#------------------------------------------------------------------------------ #$Date: 2020-09-06 12:33:13 +0300 (Sun, 06 Sep 2020) $ #$Revision: 256066 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/49/7704995.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_7704995 loop_ _publ_author_name 'Schachner, J\"org A' 'Belaj, Ferdinand' 'M\"osch-Zanetti, Nadia C' _publ_section_title ; Isomers in chlorido and alkoxido-substituted oxidorhenium(v) complexes: effects on catalytic epoxidation activity. ; _journal_issue 32 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 11142 _journal_page_last 11149 _journal_paper_doi 10.1039/d0dt02352c _journal_volume 49 _journal_year 2020 _chemical_compound_source 'synthetical product' _chemical_formula_moiety 'C29 H26 Cl2 N2 O5 P Re' _chemical_formula_sum 'C29 H26 Cl2 N2 O5 P Re' _chemical_formula_weight 770.59 _chemical_name_common cis-dichloro-[2-(4,4-dimethyl-4,5-dihydro-1,3-oxazol-2-yl)-4-nitropheno-lato-N,O]-oxo-(triphenylphosphine)-rhenium(V) _chemical_name_systematic cis-dichloro-[2-(4,4-dimethyl-4,5-dihydro-1,3-oxazol-2-yl)-4-nitropheno-lato-N,O]-oxo-(triphenylphosphine)-rhenium(V) _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 ; 2020-06-22 deposited with the CCDC. 2020-07-29 downloaded from the CCDC. ; _cell_angle_alpha 77.6402(17) _cell_angle_beta 87.6176(18) _cell_angle_gamma 82.1537(18) _cell_formula_units_Z 2 _cell_length_a 10.7088(4) _cell_length_b 10.7534(4) _cell_length_c 12.8027(5) _cell_measurement_reflns_used 9993 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 30.03 _cell_measurement_theta_min 2.27 _cell_volume 1426.54(9) _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 0.0783 _diffrn_reflns_av_unetI/netI 0.0529 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 55063 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 30.00 _diffrn_reflns_theta_max 30.00 _diffrn_reflns_theta_min 1.92 _exptl_absorpt_coefficient_mu 4.545 _exptl_absorpt_correction_T_max 0.746 _exptl_absorpt_correction_T_min 0.426 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Bruker (2001). SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.' _exptl_crystal_colour green _exptl_crystal_density_diffrn 1.794 _exptl_crystal_description block _exptl_crystal_F_000 756 _exptl_crystal_size_max 0.330 _exptl_crystal_size_mid 0.260 _exptl_crystal_size_min 0.230 _refine_diff_density_max 2.735 _refine_diff_density_min -2.273 _refine_diff_density_rms 0.170 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_hydrogen_treatment refU _refine_ls_matrix_type full _refine_ls_number_parameters 370 _refine_ls_number_reflns 8300 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.083 _refine_ls_R_factor_all 0.0327 _refine_ls_R_factor_gt 0.0297 _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^)+(0.0190P)^2^+0.4664P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0627 _refine_ls_wR_factor_ref 0.0636 _reflns_Friedel_coverage 0.000 _reflns_number_gt 7645 _reflns_number_total 8300 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0dt02352c2.cif _cod_data_source_block JS90 _cod_depositor_comments 'Adding full bibliography for 7704994--7704996.cif.' _cod_database_code 7704995 _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 0.315 _shelx_estimated_absorpt_t_max 0.421 _shelxl_version_number 2014/6 _shelx_res_file ; TITL JS90.res in P-1 J.Schachner (Me2C3H2NO-NO2C6H3O)ReOCl2(PPh3) green 100K CELL 0.71073 10.7088 10.7534 12.8027 77.6402 87.6176 82.1537 ZERR 2 0.0004 0.0004 0.0005 0.0017 0.0018 0.0018 LATT 1 SFAC C H N O P CL RE UNIT 58 52 4 10 2 4 2 TEMP -173.17 SIZE 0.23 0.26 0.33 ACTA 60.0004 MERG 2 OMIT -2 60.0004 L.S. 4 BOND $H CONF FMAP 2 PLAN 20 WGHT 0.019000 0.466400 FVAR 0.10876 0.01506 0.01690 0.02021 0.01565 0.05504 0.05186 FVAR 0.04983 RE1 7 0.463619 0.189221 0.751449 11.00000 0.00763 0.00948 = 0.00980 -0.00397 0.00027 -0.00133 O1 4 0.454994 0.131282 0.883682 11.00000 0.01717 0.01512 = 0.01369 -0.00320 -0.00222 -0.00376 CL1 6 0.589898 0.352391 0.754017 11.00000 0.01308 0.01585 = 0.01645 -0.00506 -0.00089 -0.00630 CL2 6 0.649475 0.070727 0.696784 11.00000 0.01088 0.01986 = 0.03108 -0.01201 0.00399 -0.00044 O11 4 0.251059 -0.058869 0.625476 11.00000 0.03857 0.01199 = 0.02304 -0.00129 -0.01056 -0.01208 C12 1 0.305834 0.044523 0.629782 11.00000 0.01621 0.00793 = 0.01896 -0.00753 -0.00052 -0.00217 N13 3 0.360961 0.043725 0.717663 11.00000 0.01163 0.01126 = 0.01499 -0.00150 0.00094 -0.00202 C14 1 0.351968 -0.087185 0.790657 11.00000 0.01712 0.00885 = 0.01753 -0.00006 0.00044 -0.00166 C15 1 0.251234 -0.135313 0.734742 11.00000 0.05860 0.02280 = 0.03369 0.00804 -0.02071 -0.02249 AFIX 23 H151 2 0.272706 -0.227957 0.735274 11.00000 61.00000 H152 2 0.167873 -0.121269 0.769803 11.00000 61.00000 AFIX 0 C16 1 0.305010 -0.079961 0.903111 11.00000 0.05502 0.02452 = 0.03171 -0.00640 0.02087 -0.02090 AFIX 137 H161 2 0.281174 -0.163335 0.939589 11.00000 71.00000 H162 2 0.231522 -0.014040 0.899368 11.00000 71.00000 H163 2 0.372049 -0.057848 0.942907 11.00000 71.00000 AFIX 0 C17 1 0.476805 -0.171020 0.793443 11.00000 0.02658 0.01770 = 0.08457 0.01901 0.01308 0.00807 AFIX 137 H171 2 0.539094 -0.135209 0.828269 11.00000 81.00000 H172 2 0.505077 -0.174690 0.720246 11.00000 81.00000 H173 2 0.467581 -0.257784 0.833630 11.00000 81.00000 AFIX 0 O21 4 0.433073 0.265320 0.596725 11.00000 0.00953 0.01823 = 0.00926 -0.00482 0.00179 -0.00562 C21 1 0.357826 0.252987 0.521477 11.00000 0.01005 0.01560 = 0.01175 -0.00867 0.00348 -0.00230 C22 1 0.293165 0.144950 0.532861 11.00000 0.01294 0.01122 = 0.01561 -0.00677 -0.00012 -0.00082 C23 1 0.215026 0.135133 0.450932 11.00000 0.01578 0.01291 = 0.02090 -0.00946 -0.00203 -0.00144 AFIX 43 H23 2 0.170573 0.063102 0.457741 11.00000 21.00000 AFIX 0 C24 1 0.203427 0.231400 0.360205 11.00000 0.01460 0.01654 = 0.01469 -0.00911 -0.00257 0.00165 C25 1 0.266058 0.338969 0.347195 11.00000 0.01633 0.01673 = 0.01188 -0.00280 0.00183 -0.00027 AFIX 43 H25 2 0.255927 0.404093 0.283900 11.00000 21.00000 AFIX 0 C26 1 0.342945 0.349467 0.427557 11.00000 0.01520 0.01647 = 0.01492 -0.00491 0.00270 -0.00391 AFIX 43 H26 2 0.386334 0.422386 0.419614 11.00000 21.00000 AFIX 0 N24 3 0.119668 0.220804 0.276089 11.00000 0.01969 0.02350 = 0.02351 -0.01082 -0.00765 0.00251 O23 4 0.054864 0.133424 0.293469 11.00000 0.03329 0.02511 = 0.03989 -0.01010 -0.01826 -0.00872 O25 4 0.119124 0.300557 0.191868 11.00000 0.04181 0.04214 = 0.02089 0.00249 -0.01704 -0.01176 P1 5 0.268957 0.334081 0.774998 11.00000 0.00827 0.00883 = 0.00901 -0.00241 0.00084 -0.00208 C31 1 0.228928 0.465075 0.660666 11.00000 0.01181 0.00907 = 0.00988 -0.00262 0.00107 -0.00031 C32 1 0.324756 0.536297 0.616162 11.00000 0.01284 0.01613 = 0.01652 -0.00308 0.00090 -0.00230 AFIX 43 H32 2 0.408669 0.509564 0.640619 11.00000 31.00000 AFIX 0 C33 1 0.298829 0.645598 0.536676 11.00000 0.02300 0.01586 = 0.01812 0.00050 0.00363 -0.00785 AFIX 43 H33 2 0.364620 0.693645 0.506724 11.00000 31.00000 AFIX 0 C34 1 0.176307 0.684595 0.500997 11.00000 0.02809 0.01457 = 0.01643 0.00350 -0.00222 -0.00251 AFIX 43 H34 2 0.158276 0.759502 0.446395 11.00000 31.00000 AFIX 0 C35 1 0.080586 0.615237 0.544346 11.00000 0.01843 0.01726 = 0.01874 -0.00310 -0.00634 0.00085 AFIX 43 H35 2 -0.002950 0.642501 0.519108 11.00000 31.00000 AFIX 0 C36 1 0.105225 0.505401 0.624918 11.00000 0.01568 0.01300 = 0.01507 -0.00395 0.00052 -0.00321 AFIX 43 H36 2 0.038814 0.458446 0.655225 11.00000 31.00000 AFIX 0 C41 1 0.266586 0.422366 0.882288 11.00000 0.01216 0.00731 = 0.01003 -0.00289 0.00145 -0.00334 C42 1 0.360144 0.401448 0.958044 11.00000 0.01432 0.01301 = 0.01500 -0.00336 -0.00048 0.00080 AFIX 43 H42 2 0.431865 0.339464 0.955548 11.00000 41.00000 AFIX 0 C43 1 0.347708 0.472449 1.037903 11.00000 0.01975 0.01789 = 0.01377 -0.00658 -0.00247 -0.00249 AFIX 43 H43 2 0.412121 0.459700 1.089396 11.00000 41.00000 AFIX 0 C44 1 0.242984 0.560906 1.042928 11.00000 0.02146 0.01475 = 0.01739 -0.00854 0.00034 -0.00473 AFIX 43 H44 2 0.235028 0.608194 1.098138 11.00000 41.00000 AFIX 0 C45 1 0.149207 0.580999 0.967526 11.00000 0.01713 0.01703 = 0.02284 -0.01063 -0.00023 0.00237 AFIX 43 H45 2 0.076921 0.642067 0.970795 11.00000 41.00000 AFIX 0 C46 1 0.161347 0.511914 0.887739 11.00000 0.01544 0.01778 = 0.01837 -0.00776 -0.00225 0.00009 AFIX 43 H46 2 0.097099 0.525693 0.835978 11.00000 41.00000 AFIX 0 C51 1 0.131807 0.250155 0.807325 11.00000 0.00816 0.00799 = 0.01425 -0.00350 0.00064 -0.00018 C52 1 0.071636 0.207816 0.729336 11.00000 0.01513 0.00843 = 0.01557 -0.00035 -0.00204 -0.00151 AFIX 43 H52 2 0.100908 0.225575 0.657286 11.00000 51.00000 AFIX 0 C53 1 -0.030840 0.139828 0.756106 11.00000 0.01774 0.00995 = 0.03062 -0.00257 -0.00817 -0.00425 AFIX 43 H53 2 -0.071116 0.111603 0.702307 11.00000 51.00000 AFIX 0 C54 1 -0.074223 0.113225 0.860602 11.00000 0.01401 0.01233 = 0.03710 -0.00005 0.00311 -0.00611 AFIX 43 H54 2 -0.145443 0.068634 0.878544 11.00000 51.00000 AFIX 0 C55 1 -0.013180 0.152005 0.939005 11.00000 0.02107 0.01291 = 0.02150 -0.00349 0.01115 -0.00429 AFIX 43 H55 2 -0.041692 0.132006 1.011170 11.00000 51.00000 AFIX 0 C56 1 0.089206 0.219775 0.913364 11.00000 0.01475 0.01206 = 0.01543 -0.00383 0.00417 -0.00224 AFIX 43 H56 2 0.130443 0.245586 0.967946 11.00000 51.00000 AFIX 0 HKLF 4 REM JS90.res in P-1 J.Schachner (Me2C3H2NO-NO2C6H3O)ReOCl2(PPh3) green 100K REM R1 = 0.0297 for 7645 Fo > 4sig(Fo) and 0.0327 for all 8300 data REM 370 parameters refined using 0 restraints END WGHT 0.0190 0.4664 REM Highest difference peak 2.735, deepest hole -2.273, 1-sigma level 0.170 Q1 1 0.5251 0.2018 0.7202 11.00000 0.05 2.73 Q2 1 0.4018 0.1717 0.7834 11.00000 0.05 2.42 Q3 1 0.4581 0.2656 0.7526 11.00000 0.05 2.26 Q4 1 0.4675 0.1102 0.7475 11.00000 0.05 2.18 Q5 1 0.4563 0.1023 0.8153 11.00000 0.05 1.76 Q6 1 0.4422 0.2022 0.8313 11.00000 0.05 1.60 Q7 1 0.4786 0.2803 0.6861 11.00000 0.05 1.51 Q8 1 0.3634 0.2599 0.7674 11.00000 0.05 1.40 Q9 1 0.5598 0.1209 0.7372 11.00000 0.05 1.39 Q10 1 0.4806 0.1763 0.6668 11.00000 0.05 1.29 Q11 1 0.4602 0.3545 0.6956 11.00000 0.05 1.19 Q12 1 0.4745 0.0236 0.8011 11.00000 0.05 1.12 Q13 1 0.4243 0.1317 0.7129 11.00000 0.05 1.00 Q14 1 0.3325 -0.1755 0.7138 11.00000 0.05 0.93 Q15 1 0.5799 0.2155 0.6648 11.00000 0.05 0.85 Q16 1 0.5718 0.2681 0.8026 11.00000 0.05 0.78 Q17 1 0.2506 -0.0795 0.8605 11.00000 0.05 0.78 Q18 1 0.4055 0.1929 0.7195 11.00000 0.05 0.77 Q19 1 0.4564 0.3231 0.8048 11.00000 0.05 0.72 Q20 1 0.1987 0.3120 0.8175 11.00000 0.05 0.71 ; _shelx_res_checksum 25111 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 0.46362(2) 0.18922(2) 0.75145(2) 0.00867(4) Uani 1 1 d . . . . . O1 O 0.45499(19) 0.1313(2) 0.88368(15) 0.0151(4) Uani 1 1 d . . . . . Cl1 Cl 0.58990(6) 0.35239(7) 0.75402(5) 0.01444(14) Uani 1 1 d . . . . . Cl2 Cl 0.64947(6) 0.07073(7) 0.69678(6) 0.01988(15) Uani 1 1 d . . . . . O11 O 0.2511(2) -0.0589(2) 0.62548(18) 0.0238(5) Uani 1 1 d . . . . . C12 C 0.3058(3) 0.0445(3) 0.6298(2) 0.0136(6) Uani 1 1 d . . . . . N13 N 0.3610(2) 0.0437(2) 0.71766(19) 0.0128(5) Uani 1 1 d . . . . . C14 C 0.3520(3) -0.0872(3) 0.7907(2) 0.0149(6) Uani 1 1 d . . . . . C15 C 0.2512(4) -0.1353(4) 0.7347(3) 0.0383(10) Uani 1 1 d . . . . . H151 H 0.2727 -0.2280 0.7353 0.055(10) Uiso 1 1 calc R U . . . H152 H 0.1679 -0.1213 0.7698 0.055(10) Uiso 1 1 calc R U . . . C16 C 0.3050(4) -0.0800(4) 0.9031(3) 0.0361(9) Uani 1 1 d . . . . . H161 H 0.2812 -0.1633 0.9396 0.052(8) Uiso 1 1 calc R U . . . H162 H 0.2315 -0.0140 0.8994 0.052(8) Uiso 1 1 calc R U . . . H163 H 0.3720 -0.0578 0.9429 0.052(8) Uiso 1 1 calc R U . . . C17 C 0.4768(4) -0.1710(4) 0.7934(4) 0.0489(12) Uani 1 1 d . . . . . H171 H 0.5391 -0.1352 0.8283 0.050(7) Uiso 1 1 calc R U . . . H172 H 0.5051 -0.1747 0.7202 0.050(7) Uiso 1 1 calc R U . . . H173 H 0.4676 -0.2578 0.8336 0.050(7) Uiso 1 1 calc R U . . . O21 O 0.43307(17) 0.26532(19) 0.59672(15) 0.0117(4) Uani 1 1 d . . . . . C21 C 0.3578(2) 0.2530(3) 0.5215(2) 0.0116(5) Uani 1 1 d . . . . . C22 C 0.2932(3) 0.1450(3) 0.5329(2) 0.0127(6) Uani 1 1 d . . . . . C23 C 0.2150(3) 0.1351(3) 0.4509(2) 0.0156(6) Uani 1 1 d . . . . . H23 H 0.1706 0.0631 0.4577 0.015(5) Uiso 1 1 calc R U . . . C24 C 0.2034(3) 0.2314(3) 0.3602(2) 0.0147(6) Uani 1 1 d . . . . . C25 C 0.2661(3) 0.3390(3) 0.3472(2) 0.0152(6) Uani 1 1 d . . . . . H25 H 0.2559 0.4041 0.2839 0.015(5) Uiso 1 1 calc R U . . . C26 C 0.3429(3) 0.3495(3) 0.4276(2) 0.0152(6) Uani 1 1 d . . . . . H26 H 0.3863 0.4224 0.4196 0.015(5) Uiso 1 1 calc R U . . . N24 N 0.1197(2) 0.2208(3) 0.2761(2) 0.0216(6) Uani 1 1 d . . . . . O23 O 0.0549(2) 0.1334(2) 0.2935(2) 0.0313(6) Uani 1 1 d . . . . . O25 O 0.1191(3) 0.3006(3) 0.19187(19) 0.0353(6) Uani 1 1 d . . . . . P1 P 0.26896(6) 0.33408(7) 0.77500(5) 0.00856(13) Uani 1 1 d . . . . . C31 C 0.2289(2) 0.4651(3) 0.6607(2) 0.0103(5) Uani 1 1 d . . . . . C32 C 0.3248(3) 0.5363(3) 0.6162(2) 0.0152(6) Uani 1 1 d . . . . . H32 H 0.4087 0.5096 0.6406 0.017(4) Uiso 1 1 calc R U . . . C33 C 0.2988(3) 0.6456(3) 0.5367(2) 0.0192(6) Uani 1 1 d . . . . . H33 H 0.3646 0.6936 0.5067 0.017(4) Uiso 1 1 calc R U . . . C34 C 0.1763(3) 0.6846(3) 0.5010(2) 0.0207(7) Uani 1 1 d . . . . . H34 H 0.1583 0.7595 0.4464 0.017(4) Uiso 1 1 calc R U . . . C35 C 0.0806(3) 0.6152(3) 0.5443(2) 0.0184(6) Uani 1 1 d . . . . . H35 H -0.0030 0.6425 0.5191 0.017(4) Uiso 1 1 calc R U . . . C36 C 0.1052(3) 0.5054(3) 0.6249(2) 0.0143(6) Uani 1 1 d . . . . . H36 H 0.0388 0.4584 0.6552 0.017(4) Uiso 1 1 calc R U . . . C41 C 0.2666(2) 0.4224(3) 0.8823(2) 0.0095(5) Uani 1 1 d . . . . . C42 C 0.3601(3) 0.4014(3) 0.9580(2) 0.0143(6) Uani 1 1 d . . . . . H42 H 0.4319 0.3395 0.9555 0.020(4) Uiso 1 1 calc R U . . . C43 C 0.3477(3) 0.4724(3) 1.0379(2) 0.0166(6) Uani 1 1 d . . . . . H43 H 0.4121 0.4597 1.0894 0.020(4) Uiso 1 1 calc R U . . . C44 C 0.2430(3) 0.5609(3) 1.0429(2) 0.0169(6) Uani 1 1 d . . . . . H44 H 0.2350 0.6082 1.0981 0.020(4) Uiso 1 1 calc R U . . . C45 C 0.1492(3) 0.5810(3) 0.9675(2) 0.0185(6) Uani 1 1 d . . . . . H45 H 0.0769 0.6421 0.9708 0.020(4) Uiso 1 1 calc R U . . . C46 C 0.1613(3) 0.5119(3) 0.8877(2) 0.0168(6) Uani 1 1 d . . . . . H46 H 0.0971 0.5257 0.8360 0.020(4) Uiso 1 1 calc R U . . . C51 C 0.1318(2) 0.2502(3) 0.8073(2) 0.0101(5) Uani 1 1 d . . . . . C52 C 0.0716(3) 0.2078(3) 0.7293(2) 0.0133(6) Uani 1 1 d . . . . . H52 H 0.1009 0.2256 0.6573 0.016(4) Uiso 1 1 calc R U . . . C53 C -0.0308(3) 0.1398(3) 0.7561(3) 0.0192(6) Uani 1 1 d . . . . . H53 H -0.0711 0.1116 0.7023 0.016(4) Uiso 1 1 calc R U . . . C54 C -0.0742(3) 0.1132(3) 0.8606(3) 0.0216(7) Uani 1 1 d . . . . . H54 H -0.1454 0.0686 0.8785 0.016(4) Uiso 1 1 calc R U . . . C55 C -0.0132(3) 0.1520(3) 0.9390(2) 0.0186(6) Uani 1 1 d . . . . . H55 H -0.0417 0.1320 1.0112 0.016(4) Uiso 1 1 calc R U . . . C56 C 0.0892(3) 0.2198(3) 0.9134(2) 0.0140(6) Uani 1 1 d . . . . . H56 H 0.1304 0.2456 0.9679 0.016(4) 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 0.00763(6) 0.00948(7) 0.00980(6) -0.00397(4) 0.00027(4) -0.00133(4) O1 0.0172(10) 0.0151(11) 0.0137(10) -0.0032(8) -0.0022(8) -0.0038(8) Cl1 0.0131(3) 0.0158(4) 0.0164(3) -0.0051(3) -0.0009(2) -0.0063(3) Cl2 0.0109(3) 0.0199(4) 0.0311(4) -0.0120(3) 0.0040(3) -0.0004(3) O11 0.0386(14) 0.0120(11) 0.0230(12) -0.0013(9) -0.0106(10) -0.0121(10) C12 0.0162(13) 0.0079(14) 0.0190(14) -0.0075(11) -0.0005(11) -0.0022(11) N13 0.0116(11) 0.0113(12) 0.0150(12) -0.0015(9) 0.0009(9) -0.0020(9) C14 0.0171(14) 0.0089(14) 0.0175(14) -0.0001(11) 0.0004(11) -0.0017(11) C15 0.059(3) 0.023(2) 0.034(2) 0.0080(16) -0.0207(19) -0.0225(19) C16 0.055(3) 0.025(2) 0.032(2) -0.0064(16) 0.0209(17) -0.0209(18) C17 0.027(2) 0.018(2) 0.085(3) 0.019(2) 0.013(2) 0.0081(16) O21 0.0095(9) 0.0182(11) 0.0093(9) -0.0048(8) 0.0018(7) -0.0056(8) C21 0.0101(12) 0.0156(15) 0.0118(13) -0.0087(11) 0.0035(10) -0.0023(11) C22 0.0129(13) 0.0112(14) 0.0156(14) -0.0068(11) -0.0001(10) -0.0008(11) C23 0.0158(14) 0.0129(15) 0.0209(15) -0.0095(12) -0.0020(11) -0.0014(12) C24 0.0146(13) 0.0165(16) 0.0147(14) -0.0091(12) -0.0026(11) 0.0017(12) C25 0.0163(14) 0.0167(16) 0.0119(13) -0.0028(11) 0.0018(10) -0.0003(12) C26 0.0152(13) 0.0165(16) 0.0149(14) -0.0049(12) 0.0027(10) -0.0039(12) N24 0.0197(13) 0.0235(15) 0.0235(14) -0.0108(12) -0.0077(11) 0.0025(12) O23 0.0333(14) 0.0251(14) 0.0399(15) -0.0101(11) -0.0183(11) -0.0087(11) O25 0.0418(15) 0.0421(17) 0.0209(13) 0.0025(11) -0.0170(11) -0.0118(13) P1 0.0083(3) 0.0088(4) 0.0090(3) -0.0024(3) 0.0008(2) -0.0021(3) C31 0.0118(12) 0.0091(14) 0.0099(12) -0.0026(10) 0.0011(10) -0.0003(10) C32 0.0128(13) 0.0161(16) 0.0165(14) -0.0031(12) 0.0009(10) -0.0023(11) C33 0.0230(15) 0.0159(16) 0.0181(15) 0.0005(12) 0.0036(12) -0.0078(13) C34 0.0281(17) 0.0146(16) 0.0164(15) 0.0035(12) -0.0022(12) -0.0025(13) C35 0.0184(14) 0.0173(16) 0.0187(15) -0.0031(12) -0.0063(12) 0.0008(12) C36 0.0157(13) 0.0130(15) 0.0151(14) -0.0039(11) 0.0005(10) -0.0032(11) C41 0.0122(12) 0.0073(13) 0.0100(12) -0.0029(10) 0.0015(9) -0.0033(10) C42 0.0143(13) 0.0130(15) 0.0150(14) -0.0034(11) -0.0005(10) 0.0008(11) C43 0.0197(14) 0.0179(16) 0.0138(14) -0.0066(12) -0.0025(11) -0.0025(12) C44 0.0215(15) 0.0147(16) 0.0174(14) -0.0085(12) 0.0003(11) -0.0047(12) C45 0.0171(14) 0.0170(16) 0.0228(15) -0.0106(13) -0.0002(12) 0.0024(12) C46 0.0154(14) 0.0178(16) 0.0184(15) -0.0078(12) -0.0022(11) 0.0001(12) C51 0.0082(12) 0.0080(13) 0.0142(13) -0.0035(10) 0.0006(9) -0.0002(10) C52 0.0151(13) 0.0084(14) 0.0156(14) -0.0004(11) -0.0020(10) -0.0015(11) C53 0.0177(15) 0.0099(15) 0.0306(17) -0.0026(12) -0.0082(12) -0.0042(12) C54 0.0140(14) 0.0123(16) 0.0371(19) -0.0001(14) 0.0031(13) -0.0061(12) C55 0.0211(15) 0.0129(15) 0.0215(15) -0.0035(12) 0.0111(12) -0.0043(12) C56 0.0148(13) 0.0121(15) 0.0154(14) -0.0038(11) 0.0042(10) -0.0022(11) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Cl Cl 0.1484 0.1585 '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 167.51(8) . . yes O1 Re1 N13 92.02(9) . . ? O21 Re1 N13 82.42(8) . . ? O1 Re1 Cl1 98.31(7) . . ? O21 Re1 Cl1 88.17(6) . . ? N13 Re1 Cl1 168.96(6) . . yes O1 Re1 P1 86.32(7) . . ? O21 Re1 P1 82.83(6) . . ? N13 Re1 P1 93.07(7) . . ? Cl1 Re1 P1 91.46(2) . . ? Cl2 Re1 P1 169.80(3) . . yes O1 Re1 Cl2 103.84(7) . . ? O21 Re1 Cl2 87.16(6) . . ? N13 Re1 Cl2 87.50(7) . . ? Cl1 Re1 Cl2 86.27(3) . . yes C12 O11 C15 106.1(2) . . ? N13 C12 O11 117.0(3) . . ? N13 C12 C22 128.6(3) . . ? O11 C12 C22 114.4(2) . . ? C12 N13 C14 106.9(2) . . yes C12 N13 Re1 127.3(2) . . yes C14 N13 Re1 125.55(17) . . yes C17 C14 C16 110.8(3) . . ? C17 C14 C15 112.3(3) . . ? C16 C14 C15 108.3(3) . . ? C17 C14 N13 110.1(2) . . ? C16 C14 N13 113.8(3) . . ? C15 C14 N13 101.2(2) . . ? O11 C15 C14 104.3(3) . . ? 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 137.57(18) . . yes O21 C21 C26 119.1(2) . . ? O21 C21 C22 121.4(3) . . ? C26 C21 C22 119.5(2) . . ? C23 C22 C21 119.6(3) . . ? C23 C22 C12 119.8(3) . . ? C21 C22 C12 120.6(2) . . ? C24 C23 C22 119.1(3) . . ? C24 C23 H23 120.5 . . ? C22 C23 H23 120.5 . . ? C23 C24 C25 122.4(3) . . ? C23 C24 N24 118.4(3) . . ? C25 C24 N24 119.2(3) . . ? C26 C25 C24 118.9(3) . . ? C26 C25 H25 120.6 . . ? C24 C25 H25 120.6 . . ? C25 C26 C21 120.5(3) . . ? C25 C26 H26 119.7 . . ? C21 C26 H26 119.7 . . ? O23 N24 O25 123.9(3) . . ? O23 N24 C24 118.4(3) . . ? O25 N24 C24 117.7(3) . . ? C51 P1 C31 107.39(12) . . ? C51 P1 C41 102.25(12) . . ? C31 P1 C41 100.90(13) . . ? C51 P1 Re1 112.94(9) . . ? C31 P1 Re1 114.64(9) . . ? C41 P1 Re1 117.25(9) . . ? C32 C31 C36 119.5(3) . . ? C32 C31 P1 117.2(2) . . ? C36 C31 P1 122.9(2) . . ? C33 C32 C31 120.6(3) . . ? C33 C32 H32 119.7 . . ? C31 C32 H32 119.7 . . ? C32 C33 C34 119.7(3) . . ? C32 C33 H33 120.2 . . ? C34 C33 H33 120.2 . . ? C35 C34 C33 120.3(3) . . ? C35 C34 H34 119.8 . . ? C33 C34 H34 119.8 . . ? C34 C35 C36 120.6(3) . . ? C34 C35 H35 119.7 . . ? C36 C35 H35 119.7 . . ? C35 C36 C31 119.3(3) . . ? C35 C36 H36 120.4 . . ? C31 C36 H36 120.4 . . ? C42 C41 C46 119.8(3) . . ? C42 C41 P1 123.9(2) . . ? C46 C41 P1 116.3(2) . . ? C41 C42 C43 119.2(3) . . ? C41 C42 H42 120.4 . . ? C43 C42 H42 120.4 . . ? C44 C43 C42 120.6(3) . . ? C44 C43 H43 119.7 . . ? C42 C43 H43 119.7 . . ? C43 C44 C45 120.0(3) . . ? C43 C44 H44 120.0 . . ? C45 C44 H44 120.0 . . ? C46 C45 C44 119.6(3) . . ? C46 C45 H45 120.2 . . ? C44 C45 H45 120.2 . . ? C45 C46 C41 120.6(3) . . ? C45 C46 H46 119.7 . . ? C41 C46 H46 119.7 . . ? C52 C51 C56 118.6(2) . . ? C52 C51 P1 121.3(2) . . ? C56 C51 P1 119.9(2) . . ? C53 C52 C51 120.6(3) . . ? C53 C52 H52 119.7 . . ? C51 C52 H52 119.7 . . ? C54 C53 C52 120.3(3) . . ? C54 C53 H53 119.9 . . ? C52 C53 H53 119.9 . . ? C53 C54 C55 119.5(3) . . ? C53 C54 H54 120.2 . . ? C55 C54 H54 120.2 . . ? C54 C55 C56 120.8(3) . . ? C54 C55 H55 119.6 . . ? C56 C55 H55 119.6 . . ? C55 C56 C51 120.1(3) . . ? 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 1.6775(19) . yes Re1 Cl1 2.3632(7) . yes Re1 Cl2 2.3766(7) . yes Re1 N13 2.155(2) . yes Re1 O21 1.9969(18) . yes Re1 P1 2.4749(7) . yes O11 C12 1.338(3) . ? O11 C15 1.463(4) . ? C12 N13 1.290(3) . ? C12 C22 1.458(4) . ? N13 C14 1.527(4) . ? C14 C17 1.504(5) . ? C14 C16 1.519(4) . ? C14 C15 1.523(4) . ? 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 1.320(3) . ? C21 C26 1.409(4) . ? C21 C22 1.410(4) . ? C22 C23 1.399(4) . ? C23 C24 1.378(4) . ? C23 H23 0.95 . ? C24 C25 1.391(4) . ? C24 N24 1.462(3) . ? C25 C26 1.376(4) . ? C25 H25 0.95 . ? C26 H26 0.95 . ? N24 O23 1.221(3) . ? N24 O25 1.225(4) . ? P1 C51 1.815(3) . ? P1 C31 1.821(3) . ? P1 C41 1.827(3) . ? C31 C32 1.394(4) . ? C31 C36 1.400(4) . ? C32 C33 1.384(4) . ? C32 H32 0.95 . ? C33 C34 1.387(4) . ? C33 H33 0.95 . ? C34 C35 1.378(4) . ? C34 H34 0.95 . ? C35 C36 1.395(4) . ? C35 H35 0.95 . ? C36 H36 0.95 . ? C41 C42 1.386(4) . ? C41 C46 1.389(4) . ? C42 C43 1.393(4) . ? C42 H42 0.95 . ? C43 C44 1.377(4) . ? C43 H43 0.95 . ? C44 C45 1.385(4) . ? C44 H44 0.95 . ? C45 C46 1.378(4) . ? C45 H45 0.95 . ? C46 H46 0.95 . ? C51 C52 1.396(4) . ? C51 C56 1.399(4) . ? C52 C53 1.392(4) . ? C52 H52 0.95 . ? C53 C54 1.381(4) . ? C53 H53 0.95 . ? C54 C55 1.385(4) . ? C54 H54 0.95 . ? C55 C56 1.388(4) . ? 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 10.5(4) . . . . ? C15 O11 C12 C22 -168.8(3) . . . . ? O11 C12 N13 C14 3.6(3) . . . . ? C22 C12 N13 C14 -177.3(3) . . . . ? O11 C12 N13 Re1 177.73(19) . . . . ? C22 C12 N13 Re1 -3.1(4) . . . . ? C12 N13 C14 C17 103.8(3) . . . . ? Re1 N13 C14 C17 -70.5(3) . . . . ? C12 N13 C14 C16 -131.1(3) . . . . ? Re1 N13 C14 C16 54.6(3) . . . . ? C12 N13 C14 C15 -15.2(3) . . . . ? Re1 N13 C14 C15 170.5(2) . . . . ? C12 O11 C15 C14 -19.5(4) . . . . ? C17 C14 C15 O11 -97.0(3) . . . . ? C16 C14 C15 O11 140.3(3) . . . . ? N13 C14 C15 O11 20.4(3) . . . . ? Re1 O21 C21 C26 163.3(2) . . . . ? Re1 O21 C21 C22 -17.3(4) . . . . ? O21 C21 C22 C23 -179.5(3) . . . . ? C26 C21 C22 C23 -0.1(4) . . . . ? O21 C21 C22 C12 1.3(4) . . . . ? C26 C21 C22 C12 -179.3(3) . . . . ? N13 C12 C22 C23 -171.3(3) . . . . yes O11 C12 C22 C23 7.9(4) . . . . yes N13 C12 C22 C21 7.9(5) . . . . yes O11 C12 C22 C21 -172.9(3) . . . . yes C21 C22 C23 C24 0.3(4) . . . . ? C12 C22 C23 C24 179.5(3) . . . . ? C22 C23 C24 C25 -0.5(4) . . . . ? C22 C23 C24 N24 -178.9(3) . . . . ? C23 C24 C25 C26 0.3(4) . . . . ? N24 C24 C25 C26 178.8(3) . . . . ? C24 C25 C26 C21 -0.1(4) . . . . ? O21 C21 C26 C25 179.4(3) . . . . ? C22 C21 C26 C25 0.0(4) . . . . ? C23 C24 N24 O23 6.5(4) . . . . yes C25 C24 N24 O23 -172.0(3) . . . . yes C23 C24 N24 O25 -173.3(3) . . . . yes C25 C24 N24 O25 8.1(4) . . . . yes C51 P1 C31 C32 -174.7(2) . . . . ? C41 P1 C31 C32 78.6(2) . . . . ? Re1 P1 C31 C32 -48.3(2) . . . . ? C51 P1 C31 C36 13.0(3) . . . . ? C41 P1 C31 C36 -93.7(2) . . . . ? Re1 P1 C31 C36 139.4(2) . . . . ? C36 C31 C32 C33 -0.5(4) . . . . ? P1 C31 C32 C33 -173.1(2) . . . . ? C31 C32 C33 C34 0.0(5) . . . . ? C32 C33 C34 C35 0.1(5) . . . . ? C33 C34 C35 C36 0.3(5) . . . . ? C34 C35 C36 C31 -0.8(4) . . . . ? C32 C31 C36 C35 0.9(4) . . . . ? P1 C31 C36 C35 173.0(2) . . . . ? C51 P1 C41 C42 116.1(2) . . . . ? C31 P1 C41 C42 -133.2(2) . . . . ? Re1 P1 C41 C42 -8.0(3) . . . . ? C51 P1 C41 C46 -61.7(2) . . . . ? C31 P1 C41 C46 48.9(2) . . . . ? Re1 P1 C41 C46 174.17(18) . . . . ? C46 C41 C42 C43 -0.9(4) . . . . ? P1 C41 C42 C43 -178.7(2) . . . . ? C41 C42 C43 C44 1.1(4) . . . . ? C42 C43 C44 C45 -0.6(5) . . . . ? C43 C44 C45 C46 0.1(5) . . . . ? C44 C45 C46 C41 0.0(5) . . . . ? C42 C41 C46 C45 0.4(4) . . . . ? P1 C41 C46 C45 178.3(2) . . . . ? C31 P1 C51 C52 51.4(3) . . . . ? C41 P1 C51 C52 157.1(2) . . . . ? Re1 P1 C51 C52 -76.0(2) . . . . ? C31 P1 C51 C56 -132.6(2) . . . . ? C41 P1 C51 C56 -26.9(3) . . . . ? Re1 P1 C51 C56 100.1(2) . . . . ? C56 C51 C52 C53 1.7(4) . . . . ? P1 C51 C52 C53 177.8(2) . . . . ? C51 C52 C53 C54 -0.1(5) . . . . ? C52 C53 C54 C55 -1.5(5) . . . . ? C53 C54 C55 C56 1.5(5) . . . . ? C54 C55 C56 C51 0.2(5) . . . . ? C52 C51 C56 C55 -1.8(4) . . . . ? P1 C51 C56 C55 -177.9(2) . . . . ?