#------------------------------------------------------------------------------ #$Date: 2020-09-06 12:33:13 +0300 (Sun, 06 Sep 2020) $ #$Revision: 256066 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/49/7704994.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_7704994 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 '2(C29 H27 Cl2 N O3 P Re), C2 H3 N' _chemical_formula_sum 'C60 H57 Cl4 N3 O6 P2 Re2' _chemical_formula_weight 1492.22 _chemical_name_common 'dichloro-(2-(4,4-dimethyl-4,5-dihydro-1,3-oxazol-2-yl)-pheno-lato-N,O)-oxo-triphenylphosphine-rhenium(V) acetonitrile solvate (2:1)' _chemical_name_systematic 'dichloro-(2-(4,4-dimethyl-4,5-dihydro-1,3-oxazol-2-yl)-pheno-lato-N,O)-oxo-triphenylphosphine-rhenium(V) acetonitrile solvate (2:1)' _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. 2020-07-29 downloaded from the CCDC. ; _cell_angle_alpha 81.0109(14) _cell_angle_beta 70.7506(13) _cell_angle_gamma 64.3553(12) _cell_formula_units_Z 1 _cell_length_a 10.1415(4) _cell_length_b 11.3165(5) _cell_length_c 14.1899(6) _cell_measurement_reflns_used 9876 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 30.97 _cell_measurement_theta_min 2.38 _cell_volume 1385.85(10) _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 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0245 _diffrn_reflns_av_unetI/netI 0.0159 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 41467 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_theta_full 30.00 _diffrn_reflns_theta_max 30.00 _diffrn_reflns_theta_min 2.00 _exptl_absorpt_coefficient_mu 4.669 _exptl_absorpt_correction_T_max 0.837 _exptl_absorpt_correction_T_min 0.719 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Bruker SADABS' _exptl_crystal_colour green _exptl_crystal_density_diffrn 1.788 _exptl_crystal_description block _exptl_crystal_F_000 734 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _refine_diff_density_max 2.199 _refine_diff_density_min -0.947 _refine_diff_density_rms 0.096 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_hydrogen_treatment refU _refine_ls_matrix_type full _refine_ls_number_parameters 360 _refine_ls_number_reflns 8052 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.093 _refine_ls_R_factor_all 0.0175 _refine_ls_R_factor_gt 0.0167 _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^)+(0.0208P)^2^+1.6254P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0443 _refine_ls_wR_factor_ref 0.0448 _reflns_Friedel_coverage 0.000 _reflns_number_gt 7792 _reflns_number_total 8052 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0dt02352c2.cif _cod_data_source_block JS31 _cod_depositor_comments 'Adding full bibliography for 7704994--7704996.cif.' _cod_database_code 7704994 _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 0.541 _shelx_estimated_absorpt_t_max 0.604 _shelxl_version_number 2014/6 _shelx_res_file ; TITL JS31_0m in P-1 J.Schachner (Me2C3H2NO-C6H4O)ReOCl2(PPh3)*CH3CN green 100K CELL 0.71073 10.1415 11.3165 14.1899 81.0109 70.7506 64.3553 ZERR 1 0.0004 0.0005 0.0006 0.0014 0.0013 0.0012 LATT 1 EQIV $1 1-X, 1-Y, 1-Z SFAC C H CL N O P RE UNIT 60 57 4 3 6 2 2 TEMP -173.150 SIZE 0.12 0.12 0.15 ACTA 60.0004 MERG 2 OMIT -2 60.0004 L.S. 5 FREE N61 C62_$1 FREE C61 C61_$1 FREE C61 C62_$1 FREE C62 N61_$1 FREE C62 C61_$1 FREE C62 C62_$1 BOND $H CONF HTAB FMAP 2 PLAN 20 WGHT 0.020800 1.625400 FVAR 0.12075 0.02787 0.02574 0.02779 0.02820 0.03605 0.02901 FVAR 0.03613 0.06454 O1 5 0.996515 0.794341 0.115863 11.00000 0.01981 0.01900 = 0.01281 0.00156 -0.00505 -0.00831 RE1 7 0.952703 0.799412 0.241398 11.00000 0.01375 0.01279 = 0.01112 0.00160 -0.00442 -0.00624 CL1 3 1.214080 0.709550 0.242533 11.00000 0.01581 0.01703 = 0.02100 0.00129 -0.00778 -0.00577 CL2 3 0.684927 0.868571 0.262639 11.00000 0.01478 0.02419 = 0.02178 0.00188 -0.00593 -0.00941 P1 6 0.911107 1.031636 0.239758 11.00000 0.01212 0.01201 = 0.01014 0.00075 -0.00379 -0.00529 O11 5 0.930005 0.432220 0.361039 11.00000 0.03019 0.01556 = 0.01949 -0.00072 0.00072 -0.01217 C12 1 0.915359 0.556001 0.359662 11.00000 0.01703 0.01458 = 0.01710 0.00085 -0.00412 -0.00807 N13 4 0.962516 0.604891 0.273367 11.00000 0.01796 0.01501 = 0.01421 -0.00011 -0.00501 -0.00755 C14 1 1.010078 0.507200 0.194577 11.00000 0.02681 0.01651 = 0.01637 -0.00168 -0.00566 -0.01105 C15 1 1.005013 0.386128 0.259497 11.00000 0.03232 0.01658 = 0.01889 -0.00053 -0.00575 -0.01235 AFIX 23 H151 2 0.946564 0.348596 0.239414 11.00000 61.00000 H152 2 1.109805 0.318039 0.252914 11.00000 61.00000 AFIX 0 C16 1 1.169291 0.481199 0.124045 11.00000 0.02887 0.02293 = 0.02175 -0.00556 0.00060 -0.01157 AFIX 137 H161 2 1.167853 0.560494 0.084223 11.00000 71.00000 H162 2 1.201108 0.409457 0.079581 11.00000 71.00000 H163 2 1.241557 0.456882 0.162858 11.00000 71.00000 AFIX 0 C17 1 0.889578 0.555668 0.139171 11.00000 0.03868 0.02614 = 0.02519 -0.00080 -0.01664 -0.01549 AFIX 137 H171 2 0.788215 0.575680 0.187490 11.00000 81.00000 H172 2 0.912249 0.487471 0.094140 11.00000 81.00000 H173 2 0.890921 0.634963 0.100318 11.00000 81.00000 AFIX 0 O21 5 0.894141 0.805840 0.386399 11.00000 0.02030 0.01624 = 0.01413 0.00195 -0.00501 -0.01007 C21 1 0.831733 0.745854 0.464886 11.00000 0.01527 0.01739 = 0.01210 0.00246 -0.00454 -0.00703 C22 1 0.842946 0.619915 0.455889 11.00000 0.01650 0.01692 = 0.01431 0.00144 -0.00312 -0.00696 C23 1 0.781076 0.556311 0.540211 11.00000 0.02369 0.01941 = 0.01906 0.00312 -0.00212 -0.01108 AFIX 43 H23 2 0.792579 0.469452 0.535094 11.00000 21.00000 AFIX 0 C24 1 0.703487 0.619438 0.630665 11.00000 0.02558 0.02544 = 0.01600 0.00389 -0.00150 -0.01180 AFIX 43 H24 2 0.659866 0.576798 0.687237 11.00000 21.00000 AFIX 0 C25 1 0.689453 0.745847 0.638610 11.00000 0.02369 0.02534 = 0.01380 0.00074 -0.00395 -0.00896 AFIX 43 H25 2 0.634059 0.789735 0.700476 11.00000 21.00000 AFIX 0 C26 1 0.755336 0.808325 0.557338 11.00000 0.02167 0.01883 = 0.01419 0.00004 -0.00585 -0.00785 AFIX 43 H26 2 0.748760 0.893024 0.564246 11.00000 21.00000 AFIX 0 C31 1 0.821258 1.098229 0.364840 11.00000 0.01624 0.01398 = 0.01057 0.00121 -0.00445 -0.00457 C32 1 0.672178 1.108104 0.412029 11.00000 0.01604 0.01965 = 0.01591 -0.00027 -0.00314 -0.00583 AFIX 43 H32 2 0.622487 1.082276 0.378105 11.00000 31.00000 AFIX 0 C33 1 0.596662 1.155636 0.508455 11.00000 0.01807 0.02461 = 0.01509 0.00065 -0.00028 -0.00432 AFIX 43 H33 2 0.494593 1.164108 0.539838 11.00000 31.00000 AFIX 0 C34 1 0.670239 1.190758 0.558976 11.00000 0.02782 0.02345 = 0.01235 -0.00149 -0.00434 -0.00326 AFIX 43 H34 2 0.619177 1.221439 0.625424 11.00000 31.00000 AFIX 0 C35 1 0.817916 1.181188 0.512759 11.00000 0.02897 0.02305 = 0.01477 -0.00266 -0.00872 -0.00755 AFIX 43 H35 2 0.867940 1.205347 0.547514 11.00000 31.00000 AFIX 0 C36 1 0.893207 1.136097 0.415219 11.00000 0.01903 0.01861 = 0.01427 -0.00072 -0.00531 -0.00675 AFIX 43 H36 2 0.993714 1.131227 0.383133 11.00000 31.00000 AFIX 0 C41 1 0.783932 1.141600 0.168441 11.00000 0.01190 0.01529 = 0.01232 0.00188 -0.00358 -0.00600 C42 1 0.779860 1.097105 0.083688 11.00000 0.01656 0.01626 = 0.01397 0.00166 -0.00633 -0.00728 AFIX 43 H42 2 0.835798 1.007067 0.067016 11.00000 41.00000 AFIX 0 C43 1 0.694486 1.183566 0.023324 11.00000 0.01911 0.02265 = 0.01436 0.00362 -0.00713 -0.01021 AFIX 43 H43 2 0.692971 1.152799 -0.034723 11.00000 41.00000 AFIX 0 C44 1 0.611523 1.314883 0.048095 11.00000 0.01882 0.02142 = 0.01866 0.00607 -0.00785 -0.00542 AFIX 43 H44 2 0.553187 1.373997 0.006900 11.00000 41.00000 AFIX 0 C45 1 0.613487 1.360171 0.132893 11.00000 0.02409 0.01704 = 0.02073 0.00137 -0.00651 -0.00164 AFIX 43 H45 2 0.555728 1.449955 0.149991 11.00000 41.00000 AFIX 0 C46 1 0.700326 1.273782 0.193018 11.00000 0.02181 0.01671 = 0.01564 -0.00027 -0.00635 -0.00516 AFIX 43 H46 2 0.702518 1.304948 0.250647 11.00000 41.00000 AFIX 0 C51 1 1.083710 1.060735 0.186387 11.00000 0.01343 0.01325 = 0.01269 -0.00182 -0.00363 -0.00573 C52 1 1.201026 1.002643 0.231840 11.00000 0.01641 0.01689 = 0.01910 -0.00032 -0.00753 -0.00558 AFIX 43 H52 2 1.187723 0.951822 0.291359 11.00000 51.00000 AFIX 0 C53 1 1.336782 1.019022 0.190255 11.00000 0.01490 0.02297 = 0.02971 -0.00542 -0.00826 -0.00566 AFIX 43 H53 2 1.415008 0.981333 0.222304 11.00000 51.00000 AFIX 0 C54 1 1.358228 1.090140 0.102236 11.00000 0.01608 0.02545 = 0.02979 -0.00795 0.00017 -0.01145 AFIX 43 H54 2 1.451319 1.100962 0.073829 11.00000 51.00000 AFIX 0 C55 1 1.244540 1.145493 0.055520 11.00000 0.02304 0.02156 = 0.01781 -0.00144 0.00002 -0.01328 AFIX 43 H55 2 1.260839 1.192556 -0.005697 11.00000 51.00000 AFIX 0 C56 1 1.106369 1.132780 0.097514 11.00000 0.01685 0.01653 = 0.01358 -0.00149 -0.00276 -0.00765 AFIX 43 H56 2 1.027669 1.172893 0.065936 11.00000 51.00000 AFIX 0 PART 1 10.5 EADP N61 C61 C62 N61 4 0.601487 0.486290 0.374330 10.50000 0.03516 0.03472 = 0.04923 -0.01276 -0.00544 -0.00872 C61 1 0.535194 0.496897 0.459508 10.50000 0.03516 0.03472 = 0.04923 -0.01276 -0.00544 -0.00872 C62 1 0.453850 0.509956 0.564087 10.50000 0.03516 0.03472 = 0.04923 -0.01276 -0.00544 -0.00872 AFIX 137 H621 2 0.524723 0.495026 0.602205 10.50000 91.00000 H622 2 0.409024 0.445328 0.584737 10.50000 91.00000 H623 2 0.372265 0.598431 0.576720 10.50000 91.00000 AFIX 0 HKLF 4 REM JS31_0m in P-1 J.Schachner (Me2C3H2NO-C6H4O)ReOCl2(PPh3)*CH3CN green 100K REM R1 = 0.0167 for 7792 Fo > 4sig(Fo) and 0.0175 for all 8052 data REM 360 parameters refined using 0 restraints END WGHT 0.0208 1.6255 REM Instructions for potential hydrogen bonds HTAB C16 O1 HTAB C17 O1 HTAB C32 Cl2 HTAB C42 O1 EQIV $2 x, y+1, z HTAB C46 N61_$2 EQIV $3 -x+2, -y+2, -z HTAB C56 O1_$3 REM Highest difference peak 2.199, deepest hole -0.947, 1-sigma level 0.096 Q1 1 0.9102 0.7976 0.2942 11.00000 0.05 2.20 Q2 1 0.8628 0.8250 0.2426 11.00000 0.05 1.35 Q3 1 1.0372 0.7810 0.2458 11.00000 0.05 1.24 Q4 1 0.9642 0.7432 0.2240 11.00000 0.05 1.15 Q5 1 0.9027 0.8764 0.2575 11.00000 0.05 1.06 Q6 1 0.5550 0.7015 0.1418 11.00000 0.05 0.87 Q7 1 0.9767 0.8043 0.1678 11.00000 0.05 0.72 Q8 1 0.9034 0.9761 0.2444 11.00000 0.05 0.63 Q9 1 0.7796 0.7789 0.5106 11.00000 0.05 0.55 Q10 1 0.7756 1.1226 0.1286 11.00000 0.05 0.54 Q11 1 1.1767 1.1358 0.0764 11.00000 0.05 0.53 Q12 1 1.0135 1.0568 0.2022 11.00000 0.05 0.53 Q13 1 1.1379 1.0325 0.2089 11.00000 0.05 0.53 Q14 1 0.6496 1.3162 0.1684 11.00000 0.05 0.52 Q15 1 0.8531 1.1578 0.4639 11.00000 0.05 0.52 Q16 1 0.6315 1.1311 0.4576 11.00000 0.05 0.52 Q17 1 0.7511 1.2009 0.1755 11.00000 0.05 0.52 Q18 1 1.1605 0.7150 0.2944 11.00000 0.05 0.51 Q19 1 0.5817 1.3332 0.1008 11.00000 0.05 0.50 Q20 1 0.7572 0.8550 0.2703 11.00000 0.05 0.50 ; _shelx_res_checksum 6111 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 O1 O 0.99652(16) 0.79434(14) 0.11586(10) 0.0172(3) Uani 1 1 d . . . . . Re1 Re 0.95270(2) 0.79941(2) 0.24140(2) 0.01226(3) Uani 1 1 d . . . . . Cl1 Cl 1.21408(5) 0.70955(4) 0.24253(3) 0.01785(8) Uani 1 1 d . . . . . Cl2 Cl 0.68493(5) 0.86857(5) 0.26264(4) 0.01984(9) Uani 1 1 d . . . . . P1 P 0.91111(5) 1.03164(4) 0.23976(3) 0.01127(8) Uani 1 1 d . . . . . O11 O 0.93001(18) 0.43222(14) 0.36104(11) 0.0228(3) Uani 1 1 d . . . . . C12 C 0.9154(2) 0.55600(18) 0.35966(14) 0.0160(3) Uani 1 1 d . . . . . N13 N 0.96252(18) 0.60489(16) 0.27337(12) 0.0154(3) Uani 1 1 d . . . . . C14 C 1.0101(2) 0.50720(19) 0.19458(15) 0.0191(4) Uani 1 1 d . . . . . C15 C 1.0050(3) 0.3861(2) 0.25950(15) 0.0222(4) Uani 1 1 d . . . . . H151 H 0.9466 0.3486 0.2394 0.036(6) Uiso 1 1 calc R U . . . H152 H 1.1098 0.3180 0.2529 0.036(6) Uiso 1 1 calc R U . . . C16 C 1.1693(3) 0.4812(2) 0.12404(16) 0.0257(4) Uani 1 1 d . . . . . H161 H 1.1679 0.5605 0.0842 0.029(4) Uiso 1 1 calc R U . . . H162 H 1.2011 0.4095 0.0796 0.029(4) Uiso 1 1 calc R U . . . H163 H 1.2416 0.4569 0.1629 0.029(4) Uiso 1 1 calc R U . . . C17 C 0.8896(3) 0.5557(2) 0.13917(17) 0.0272(4) Uani 1 1 d . . . . . H171 H 0.7882 0.5757 0.1875 0.036(5) Uiso 1 1 calc R U . . . H172 H 0.9122 0.4875 0.0941 0.036(5) Uiso 1 1 calc R U . . . H173 H 0.8909 0.6350 0.1003 0.036(5) Uiso 1 1 calc R U . . . O21 O 0.89414(16) 0.80584(13) 0.38640(10) 0.0162(2) Uani 1 1 d . . . . . C21 C 0.8317(2) 0.74585(18) 0.46489(13) 0.0150(3) Uani 1 1 d . . . . . C22 C 0.8429(2) 0.61991(19) 0.45589(14) 0.0164(3) Uani 1 1 d . . . . . C23 C 0.7811(2) 0.5563(2) 0.54021(15) 0.0214(4) Uani 1 1 d . . . . . H23 H 0.7926 0.4695 0.5351 0.028(4) Uiso 1 1 calc R U . . . C24 C 0.7035(2) 0.6194(2) 0.63067(15) 0.0236(4) Uani 1 1 d . . . . . H24 H 0.6599 0.5768 0.6872 0.028(4) Uiso 1 1 calc R U . . . C25 C 0.6895(2) 0.7458(2) 0.63861(15) 0.0219(4) Uani 1 1 d . . . . . H25 H 0.6341 0.7897 0.7005 0.028(4) Uiso 1 1 calc R U . . . C26 C 0.7553(2) 0.8083(2) 0.55734(14) 0.0183(3) Uani 1 1 d . . . . . H26 H 0.7488 0.8930 0.5642 0.028(4) Uiso 1 1 calc R U . . . C31 C 0.8213(2) 1.09823(18) 0.36484(13) 0.0142(3) Uani 1 1 d . . . . . C32 C 0.6722(2) 1.10810(19) 0.41203(14) 0.0182(3) Uani 1 1 d . . . . . H32 H 0.6225 1.0823 0.3781 0.026(3) Uiso 1 1 calc R U . . . C33 C 0.5967(2) 1.1556(2) 0.50846(15) 0.0223(4) Uani 1 1 d . . . . . H33 H 0.4946 1.1641 0.5398 0.026(3) Uiso 1 1 calc R U . . . C34 C 0.6702(3) 1.1908(2) 0.55898(15) 0.0242(4) Uani 1 1 d . . . . . H34 H 0.6192 1.2214 0.6254 0.026(3) Uiso 1 1 calc R U . . . C35 C 0.8179(3) 1.1812(2) 0.51276(15) 0.0225(4) Uani 1 1 d . . . . . H35 H 0.8679 1.2053 0.5475 0.026(3) Uiso 1 1 calc R U . . . C36 C 0.8932(2) 1.13610(19) 0.41522(14) 0.0175(3) Uani 1 1 d . . . . . H36 H 0.9937 1.1312 0.3831 0.026(3) Uiso 1 1 calc R U . . . C41 C 0.7839(2) 1.14160(18) 0.16844(13) 0.0133(3) Uani 1 1 d . . . . . C42 C 0.7799(2) 1.09711(18) 0.08369(13) 0.0151(3) Uani 1 1 d . . . . . H42 H 0.8358 1.0071 0.0670 0.028(3) Uiso 1 1 calc R U . . . C43 C 0.6945(2) 1.1836(2) 0.02332(14) 0.0180(3) Uani 1 1 d . . . . . H43 H 0.6930 1.1528 -0.0347 0.028(3) Uiso 1 1 calc R U . . . C44 C 0.6115(2) 1.3149(2) 0.04810(15) 0.0208(4) Uani 1 1 d . . . . . H44 H 0.5532 1.3740 0.0069 0.028(3) Uiso 1 1 calc R U . . . C45 C 0.6135(2) 1.3602(2) 0.13289(16) 0.0234(4) Uani 1 1 d . . . . . H45 H 0.5557 1.4500 0.1500 0.028(3) Uiso 1 1 calc R U . . . C46 C 0.7003(2) 1.27378(19) 0.19302(14) 0.0188(4) Uani 1 1 d . . . . . H46 H 0.7025 1.3049 0.2506 0.028(3) Uiso 1 1 calc R U . . . C51 C 1.0837(2) 1.06074(17) 0.18639(13) 0.0129(3) Uani 1 1 d . . . . . C52 C 1.2010(2) 1.00264(19) 0.23184(15) 0.0173(3) Uani 1 1 d . . . . . H52 H 1.1877 0.9518 0.2914 0.028(3) Uiso 1 1 calc R U . . . C53 C 1.3368(2) 1.0190(2) 0.19025(17) 0.0222(4) Uani 1 1 d . . . . . H53 H 1.4150 0.9813 0.2223 0.028(3) Uiso 1 1 calc R U . . . C54 C 1.3582(2) 1.0901(2) 0.10224(17) 0.0236(4) Uani 1 1 d . . . . . H54 H 1.4513 1.1010 0.0738 0.028(3) Uiso 1 1 calc R U . . . C55 C 1.2445(2) 1.1455(2) 0.05552(15) 0.0207(4) Uani 1 1 d . . . . . H55 H 1.2608 1.1926 -0.0057 0.028(3) Uiso 1 1 calc R U . . . C56 C 1.1064(2) 1.13278(18) 0.09751(14) 0.0157(3) Uani 1 1 d . . . . . H56 H 1.0277 1.1729 0.0659 0.028(3) Uiso 1 1 calc R U . . . N61 N 0.6015(6) 0.4863(5) 0.3743(4) 0.0422(10) Uani 0.5 1 d . . P A 1 C61 C 0.5352(14) 0.4969(12) 0.4595(7) 0.0422(10) Uani 0.5 1 d . . P A 1 C62 C 0.4538(15) 0.5100(12) 0.5641(8) 0.0422(10) Uani 0.5 1 d . . P A 1 H621 H 0.5247 0.4950 0.6022 0.065(14) Uiso 0.5 1 calc R U P A 1 H622 H 0.4090 0.4453 0.5847 0.065(14) Uiso 0.5 1 calc R U P A 1 H623 H 0.3723 0.5984 0.5767 0.065(14) Uiso 0.5 1 calc R U P A 1 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 O1 0.0198(6) 0.0190(6) 0.0128(6) 0.0016(5) -0.0051(5) -0.0083(5) Re1 0.01375(4) 0.01279(4) 0.01112(4) 0.00160(2) -0.00442(2) -0.00624(3) Cl1 0.01581(18) 0.01703(19) 0.0210(2) 0.00129(15) -0.00778(16) -0.00577(15) Cl2 0.01478(18) 0.0242(2) 0.0218(2) 0.00188(17) -0.00593(16) -0.00941(16) P1 0.01212(18) 0.01201(18) 0.01014(18) 0.00075(14) -0.00379(15) -0.00529(15) O11 0.0302(8) 0.0156(6) 0.0195(7) -0.0007(5) 0.0007(6) -0.0122(6) C12 0.0170(8) 0.0146(8) 0.0171(8) 0.0009(6) -0.0041(6) -0.0081(6) N13 0.0180(7) 0.0150(7) 0.0142(7) -0.0001(5) -0.0050(6) -0.0075(6) C14 0.0268(9) 0.0165(8) 0.0164(8) -0.0017(7) -0.0057(7) -0.0110(7) C15 0.0323(10) 0.0166(8) 0.0189(9) -0.0005(7) -0.0058(8) -0.0123(8) C16 0.0289(10) 0.0229(10) 0.0217(10) -0.0056(8) 0.0006(8) -0.0116(8) C17 0.0387(12) 0.0261(10) 0.0252(10) -0.0008(8) -0.0166(9) -0.0155(9) O21 0.0203(6) 0.0162(6) 0.0141(6) 0.0020(5) -0.0050(5) -0.0101(5) C21 0.0153(8) 0.0174(8) 0.0121(7) 0.0025(6) -0.0045(6) -0.0070(6) C22 0.0165(8) 0.0169(8) 0.0143(8) 0.0014(6) -0.0031(6) -0.0070(7) C23 0.0237(9) 0.0194(9) 0.0191(9) 0.0031(7) -0.0021(7) -0.0111(8) C24 0.0256(10) 0.0254(10) 0.0160(9) 0.0039(7) -0.0015(7) -0.0118(8) C25 0.0237(9) 0.0253(10) 0.0138(8) 0.0007(7) -0.0039(7) -0.0090(8) C26 0.0217(9) 0.0188(8) 0.0142(8) 0.0000(6) -0.0058(7) -0.0079(7) C31 0.0162(8) 0.0140(7) 0.0106(7) 0.0012(6) -0.0044(6) -0.0046(6) C32 0.0160(8) 0.0196(9) 0.0159(8) -0.0003(7) -0.0031(6) -0.0058(7) C33 0.0181(8) 0.0246(10) 0.0151(8) 0.0006(7) -0.0003(7) -0.0043(7) C34 0.0278(10) 0.0235(10) 0.0123(8) -0.0015(7) -0.0043(7) -0.0033(8) C35 0.0290(10) 0.0231(9) 0.0148(8) -0.0027(7) -0.0087(7) -0.0076(8) C36 0.0190(8) 0.0186(8) 0.0143(8) -0.0007(6) -0.0053(7) -0.0068(7) C41 0.0119(7) 0.0153(8) 0.0123(7) 0.0019(6) -0.0036(6) -0.0060(6) C42 0.0166(8) 0.0163(8) 0.0140(8) 0.0017(6) -0.0063(6) -0.0073(6) C43 0.0191(8) 0.0226(9) 0.0144(8) 0.0036(7) -0.0071(7) -0.0102(7) C44 0.0188(8) 0.0214(9) 0.0187(9) 0.0061(7) -0.0078(7) -0.0054(7) C45 0.0241(9) 0.0170(9) 0.0207(9) 0.0014(7) -0.0065(8) -0.0016(7) C46 0.0218(9) 0.0167(8) 0.0156(8) -0.0003(7) -0.0064(7) -0.0052(7) C51 0.0134(7) 0.0133(7) 0.0127(7) -0.0018(6) -0.0036(6) -0.0057(6) C52 0.0164(8) 0.0169(8) 0.0191(8) -0.0003(7) -0.0075(7) -0.0056(7) C53 0.0149(8) 0.0230(9) 0.0297(10) -0.0054(8) -0.0083(7) -0.0057(7) C54 0.0161(8) 0.0255(10) 0.0298(11) -0.0080(8) 0.0002(8) -0.0114(8) C55 0.0230(9) 0.0216(9) 0.0178(8) -0.0014(7) 0.0000(7) -0.0133(8) C56 0.0168(8) 0.0165(8) 0.0136(8) -0.0015(6) -0.0028(6) -0.0076(7) N61 0.0352(17) 0.0347(14) 0.049(3) -0.013(2) -0.005(2) -0.0087(13) C61 0.0352(17) 0.0347(14) 0.049(3) -0.013(2) -0.005(2) -0.0087(13) C62 0.0352(17) 0.0347(14) 0.049(3) -0.013(2) -0.005(2) -0.0087(13) 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 177.71(6) . . yes Cl1 Re1 Cl2 171.181(16) . . yes N13 Re1 P1 168.60(4) . . yes O1 Re1 Cl1 94.60(5) . . yes O1 Re1 Cl2 92.14(5) . . yes O1 Re1 N13 97.08(6) . . yes O1 Re1 P1 93.67(5) . . yes O21 Re1 Cl1 87.57(4) . . yes O21 Re1 Cl2 85.62(4) . . yes O21 Re1 N13 82.30(6) . . yes O21 Re1 P1 86.81(4) . . yes N13 Re1 Cl1 87.10(4) . . ? N13 Re1 Cl2 86.43(4) . . ? Cl1 Re1 P1 95.835(15) . . ? Cl2 Re1 P1 89.387(16) . . ? C51 P1 C31 107.57(8) . . ? C51 P1 C41 103.73(8) . . ? C31 P1 C41 104.33(8) . . ? C51 P1 Re1 114.42(6) . . ? C31 P1 Re1 111.34(6) . . ? C41 P1 Re1 114.61(6) . . ? C12 O11 C15 107.04(15) . . ? N13 C12 O11 116.40(17) . . ? N13 C12 C22 128.09(17) . . ? O11 C12 C22 115.47(16) . . ? C12 N13 C14 108.53(16) . . yes C12 N13 Re1 127.05(13) . . yes C14 N13 Re1 124.05(12) . . yes N13 C14 C16 112.01(17) . . ? N13 C14 C17 108.95(16) . . ? C16 C14 C17 112.12(18) . . ? N13 C14 C15 101.05(15) . . ? C16 C14 C15 111.95(17) . . ? C17 C14 C15 110.22(18) . . ? O11 C15 C14 105.70(15) . . ? O11 C15 H151 110.6 . . ? C14 C15 H151 110.6 . . ? O11 C15 H152 110.6 . . ? C14 C15 H152 110.6 . . ? H151 C15 H152 108.7 . . ? 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 137.74(12) . . yes O21 C21 C26 119.92(17) . . ? O21 C21 C22 120.37(17) . . ? C26 C21 C22 119.71(17) . . ? C21 C22 C23 119.60(18) . . ? C21 C22 C12 120.54(17) . . ? C23 C22 C12 119.85(18) . . ? C24 C23 C22 120.33(19) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? C23 C24 C25 119.79(19) . . ? C23 C24 H24 120.1 . . ? C25 C24 H24 120.1 . . ? C26 C25 C24 120.82(19) . . ? C26 C25 H25 119.6 . . ? C24 C25 H25 119.6 . . ? C25 C26 C21 119.66(19) . . ? C25 C26 H26 120.2 . . ? C21 C26 H26 120.2 . . ? C36 C31 C32 119.53(17) . . ? C36 C31 P1 123.89(14) . . ? C32 C31 P1 116.56(14) . . ? C33 C32 C31 120.09(19) . . ? C33 C32 H32 120.0 . . ? C31 C32 H32 120.0 . . ? C34 C33 C32 120.05(19) . . ? C34 C33 H33 120.0 . . ? C32 C33 H33 120.0 . . ? C35 C34 C33 120.18(18) . . ? C35 C34 H34 119.9 . . ? C33 C34 H34 119.9 . . ? C34 C35 C36 120.04(19) . . ? C34 C35 H35 120.0 . . ? C36 C35 H35 120.0 . . ? C31 C36 C35 120.08(18) . . ? C31 C36 H36 120.0 . . ? C35 C36 H36 120.0 . . ? C42 C41 C46 119.46(17) . . ? C42 C41 P1 120.14(14) . . ? C46 C41 P1 120.15(14) . . ? C43 C42 C41 120.48(18) . . ? C43 C42 H42 119.8 . . ? C41 C42 H42 119.8 . . ? C44 C43 C42 119.84(18) . . ? C44 C43 H43 120.1 . . ? C42 C43 H43 120.1 . . ? C43 C44 C45 120.23(18) . . ? C43 C44 H44 119.9 . . ? C45 C44 H44 119.9 . . ? C44 C45 C46 120.01(19) . . ? C44 C45 H45 120.0 . . ? C46 C45 H45 120.0 . . ? C41 C46 C45 119.98(18) . . ? C41 C46 H46 120.0 . . ? C45 C46 H46 120.0 . . ? C56 C51 C52 119.20(17) . . ? C56 C51 P1 121.58(13) . . ? C52 C51 P1 119.09(14) . . ? C53 C52 C51 120.26(18) . . ? C53 C52 H52 119.9 . . ? C51 C52 H52 119.9 . . ? C54 C53 C52 120.08(19) . . ? C54 C53 H53 120.0 . . ? C52 C53 H53 120.0 . . ? C55 C54 C53 120.15(19) . . ? C55 C54 H54 119.9 . . ? C53 C54 H54 119.9 . . ? C54 C55 C56 120.47(19) . . ? C54 C55 H55 119.8 . . ? C56 C55 H55 119.8 . . ? C55 C56 C51 119.80(18) . . ? C55 C56 H56 120.1 . . ? C51 C56 H56 120.1 . . ? N61 C61 C62 180.0(10) . . ? C61 C62 H621 109.5 . . ? C61 C62 H622 109.5 . . ? H621 C62 H622 109.5 . . ? C61 C62 H623 109.5 . . ? H621 C62 H623 109.5 . . ? H622 C62 H623 109.5 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 Re1 1.6917(13) . yes Re1 O21 1.9481(13) . yes Re1 N13 2.1423(16) . yes Re1 Cl1 2.3981(5) . yes Re1 Cl2 2.4026(5) . yes Re1 P1 2.4723(5) . yes P1 C51 1.8147(18) . ? P1 C31 1.8182(18) . ? P1 C41 1.8204(18) . ? O11 C12 1.341(2) . ? O11 C15 1.448(2) . ? C12 N13 1.291(2) . ? C12 C22 1.454(3) . ? N13 C14 1.508(2) . ? C14 C16 1.520(3) . ? C14 C17 1.527(3) . ? C14 C15 1.537(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 1.331(2) . ? C21 C26 1.402(3) . ? C21 C22 1.403(3) . ? C22 C23 1.404(3) . ? C23 C24 1.382(3) . ? C23 H23 0.95 . ? C24 C25 1.394(3) . ? C24 H24 0.95 . ? C25 C26 1.386(3) . ? C25 H25 0.95 . ? C26 H26 0.95 . ? C31 C36 1.392(3) . ? C31 C32 1.399(3) . ? C32 C33 1.389(3) . ? C32 H32 0.95 . ? C33 C34 1.388(3) . ? C33 H33 0.95 . ? C34 C35 1.385(3) . ? C34 H34 0.95 . ? C35 C36 1.395(3) . ? C35 H35 0.95 . ? C36 H36 0.95 . ? C41 C42 1.393(2) . ? C41 C46 1.396(3) . ? C42 C43 1.391(2) . ? C42 H42 0.95 . ? C43 C44 1.388(3) . ? C43 H43 0.95 . ? C44 C45 1.389(3) . ? C44 H44 0.95 . ? C45 C46 1.396(3) . ? C45 H45 0.95 . ? C46 H46 0.95 . ? C51 C56 1.399(2) . ? C51 C52 1.400(2) . ? C52 C53 1.389(3) . ? C52 H52 0.95 . ? C53 C54 1.383(3) . ? C53 H53 0.95 . ? C54 C55 1.382(3) . ? C54 H54 0.95 . ? C55 C56 1.392(3) . ? C55 H55 0.95 . ? C56 H56 0.95 . ? N61 C61 1.169(11) . ? C61 C62 1.435(8) . ? C62 H621 0.98 . ? C62 H622 0.98 . ? C62 H623 0.98 . ? 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 2.6(2) . . . . ? C15 O11 C12 C22 -179.50(17) . . . . ? O11 C12 N13 C14 5.1(2) . . . . ? C22 C12 N13 C14 -172.55(18) . . . . ? O11 C12 N13 Re1 178.35(13) . . . . ? C22 C12 N13 Re1 0.7(3) . . . . ? C12 N13 C14 C16 -129.08(18) . . . . ? Re1 N13 C14 C16 57.4(2) . . . . ? C12 N13 C14 C17 106.29(19) . . . . ? Re1 N13 C14 C17 -67.2(2) . . . . ? C12 N13 C14 C15 -9.8(2) . . . . ? Re1 N13 C14 C15 176.71(12) . . . . ? C12 O11 C15 C14 -8.8(2) . . . . ? N13 C14 C15 O11 10.9(2) . . . . ? C16 C14 C15 O11 130.26(18) . . . . ? C17 C14 C15 O11 -104.23(19) . . . . ? Re1 O21 C21 C26 -156.12(15) . . . . ? Re1 O21 C21 C22 24.4(3) . . . . ? O21 C21 C22 C23 177.81(17) . . . . ? C26 C21 C22 C23 -1.7(3) . . . . ? O21 C21 C22 C12 -3.4(3) . . . . ? C26 C21 C22 C12 177.09(17) . . . . ? N13 C12 C22 C21 -7.1(3) . . . . ? O11 C12 C22 C21 175.23(17) . . . . ? N13 C12 C22 C23 171.6(2) . . . . ? O11 C12 C22 C23 -6.0(3) . . . . ? C21 C22 C23 C24 2.9(3) . . . . ? C12 C22 C23 C24 -175.89(19) . . . . ? C22 C23 C24 C25 -1.3(3) . . . . ? C23 C24 C25 C26 -1.4(3) . . . . ? C24 C25 C26 C21 2.6(3) . . . . ? O21 C21 C26 C25 179.46(18) . . . . ? C22 C21 C26 C25 -1.0(3) . . . . ? C51 P1 C31 C36 -13.06(18) . . . . ? C41 P1 C31 C36 -122.80(16) . . . . ? Re1 P1 C31 C36 113.06(15) . . . . ? C51 P1 C31 C32 168.37(14) . . . . ? C41 P1 C31 C32 58.62(16) . . . . ? Re1 P1 C31 C32 -65.52(15) . . . . ? C36 C31 C32 C33 0.1(3) . . . . ? P1 C31 C32 C33 178.75(15) . . . . ? C31 C32 C33 C34 -1.4(3) . . . . ? C32 C33 C34 C35 1.4(3) . . . . ? C33 C34 C35 C36 0.0(3) . . . . ? C32 C31 C36 C35 1.2(3) . . . . ? P1 C31 C36 C35 -177.33(15) . . . . ? C34 C35 C36 C31 -1.3(3) . . . . ? C51 P1 C41 C42 92.68(16) . . . . ? C31 P1 C41 C42 -154.79(15) . . . . ? Re1 P1 C41 C42 -32.77(16) . . . . ? C51 P1 C41 C46 -81.56(16) . . . . ? C31 P1 C41 C46 30.97(17) . . . . ? Re1 P1 C41 C46 152.99(14) . . . . ? C46 C41 C42 C43 0.6(3) . . . . ? P1 C41 C42 C43 -173.68(14) . . . . ? C41 C42 C43 C44 -0.6(3) . . . . ? C42 C43 C44 C45 0.0(3) . . . . ? C43 C44 C45 C46 0.6(3) . . . . ? C42 C41 C46 C45 0.0(3) . . . . ? P1 C41 C46 C45 174.32(16) . . . . ? C44 C45 C46 C41 -0.7(3) . . . . ? C31 P1 C51 C56 -121.74(15) . . . . ? C41 P1 C51 C56 -11.58(17) . . . . ? Re1 P1 C51 C56 114.00(14) . . . . ? C31 P1 C51 C52 62.41(16) . . . . ? C41 P1 C51 C52 172.57(15) . . . . ? Re1 P1 C51 C52 -61.86(16) . . . . ? C56 C51 C52 C53 1.5(3) . . . . ? P1 C51 C52 C53 177.42(15) . . . . ? C51 C52 C53 C54 -1.6(3) . . . . ? C52 C53 C54 C55 0.2(3) . . . . ? C53 C54 C55 C56 1.4(3) . . . . ? C54 C55 C56 C51 -1.6(3) . . . . ? C52 C51 C56 C55 0.1(3) . . . . ? P1 C51 C56 C55 -175.71(14) . . . . ?