#------------------------------------------------------------------------------ #$Date: 2024-12-24 04:15:53 +0200 (Tue, 24 Dec 2024) $ #$Revision: 296957 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/97/7249715.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_7249715 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 'C29 H25 Cl5 N O3 P Re' _chemical_formula_sum 'C29 H25 Cl5 N O3 P Re' _chemical_formula_weight 829.92 _chemical_name_common 'trichloro-[2,4-dichloro-6-(4,4-dimethyl-4,5-dihydro-1,3-oxa-zol-2-yl)phenolato-N,O]-(triphenylphosphine oxide-O)-rhenium(IV)' _chemical_name_systematic 'trichloro-[2,4-dichloro-6-(4,4-dimethyl-4,5-dihydro-1,3-oxa-zol-2-yl)phenolato-N,O]-(triphenylphosphine oxide-O)-rhenium(IV)' _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 geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method 'manual edited SHELXL-2014/6.cif file' _audit_update_record ; 2018-07-10 deposited with the CCDC. 2024-12-12 downloaded from the CCDC. ; _cell_angle_alpha 73.649(5) _cell_angle_beta 76.698(5) _cell_angle_gamma 71.136(6) _cell_formula_units_Z 2 _cell_length_a 9.9619(18) _cell_length_b 10.0674(18) _cell_length_c 17.161(3) _cell_measurement_reflns_used 5384 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 23.47 _cell_measurement_theta_min 2.35 _cell_volume 1544.3(5) _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 0.0893 _diffrn_reflns_av_unetI/netI 0.0721 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _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 27366 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_reflns_theta_max 26.00 _diffrn_reflns_theta_min 2.19 _exptl_absorpt_coefficient_mu 4.451 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.624 _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 1.785 _exptl_crystal_description plate _exptl_crystal_F_000 810 _exptl_crystal_size_max 0.160 _exptl_crystal_size_mid 0.080 _exptl_crystal_size_min 0.040 _refine_diff_density_max 0.973 _refine_diff_density_min -1.207 _refine_diff_density_rms 0.167 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_hydrogen_treatment refU _refine_ls_matrix_type full _refine_ls_number_parameters 370 _refine_ls_number_reflns 6063 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.029 _refine_ls_R_factor_all 0.0534 _refine_ls_R_factor_gt 0.0359 _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^)+(0.0174P)^2^+1.0201P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0630 _refine_ls_wR_factor_ref 0.0685 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4977 _reflns_number_total 6063 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4ra07391f2.cif _cod_data_source_block JS76V _cod_database_code 7249715 _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 0.536 _shelx_estimated_absorpt_t_max 0.842 _shelxl_version_number 2014/6 _shelx_res_file ; TITL JS76v_0m_a.res P-1 J.Schachner (Me2C3H2NOC6H2Cl2O)ReCl3(OPPh3) orange 100K CELL 0.71073 9.9619 10.0674 17.1607 73.649 76.698 71.136 ZERR 2 0.0018 0.0018 0.0031 0.005 0.005 0.006 LATT 1 SFAC C H CL N O P RE UNIT 58 50 10 2 6 2 2 TEMP -173.18 SIZE 0.04 0.08 0.16 ACTA 52.0004 MERG 2 OMIT -2 52.0004 OMIT 0 0 1 L.S. 3 LIST 4 BOND $H CONF FMAP 2 PLAN 20 WGHT 0.017400 1.020100 FVAR 0.11473 0.03588 0.03951 0.03435 0.03593 0.02878 0.02833 FVAR 0.02791 RE1 7 0.743539 0.570655 0.728192 11.00000 0.01207 0.01142 = 0.01161 -0.00296 -0.00186 -0.00334 CL1 3 0.517461 0.538448 0.790883 11.00000 0.01255 0.02442 = 0.01900 -0.00583 -0.00083 -0.00570 CL2 3 0.967694 0.598949 0.656410 11.00000 0.01804 0.02208 = 0.01802 -0.00538 0.00232 -0.01051 CL3 3 0.784920 0.619924 0.843795 11.00000 0.02167 0.01978 = 0.01594 -0.00780 -0.00297 -0.00849 O11 5 0.597168 0.608985 0.506448 11.00000 0.02980 0.02505 = 0.01764 -0.00781 -0.01189 -0.00058 C12 1 0.611347 0.642012 0.574534 11.00000 0.01966 0.02038 = 0.01243 -0.00615 -0.00059 -0.00957 N13 4 0.701921 0.545238 0.619176 11.00000 0.00942 0.01798 = 0.01568 -0.00242 -0.00242 -0.00279 C14 1 0.751011 0.413054 0.583838 11.00000 0.02244 0.01713 = 0.01884 -0.00866 -0.00506 -0.00406 C15 1 0.712950 0.479433 0.497713 11.00000 0.02587 0.02460 = 0.01809 -0.00750 -0.00683 -0.00237 AFIX 23 H151 2 0.796327 0.503365 0.458612 11.00000 61.00000 H152 2 0.680769 0.412872 0.478126 11.00000 61.00000 AFIX 0 C16 1 0.658000 0.314328 0.633695 11.00000 0.03204 0.02166 = 0.02615 -0.00865 -0.00894 -0.00720 AFIX 137 H161 2 0.660101 0.299654 0.692380 11.00000 71.00000 H162 2 0.695196 0.221263 0.617931 11.00000 71.00000 H163 2 0.558992 0.358689 0.622781 11.00000 71.00000 AFIX 0 C17 1 0.909195 0.337466 0.581986 11.00000 0.02265 0.02304 = 0.01969 -0.00893 -0.00348 -0.00164 AFIX 137 H171 2 0.964706 0.406363 0.553191 11.00000 81.00000 H172 2 0.935406 0.259150 0.553212 11.00000 81.00000 H173 2 0.930172 0.297809 0.638355 11.00000 81.00000 AFIX 0 O21 5 0.649230 0.777964 0.691679 11.00000 0.02064 0.01208 = 0.01972 -0.00259 -0.00800 0.00478 C21 1 0.541930 0.837859 0.648540 11.00000 0.02484 0.01254 = 0.01578 0.00413 0.00113 -0.00212 C22 1 0.448509 0.975001 0.657497 11.00000 0.03221 0.01631 = 0.01741 -0.00451 0.00678 -0.00214 C23 1 0.336112 1.043986 0.613069 11.00000 0.02896 0.01661 = 0.02951 0.00685 0.00376 0.00964 AFIX 43 H23 2 0.272155 1.133488 0.621954 11.00000 21.00000 AFIX 0 C24 1 0.317609 0.981515 0.555558 11.00000 0.02524 0.02890 = 0.02020 -0.00037 -0.00373 0.00679 C25 1 0.407125 0.852058 0.543001 11.00000 0.02454 0.02883 = 0.01897 0.00157 -0.00349 -0.00054 AFIX 43 H25 2 0.394017 0.811282 0.502611 11.00000 21.00000 AFIX 0 C26 1 0.518881 0.778929 0.589883 11.00000 0.01970 0.02220 = 0.01689 -0.00300 -0.00233 0.00188 CL22 3 0.474143 1.053242 0.728671 11.00000 0.04910 0.01666 = 0.03072 -0.00693 0.00297 -0.00414 CL24 3 0.181061 1.071741 0.495825 11.00000 0.02890 0.06046 = 0.03621 0.00233 -0.01152 0.01946 O1 5 0.833504 0.354099 0.769270 11.00000 0.00700 0.00950 = 0.01392 -0.00345 0.00037 -0.00057 P1 6 0.894964 0.237528 0.841464 11.00000 0.01212 0.01193 = 0.01277 -0.00268 -0.00388 -0.00303 C31 1 1.025043 0.286602 0.875750 11.00000 0.01321 0.00754 = 0.02537 -0.00734 -0.00636 0.00192 C32 1 1.017525 0.283556 0.958963 11.00000 0.02518 0.02012 = 0.02990 -0.00802 -0.01249 -0.00158 AFIX 43 H32 2 0.944660 0.251576 0.999190 11.00000 31.00000 AFIX 0 C33 1 1.118186 0.327986 0.981293 11.00000 0.03824 0.03548 = 0.04076 -0.01943 -0.02328 0.00030 AFIX 43 H33 2 1.113406 0.327788 1.037255 11.00000 31.00000 AFIX 0 C34 1 1.225346 0.372542 0.923230 11.00000 0.03498 0.02587 = 0.07261 -0.01302 -0.03524 -0.00549 AFIX 43 H34 2 1.292735 0.404569 0.939108 11.00000 31.00000 AFIX 0 C35 1 1.234706 0.370563 0.841417 11.00000 0.02305 0.02654 = 0.05393 0.00329 -0.01707 -0.01187 AFIX 43 H35 2 1.311265 0.396805 0.801917 11.00000 31.00000 AFIX 0 C36 1 1.133230 0.330641 0.817524 11.00000 0.01895 0.02157 = 0.03604 -0.00584 -0.00676 -0.00507 AFIX 43 H36 2 1.137406 0.333294 0.761257 11.00000 31.00000 AFIX 0 C41 1 0.758334 0.202315 0.926529 11.00000 0.01366 0.01748 = 0.01294 -0.00102 -0.00854 -0.00333 C42 1 0.741578 0.063705 0.958471 11.00000 0.02269 0.01793 = 0.01865 -0.00099 -0.00366 -0.00729 AFIX 43 H42 2 0.801809 -0.013701 0.934416 11.00000 41.00000 AFIX 0 C43 1 0.636756 0.039487 1.025395 11.00000 0.03054 0.02371 = 0.02901 -0.00066 -0.00196 -0.01174 AFIX 43 H43 2 0.624994 -0.054619 1.046892 11.00000 41.00000 AFIX 0 C44 1 0.549608 0.151069 1.060876 11.00000 0.01955 0.03366 = 0.01905 0.00248 -0.00198 -0.00496 AFIX 43 H44 2 0.477907 0.133603 1.106604 11.00000 41.00000 AFIX 0 C45 1 0.566014 0.288116 1.030277 11.00000 0.02093 0.02735 = 0.01727 -0.00510 0.00100 -0.00259 AFIX 43 H45 2 0.505554 0.364945 1.054742 11.00000 41.00000 AFIX 0 C46 1 0.671177 0.313326 0.963621 11.00000 0.02033 0.01607 = 0.01931 0.00163 -0.00339 -0.00443 AFIX 43 H46 2 0.683590 0.407320 0.943227 11.00000 41.00000 AFIX 0 C51 1 0.981846 0.072288 0.807252 11.00000 0.01781 0.01741 = 0.01701 -0.00212 -0.00332 -0.00778 C52 1 1.114438 -0.014689 0.828749 11.00000 0.01619 0.02294 = 0.02041 -0.00409 -0.00279 -0.00425 AFIX 43 H52 2 1.163354 0.015505 0.859086 11.00000 51.00000 AFIX 0 C53 1 1.174545 -0.145060 0.805778 11.00000 0.02564 0.01838 = 0.03804 -0.00421 -0.00541 0.00199 AFIX 43 H53 2 1.265393 -0.204209 0.819790 11.00000 51.00000 AFIX 0 C54 1 1.101874 -0.189460 0.762160 11.00000 0.04617 0.01593 = 0.03263 -0.00851 -0.00299 -0.00350 AFIX 43 H54 2 1.143219 -0.279188 0.746535 11.00000 51.00000 AFIX 0 C55 1 0.970419 -0.104268 0.741467 11.00000 0.04981 0.01624 = 0.03229 -0.00799 -0.01214 -0.00907 AFIX 43 H55 2 0.921289 -0.135335 0.711691 11.00000 51.00000 AFIX 0 C56 1 0.909876 0.026174 0.763896 11.00000 0.02830 0.01681 = 0.02916 -0.00179 -0.01143 -0.00644 AFIX 43 H56 2 0.818917 0.084653 0.749740 11.00000 51.00000 AFIX 0 HKLF 4 REM JS76v_0m_a.res P-1 J.Schachner (Me2C3H2NOC6H2Cl2O)ReCl3(OPPh3) orange 100K REM R1 = 0.0359 for 4977 Fo > 4sig(Fo) and 0.0534 for all 6063 data REM 370 parameters refined using 0 restraints END WGHT 0.0174 1.0201 REM Highest difference peak 0.973, deepest hole -1.207, 1-sigma level 0.167 Q1 1 0.8379 0.5769 0.7167 11.00000 0.05 0.97 Q2 1 0.6947 0.5658 0.7507 11.00000 0.05 0.91 Q3 1 0.8250 0.4866 0.6711 11.00000 0.05 0.88 Q4 1 0.6817 0.5495 0.8155 11.00000 0.05 0.84 Q5 1 0.6553 0.6662 0.7802 11.00000 0.05 0.80 Q6 1 0.6453 0.6440 0.6888 11.00000 0.05 0.78 Q7 1 0.7679 0.4450 0.7256 11.00000 0.05 0.77 Q8 1 0.7416 0.5819 0.6453 11.00000 0.05 0.74 Q9 1 0.2161 1.1195 0.5270 11.00000 0.05 0.72 Q10 1 0.8613 0.3030 0.8133 11.00000 0.05 0.69 Q11 1 0.4902 0.2116 1.1570 11.00000 0.05 0.66 Q12 1 0.8655 0.6199 0.6662 11.00000 0.05 0.66 Q13 1 0.7068 0.6646 0.7080 11.00000 0.05 0.65 Q14 1 0.5169 0.4337 0.8267 11.00000 0.05 0.64 Q15 1 0.6136 0.4588 0.9196 11.00000 0.05 0.63 Q16 1 0.1972 1.0213 0.5648 11.00000 0.05 0.62 Q17 1 0.8534 0.2243 0.8705 11.00000 0.05 0.62 Q18 1 0.6231 0.5447 0.7266 11.00000 0.05 0.61 Q19 1 0.6552 0.4425 0.9858 11.00000 0.05 0.61 Q20 1 0.3028 1.1896 0.5973 11.00000 0.05 0.61 ; _shelx_res_checksum 46983 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 Re1 Re 0.74354(2) 0.57065(2) 0.72819(2) 0.01159(7) Uani 1 1 d . . . . . Cl1 Cl 0.51746(12) 0.53845(14) 0.79088(8) 0.0186(3) Uani 1 1 d . . . . . Cl2 Cl 0.96769(12) 0.59895(13) 0.65641(8) 0.0188(3) Uani 1 1 d . . . . . Cl3 Cl 0.78492(12) 0.61992(13) 0.84380(7) 0.0176(3) Uani 1 1 d . . . . . O11 O 0.5972(4) 0.6090(4) 0.5064(2) 0.0238(9) Uani 1 1 d . . . . . C12 C 0.6113(5) 0.6420(5) 0.5745(3) 0.0163(11) Uani 1 1 d . . . . . N13 N 0.7019(4) 0.5452(4) 0.6192(2) 0.0148(9) Uani 1 1 d . . . . . C14 C 0.7510(5) 0.4131(5) 0.5838(3) 0.0185(12) Uani 1 1 d . . . . . C15 C 0.7129(5) 0.4794(6) 0.4977(3) 0.0228(12) Uani 1 1 d . . . . . H151 H 0.7963 0.5034 0.4586 0.029(11) Uiso 1 1 calc R U . . . H152 H 0.6808 0.4129 0.4781 0.029(11) Uiso 1 1 calc R U . . . C16 C 0.6580(6) 0.3143(6) 0.6337(3) 0.0252(13) Uani 1 1 d . . . . . H161 H 0.6601 0.2997 0.6924 0.028(8) Uiso 1 1 calc R U . . . H162 H 0.6952 0.2213 0.6179 0.028(8) Uiso 1 1 calc R U . . . H163 H 0.5590 0.3587 0.6228 0.028(8) Uiso 1 1 calc R U . . . C17 C 0.9092(5) 0.3375(6) 0.5820(3) 0.0220(12) Uani 1 1 d . . . . . H171 H 0.9647 0.4064 0.5532 0.028(9) Uiso 1 1 calc R U . . . H172 H 0.9354 0.2591 0.5532 0.028(9) Uiso 1 1 calc R U . . . H173 H 0.9302 0.2978 0.6384 0.028(9) Uiso 1 1 calc R U . . . O21 O 0.6492(3) 0.7780(3) 0.6917(2) 0.0192(8) Uani 1 1 d . . . . . C21 C 0.5419(5) 0.8379(5) 0.6485(3) 0.0208(12) Uani 1 1 d . . . . . C22 C 0.4485(6) 0.9750(6) 0.6575(3) 0.0248(13) Uani 1 1 d . . . . . C23 C 0.3361(6) 1.0440(6) 0.6131(4) 0.0330(15) Uani 1 1 d . . . . . H23 H 0.2722 1.1335 0.6220 0.036(12) Uiso 1 1 calc R U . . . C24 C 0.3176(6) 0.9815(6) 0.5556(3) 0.0294(14) Uani 1 1 d . . . . . C25 C 0.4071(5) 0.8521(6) 0.5430(3) 0.0273(13) Uani 1 1 d . . . . . H25 H 0.3940 0.8113 0.5026 0.036(12) Uiso 1 1 calc R U . . . C26 C 0.5189(5) 0.7789(6) 0.5899(3) 0.0219(12) Uani 1 1 d . . . . . Cl22 Cl 0.47414(16) 1.05324(15) 0.72867(9) 0.0346(4) Uani 1 1 d . . . . . Cl24 Cl 0.18106(16) 1.07174(19) 0.49582(10) 0.0515(5) Uani 1 1 d . . . . . O1 O 0.8335(3) 0.3541(3) 0.76927(19) 0.0107(7) Uani 1 1 d . . . . . P1 P 0.89496(12) 0.23753(13) 0.84146(8) 0.0120(3) Uani 1 1 d . . . . . C31 C 1.0250(5) 0.2866(5) 0.8758(3) 0.0152(11) Uani 1 1 d . . . . . C32 C 1.0175(6) 0.2836(6) 0.9590(3) 0.0243(13) Uani 1 1 d . . . . . H32 H 0.9447 0.2516 0.9992 0.040(8) Uiso 1 1 calc R U . . . C33 C 1.1182(6) 0.3280(6) 0.9813(4) 0.0355(15) Uani 1 1 d . . . . . H33 H 1.1134 0.3278 1.0373 0.040(8) Uiso 1 1 calc R U . . . C34 C 1.2253(6) 0.3725(6) 0.9232(4) 0.0401(17) Uani 1 1 d . . . . . H34 H 1.2927 0.4046 0.9391 0.040(8) Uiso 1 1 calc R U . . . C35 C 1.2347(6) 0.3706(6) 0.8414(4) 0.0340(15) Uani 1 1 d . . . . . H35 H 1.3113 0.3968 0.8019 0.040(8) Uiso 1 1 calc R U . . . C36 C 1.1332(5) 0.3306(6) 0.8175(4) 0.0254(13) Uani 1 1 d . . . . . H36 H 1.1374 0.3333 0.7613 0.040(8) Uiso 1 1 calc R U . . . C41 C 0.7583(5) 0.2023(5) 0.9265(3) 0.0143(11) Uani 1 1 d . . . . . C42 C 0.7416(5) 0.0637(6) 0.9585(3) 0.0199(12) Uani 1 1 d . . . . . H42 H 0.8018 -0.0137 0.9344 0.034(7) Uiso 1 1 calc R U . . . C43 C 0.6368(6) 0.0395(6) 1.0254(3) 0.0283(14) Uani 1 1 d . . . . . H43 H 0.6250 -0.0546 1.0469 0.034(7) Uiso 1 1 calc R U . . . C44 C 0.5496(5) 0.1511(6) 1.0609(3) 0.0267(13) Uani 1 1 d . . . . . H44 H 0.4779 0.1336 1.1066 0.034(7) Uiso 1 1 calc R U . . . C45 C 0.5660(5) 0.2881(6) 1.0303(3) 0.0235(13) Uani 1 1 d . . . . . H45 H 0.5056 0.3649 1.0547 0.034(7) Uiso 1 1 calc R U . . . C46 C 0.6712(5) 0.3133(6) 0.9636(3) 0.0199(12) Uani 1 1 d . . . . . H46 H 0.6836 0.4073 0.9432 0.034(7) Uiso 1 1 calc R U . . . C51 C 0.9818(5) 0.0723(5) 0.8073(3) 0.0169(11) Uani 1 1 d . . . . . C52 C 1.1144(5) -0.0147(6) 0.8287(3) 0.0203(12) Uani 1 1 d . . . . . H52 H 1.1634 0.0155 0.8591 0.036(7) Uiso 1 1 calc R U . . . C53 C 1.1745(6) -0.1451(6) 0.8058(4) 0.0297(14) Uani 1 1 d . . . . . H53 H 1.2654 -0.2042 0.8198 0.036(7) Uiso 1 1 calc R U . . . C54 C 1.1019(6) -0.1895(6) 0.7622(4) 0.0327(15) Uani 1 1 d . . . . . H54 H 1.1432 -0.2792 0.7465 0.036(7) Uiso 1 1 calc R U . . . C55 C 0.9704(6) -0.1043(6) 0.7415(3) 0.0312(14) Uani 1 1 d . . . . . H55 H 0.9213 -0.1353 0.7117 0.036(7) Uiso 1 1 calc R U . . . C56 C 0.9099(6) 0.0262(6) 0.7639(3) 0.0242(13) Uani 1 1 d . . . . . H56 H 0.8189 0.0847 0.7497 0.036(7) Uiso 1 1 calc R U . . . 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 0.01207(10) 0.01142(11) 0.01161(11) -0.00296(8) -0.00186(7) -0.00334(8) Cl1 0.0126(6) 0.0244(7) 0.0190(7) -0.0058(6) -0.0008(5) -0.0057(5) Cl2 0.0180(6) 0.0221(7) 0.0180(7) -0.0054(6) 0.0023(5) -0.0105(5) Cl3 0.0217(6) 0.0198(7) 0.0159(7) -0.0078(5) -0.0030(5) -0.0085(5) O11 0.030(2) 0.025(2) 0.018(2) -0.0078(17) -0.0119(16) -0.0006(17) C12 0.020(3) 0.020(3) 0.012(3) -0.006(2) -0.001(2) -0.010(2) N13 0.009(2) 0.018(2) 0.016(2) -0.0024(19) -0.0024(18) -0.0028(18) C14 0.022(3) 0.017(3) 0.019(3) -0.009(2) -0.005(2) -0.004(2) C15 0.026(3) 0.025(3) 0.018(3) -0.008(2) -0.007(2) -0.002(3) C16 0.032(3) 0.022(3) 0.026(3) -0.009(3) -0.009(3) -0.007(3) C17 0.023(3) 0.023(3) 0.020(3) -0.009(2) -0.003(2) -0.002(2) O21 0.0206(18) 0.0121(19) 0.020(2) -0.0026(16) -0.0080(16) 0.0048(15) C21 0.025(3) 0.013(3) 0.016(3) 0.004(2) 0.001(2) -0.002(2) C22 0.032(3) 0.016(3) 0.017(3) -0.005(2) 0.007(2) -0.002(3) C23 0.029(3) 0.017(3) 0.030(4) 0.007(3) 0.004(3) 0.010(3) C24 0.025(3) 0.029(4) 0.020(3) 0.000(3) -0.004(2) 0.007(3) C25 0.025(3) 0.029(3) 0.019(3) 0.002(3) -0.003(2) -0.001(3) C26 0.020(3) 0.022(3) 0.017(3) -0.003(2) -0.002(2) 0.002(2) Cl22 0.0491(9) 0.0167(7) 0.0307(8) -0.0069(6) 0.0030(7) -0.0041(7) Cl24 0.0289(8) 0.0605(12) 0.0362(10) 0.0023(8) -0.0115(7) 0.0195(8) O1 0.0070(15) 0.0095(17) 0.0139(18) -0.0034(14) 0.0004(13) -0.0006(13) P1 0.0121(6) 0.0119(7) 0.0128(7) -0.0027(5) -0.0039(5) -0.0030(5) C31 0.013(2) 0.008(3) 0.025(3) -0.007(2) -0.006(2) 0.002(2) C32 0.025(3) 0.020(3) 0.030(3) -0.008(3) -0.012(3) -0.002(2) C33 0.038(4) 0.035(4) 0.041(4) -0.019(3) -0.023(3) 0.000(3) C34 0.035(4) 0.026(4) 0.073(5) -0.013(3) -0.035(4) -0.005(3) C35 0.023(3) 0.027(3) 0.054(4) 0.003(3) -0.017(3) -0.012(3) C36 0.019(3) 0.022(3) 0.036(4) -0.006(3) -0.007(2) -0.005(2) C41 0.014(2) 0.017(3) 0.013(3) -0.001(2) -0.009(2) -0.003(2) C42 0.023(3) 0.018(3) 0.019(3) -0.001(2) -0.004(2) -0.007(2) C43 0.031(3) 0.024(3) 0.029(3) -0.001(3) -0.002(3) -0.012(3) C44 0.020(3) 0.034(4) 0.019(3) 0.002(3) -0.002(2) -0.005(3) C45 0.021(3) 0.027(3) 0.017(3) -0.005(2) 0.001(2) -0.003(2) C46 0.020(3) 0.016(3) 0.019(3) 0.002(2) -0.003(2) -0.004(2) C51 0.018(3) 0.017(3) 0.017(3) -0.002(2) -0.003(2) -0.008(2) C52 0.016(3) 0.023(3) 0.020(3) -0.004(2) -0.003(2) -0.004(2) C53 0.026(3) 0.018(3) 0.038(4) -0.004(3) -0.005(3) 0.002(3) C54 0.046(4) 0.016(3) 0.033(4) -0.009(3) -0.003(3) -0.004(3) C55 0.050(4) 0.016(3) 0.032(4) -0.008(3) -0.012(3) -0.009(3) C56 0.028(3) 0.017(3) 0.029(3) -0.002(2) -0.011(3) -0.006(2) 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' P P 0.1023 0.0942 '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 O21 177.55(13) . . yes O21 Re1 N13 86.75(15) . . ? O1 Re1 N13 93.58(14) . . ? O21 Re1 Cl3 88.48(10) . . ? O1 Re1 Cl3 91.24(9) . . ? N13 Re1 Cl3 175.08(11) . . yes O21 Re1 Cl1 88.45(10) . . ? O1 Re1 Cl1 89.14(9) . . ? N13 Re1 Cl1 87.75(10) . . ? Cl3 Re1 Cl1 93.32(4) . . ? O21 Re1 Cl2 91.74(10) . . ? O1 Re1 Cl2 90.70(9) . . ? N13 Re1 Cl2 87.94(10) . . ? Cl3 Re1 Cl2 91.01(4) . . ? Cl1 Re1 Cl2 175.67(4) . . yes C12 O11 C15 105.4(4) . . ? N13 C12 O11 116.1(4) . . ? N13 C12 C26 128.4(5) . . ? O11 C12 C26 115.5(4) . . ? C12 N13 C14 107.0(4) . . yes C12 N13 Re1 123.5(3) . . yes C14 N13 Re1 129.1(3) . . yes N13 C14 C17 113.9(4) . . ? N13 C14 C15 100.5(4) . . ? C17 C14 C15 111.7(4) . . ? N13 C14 C16 106.8(4) . . ? C17 C14 C16 112.1(4) . . ? C15 C14 C16 111.2(4) . . ? O11 C15 C14 104.2(4) . . ? O11 C15 H151 110.9 . . ? C14 C15 H151 110.9 . . ? O11 C15 H152 110.9 . . ? C14 C15 H152 110.9 . . ? 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 127.6(3) . . yes O21 C21 C26 124.0(4) . . ? O21 C21 C22 119.1(5) . . ? C26 C21 C22 116.8(5) . . ? C23 C22 C21 121.7(5) . . ? C23 C22 Cl22 119.8(4) . . ? C21 C22 Cl22 118.4(4) . . ? C22 C23 C24 119.4(5) . . ? C22 C23 H23 120.3 . . ? C24 C23 H23 120.3 . . ? C25 C24 C23 121.0(5) . . ? C25 C24 Cl24 119.3(5) . . ? C23 C24 Cl24 119.7(4) . . ? C24 C25 C26 119.9(5) . . ? C24 C25 H25 120.0 . . ? C26 C25 H25 120.0 . . ? C21 C26 C25 121.1(5) . . ? C21 C26 C12 120.8(5) . . ? C25 C26 C12 118.1(5) . . ? P1 O1 Re1 144.71(19) . . yes O1 P1 C31 110.9(2) . . ? O1 P1 C41 112.42(19) . . ? C31 P1 C41 109.1(2) . . ? O1 P1 C51 108.5(2) . . ? C31 P1 C51 108.4(2) . . ? C41 P1 C51 107.3(2) . . ? C36 C31 C32 120.4(5) . . ? C36 C31 P1 118.1(4) . . ? C32 C31 P1 121.5(4) . . ? C33 C32 C31 118.8(5) . . ? C33 C32 H32 120.6 . . ? C31 C32 H32 120.6 . . ? C34 C33 C32 120.8(6) . . ? C34 C33 H33 119.6 . . ? C32 C33 H33 119.6 . . ? C33 C34 C35 120.0(5) . . ? C33 C34 H34 120.0 . . ? C35 C34 H34 120.0 . . ? C36 C35 C34 120.2(6) . . ? C36 C35 H35 119.9 . . ? C34 C35 H35 119.9 . . ? C35 C36 C31 119.9(5) . . ? C35 C36 H36 120.1 . . ? C31 C36 H36 120.1 . . ? C46 C41 C42 119.2(5) . . ? C46 C41 P1 119.5(4) . . ? C42 C41 P1 121.2(4) . . ? C43 C42 C41 119.8(5) . . ? C43 C42 H42 120.1 . . ? C41 C42 H42 120.1 . . ? C44 C43 C42 120.4(5) . . ? C44 C43 H43 119.8 . . ? C42 C43 H43 119.8 . . ? C43 C44 C45 120.3(5) . . ? C43 C44 H44 119.9 . . ? C45 C44 H44 119.9 . . ? C44 C45 C46 119.8(5) . . ? C44 C45 H45 120.1 . . ? C46 C45 H45 120.1 . . ? C41 C46 C45 120.5(5) . . ? C41 C46 H46 119.7 . . ? C45 C46 H46 119.7 . . ? C56 C51 C52 119.7(5) . . ? C56 C51 P1 119.1(4) . . ? C52 C51 P1 121.0(4) . . ? C53 C52 C51 119.8(5) . . ? C53 C52 H52 120.1 . . ? C51 C52 H52 120.1 . . ? C52 C53 C54 119.9(5) . . ? C52 C53 H53 120.0 . . ? C54 C53 H53 120.0 . . ? C55 C54 C53 120.4(5) . . ? C55 C54 H54 119.8 . . ? C53 C54 H54 119.8 . . ? C54 C55 C56 120.1(5) . . ? C54 C55 H55 120.0 . . ? C56 C55 H55 120.0 . . ? C55 C56 C51 120.1(5) . . ? C55 C56 H56 119.9 . . ? C51 C56 H56 119.9 . . ? 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 2.053(3) . yes Re1 N13 2.105(4) . yes Re1 O21 1.974(3) . yes Re1 Cl1 2.3443(12) . yes Re1 Cl2 2.3522(12) . yes Re1 Cl3 2.3268(12) . yes O11 C12 1.349(6) . ? O11 C15 1.453(6) . ? C12 N13 1.296(6) . ? C12 C26 1.446(7) . ? N13 C14 1.508(6) . ? C14 C17 1.509(7) . ? C14 C15 1.521(7) . ? C14 C16 1.527(7) . ? 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 1.323(6) . ? C21 C26 1.396(7) . ? C21 C22 1.421(7) . ? C22 C23 1.382(8) . ? C22 Cl22 1.730(6) . ? C23 C24 1.383(8) . ? C23 H23 0.95 . ? C24 C25 1.363(8) . ? C24 Cl24 1.745(6) . ? C25 C26 1.406(7) . ? C25 H25 0.95 . ? O1 P1 1.534(3) . yes P1 C31 1.788(5) . ? P1 C41 1.793(5) . ? P1 C51 1.802(5) . ? C31 C36 1.386(7) . ? C31 C32 1.405(7) . ? C32 C33 1.384(7) . ? C32 H32 0.95 . ? C33 C34 1.379(8) . ? C33 H33 0.95 . ? C34 C35 1.391(8) . ? C34 H34 0.95 . ? C35 C36 1.378(7) . ? C35 H35 0.95 . ? C36 H36 0.95 . ? C41 C46 1.388(7) . ? C41 C42 1.398(7) . ? C42 C43 1.387(7) . ? C42 H42 0.95 . ? C43 C44 1.378(8) . ? C43 H43 0.95 . ? C44 C45 1.380(7) . ? C44 H44 0.95 . ? C45 C46 1.388(7) . ? C45 H45 0.95 . ? C46 H46 0.95 . ? C51 C56 1.392(7) . ? C51 C52 1.394(7) . ? C52 C53 1.382(7) . ? C52 H52 0.95 . ? C53 C54 1.390(8) . ? C53 H53 0.95 . ? C54 C55 1.376(8) . ? C54 H54 0.95 . ? C55 C56 1.379(7) . ? C55 H55 0.95 . ? C56 H56 0.95 . ? 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 -10.3(6) . . . . ? C15 O11 C12 C26 172.1(4) . . . . ? O11 C12 N13 C14 -7.1(6) . . . . ? C26 C12 N13 C14 170.2(5) . . . . ? O11 C12 N13 Re1 180.0(3) . . . . ? C26 C12 N13 Re1 -2.7(7) . . . . ? C12 N13 C14 C17 139.7(4) . . . . ? Re1 N13 C14 C17 -47.9(6) . . . . ? C12 N13 C14 C15 20.2(5) . . . . ? Re1 N13 C14 C15 -167.4(3) . . . . ? C12 N13 C14 C16 -95.9(5) . . . . ? Re1 N13 C14 C16 76.4(5) . . . . ? C12 O11 C15 C14 22.6(5) . . . . ? N13 C14 C15 O11 -25.4(5) . . . . ? C17 C14 C15 O11 -146.5(4) . . . . ? C16 C14 C15 O11 87.4(5) . . . . ? Re1 O21 C21 C26 -31.5(7) . . . . ? Re1 O21 C21 C22 152.8(4) . . . . ? O21 C21 C22 C23 178.9(5) . . . . ? C26 C21 C22 C23 2.9(8) . . . . ? O21 C21 C22 Cl22 -3.3(6) . . . . ? C26 C21 C22 Cl22 -179.3(4) . . . . ? C21 C22 C23 C24 -3.1(8) . . . . ? Cl22 C22 C23 C24 179.2(4) . . . . ? C22 C23 C24 C25 1.0(8) . . . . ? C22 C23 C24 Cl24 -177.1(4) . . . . ? C23 C24 C25 C26 1.1(8) . . . . ? Cl24 C24 C25 C26 179.1(4) . . . . ? O21 C21 C26 C25 -176.5(5) . . . . ? C22 C21 C26 C25 -0.7(7) . . . . ? O21 C21 C26 C12 2.2(8) . . . . ? C22 C21 C26 C12 178.0(5) . . . . ? C24 C25 C26 C21 -1.2(8) . . . . ? C24 C25 C26 C12 -180.0(5) . . . . ? N13 C12 C26 C21 15.1(8) . . . . ? O11 C12 C26 C21 -167.6(4) . . . . ? N13 C12 C26 C25 -166.1(5) . . . . ? O11 C12 C26 C25 11.2(7) . . . . ? Re1 O1 P1 C31 -50.1(4) . . . . ? Re1 O1 P1 C41 72.4(4) . . . . ? Re1 O1 P1 C51 -169.0(3) . . . . ? O1 P1 C31 C36 -50.0(4) . . . . ? C41 P1 C31 C36 -174.4(4) . . . . ? C51 P1 C31 C36 69.0(4) . . . . ? O1 P1 C31 C32 128.9(4) . . . . ? C41 P1 C31 C32 4.5(5) . . . . ? C51 P1 C31 C32 -112.1(4) . . . . ? C36 C31 C32 C33 1.3(7) . . . . ? P1 C31 C32 C33 -177.6(4) . . . . ? C31 C32 C33 C34 -0.9(8) . . . . ? C32 C33 C34 C35 -1.2(9) . . . . ? C33 C34 C35 C36 3.1(9) . . . . ? C34 C35 C36 C31 -2.7(8) . . . . ? C32 C31 C36 C35 0.5(7) . . . . ? P1 C31 C36 C35 179.4(4) . . . . ? O1 P1 C41 C46 -59.0(4) . . . . ? C31 P1 C41 C46 64.5(4) . . . . ? C51 P1 C41 C46 -178.2(4) . . . . ? O1 P1 C41 C42 123.7(4) . . . . ? C31 P1 C41 C42 -112.8(4) . . . . ? C51 P1 C41 C42 4.5(5) . . . . ? C46 C41 C42 C43 1.3(7) . . . . ? P1 C41 C42 C43 178.7(4) . . . . ? C41 C42 C43 C44 -0.4(8) . . . . ? C42 C43 C44 C45 -0.2(8) . . . . ? C43 C44 C45 C46 -0.2(8) . . . . ? C42 C41 C46 C45 -1.7(7) . . . . ? P1 C41 C46 C45 -179.1(4) . . . . ? C44 C45 C46 C41 1.2(8) . . . . ? O1 P1 C51 C56 -47.8(5) . . . . ? C31 P1 C51 C56 -168.3(4) . . . . ? C41 P1 C51 C56 73.9(4) . . . . ? O1 P1 C51 C52 137.0(4) . . . . ? C31 P1 C51 C52 16.5(5) . . . . ? C41 P1 C51 C52 -101.3(4) . . . . ? C56 C51 C52 C53 1.0(8) . . . . ? P1 C51 C52 C53 176.1(4) . . . . ? C51 C52 C53 C54 -0.7(8) . . . . ? C52 C53 C54 C55 0.2(9) . . . . ? C53 C54 C55 C56 0.1(9) . . . . ? C54 C55 C56 C51 0.3(8) . . . . ? C52 C51 C56 C55 -0.8(8) . . . . ? P1 C51 C56 C55 -176.0(4) . . . . ?