 0.0554 8 3 4 -1.9906 0.0084 8 3 5 0.3364 -0.0942 8 3 6 1.9168 -0.0894 8 3 7 0.9820 0.0455 8 3 8 -0.8305 0.0708 8 3 9 -1.6758 -0.0718 8 3 10 -0.8949 -0.0700 8 3 11 0.5895 0.1723 8 3 12 0.9366 0.2561 8 4 0 1.7331 -0.1131 8 4 1 0.6621 0.1165 8 4 2 -0.9285 0.1486 8 4 3 -1.2569 -0.0297 8 4 4 0.0356 -0.1476 8 4 5 1.0197 -0.0801 8 4 6 0.7020 0.0462 8 4 7 -0.2370 0.0898 8 4 8 -1.1667 0.0427 8 4 9 -1.0935 0.0052 8 4 10 0.4380 0.0512 8 4 11 1.4144 0.0824 8 4 12 0.4242 -0.0380 8 5 0 0.4872 0.0189 8 5 1 -1.0970 0.1454 8 5 2 -1.1735 -0.0010 8 5 3 0.2049 -0.1116 8 5 4 0.9289 -0.0134 8 5 5 0.4986 0.0627 8 5 6 0.0833 0.0191 8 5 7 -0.4008 0.0178 8 5 8 -0.9840 0.0590 8 5 9 -0.3022 0.0114 8 5 10 1.0783 -0.0783 8 5 11 0.8417 -0.1040 8 6 0 -0.9439 -0.0020 8 6 1 -1.3440 -0.0008 8 6 2 0.0817 -0.0166 8 6 3 1.1802 0.0801 8 6 4 0.8077 0.0868 8 6 5 0.2055 -0.0626 8 6 6 -0.1839 -0.0940 8 6 7 -0.8896 0.0208 8 6 8 -0.9165 0.0219 8 6 9 0.3379 -0.0668 8 6 10 0.9834 -0.0463 8 7 0 -0.9675 -0.0513 8 7 1 -0.0608 0.0149 8 7 2 0.9014 0.1439 8 7 3 0.8849 0.1270 8 7 4 0.3382 -0.1096 8 7 5 -0.2667 -0.2033 8 7 6 -0.9439 -0.0265 8 7 7 -1.0424 0.0744 8 7 8 -0.0619 0.0295 9 0 0 0.8292 0.2091 9 0 1 -1.8482 -0.0811 9 0 2 -2.8182 -0.2618 9 0 3 0.5956 0.0731 9 0 4 3.4641 0.3128 9 1 0 -1.4364 -0.0451 9 1 1 -3.0229 -0.1892 9 1 2 -0.6904 0.0321 9 1 3 3.3863 0.2458 9 1 4 2.9191 0.0117 9 1 5 -1.4687 -0.2478 9 2 0 -2.0790 -0.0642 9 2 1 -1.1475 -0.0117 9 2 2 1.6832 0.1092 9 2 3 2.9523 0.0224 9 2 4 0.1182 -0.1257 9 2 5 -2.6864 -0.0176 9 2 6 -1.4890 0.1374 9 3 0 -0.5415 -0.0172 9 3 1 0.4354 -0.0301 9 3 2 1.6096 0.0136 9 3 3 0.9980 0.0144 9 3 4 -1.1139 0.0173 9 3 5 -1.5507 0.0364 9 4 2 0.8032 0.0559 9 4 3 -0.1012 0.0163 9 4 4 -0.8674 -0.0658 0 0 0 0.0 0.0 ; _shelx_fab_checksum 61091 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 C1 C 0.2827(17) 0.2299(9) 0.7128(6) 0.051(3) Uani 1 1 d . . . . . C2 C 0.017(2) 0.1331(10) 0.6752(6) 0.062(4) Uani 1 1 d . . . . . C3 C 0.0547(18) 0.3815(12) 0.6110(6) 0.0563(14) Uani 1 1 d . . . . . C4 C -0.0056(12) 0.1561(7) 0.4951(5) 0.031(2) Uani 1 1 d . . . . . H4 H -0.083189 0.123910 0.535909 0.037 Uiso 1 1 calc R U . . . C17 C -0.0421(12) 0.1523(8) 0.4223(5) 0.0283(19) Uani 1 1 d . . . . . H17 H -0.142612 0.118961 0.414090 0.034 Uiso 1 1 calc R U . . . C6 C 0.0695(10) 0.1974(7) 0.3631(5) 0.0237(18) Uani 1 1 d . . . . . H6 H 0.046065 0.196814 0.313271 0.028 Uiso 1 1 calc R U . . . C7 C 0.2201(11) 0.2451(8) 0.3765(5) 0.0258(18) Uani 1 1 d . . . . . C8 C 0.2445(12) 0.2472(8) 0.4514(5) 0.0276(19) Uani 1 1 d . . . . . C9 C 0.3928(12) 0.2951(8) 0.4686(5) 0.034(2) Uani 1 1 d . . . . . C10 C 0.5466(16) 0.3351(10) 0.5607(7) 0.053(3) Uani 1 1 d . . . . . H10 H 0.561361 0.332001 0.612061 0.064 Uiso 1 1 calc R U . . . C11 C 0.6736(15) 0.3824(10) 0.5060(8) 0.057(4) Uani 1 1 d . . . . . H11 H 0.771021 0.411226 0.520973 0.068 Uiso 1 1 calc R U . . . C12 C 0.6590(12) 0.3876(9) 0.4314(6) 0.040(2) Uani 1 1 d . . . . . H12 H 0.744252 0.420456 0.394324 0.048 Uiso 1 1 calc R U . . . C13 C 0.5121(12) 0.3422(8) 0.4108(5) 0.032(2) Uani 1 1 d . . . . . C14 C 0.4861(11) 0.3410(9) 0.3350(5) 0.032(2) Uani 1 1 d . . . . . H14 H 0.567109 0.373003 0.295542 0.039 Uiso 1 1 calc R U . . . C15 C 0.3458(11) 0.2943(8) 0.3191(5) 0.0268(19) Uani 1 1 d . . . . . C16 C 0.3345(11) 0.1848(10) 0.2247(6) 0.039(2) Uani 1 1 d . . . . . H16 H 0.363027 0.118963 0.267309 0.047 Uiso 0.491(5) 1 calc R U P A 1 H16A H 0.375704 0.110450 0.259996 0.047 Uiso 0.509(5) 1 calc R U P A 2 Br1 Br 0.3980(2) 0.00357(10) 0.62214(7) 0.0633(4) Uani 1 1 d . . . . . N1 N 0.4051(11) 0.2942(7) 0.5431(4) 0.040(2) Uani 1 1 d . . . . . N2 N 0.1328(10) 0.2028(6) 0.5099(4) 0.0309(17) Uani 1 1 d . . . . . N3 N 0.3177(10) 0.2957(7) 0.2423(4) 0.0328(17) Uani 1 1 d . . . . . O1 O 0.3306(12) 0.2364(7) 0.7699(4) 0.062(2) Uani 1 1 d . . . . . O2 O -0.1031(12) 0.0808(7) 0.7058(4) 0.0563(14) Uani 1 1 d . . . . . O3 O -0.0173(12) 0.4709(8) 0.6045(4) 0.0563(14) Uani 1 1 d . . . . . Re2 Re 0.19952(7) 0.21747(4) 0.61953(2) 0.04345(19) Uani 1 1 d . . . . . C22B C 0.285(2) 0.2234(18) 0.0980(10) 0.025(2) Uani 0.491(5) 1 d . . P A 1 C17B C 0.324(3) 0.1367(19) 0.1655(11) 0.025(2) Uani 0.491(5) 1 d . . P A 1 C18B C 0.348(2) 0.0036(18) 0.1663(10) 0.025(2) Uani 0.491(5) 1 d . . P A 1 H18B H 0.378706 -0.055638 0.211351 0.030 Uiso 0.491(5) 1 calc R U P A 1 C19B C 0.326(2) -0.0406(18) 0.1033(10) 0.025(4) Uani 0.491(5) 1 d . . P A 1 H19B H 0.342575 -0.128986 0.104823 0.030 Uiso 0.491(5) 1 calc R U P A 1 C20B C 0.280(2) 0.0500(19) 0.0352(11) 0.025(2) Uani 0.491(5) 1 d . . P A 1 C21B C 0.265(2) 0.1743(18) 0.0344(9) 0.025(2) Uani 0.491(5) 1 d . . P A 1 H21B H 0.240575 0.233112 -0.011604 0.030 Uiso 0.491(5) 1 calc R U P A 1 C23B C 0.253(3) -0.001(2) -0.0330(12) 0.041(4) Uani 0.491(5) 1 d . . P A 1 H23A H 0.270066 -0.094063 -0.019545 0.062 Uiso 0.491(5) 1 calc R U P A 1 H23B H 0.135786 0.028650 -0.049141 0.062 Uiso 0.491(5) 1 calc R U P A 1 H23C H 0.337546 0.029157 -0.074077 0.062 Uiso 0.491(5) 1 calc R U P A 1 O9 O 0.257(2) 0.3477(12) 0.0900(6) 0.026(3) Uani 0.491(5) 1 d . . P A 1 O2A O 0.2378(18) 0.7033(12) 0.0414(7) 0.041(2) Uani 0.491(5) 1 d . . P A 1 C2A C 0.255(3) 0.6120(19) 0.0889(11) 0.041(2) Uani 0.491(5) 1 d . . P A 1 Re1A Re 0.2808(4) 0.46070(14) 0.16673(6) 0.0228(4) Uani 0.491(5) 1 d D . P A 1 O1A O -0.101(2) 0.4974(17) 0.2205(13) 0.047(4) Uani 0.491(5) 1 d . . P A 1 C1A C 0.030(3) 0.486(3) 0.1978(18) 0.047(4) Uani 0.491(5) 1 d . . P A 1 O3A O 0.340(3) 0.637(2) 0.2674(12) 0.033(5) Uani 0.491(5) 1 d . . P A 1 C3A C 0.314(3) 0.567(3) 0.2291(15) 0.033(5) Uani 0.491(5) 1 d . . P A 1 O4A O 0.5558(16) 0.4080(12) 0.1379(7) 0.034(2) Uani 0.491(5) 1 d D . P A 1 H4A H 0.621(4) 0.341(6) 0.161(6) 0.051 Uiso 0.491(5) 1 d D U P A 1 C4A C 0.672(3) 0.4995(19) 0.0956(11) 0.042(5) Uani 0.491(5) 1 d D . P A 1 H4AA H 0.628168 0.538445 0.045974 0.063 Uiso 0.491(5) 1 calc R U P A 1 H4AB H 0.788652 0.455224 0.089455 0.063 Uiso 0.491(5) 1 calc R U P A 1 H4AC H 0.675799 0.565597 0.123329 0.063 Uiso 0.491(5) 1 calc R U P A 1 C23A C 0.183(3) 0.075(2) -0.0565(11) 0.041(4) Uani 0.509(5) 1 d . . P A 2 H23D H 0.124446 0.149293 -0.089815 0.062 Uiso 0.509(5) 1 calc R U P A 2 H23E H 0.294423 0.047709 -0.081131 0.062 Uiso 0.509(5) 1 calc R U P A 2 H23F H 0.110974 0.005878 -0.045478 0.062 Uiso 0.509(5) 1 calc R U P A 2 C22A C 0.2046(17) 0.2657(9) 0.0898(6) 0.029(2) Uani 0.509(5) 1 d G . P A 2 C17A C 0.2871(17) 0.1753(11) 0.1463(6) 0.027(3) Uani 0.509(5) 1 d G . P A 2 C18A C 0.3336(15) 0.0516(10) 0.1377(7) 0.027(3) Uani 0.509(5) 1 d G . P A 2 H18A H 0.390015 -0.010219 0.176346 0.032 Uiso 0.509(5) 1 calc R U P A 2 C19A C 0.2976(16) 0.0184(10) 0.0725(8) 0.027(3) Uani 0.509(5) 1 d G . P A 2 H19A H 0.329404 -0.066135 0.066573 0.032 Uiso 0.509(5) 1 calc R U P A 2 C20A C 0.2151(17) 0.1088(12) 0.0159(6) 0.029(2) Uani 0.509(5) 1 d G . P A 2 C21A C 0.1686(17) 0.2325(11) 0.0246(5) 0.029(2) Uani 0.509(5) 1 d G . P A 2 H21A H 0.112226 0.294304 -0.014106 0.035 Uiso 0.509(5) 1 calc R U P A 2 O4 O 0.149(2) 0.3881(13) 0.0953(7) 0.035(3) Uani 0.509(5) 1 d . . P A 2 O2B O 0.048(2) 0.7520(12) 0.0853(8) 0.051(4) Uani 0.509(5) 1 d . . P A 2 C2B C 0.099(3) 0.6520(18) 0.1170(11) 0.041(2) Uani 0.509(5) 1 d . . P A 2 Re1B Re 0.1928(4) 0.48966(14) 0.17520(6) 0.0232(4) Uani 0.509(5) 1 d D . P A 2 O1B O -0.1624(19) 0.4770(13) 0.2621(9) 0.036(3) Uani 0.509(5) 1 d . . P A 2 C1B C -0.018(4) 0.484(2) 0.2247(16) 0.036(3) Uani 0.509(5) 1 d . . P A 2 C3B C 0.256(3) 0.582(2) 0.2439(13) 0.021(3) Uani 0.509(5) 1 d . . P A 2 O3B O 0.287(2) 0.638(2) 0.2850(11) 0.021(3) Uani 0.509(5) 1 d . . P A 2 O4B O 0.4462(15) 0.4860(11) 0.1133(7) 0.034(2) Uani 0.509(5) 1 d D . P A 2 H4B H 0.528(6) 0.422(4) 0.123(6) 0.051 Uiso 0.509(5) 1 d D U P A 2 C4B C 0.525(3) 0.5972(19) 0.0766(12) 0.053(6) Uani 0.509(5) 1 d D . P A 2 H4BA H 0.637558 0.572162 0.052674 0.080 Uiso 0.509(5) 1 calc R U P A 2 H4BB H 0.449765 0.649927 0.038215 0.080 Uiso 0.509(5) 1 calc R U P A 2 H4BC H 0.540150 0.645657 0.113765 0.080 Uiso 0.509(5) 1 calc R U P A 2 O5 O 0.9352(19) 0.4377(16) 0.0354(10) 0.063(3) Uani 0.509(5) 1 d G . P A 2 H5A H 0.922879 0.507304 0.000621 0.095 Uiso 0.509(5) 1 d G U P A 2 H5B H 1.045106 0.410413 0.031725 0.095 Uiso 0.509(5) 1 d G U P A 2 O6 O 0.695(2) 0.3090(16) 0.1196(10) 0.063(3) Uani 0.509(5) 1 d G . P A 2 H6A H 0.717051 0.349440 0.152682 0.095 Uiso 0.509(5) 1 d G U P A 2 H6B H 0.761423 0.336974 0.079998 0.095 Uiso 0.509(5) 1 d G 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 C1 0.096(9) 0.023(5) 0.032(6) -0.004(4) -0.016(6) 0.005(5) C2 0.133(12) 0.030(6) 0.026(5) -0.006(4) -0.007(6) -0.022(7) C3 0.092(4) 0.049(3) 0.037(2) -0.011(3) -0.008(3) -0.033(3) C4 0.047(6) 0.011(4) 0.029(5) -0.003(3) 0.003(4) 0.006(4) C17 0.039(5) 0.018(4) 0.026(4) -0.004(3) -0.005(4) 0.003(4) C6 0.026(4) 0.020(4) 0.027(4) -0.009(3) -0.011(3) 0.006(3) C7 0.031(5) 0.022(4) 0.025(4) -0.008(3) -0.006(4) 0.004(4) C8 0.042(5) 0.017(4) 0.024(4) -0.007(3) -0.016(4) 0.013(4) C9 0.041(5) 0.021(4) 0.044(6) -0.018(4) -0.022(4) 0.011(4) C10 0.068(8) 0.039(6) 0.063(7) -0.030(6) -0.044(7) 0.019(6) C11 0.050(7) 0.037(6) 0.098(10) -0.045(7) -0.044(7) 0.021(5) C12 0.021(5) 0.039(6) 0.072(7) -0.038(5) -0.015(5) 0.007(4) C13 0.031(5) 0.021(4) 0.048(6) -0.018(4) -0.013(4) 0.010(4) C14 0.023(5) 0.035(5) 0.046(6) -0.024(4) -0.001(4) -0.006(4) C15 0.028(5) 0.023(4) 0.033(5) -0.015(4) -0.008(4) 0.003(4) C16 0.026(5) 0.059(7) 0.044(6) -0.034(5) 0.001(4) -0.010(4) Br1 0.1174(11) 0.0240(6) 0.0501(7) -0.0122(5) -0.0472(7) 0.0199(6) N1 0.062(5) 0.020(4) 0.040(5) -0.016(3) -0.032(4) 0.018(4) N2 0.056(5) 0.014(3) 0.023(4) -0.004(3) -0.015(3) 0.006(3) N3 0.035(4) 0.042(5) 0.027(4) -0.017(3) 0.005(3) -0.013(4) O1 0.113(7) 0.046(5) 0.029(4) -0.005(3) -0.031(4) -0.003(4) O2 0.092(4) 0.049(3) 0.037(2) -0.011(3) -0.008(3) -0.033(3) O3 0.092(4) 0.049(3) 0.037(2) -0.011(3) -0.008(3) -0.033(3) Re2 0.0886(4) 0.0187(2) 0.0237(2) -0.00592(17) -0.0223(2) 0.0053(2) C22B 0.026(5) 0.027(5) 0.021(5) -0.004(4) -0.006(4) -0.002(4) C17B 0.026(5) 0.027(5) 0.021(5) -0.004(4) -0.006(4) -0.002(4) C18B 0.026(5) 0.027(5) 0.021(5) -0.004(4) -0.006(4) -0.002(4) C19B 0.021(9) 0.026(10) 0.029(10) -0.012(8) -0.001(7) 0.003(8) C20B 0.026(5) 0.027(5) 0.021(5) -0.004(4) -0.006(4) -0.002(4) C21B 0.026(5) 0.027(5) 0.021(5) -0.004(4) -0.006(4) -0.002(4) C23B 0.056(11) 0.044(11) 0.033(9) -0.021(8) 0.003(7) -0.019(8) O9 0.046(9) 0.019(7) 0.015(6) -0.008(5) 0.002(6) 0.001(6) O2A 0.054(6) 0.029(5) 0.038(6) 0.001(4) -0.014(5) -0.008(5) C2A 0.054(6) 0.029(5) 0.038(6) 0.001(4) -0.014(5) -0.008(5) Re1A 0.0333(11) 0.0162(5) 0.0187(4) -0.0022(3) -0.0057(5) -0.0028(6) O1A 0.016(7) 0.057(9) 0.073(12) -0.036(8) 0.005(7) 0.007(6) C1A 0.016(7) 0.057(9) 0.073(12) -0.036(8) 0.005(7) 0.007(6) O3A 0.043(13) 0.039(8) 0.016(9) 0.000(6) 0.010(8) -0.017(9) C3A 0.043(13) 0.039(8) 0.016(9) 0.000(6) 0.010(8) -0.017(9) O4A 0.030(5) 0.027(5) 0.039(5) 0.002(4) 0.014(4) -0.013(3) C4A 0.040(12) 0.043(12) 0.038(11) 0.002(9) -0.005(9) -0.009(9) C23A 0.056(11) 0.044(11) 0.033(9) -0.021(8) 0.003(7) -0.019(8) C22A 0.036(7) 0.036(7) 0.018(5) -0.007(5) 0.003(5) -0.015(5) C17A 0.027(6) 0.026(7) 0.028(7) -0.010(6) -0.002(5) -0.002(5) C18A 0.027(6) 0.026(7) 0.028(7) -0.010(6) -0.002(5) -0.002(5) C19A 0.027(6) 0.026(7) 0.028(7) -0.010(6) -0.002(5) -0.002(5) C20A 0.036(7) 0.036(7) 0.018(5) -0.007(5) 0.003(5) -0.015(5) C21A 0.036(7) 0.036(7) 0.018(5) -0.007(5) 0.003(5) -0.015(5) O4 0.053(9) 0.027(7) 0.026(7) -0.013(6) -0.003(7) 0.001(7) O2B 0.077(11) 0.024(7) 0.051(9) 0.006(6) -0.037(8) -0.002(7) C2B 0.054(6) 0.029(5) 0.038(6) 0.001(4) -0.014(5) -0.008(5) Re1B 0.0330(11) 0.0190(5) 0.0180(4) -0.0035(3) -0.0038(5) -0.0038(6) O1B 0.030(8) 0.035(7) 0.046(8) -0.023(6) -0.001(6) 0.004(6) C1B 0.030(8) 0.035(7) 0.046(8) -0.023(6) -0.001(6) 0.004(6) C3B 0.018(8) 0.032(6) 0.017(9) -0.011(6) 0.007(6) -0.010(6) O3B 0.018(8) 0.032(6) 0.017(9) -0.011(6) 0.007(6) -0.010(6) O4B 0.030(5) 0.027(5) 0.039(5) 0.002(4) 0.014(4) -0.013(3) C4B 0.067(15) 0.037(12) 0.046(13) -0.005(10) 0.031(11) -0.009(11) O5 0.036(6) 0.061(8) 0.070(8) 0.017(6) 0.008(6) 0.007(5) O6 0.036(6) 0.061(8) 0.070(8) 0.017(6) 0.008(6) 0.007(5) 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' Br Br -0.6763 1.2805 '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' Re Re -5.2083 5.8923 '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 O1 C1 Re2 178.8(11) . . ? O2 C2 Re2 175.7(10) . . ? O3 C3 Re2 177.0(12) . . ? N2 C4 C17 123.2(8) . . ? N2 C4 H4 118.4 . . ? C17 C4 H4 118.4 . . ? C6 C17 C4 118.9(8) . . ? C6 C17 H17 120.6 . . ? C4 C17 H17 120.6 . . ? C17 C6 C7 119.8(8) . . ? C17 C6 H6 120.1 . . ? C7 C6 H6 120.1 . . ? C8 C7 C6 117.3(8) . . ? C8 C7 C15 118.1(8) . . ? C6 C7 C15 124.5(7) . . ? N2 C8 C7 122.7(8) . . ? N2 C8 C9 117.2(8) . . ? C7 C8 C9 120.1(9) . . ? N1 C9 C13 124.1(9) . . ? N1 C9 C8 116.0(9) . . ? C13 C9 C8 119.9(8) . . ? N1 C10 C11 122.4(10) . . ? N1 C10 H10 118.8 . . ? C11 C10 H10 118.8 . . ? C12 C11 C10 120.9(10) . . ? C12 C11 H11 119.5 . . ? C10 C11 H11 119.5 . . ? C11 C12 C13 118.2(11) . . ? C11 C12 H12 120.9 . . ? C13 C12 H12 120.9 . . ? C9 C13 C14 119.8(8) . . ? C9 C13 C12 117.4(9) . . ? C14 C13 C12 122.7(9) . . ? C15 C14 C13 120.0(9) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C14 C15 C7 122.1(8) . . ? C14 C15 N3 119.9(8) . . ? C7 C15 N3 118.0(7) . . ? N3 C16 C17B 139.4(13) . . ? N3 C16 C17A 120.0(10) . . ? N3 C16 H16 110.3 . . ? C17B C16 H16 110.3 . . ? N3 C16 H16A 120.0 . . ? C17A C16 H16A 120.0 . . ? C10 N1 C9 116.9(10) . . ? C10 N1 Re2 127.3(8) . . ? C9 N1 Re2 115.8(7) . . ? C4 N2 C8 118.1(7) . . ? C4 N2 Re2 126.6(6) . . ? C8 N2 Re2 115.3(6) . . ? C16 N3 C15 116.2(8) . . ? C16 N3 Re1A 123.3(7) . . ? C15 N3 Re1A 120.2(6) . . ? C16 N3 Re1B 128.4(7) . . ? C15 N3 Re1B 114.1(5) . . ? C2 Re2 C1 88.9(5) . . ? C2 Re2 C3 90.5(5) . . ? C1 Re2 C3 91.5(4) . . ? C2 Re2 N1 170.5(4) . . ? C1 Re2 N1 99.1(4) . . ? C3 Re2 N1 94.3(4) . . ? C2 Re2 N2 96.1(4) . . ? C1 Re2 N2 174.2(4) . . ? C3 Re2 N2 91.4(4) . . ? N1 Re2 N2 75.6(3) . . ? C2 Re2 Br1 91.9(4) . . ? C1 Re2 Br1 91.0(3) . . ? C3 Re2 Br1 176.5(3) . . ? N1 Re2 Br1 82.91(19) . . ? N2 Re2 Br1 85.89(18) . . ? O9 C22B C17B 124.7(16) . . ? O9 C22B C21B 117.4(15) . . ? C17B C22B C21B 117.9(17) . . ? C16 C17B C22B 116.6(17) . . ? C16 C17B C18B 124.8(16) . . ? C22B C17B C18B 118.6(16) . . ? C19B C18B C17B 121.8(16) . . ? C19B C18B H18B 119.1 . . ? C17B C18B H18B 119.1 . . ? C18B C19B C20B 118.7(16) . . ? C18B C19B H19B 120.7 . . ? C20B C19B H19B 120.7 . . ? C21B C20B C19B 118.8(16) . . ? C21B C20B C23B 123.5(19) . . ? C19B C20B C23B 117.7(17) . . ? C20B C21B C22B 124.2(16) . . ? C20B C21B H21B 117.9 . . ? C22B C21B H21B 117.9 . . ? C20B C23B H23A 109.5 . . ? C20B C23B H23B 109.5 . . ? H23A C23B H23B 109.5 . . ? C20B C23B H23C 109.5 . . ? H23A C23B H23C 109.5 . . ? H23B C23B H23C 109.5 . . ? C22B O9 Re1A 130.2(11) . . ? O2A C2A Re1A 179.3(19) . . ? C3A Re1A C2A 85.7(10) . . ? C3A Re1A C1A 87.4(11) . . ? C2A Re1A C1A 90.8(11) . . ? C3A Re1A N3 97.7(9) . . ? C2A Re1A N3 175.6(7) . . ? C1A Re1A N3 92.1(9) . . ? C3A Re1A O9 175.5(8) . . ? C2A Re1A O9 91.2(7) . . ? C1A Re1A O9 95.9(9) . . ? N3 Re1A O9 85.2(4) . . ? C3A Re1A O4A 96.4(8) . . ? C2A Re1A O4A 95.6(7) . . ? C1A Re1A O4A 172.9(9) . . ? N3 Re1A O4A 81.4(4) . . ? O9 Re1A O4A 80.6(6) . . ? O1A C1A Re1A 174(3) . . ? O3A C3A Re1A 178.0(16) . . ? C4A O4A Re1A 123.5(11) . . ? C4A O4A H4A 108(2) . . ? Re1A O4A H4A 126(2) . . ? O4A C4A H4AA 109.5 . . ? O4A C4A H4AB 109.5 . . ? H4AA C4A H4AB 109.5 . . ? O4A C4A H4AC 109.5 . . ? H4AA C4A H4AC 109.5 . . ? H4AB C4A H4AC 109.5 . . ? C20A C23A H23D 109.5 . . ? C20A C23A H23E 109.5 . . ? H23D C23A H23E 109.5 . . ? C20A C23A H23F 109.5 . . ? H23D C23A H23F 109.5 . . ? H23E C23A H23F 109.5 . . ? O4 C22A C17A 123.4(9) . . ? O4 C22A C21A 116.5(9) . . ? C17A C22A C21A 120.0 . . ? C18A C17A C22A 120.0 . . ? C18A C17A C16 109.4(8) . . ? C22A C17A C16 130.6(8) . . ? C19A C18A C17A 120.0 . . ? C19A C18A H18A 120.0 . . ? C17A C18A H18A 120.0 . . ? C20A C19A C18A 120.0 . . ? C20A C19A H19A 120.0 . . ? C18A C19A H19A 120.0 . . ? C19A C20A C21A 120.0 . . ? C19A C20A C23A 120.2(12) . . ? C21A C20A C23A 119.7(12) . . ? C20A C21A C22A 120.0 . . ? C20A C21A H21A 120.0 . . ? C22A C21A H21A 120.0 . . ? C22A O4 Re1B 131.3(10) . . ? O2B C2B Re1B 175.8(17) . . ? C1B Re1B C3B 88.8(10) . . ? C1B Re1B C2B 86.4(11) . . ? C3B Re1B C2B 86.2(10) . . ? C1B Re1B O4 96.8(9) . . ? C3B Re1B O4 174.4(7) . . ? C2B Re1B O4 94.6(7) . . ? C1B Re1B O4B 176.6(8) . . ? C3B Re1B O4B 94.2(6) . . ? C2B Re1B O4B 95.3(7) . . ? O4 Re1B O4B 80.2(6) . . ? C1B Re1B N3 96.2(9) . . ? C3B Re1B N3 93.6(8) . . ? C2B Re1B N3 177.4(7) . . ? O4 Re1B N3 85.3(4) . . ? O4B Re1B N3 82.1(4) . . ? O1B C1B Re1B 177(2) . . ? O3B C3B Re1B 177.9(14) . . ? C4B O4B Re1B 124.1(11) . . ? C4B O4B H4B 109(3) . . ? Re1B O4B H4B 123(2) . . ? O4B C4B H4BA 109.5 . . ? O4B C4B H4BB 109.5 . . ? H4BA C4B H4BB 109.5 . . ? O4B C4B H4BC 109.5 . . ? H4BA C4B H4BC 109.5 . . ? H4BB C4B H4BC 109.5 . . ? H5A O5 H5B 104.4 . . ? H6A O6 H6B 104.6 . . ? 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 O1 1.164(12) . ? C1 Re2 1.924(11) . ? C2 O2 1.191(15) . ? C2 Re2 1.896(14) . ? C3 O3 1.043(14) . ? C3 Re2 1.960(14) . ? C4 N2 1.334(12) . ? C4 C17 1.401(12) . ? C4 H4 0.9500 . ? C17 C6 1.367(12) . ? C17 H17 0.9500 . ? C6 C7 1.417(12) . ? C6 H6 0.9500 . ? C7 C8 1.408(11) . ? C7 C15 1.432(12) . ? C8 N2 1.359(12) . ? C8 C9 1.427(13) . ? C9 N1 1.375(12) . ? C9 C13 1.396(14) . ? C10 N1 1.343(14) . ? C10 C11 1.404(18) . ? C10 H10 0.9500 . ? C11 C12 1.370(16) . ? C11 H11 0.9500 . ? C12 C13 1.427(13) . ? C12 H12 0.9500 . ? C13 C14 1.426(13) . ? C14 C15 1.356(12) . ? C14 H14 0.9500 . ? C15 N3 1.439(11) . ? C16 N3 1.311(12) . ? C16 C17B 1.32(2) . ? C16 C17A 1.545(13) . ? C16 H16 0.9500 . ? C16 H16A 0.9500 . ? Br1 Re2 2.6080(12) . ? N1 Re2 2.157(10) . ? N2 Re2 2.167(7) . ? N3 Re1A 2.002(8) . ? N3 Re1B 2.319(8) . ? C22B O9 1.32(2) . ? C22B C17B 1.40(2) . ? C22B C21B 1.42(2) . ? C17B C18B 1.44(2) . ? C18B C19B 1.38(2) . ? C18B H18B 0.9500 . ? C19B C20B 1.44(3) . ? C19B H19B 0.9500 . ? C20B C21B 1.34(3) . ? C20B C23B 1.52(3) . ? C21B H21B 0.9500 . ? C23B H23A 0.9800 . ? C23B H23B 0.9800 . ? C23B H23C 0.9800 . ? O9 Re1A 2.112(12) . ? O2A C2A 1.16(2) . ? C2A Re1A 1.914(19) . ? Re1A C3A 1.87(3) . ? Re1A C1A 1.99(2) . ? Re1A O4A 2.193(13) . ? O1A C1A 1.07(3) . ? O3A C3A 1.20(3) . ? O4A C4A 1.48(2) . ? O4A H4A 0.876(10) . ? C4A H4AA 0.9800 . ? C4A H4AB 0.9800 . ? C4A H4AC 0.9800 . ? C23A C20A 1.51(2) . ? C23A H23D 0.9800 . ? C23A H23E 0.9800 . ? C23A H23F 0.9800 . ? C22A O4 1.371(16) . ? C22A C17A 1.3900 . ? C22A C21A 1.3900 . ? C17A C18A 1.3900 . ? C18A C19A 1.3900 . ? C18A H18A 0.9500 . ? C19A C20A 1.3900 . ? C19A H19A 0.9500 . ? C20A C21A 1.3900 . ? C21A H21A 0.9500 . ? O4 Re1B 2.110(12) . ? O2B C2B 1.15(2) . ? C2B Re1B 1.926(19) . ? Re1B C1B 1.81(3) . ? Re1B C3B 1.92(2) . ? Re1B O4B 2.187(11) . ? O1B C1B 1.27(3) . ? C3B O3B 1.14(2) . ? O4B C4B 1.43(2) . ? O4B H4B 0.874(10) . ? C4B H4BA 0.9800 . ? C4B H4BB 0.9800 . ? C4B H4BC 0.9800 . ? O5 H5A 0.8701 . ? O5 H5B 0.8702 . ? O6 H6A 0.8695 . ? O6 H6B 0.8702 . ? 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 _geom_hbond_publ_flag C23A^b H23D^b O2B^b 0.98 1.61 2.42(3) 137.1 2_565 yes C21A^b H21A^b O2B^b 0.95 2.08 2.709(17) 122.5 2_565 yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 C4 C17 C6 0.5(12) . . . . ? C4 C17 C6 C7 0.9(12) . . . . ? C17 C6 C7 C8 -2.0(11) . . . . ? C17 C6 C7 C15 179.8(8) . . . . ? C6 C7 C8 N2 1.7(12) . . . . ? C15 C7 C8 N2 -180.0(7) . . . . ? C6 C7 C8 C9 -179.4(7) . . . . ? C15 C7 C8 C9 -1.1(12) . . . . ? N2 C8 C9 N1 -1.5(11) . . . . ? C7 C8 C9 N1 179.6(7) . . . . ? N2 C8 C9 C13 -179.9(7) . . . . ? C7 C8 C9 C13 1.1(12) . . . . ? N1 C10 C11 C12 -0.7(15) . . . . ? C10 C11 C12 C13 -0.7(14) . . . . ? N1 C9 C13 C14 -178.8(8) . . . . ? C8 C9 C13 C14 -0.6(12) . . . . ? N1 C9 C13 C12 2.4(13) . . . . ? C8 C9 C13 C12 -179.3(8) . . . . ? C11 C12 C13 C9 -0.1(12) . . . . ? C11 C12 C13 C14 -178.8(9) . . . . ? C9 C13 C14 C15 0.0(13) . . . . ? C12 C13 C14 C15 178.6(8) . . . . ? C13 C14 C15 C7 0.0(13) . . . . ? C13 C14 C15 N3 178.7(8) . . . . ? C8 C7 C15 C14 0.5(12) . . . . ? C6 C7 C15 C14 178.7(8) . . . . ? C8 C7 C15 N3 -178.1(7) . . . . ? C6 C7 C15 N3 0.1(12) . . . . ? C11 C10 N1 C9 2.8(13) . . . . ? C11 C10 N1 Re2 179.4(7) . . . . ? C13 C9 N1 C10 -3.8(12) . . . . ? C8 C9 N1 C10 177.9(8) . . . . ? C13 C9 N1 Re2 179.3(6) . . . . ? C8 C9 N1 Re2 0.9(9) . . . . ? C17 C4 N2 C8 -0.9(12) . . . . ? C17 C4 N2 Re2 178.5(6) . . . . ? C7 C8 N2 C4 -0.3(11) . . . . ? C9 C8 N2 C4 -179.2(7) . . . . ? C7 C8 N2 Re2 -179.8(6) . . . . ? C9 C8 N2 Re2 1.3(9) . . . . ? C17B C16 N3 C15 -179.7(16) . . . . ? C17A C16 N3 C15 173.2(9) . . . . ? C17B C16 N3 Re1A -6(2) . . . . ? C17A C16 N3 Re1B 7.7(13) . . . . ? C14 C15 N3 C16 111.6(9) . . . . ? C7 C15 N3 C16 -69.8(10) . . . . ? C14 C15 N3 Re1A -62.2(10) . . . . ? C7 C15 N3 Re1A 116.5(7) . . . . ? C14 C15 N3 Re1B -80.9(9) . . . . ? C7 C15 N3 Re1B 97.8(7) . . . . ? N3 C16 C17B C22B 1(3) . . . . ? N3 C16 C17B C18B -178.5(13) . . . . ? O9 C22B C17B C16 -1(3) . . . . ? C21B C22B C17B C16 -177.4(15) . . . . ? O9 C22B C17B C18B 178.8(17) . . . . ? C21B C22B C17B C18B 2(3) . . . . ? C16 C17B C18B C19B 176.9(17) . . . . ? C22B C17B C18B C19B -3(3) . . . . ? C17B C18B C19B C20B 0(3) . . . . ? C18B C19B C20B C21B 3(3) . . . . ? C18B C19B C20B C23B -178.8(17) . . . . ? C19B C20B C21B C22B -3(3) . . . . ? C23B C20B C21B C22B 178.3(17) . . . . ? O9 C22B C21B C20B -176.1(17) . . . . ? C17B C22B C21B C20B 1(3) . . . . ? C17B C22B O9 Re1A 6(3) . . . . ? C21B C22B O9 Re1A -177.1(12) . . . . ? O4 C22A C17A C18A 177.5(14) . . . . ? C21A C22A C17A C18A 0.0 . . . . ? O4 C22A C17A C16 0.5(15) . . . . ? C21A C22A C17A C16 -177.0(13) . . . . ? N3 C16 C17A C18A 173.4(8) . . . . ? N3 C16 C17A C22A -9.4(15) . . . . ? C22A C17A C18A C19A 0.0 . . . . ? C16 C17A C18A C19A 177.5(10) . . . . ? C17A C18A C19A C20A 0.0 . . . . ? C18A C19A C20A C21A 0.0 . . . . ? C18A C19A C20A C23A 177.0(14) . . . . ? C19A C20A C21A C22A 0.0 . . . . ? C23A C20A C21A C22A -177.1(14) . . . . ? O4 C22A C21A C20A -177.6(13) . . . . ? C17A C22A C21A C20A 0.0 . . . . ? C17A C22A O4 Re1B 9.8(19) . . . . ? C21A C22A O4 Re1B -172.7(9) . . . . ?