#------------------------------------------------------------------------------ #$Date: 2024-12-24 04:15:53 +0200 (Tue, 24 Dec 2024) $ #$Revision: 296957 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/97/7249714.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_7249714 loop_ _publ_author_name 'Gradenegger, A.' 'Schachner, J. A.' 'Belaj, F.' 'M\"osch-Zanetti, N. C.' _publ_section_title ; An oxidorhenium(v) complex with an electron-withdrawing ligand: benefits and drawbacks for a dual role catalyst ; _journal_issue 54 _journal_name_full 'RSC Advances' _journal_page_first 40058 _journal_page_last 40068 _journal_paper_doi 10.1039/D4RA07391F _journal_volume 14 _journal_year 2024 _chemical_compound_source 'synthetical product' _chemical_formula_moiety 'C22 H20 Cl4 N2 O6 Re' _chemical_formula_sum 'C22 H20 Cl4 N2 O6 Re' _chemical_formula_weight 736.40 _chemical_name_common bis[2-(4,4-dimethyl-4,5-dihydro-1,3-oxazol-2-yl)-4,6-dichlo-rophenolato-N,O]-dioxo-rhenium(VI) _chemical_name_systematic bis[2-(4,4-dimethyl-4,5-dihydro-1,3-oxazol-2-yl)-4,6-dichlo-rophenolato-N,O]-dioxo-rhenium(VI) _space_group_crystal_system orthorhombic _space_group_IT_number 56 _space_group_name_Hall '-P 2ab 2ac' _space_group_name_H-M_alt 'P c c n' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method 'manual edited SHELXL-2014/6.cif file' _audit_update_record ; 2020-04-08 deposited with the CCDC. 2024-12-12 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 16.202(3) _cell_length_b 16.335(3) _cell_length_c 18.805(3) _cell_measurement_reflns_used 9744 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 40.71 _cell_measurement_theta_min 2.50 _cell_volume 4976.9(15) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'modified ORTEP (Johnson, 1965)' _computing_publication_material 'SHELXL-2014/6 (Sheldrick, 2015)' _computing_structure_refinement 'SHELXL-2014/6 (Sheldrick, 2015)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator 'multilayer monochromator' _diffrn_radiation_source 'Incoatec microfocus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0542 _diffrn_reflns_av_unetI/netI 0.0424 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_number 77915 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 40.00 _diffrn_reflns_theta_max 40.00 _diffrn_reflns_theta_min 1.77 _exptl_absorpt_coefficient_mu 5.355 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.593 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Bruker (2001). SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.' _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.966 _exptl_crystal_description block _exptl_crystal_F_000 2856 _exptl_crystal_size_max 0.280 _exptl_crystal_size_mid 0.130 _exptl_crystal_size_min 0.090 _refine_diff_density_max 1.776 _refine_diff_density_min -1.583 _refine_diff_density_rms 0.168 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_hydrogen_treatment refU _refine_ls_matrix_type full _refine_ls_number_parameters 330 _refine_ls_number_reflns 15402 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.018 _refine_ls_R_factor_all 0.0501 _refine_ls_R_factor_gt 0.0283 _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^)+(0.0217P)^2^+2.4883P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0605 _refine_ls_wR_factor_ref 0.0686 _reflns_Friedel_coverage 0.000 _reflns_number_gt 10723 _reflns_number_total 15402 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4ra07391f2.cif _cod_data_source_block JSJZ21 _cod_database_code 7249714 _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 0.316 _shelx_estimated_absorpt_t_max 0.644 _shelxl_version_number 2014/6 _shelx_res_file ; TITL JSJZ21_0m_a.res Pccn J.S./J.Zechner (Me2C3H2NO-C6H2Cl2O)ReO2 orange 100K CELL 0.71073 16.2023 16.3348 18.8049 90.000 90.000 90.000 ZERR 8 0.0028 0.0028 0.0032 0.000 0.000 0.000 LATT 1 SYMM 1/2-X, 1/2-Y, Z SYMM -X, 1/2+Y, 1/2-Z SYMM 1/2+X, -Y, 1/2-Z SFAC C H CL N O RE UNIT 176 160 32 16 48 8 TEMP -173.120 SIZE 0.09 0.13 0.28 ACTA 80.0004 MERG 2 OMIT -2 80.0004 OMIT 0 0 2 L.S. 3 BOND $H CONF FMAP 2 PLAN 20 WGHT 0.021700 2.488300 FVAR 0.03501 0.02092 0.02147 0.01878 0.02825 0.02562 0.02488 FVAR 0.01836 0.02337 0.03000 RE1 6 0.250000 0.250000 0.249198 10.50000 0.00774 0.00920 = 0.00984 0.00000 0.00000 0.00008 O1 5 0.280839 0.169073 0.195244 11.00000 0.01157 0.01328 = 0.01703 -0.00150 0.00056 0.00032 O11 5 0.480087 0.353949 0.310437 11.00000 0.01190 0.01994 = 0.01794 -0.00358 0.00068 -0.00455 C12 1 0.400447 0.331954 0.315458 11.00000 0.01132 0.01215 = 0.01286 -0.00009 -0.00027 -0.00086 N13 4 0.371088 0.293521 0.259839 11.00000 0.00917 0.01106 = 0.01259 0.00055 0.00075 -0.00014 C14 1 0.441466 0.277414 0.209370 11.00000 0.01010 0.01430 = 0.01470 -0.00031 0.00155 -0.00033 C15 1 0.504218 0.339405 0.236961 11.00000 0.01378 0.01964 = 0.01695 -0.00165 0.00301 -0.00404 AFIX 23 H151 2 0.560891 0.316942 0.234412 11.00000 21.00000 H152 2 0.501870 0.390708 0.209006 11.00000 21.00000 AFIX 0 C16 1 0.417360 0.294489 0.132997 11.00000 0.01715 0.02515 = 0.01424 0.00241 0.00218 -0.00269 AFIX 137 H161 2 0.375687 0.254714 0.117737 11.00000 41.00000 H162 2 0.466160 0.289874 0.102469 11.00000 41.00000 H163 2 0.394634 0.349930 0.129360 11.00000 41.00000 AFIX 0 C17 1 0.472183 0.189719 0.220883 11.00000 0.01332 0.01538 = 0.02269 -0.00202 0.00076 0.00224 AFIX 137 H171 2 0.427817 0.151076 0.209572 11.00000 51.00000 H172 2 0.488791 0.182711 0.270623 11.00000 51.00000 H173 2 0.519592 0.179266 0.189820 11.00000 51.00000 AFIX 0 O21 5 0.224533 0.325121 0.334957 11.00000 0.01208 0.01223 = 0.01320 -0.00185 -0.00076 0.00087 C21 1 0.273258 0.345774 0.387600 11.00000 0.01470 0.00793 = 0.01184 0.00026 -0.00055 -0.00009 C22 1 0.359479 0.352984 0.381605 11.00000 0.01466 0.01186 = 0.01340 -0.00027 0.00044 -0.00067 C23 1 0.407825 0.382281 0.438103 11.00000 0.01639 0.01463 = 0.01404 -0.00198 -0.00270 0.00008 AFIX 43 H23 2 0.465793 0.388390 0.432675 11.00000 81.00000 AFIX 0 C24 1 0.370202 0.402049 0.501469 11.00000 0.02319 0.01325 = 0.01346 -0.00163 -0.00324 -0.00184 C25 1 0.285219 0.392041 0.511052 11.00000 0.02337 0.01512 = 0.01253 -0.00046 0.00061 -0.00034 AFIX 43 H25 2 0.260342 0.403826 0.555638 11.00000 81.00000 AFIX 0 C26 1 0.238048 0.364773 0.454719 11.00000 0.01622 0.01337 = 0.01289 -0.00056 0.00209 0.00025 CL24 3 0.429589 0.439512 0.571152 11.00000 0.02827 0.02247 = 0.01502 -0.00399 -0.00545 -0.00346 CL26 3 0.132675 0.352965 0.464348 11.00000 0.01640 0.02082 = 0.01739 -0.00114 0.00492 0.00001 RE2 6 0.750000 0.250000 0.709332 10.50000 0.00922 0.00785 = 0.01131 0.00000 0.00000 0.00033 O2 5 0.667919 0.278926 0.762922 11.00000 0.01355 0.01301 = 0.01881 -0.00090 0.00180 -0.00044 O31 5 0.852803 0.480921 0.653061 11.00000 0.02420 0.00995 = 0.01840 -0.00031 0.00307 -0.00360 C32 1 0.830010 0.402373 0.646039 11.00000 0.01405 0.00863 = 0.01569 0.00087 -0.00079 -0.00055 N33 4 0.790019 0.371681 0.699813 11.00000 0.01354 0.00870 = 0.01332 -0.00116 0.00016 0.00084 C34 1 0.772318 0.440715 0.751040 11.00000 0.01710 0.01001 = 0.01651 -0.00127 0.00071 0.00177 C35 1 0.837159 0.502824 0.727193 11.00000 0.02036 0.00966 = 0.01962 -0.00255 0.00007 -0.00036 AFIX 23 H351 2 0.815810 0.559440 0.731023 11.00000 31.00000 H352 2 0.888038 0.497983 0.756040 11.00000 31.00000 AFIX 0 C36 1 0.784679 0.415015 0.828063 11.00000 0.02787 0.01640 = 0.01370 -0.00248 -0.00142 0.00065 AFIX 137 H361 2 0.742353 0.374942 0.841262 11.00000 61.00000 H362 2 0.780172 0.463124 0.858957 11.00000 61.00000 H363 2 0.839476 0.390425 0.833589 11.00000 61.00000 AFIX 0 C37 1 0.684928 0.471859 0.736237 11.00000 0.01995 0.01525 = 0.02311 0.00001 0.00245 0.00635 AFIX 137 H371 2 0.680486 0.488260 0.686254 11.00000 71.00000 H372 2 0.673260 0.519052 0.766803 11.00000 71.00000 H373 2 0.645063 0.428212 0.746172 11.00000 71.00000 AFIX 0 O41 5 0.827000 0.227490 0.623770 11.00000 0.01521 0.01131 = 0.01727 0.00082 0.00433 0.00125 C41 1 0.848297 0.277280 0.572267 11.00000 0.01095 0.01295 = 0.01406 -0.00036 0.00059 -0.00050 C42 1 0.853235 0.363203 0.579896 11.00000 0.01327 0.01358 = 0.01300 0.00012 0.00085 -0.00077 C43 1 0.883560 0.413190 0.524408 11.00000 0.01662 0.01576 = 0.01565 0.00179 0.00022 -0.00197 AFIX 43 H43 2 0.888546 0.470667 0.530805 11.00000 91.00000 AFIX 0 C44 1 0.905705 0.377517 0.461145 11.00000 0.01720 0.02194 = 0.01473 0.00278 0.00157 -0.00219 C45 1 0.899568 0.293072 0.450384 11.00000 0.01961 0.02358 = 0.01514 -0.00057 0.00236 -0.00126 AFIX 43 H45 2 0.914399 0.269487 0.406009 11.00000 91.00000 AFIX 0 C46 1 0.871545 0.244573 0.505463 11.00000 0.01645 0.01745 = 0.01490 -0.00375 0.00232 -0.00048 CL44 3 0.943253 0.439343 0.392813 11.00000 0.02851 0.03102 = 0.01797 0.00720 0.00448 -0.00560 CL46 3 0.864731 0.139112 0.494378 11.00000 0.03021 0.01625 = 0.02160 -0.00675 0.00532 -0.00015 HKLF 4 REM JSJZ21_0m_a.res Pccn J.S./J.Zechner (Me2C3H2NO-C6H2Cl2O)ReO2 orange 100K REM R1 = 0.0283 for 10723 Fo > 4sig(Fo) and 0.0501 for all 15402 data REM 330 parameters refined using 0 restraints END WGHT 0.0217 2.4765 REM Highest difference peak 1.776, deepest hole -1.583, 1-sigma level 0.168 Q1 1 0.7547 0.2815 0.6885 11.00000 0.05 1.78 Q2 1 0.2542 0.2211 0.2224 11.00000 0.05 1.46 Q3 1 0.7531 0.2828 0.7345 11.00000 0.05 1.31 Q4 1 0.2545 0.2180 0.2720 11.00000 0.05 1.28 Q5 1 0.6800 0.2693 0.7224 11.00000 0.05 1.12 Q6 1 0.3224 0.2699 0.2516 11.00000 0.05 1.05 Q7 1 0.6785 0.2291 0.7246 11.00000 0.05 0.88 Q8 1 0.7500 0.2500 0.6230 10.50000 0.05 0.83 Q9 1 0.8202 0.2401 0.6621 11.00000 0.05 0.77 Q10 1 0.8230 0.2568 0.6944 11.00000 0.05 0.76 Q11 1 0.6577 0.2789 0.7952 11.00000 0.05 0.72 Q12 1 0.3206 0.3013 0.2684 11.00000 0.05 0.70 Q13 1 0.7985 0.3238 0.7090 11.00000 0.05 0.69 Q14 1 0.2438 0.3609 0.4212 11.00000 0.05 0.69 Q15 1 0.2481 0.3260 0.2696 11.00000 0.05 0.67 Q16 1 0.3246 0.2382 0.2360 11.00000 0.05 0.65 Q17 1 0.2509 0.1745 0.2291 11.00000 0.05 0.64 Q18 1 0.7567 0.3260 0.6933 11.00000 0.05 0.64 Q19 1 0.7569 0.2728 0.5811 11.00000 0.05 0.64 Q20 1 0.3213 0.2284 0.2654 11.00000 0.05 0.63 ; _shelx_res_checksum 71571 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' 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 Re1 Re 0.2500 0.2500 0.24920(2) 0.00892(2) Uani 1 2 d S T P . . O1 O 0.28084(8) 0.16907(8) 0.19524(7) 0.0140(2) Uani 1 1 d . . . . . O11 O 0.48009(8) 0.35395(8) 0.31044(7) 0.0166(2) Uani 1 1 d . . . . . C12 C 0.40045(10) 0.33195(10) 0.31546(8) 0.0121(2) Uani 1 1 d . . . . . N13 N 0.37109(9) 0.29352(9) 0.25984(7) 0.0109(2) Uani 1 1 d . . . . . C14 C 0.44147(10) 0.27741(11) 0.20937(8) 0.0130(3) Uani 1 1 d . . . . . C15 C 0.50422(11) 0.33940(12) 0.23696(9) 0.0168(3) Uani 1 1 d . . . . . H151 H 0.5609 0.3169 0.2344 0.021(5) Uiso 1 1 calc R U . . . H152 H 0.5019 0.3907 0.2090 0.021(5) Uiso 1 1 calc R U . . . C16 C 0.41736(12) 0.29449(13) 0.13300(9) 0.0188(3) Uani 1 1 d . . . . . H161 H 0.3757 0.2547 0.1177 0.019(4) Uiso 1 1 calc R U . . . H162 H 0.4662 0.2899 0.1025 0.019(4) Uiso 1 1 calc R U . . . H163 H 0.3946 0.3499 0.1294 0.019(4) Uiso 1 1 calc R U . . . C17 C 0.47218(11) 0.18972(11) 0.22088(10) 0.0171(3) Uani 1 1 d . . . . . H171 H 0.4278 0.1511 0.2096 0.028(4) Uiso 1 1 calc R U . . . H172 H 0.4888 0.1827 0.2706 0.028(4) Uiso 1 1 calc R U . . . H173 H 0.5196 0.1793 0.1898 0.028(4) Uiso 1 1 calc R U . . . O21 O 0.22453(8) 0.32512(8) 0.33496(6) 0.01250(19) Uani 1 1 d . . . . . C21 C 0.27326(11) 0.34577(10) 0.38760(8) 0.0115(2) Uani 1 1 d . . . . . C22 C 0.35948(10) 0.35298(10) 0.38161(8) 0.0133(3) Uani 1 1 d . . . . . C23 C 0.40782(11) 0.38228(11) 0.43810(8) 0.0150(3) Uani 1 1 d . . . . . H23 H 0.4658 0.3884 0.4327 0.018(5) Uiso 1 1 calc R U . . . C24 C 0.37020(13) 0.40205(11) 0.50147(8) 0.0166(3) Uani 1 1 d . . . . . C25 C 0.28522(12) 0.39204(11) 0.51105(9) 0.0170(3) Uani 1 1 d . . . . . H25 H 0.2603 0.4038 0.5556 0.018(5) Uiso 1 1 calc R U . . . C26 C 0.23805(10) 0.36477(11) 0.45472(8) 0.0142(3) Uani 1 1 d . . . . . Cl24 Cl 0.42959(3) 0.43951(3) 0.57115(2) 0.02192(8) Uani 1 1 d . . . . . Cl26 Cl 0.13268(3) 0.35296(3) 0.46435(2) 0.01821(7) Uani 1 1 d . . . . . Re2 Re 0.7500 0.2500 0.70933(2) 0.00946(2) Uani 1 2 d S T P . . O2 O 0.66792(8) 0.27893(8) 0.76292(7) 0.0151(2) Uani 1 1 d . . . . . O31 O 0.85280(9) 0.48092(8) 0.65306(7) 0.0175(2) Uani 1 1 d . . . . . C32 C 0.83001(10) 0.40237(10) 0.64604(8) 0.0128(3) Uani 1 1 d . . . . . N33 N 0.79002(9) 0.37168(9) 0.69981(7) 0.0119(2) Uani 1 1 d . . . . . C34 C 0.77232(12) 0.44072(11) 0.75104(9) 0.0145(3) Uani 1 1 d . . . . . C35 C 0.83716(12) 0.50282(10) 0.72719(9) 0.0165(3) Uani 1 1 d . . . . . H351 H 0.8158 0.5594 0.7310 0.021(5) Uiso 1 1 calc R U . . . H352 H 0.8880 0.4980 0.7560 0.021(5) Uiso 1 1 calc R U . . . C36 C 0.78468(13) 0.41502(12) 0.82806(9) 0.0193(3) Uani 1 1 d . . . . . H361 H 0.7424 0.3749 0.8413 0.026(4) Uiso 1 1 calc R U . . . H362 H 0.7802 0.4631 0.8590 0.026(4) Uiso 1 1 calc R U . . . H363 H 0.8395 0.3904 0.8336 0.026(4) Uiso 1 1 calc R U . . . C37 C 0.68493(12) 0.47186(12) 0.73624(10) 0.0194(3) Uani 1 1 d . . . . . H371 H 0.6805 0.4883 0.6863 0.025(4) Uiso 1 1 calc R U . . . H372 H 0.6733 0.5191 0.7668 0.025(4) Uiso 1 1 calc R U . . . H373 H 0.6451 0.4282 0.7462 0.025(4) Uiso 1 1 calc R U . . . O41 O 0.82700(8) 0.22749(8) 0.62377(7) 0.0146(2) Uani 1 1 d . . . . . C41 C 0.84830(10) 0.27728(11) 0.57227(8) 0.0126(2) Uani 1 1 d . . . . . C42 C 0.85324(10) 0.36320(10) 0.57990(8) 0.0133(3) Uani 1 1 d . . . . . C43 C 0.88356(11) 0.41319(12) 0.52441(9) 0.0160(3) Uani 1 1 d . . . . . H43 H 0.8885 0.4707 0.5308 0.023(5) Uiso 1 1 calc R U . . . C44 C 0.90570(12) 0.37752(12) 0.46115(9) 0.0180(3) Uani 1 1 d . . . . . C45 C 0.89957(12) 0.29307(13) 0.45038(9) 0.0194(3) Uani 1 1 d . . . . . H45 H 0.9144 0.2695 0.4060 0.023(5) Uiso 1 1 calc R U . . . C46 C 0.87154(12) 0.24457(11) 0.50546(9) 0.0163(3) Uani 1 1 d . . . . . Cl44 Cl 0.94325(3) 0.43934(3) 0.39281(2) 0.02583(10) Uani 1 1 d . . . . . Cl46 Cl 0.86473(3) 0.13911(3) 0.49438(2) 0.02269(9) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.00774(3) 0.00920(4) 0.00984(3) 0.000 0.000 0.00008(3) O1 0.0116(5) 0.0133(5) 0.0170(5) -0.0015(4) 0.0006(4) 0.0003(4) O11 0.0119(5) 0.0199(6) 0.0179(5) -0.0036(4) 0.0007(4) -0.0045(4) C12 0.0113(6) 0.0121(7) 0.0129(6) -0.0001(5) -0.0003(5) -0.0009(5) N13 0.0092(5) 0.0111(6) 0.0126(5) 0.0006(4) 0.0007(4) -0.0001(4) C14 0.0101(6) 0.0143(7) 0.0147(6) -0.0003(5) 0.0016(5) -0.0003(5) C15 0.0138(7) 0.0196(8) 0.0170(6) -0.0017(6) 0.0030(6) -0.0040(6) C16 0.0172(7) 0.0252(9) 0.0142(6) 0.0024(6) 0.0022(6) -0.0027(6) C17 0.0133(7) 0.0154(8) 0.0227(7) -0.0020(6) 0.0008(6) 0.0022(6) O21 0.0121(4) 0.0122(5) 0.0132(4) -0.0019(4) -0.0008(4) 0.0009(4) C21 0.0147(6) 0.0079(6) 0.0118(6) 0.0003(4) -0.0005(5) -0.0001(5) C22 0.0147(6) 0.0119(7) 0.0134(6) -0.0003(5) 0.0004(5) -0.0007(5) C23 0.0164(7) 0.0146(7) 0.0140(6) -0.0020(5) -0.0027(5) 0.0001(5) C24 0.0232(8) 0.0133(8) 0.0135(6) -0.0016(5) -0.0032(5) -0.0018(6) C25 0.0234(9) 0.0151(8) 0.0125(6) -0.0005(5) 0.0006(6) -0.0003(6) C26 0.0162(8) 0.0134(7) 0.0129(6) -0.0006(5) 0.0021(5) 0.0003(5) Cl24 0.0283(2) 0.0225(2) 0.01502(15) -0.00399(14) -0.00545(15) -0.00346(17) Cl26 0.01640(17) 0.0208(2) 0.01739(16) -0.00114(14) 0.00492(13) 0.00001(15) Re2 0.00922(3) 0.00785(3) 0.01131(3) 0.000 0.000 0.00033(3) O2 0.0135(5) 0.0130(6) 0.0188(5) -0.0009(4) 0.0018(4) -0.0004(4) O31 0.0242(6) 0.0100(5) 0.0184(5) -0.0003(4) 0.0031(5) -0.0036(4) C32 0.0140(6) 0.0086(6) 0.0157(6) 0.0009(5) -0.0008(5) -0.0006(5) N33 0.0135(6) 0.0087(6) 0.0133(5) -0.0012(4) 0.0002(4) 0.0008(4) C34 0.0171(7) 0.0100(7) 0.0165(7) -0.0013(5) 0.0007(5) 0.0018(6) C35 0.0204(8) 0.0097(7) 0.0196(7) -0.0025(6) 0.0001(6) -0.0004(5) C36 0.0279(9) 0.0164(8) 0.0137(6) -0.0025(6) -0.0014(6) 0.0007(7) C37 0.0200(8) 0.0153(8) 0.0231(8) 0.0000(6) 0.0025(7) 0.0063(6) O41 0.0152(5) 0.0113(5) 0.0173(5) 0.0008(4) 0.0043(4) 0.0013(4) C41 0.0109(6) 0.0129(7) 0.0141(6) -0.0004(5) 0.0006(5) -0.0005(5) C42 0.0133(6) 0.0136(7) 0.0130(6) 0.0001(5) 0.0009(5) -0.0008(5) C43 0.0166(7) 0.0158(8) 0.0156(6) 0.0018(5) 0.0002(5) -0.0020(6) C44 0.0172(7) 0.0219(9) 0.0147(6) 0.0028(6) 0.0016(5) -0.0022(6) C45 0.0196(8) 0.0236(9) 0.0151(6) -0.0006(6) 0.0024(6) -0.0013(7) C46 0.0164(7) 0.0175(8) 0.0149(6) -0.0037(5) 0.0023(5) -0.0005(6) Cl44 0.0285(2) 0.0310(3) 0.01797(17) 0.00720(17) 0.00448(16) -0.00560(19) Cl46 0.0302(2) 0.0162(2) 0.02160(18) -0.00675(14) 0.00532(16) -0.00015(17) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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 O1 Re1 O1 108.65(8) . 2 ? O1 Re1 O21 164.36(5) . . yes O1 Re1 O21 86.94(5) . 2 ? O21 Re1 O21 77.51(7) . 2 ? O1 Re1 N13 93.83(6) . 2 ? O21 Re1 N13 86.56(5) . 2 ? O1 Re1 N13 92.55(6) . . ? O21 Re1 N13 84.90(5) . . ? N13 Re1 N13 169.04(7) . 2 yes C12 O11 C15 106.33(13) . . ? N13 C12 O11 114.91(14) . . ? N13 C12 C22 129.20(15) . . ? O11 C12 C22 115.88(14) . . ? C12 N13 C14 108.18(13) . . yes C12 N13 Re1 125.37(11) . . yes C14 N13 Re1 126.08(10) . . yes N13 C14 C16 111.72(14) . . ? N13 C14 C15 100.03(13) . . ? C16 C14 C15 111.85(15) . . ? N13 C14 C17 108.67(14) . . ? C16 C14 C17 112.96(15) . . ? C15 C14 C17 110.86(15) . . ? O11 C15 C14 104.60(13) . . ? O11 C15 H151 110.8 . . ? C14 C15 H151 110.8 . . ? O11 C15 H152 110.8 . . ? C14 C15 H152 110.8 . . ? H151 C15 H152 108.9 . . ? C14 C16 H161 109.5 . . ? C14 C16 H162 109.5 . . ? H161 C16 H162 109.5 . . ? C14 C16 H163 109.5 . . ? H161 C16 H163 109.5 . . ? H162 C16 H163 109.5 . . ? C14 C17 H171 109.5 . . ? C14 C17 H172 109.5 . . ? H171 C17 H172 109.5 . . ? C14 C17 H173 109.5 . . ? H171 C17 H173 109.5 . . ? H172 C17 H173 109.5 . . ? C21 O21 Re1 128.44(11) . . yes O21 C21 C22 124.02(14) . . ? O21 C21 C26 119.07(15) . . ? C22 C21 C26 116.88(14) . . ? C23 C22 C21 121.47(15) . . ? C23 C22 C12 118.30(15) . . ? C21 C22 C12 120.21(14) . . ? C24 C23 C22 119.20(17) . . ? C24 C23 H23 120.4 . . ? C22 C23 H23 120.4 . . ? C23 C24 C25 121.34(16) . . ? C23 C24 Cl24 119.36(15) . . ? C25 C24 Cl24 119.30(13) . . ? C26 C25 C24 118.96(16) . . ? C26 C25 H25 120.5 . . ? C24 C25 H25 120.5 . . ? C25 C26 C21 122.04(16) . . ? C25 C26 Cl26 120.19(13) . . ? C21 C26 Cl26 117.77(13) . . ? O2 Re2 O2 108.94(9) . 2_655 ? O2 Re2 O41 86.62(6) . 2_655 ? O2 Re2 O41 164.32(6) . . yes O41 Re2 O41 77.90(7) . 2_655 ? O2 Re2 N33 94.05(6) . 2_655 ? O41 Re2 N33 87.23(5) . 2_655 ? O2 Re2 N33 91.63(6) . . ? O41 Re2 N33 85.16(5) . . ? N33 Re2 N33 170.21(7) . 2_655 yes C32 O31 C35 106.28(13) . . ? N33 C32 O31 115.40(15) . . ? N33 C32 C42 128.78(15) . . ? O31 C32 C42 115.81(14) . . ? C32 N33 C34 107.60(14) . . yes C32 N33 Re2 125.81(11) . . yes C34 N33 Re2 126.44(11) . . yes N33 C34 C36 112.10(15) . . ? N33 C34 C35 100.25(13) . . ? C36 C34 C35 111.85(16) . . ? N33 C34 C37 107.93(14) . . ? C36 C34 C37 112.76(16) . . ? C35 C34 C37 111.23(16) . . ? O31 C35 C34 103.69(13) . . ? O31 C35 H351 111.0 . . ? C34 C35 H351 111.0 . . ? O31 C35 H352 111.0 . . ? C34 C35 H352 111.0 . . ? H351 C35 H352 109.0 . . ? C34 C36 H361 109.5 . . ? C34 C36 H362 109.5 . . ? H361 C36 H362 109.5 . . ? C34 C36 H363 109.5 . . ? H361 C36 H363 109.5 . . ? H362 C36 H363 109.5 . . ? C34 C37 H371 109.5 . . ? C34 C37 H372 109.5 . . ? H371 C37 H372 109.5 . . ? C34 C37 H373 109.5 . . ? H371 C37 H373 109.5 . . ? H372 C37 H373 109.5 . . ? C41 O41 Re2 128.54(11) . . yes O41 C41 C42 123.79(15) . . ? O41 C41 C46 119.43(16) . . ? C42 C41 C46 116.73(15) . . ? C43 C42 C41 121.24(15) . . ? C43 C42 C32 117.98(15) . . ? C41 C42 C32 120.74(14) . . ? C44 C43 C42 119.05(17) . . ? C44 C43 H43 120.5 . . ? C42 C43 H43 120.5 . . ? C43 C44 C45 121.73(16) . . ? C43 C44 Cl44 118.95(15) . . ? C45 C44 Cl44 119.32(14) . . ? C46 C45 C44 118.75(16) . . ? C46 C45 H45 120.6 . . ? C44 C45 H45 120.6 . . ? C45 C46 C41 122.44(17) . . ? C45 C46 Cl46 119.96(13) . . ? C41 C46 Cl46 117.60(13) . . ? 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 Re1 O1 1.7397(13) . yes Re1 O21 2.0680(12) . yes Re1 N13 2.0963(14) . yes O11 C12 1.343(2) . ? O11 C15 1.455(2) . ? C12 N13 1.309(2) . ? C12 C22 1.451(2) . ? N13 C14 1.507(2) . ? C14 C16 1.514(2) . ? C14 C15 1.526(2) . ? C14 C17 1.532(3) . ? C15 H151 0.99 . ? C15 H152 0.99 . ? C16 H161 0.98 . ? C16 H162 0.98 . ? C16 H163 0.98 . ? C17 H171 0.98 . ? C17 H172 0.98 . ? C17 H173 0.98 . ? O21 C21 1.310(2) . ? C21 C22 1.406(2) . ? C21 C26 1.419(2) . ? C22 C23 1.404(2) . ? C23 C24 1.377(2) . ? C23 H23 0.95 . ? C24 C25 1.398(3) . ? C24 Cl24 1.7371(17) . ? C25 C26 1.380(2) . ? C25 H25 0.95 . ? C26 Cl26 1.7277(17) . ? Re2 O2 1.7342(13) . yes Re2 O41 2.0689(12) . yes Re2 N33 2.0984(15) . yes O31 C32 1.342(2) . ? O31 C35 1.461(2) . ? C32 N33 1.301(2) . ? C32 C42 1.448(2) . ? N33 C34 1.511(2) . ? C34 C36 1.521(2) . ? C34 C35 1.528(3) . ? C34 C37 1.530(3) . ? C35 H351 0.99 . ? C35 H352 0.99 . ? C36 H361 0.98 . ? C36 H362 0.98 . ? C36 H363 0.98 . ? C37 H371 0.98 . ? C37 H372 0.98 . ? C37 H373 0.98 . ? O41 C41 1.311(2) . ? C41 C42 1.413(2) . ? C41 C46 1.416(2) . ? C42 C43 1.413(2) . ? C43 C44 1.372(3) . ? C43 H43 0.95 . ? C44 C45 1.398(3) . ? C44 Cl44 1.7439(18) . ? C45 C46 1.381(3) . ? C45 H45 0.95 . ? C46 Cl46 1.7388(19) . ? 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 C15 O11 C12 N13 9.9(2) . . . . ? C15 O11 C12 C22 -170.88(15) . . . . ? O11 C12 N13 C14 6.4(2) . . . . ? C22 C12 N13 C14 -172.68(16) . . . . ? O11 C12 N13 Re1 179.79(11) . . . . ? C22 C12 N13 Re1 0.7(3) . . . . ? C12 N13 C14 C16 -137.20(16) . . . . ? Re1 N13 C14 C16 49.52(19) . . . . ? C12 N13 C14 C15 -18.69(17) . . . . ? Re1 N13 C14 C15 168.03(11) . . . . ? C12 N13 C14 C17 97.51(16) . . . . ? Re1 N13 C14 C17 -75.78(16) . . . . ? C12 O11 C15 C14 -21.36(18) . . . . ? N13 C14 C15 O11 23.53(17) . . . . ? C16 C14 C15 O11 141.94(15) . . . . ? C17 C14 C15 O11 -91.01(17) . . . . ? Re1 O21 C21 C22 30.6(2) . . . . ? Re1 O21 C21 C26 -151.43(13) . . . . ? O21 C21 C22 C23 174.31(16) . . . . ? C26 C21 C22 C23 -3.7(2) . . . . ? O21 C21 C22 C12 -4.1(3) . . . . ? C26 C21 C22 C12 177.88(15) . . . . ? N13 C12 C22 C23 169.52(17) . . . . ? O11 C12 C22 C23 -9.6(2) . . . . ? N13 C12 C22 C21 -12.0(3) . . . . ? O11 C12 C22 C21 168.88(15) . . . . ? C21 C22 C23 C24 2.0(3) . . . . ? C12 C22 C23 C24 -179.56(16) . . . . ? C22 C23 C24 C25 1.2(3) . . . . ? C22 C23 C24 Cl24 -179.21(13) . . . . ? C23 C24 C25 C26 -2.5(3) . . . . ? Cl24 C24 C25 C26 177.91(14) . . . . ? C24 C25 C26 C21 0.7(3) . . . . ? C24 C25 C26 Cl26 -179.17(14) . . . . ? O21 C21 C26 C25 -175.74(16) . . . . ? C22 C21 C26 C25 2.4(3) . . . . ? O21 C21 C26 Cl26 4.1(2) . . . . ? C22 C21 C26 Cl26 -177.79(13) . . . . ? C35 O31 C32 N33 10.2(2) . . . . ? C35 O31 C32 C42 -169.74(15) . . . . ? O31 C32 N33 C34 7.2(2) . . . . ? C42 C32 N33 C34 -172.86(17) . . . . ? O31 C32 N33 Re2 -176.93(11) . . . . ? C42 C32 N33 Re2 3.0(3) . . . . ? C32 N33 C34 C36 -139.02(16) . . . . ? Re2 N33 C34 C36 45.2(2) . . . . ? C32 N33 C34 C35 -20.23(17) . . . . ? Re2 N33 C34 C35 163.97(11) . . . . ? C32 N33 C34 C37 96.21(17) . . . . ? Re2 N33 C34 C37 -79.58(16) . . . . ? C32 O31 C35 C34 -22.48(18) . . . . ? N33 C34 C35 O31 25.05(16) . . . . ? C36 C34 C35 O31 144.02(15) . . . . ? C37 C34 C35 O31 -88.90(17) . . . . ? Re2 O41 C41 C42 29.1(2) . . . . ? Re2 O41 C41 C46 -153.78(13) . . . . ? O41 C41 C42 C43 174.32(16) . . . . ? C46 C41 C42 C43 -2.8(2) . . . . ? O41 C41 C42 C32 -3.4(3) . . . . ? C46 C41 C42 C32 179.41(16) . . . . ? N33 C32 C42 C43 168.92(17) . . . . ? O31 C32 C42 C43 -11.2(2) . . . . ? N33 C32 C42 C41 -13.2(3) . . . . ? O31 C32 C42 C41 166.66(15) . . . . ? C41 C42 C43 C44 2.4(3) . . . . ? C32 C42 C43 C44 -179.78(16) . . . . ? C42 C43 C44 C45 -0.4(3) . . . . ? C42 C43 C44 Cl44 -179.90(14) . . . . ? C43 C44 C45 C46 -0.9(3) . . . . ? Cl44 C44 C45 C46 178.52(15) . . . . ? C44 C45 C46 C41 0.4(3) . . . . ? C44 C45 C46 Cl46 -178.96(15) . . . . ? O41 C41 C46 C45 -175.85(17) . . . . ? C42 C41 C46 C45 1.4(3) . . . . ? O41 C41 C46 Cl46 3.5(2) . . . . ? C42 C41 C46 Cl46 -179.19(13) . . . . ?