#------------------------------------------------------------------------------ #$Date: 2020-09-06 12:33:13 +0300 (Sun, 06 Sep 2020) $ #$Revision: 256066 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/49/7704996.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_7704996 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 H27 Cl2 N O3 P Re' _chemical_formula_sum 'C29 H27 Cl2 N O3 P Re' _chemical_formula_weight 725.58 _chemical_name_common cis-dichloro-[2-(4,4-dimethyl-4,5-dihydro-1,3-oxazol-2-yl)pheno-lato-N,O]-oxo-(triphenylphosphine-P)-rhenium(V) _chemical_name_systematic cis-dichloro-[2-(4,4-dimethyl-4,5-dihydro-1,3-oxazol-2-yl)pheno-lato-N,O]-oxo-(triphenylphosphine-P)-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 ; 2018-07-10 deposited with the CCDC. 2020-07-29 downloaded from the CCDC. ; _cell_angle_alpha 79.637(3) _cell_angle_beta 79.537(2) _cell_angle_gamma 69.695(2) _cell_formula_units_Z 2 _cell_length_a 9.945(2) _cell_length_b 10.196(2) _cell_length_c 14.358(3) _cell_measurement_reflns_used 9524 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 30.42 _cell_measurement_theta_min 2.44 _cell_volume 1331.9(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 0.0549 _diffrn_reflns_av_unetI/netI 0.0548 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 25679 _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 2.20 _exptl_absorpt_coefficient_mu 4.856 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.545 _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 1.809 _exptl_crystal_description plate _exptl_crystal_F_000 712 _exptl_crystal_size_max 0.210 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.050 _refine_diff_density_max 1.845 _refine_diff_density_min -1.996 _refine_diff_density_rms 0.171 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_hydrogen_treatment refU _refine_ls_matrix_type full _refine_ls_number_parameters 343 _refine_ls_number_reflns 7766 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.045 _refine_ls_R_factor_all 0.0431 _refine_ls_R_factor_gt 0.0343 _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^)+(0.0278P)^2^+4.2745P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0809 _refine_ls_wR_factor_ref 0.0853 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6840 _reflns_number_total 7766 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0dt02352c2.cif _cod_data_source_block JS31A _cod_depositor_comments 'Adding full bibliography for 7704994--7704996.cif.' _cod_original_cell_volume 1331.8(5) _cod_database_code 7704996 _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 0.429 _shelx_estimated_absorpt_t_max 0.793 _shelxl_version_number 2014/6 _shelx_res_file ; TITL JS31A_0m_a.res in P-1 J.Schachner (Me2C3H2NO-C6H4O)ReOCl2(PPh3) green 100K CELL 0.71073 9.9447 10.1955 14.3580 79.637 79.537 69.695 ZERR 2 0.0021 0.0021 0.0029 0.003 0.002 0.002 LATT 1 SFAC C H CL N O P RE UNIT 58 54 4 2 6 2 2 TEMP -173.15 SIZE 0.05 0.10 0.21 ACTA 60.0004 MERG 2 OMIT -2 60.0004 L.S. 4 BOND $H CONF FMAP 2 PLAN 20 WGHT 0.027800 4.274500 FVAR 0.10278 0.02624 0.03198 0.03178 0.03389 0.06733 0.04403 FVAR 0.04461 RE1 7 0.737467 0.494514 0.762766 11.00000 0.01435 0.01533 = 0.01322 0.00030 -0.00237 -0.00196 O1 5 0.691512 0.500890 0.881061 11.00000 0.02215 0.02801 = 0.01525 0.00217 -0.00253 -0.00513 CL1 3 0.992096 0.406300 0.762643 11.00000 0.01486 0.02006 = 0.01913 0.00212 -0.00562 0.00092 CL2 3 0.753364 0.256819 0.752786 11.00000 0.02558 0.01398 = 0.03409 -0.00022 -0.00435 -0.00519 O11 5 0.314300 0.633984 0.668995 11.00000 0.01177 0.02480 = 0.02207 -0.00376 -0.00250 -0.00271 C12 1 0.457925 0.602728 0.663386 11.00000 0.01135 0.01356 = 0.02092 -0.00290 -0.00280 -0.00088 N13 4 0.511469 0.556866 0.744077 11.00000 0.01354 0.01976 = 0.01729 0.00009 -0.00106 -0.00441 C14 1 0.390682 0.546717 0.822849 11.00000 0.01485 0.02919 = 0.01941 -0.00221 0.00217 -0.00740 C15 1 0.259898 0.599550 0.766313 11.00000 0.01614 0.04678 = 0.02971 -0.00360 -0.00177 -0.01082 AFIX 23 H151 2 0.215113 0.525188 0.771648 11.00000 61.00000 H152 2 0.186243 0.683742 0.791216 11.00000 61.00000 AFIX 0 C16 1 0.371583 0.644547 0.896350 11.00000 0.02362 0.02606 = 0.02180 -0.00024 0.00247 -0.00951 AFIX 137 H161 2 0.459876 0.615642 0.926670 11.00000 71.00000 H162 2 0.289942 0.639411 0.945012 11.00000 71.00000 H163 2 0.352642 0.741545 0.864669 11.00000 71.00000 AFIX 0 C17 1 0.414887 0.395749 0.868474 11.00000 0.02901 0.02883 = 0.03006 -0.00475 0.01143 -0.01427 AFIX 137 H171 2 0.434386 0.334870 0.818652 11.00000 81.00000 H172 2 0.328300 0.389727 0.911785 11.00000 81.00000 H173 2 0.497639 0.364958 0.904510 11.00000 81.00000 AFIX 0 O21 5 0.762247 0.526443 0.623782 11.00000 0.01174 0.01558 = 0.01604 0.00138 -0.00449 -0.00322 C21 1 0.683615 0.590358 0.552106 11.00000 0.01394 0.00899 = 0.01716 -0.00027 -0.00686 -0.00108 C22 1 0.531445 0.628305 0.568871 11.00000 0.01328 0.01008 = 0.01593 -0.00161 -0.00309 -0.00024 C23 1 0.452047 0.688141 0.490685 11.00000 0.01515 0.01406 = 0.02817 -0.00533 -0.01129 0.00289 AFIX 43 H23 2 0.349833 0.711159 0.500560 11.00000 21.00000 AFIX 0 C24 1 0.520459 0.713396 0.400875 11.00000 0.02498 0.01103 = 0.01887 0.00101 -0.01059 0.00131 AFIX 43 H24 2 0.466043 0.754407 0.348875 11.00000 21.00000 AFIX 0 C25 1 0.669561 0.678690 0.386448 11.00000 0.02713 0.01460 = 0.01747 -0.00003 -0.00614 -0.00399 AFIX 43 H25 2 0.716618 0.698142 0.324352 11.00000 21.00000 AFIX 0 C26 1 0.751426 0.616201 0.460726 11.00000 0.01658 0.01186 = 0.01869 -0.00321 -0.00255 -0.00277 AFIX 43 H26 2 0.853793 0.591090 0.449122 11.00000 21.00000 AFIX 0 P1 6 0.740269 0.741192 0.748687 11.00000 0.01262 0.01244 = 0.01151 -0.00069 -0.00326 -0.00037 C31 1 0.817107 0.803537 0.630990 11.00000 0.01415 0.01263 = 0.01130 -0.00152 -0.00367 -0.00096 C32 1 0.952761 0.715933 0.592771 11.00000 0.01438 0.01410 = 0.01469 0.00025 -0.00293 -0.00206 AFIX 43 H32 2 1.000236 0.629704 0.628962 11.00000 31.00000 AFIX 0 C33 1 1.016790 0.753824 0.504048 11.00000 0.01321 0.01747 = 0.02192 -0.00461 0.00041 -0.00258 AFIX 43 H33 2 1.107901 0.693710 0.478885 11.00000 31.00000 AFIX 0 C34 1 0.947995 0.881138 0.450426 11.00000 0.02038 0.02102 = 0.01462 -0.00038 -0.00075 -0.00784 AFIX 43 H34 2 0.991286 0.906966 0.388416 11.00000 31.00000 AFIX 0 C35 1 0.816488 0.969031 0.488445 11.00000 0.02412 0.01415 = 0.01673 0.00280 -0.00575 -0.00185 AFIX 43 H35 2 0.770545 1.056401 0.452809 11.00000 31.00000 AFIX 0 C36 1 0.751599 0.930996 0.577483 11.00000 0.02013 0.01088 = 0.01681 -0.00114 -0.00165 0.00102 AFIX 43 H36 2 0.661239 0.992345 0.602642 11.00000 31.00000 AFIX 0 C41 1 0.847786 0.769439 0.829481 11.00000 0.01264 0.01984 = 0.01093 -0.00257 -0.00255 -0.00006 C42 1 0.879957 0.678417 0.913598 11.00000 0.01682 0.02099 = 0.01511 -0.00095 -0.00496 -0.00215 AFIX 43 H42 2 0.853299 0.595386 0.927453 11.00000 41.00000 AFIX 0 C43 1 0.951171 0.710235 0.976775 11.00000 0.01944 0.02977 = 0.01249 -0.00695 -0.00327 0.00424 AFIX 43 H43 2 0.973266 0.648560 1.033996 11.00000 41.00000 AFIX 0 C44 1 0.989907 0.830115 0.957206 11.00000 0.01956 0.03479 = 0.02345 -0.01848 -0.00585 0.00060 AFIX 43 H44 2 1.039224 0.850382 1.000760 11.00000 41.00000 AFIX 0 C45 1 0.957719 0.921473 0.874679 11.00000 0.02826 0.02815 = 0.03309 -0.01240 -0.00228 -0.01058 AFIX 43 H45 2 0.983766 1.004834 0.861866 11.00000 41.00000 AFIX 0 C46 1 0.887193 0.890961 0.810594 11.00000 0.02450 0.01791 = 0.02501 -0.00155 -0.00474 -0.00475 AFIX 43 H46 2 0.865666 0.953264 0.753539 11.00000 41.00000 AFIX 0 C51 1 0.563113 0.871774 0.775759 11.00000 0.01445 0.01505 = 0.01581 -0.00284 -0.00175 -0.00048 C52 1 0.458732 0.908489 0.713916 11.00000 0.01721 0.01436 = 0.01357 -0.00138 -0.00181 -0.00312 AFIX 43 H52 2 0.481834 0.869665 0.655371 11.00000 51.00000 AFIX 0 C53 1 0.321317 1.001487 0.737595 11.00000 0.01501 0.01504 = 0.02382 0.00085 -0.00655 0.00000 AFIX 43 H53 2 0.251327 1.027330 0.694736 11.00000 51.00000 AFIX 0 C54 1 0.286004 1.056859 0.823989 11.00000 0.01411 0.01973 = 0.02318 -0.00384 0.00097 0.00262 AFIX 43 H54 2 0.191665 1.119667 0.840344 11.00000 51.00000 AFIX 0 C55 1 0.386849 1.020964 0.885219 11.00000 0.02544 0.03864 = 0.02189 -0.01867 -0.00287 0.00201 AFIX 43 H55 2 0.362674 1.059041 0.944091 11.00000 51.00000 AFIX 0 C56 1 0.525065 0.928671 0.861589 11.00000 0.02134 0.03366 = 0.01874 -0.00997 -0.00630 0.00141 AFIX 43 H56 2 0.594449 0.904184 0.904747 11.00000 51.00000 AFIX 0 HKLF 4 REM JS31A_0m_a.res in P-1 J.Schachner (Me2C3H2NO-C6H4O)ReOCl2(PPh3) green 100K REM R1 = 0.0343 for 6840 Fo > 4sig(Fo) and 0.0431 for all 7766 data REM 343 parameters refined using 0 restraints END WGHT 0.0278 4.2747 REM Highest difference peak 1.845, deepest hole -1.996, 1-sigma level 0.171 Q1 1 0.7587 0.4231 0.7706 11.00000 0.05 1.85 Q2 1 0.7153 0.4812 0.8242 11.00000 0.05 1.51 Q3 1 0.7401 0.4033 0.7179 11.00000 0.05 1.44 Q4 1 0.7991 0.4951 0.7724 11.00000 0.05 1.22 Q5 1 0.7727 0.4984 0.7078 11.00000 0.05 1.11 Q6 1 0.6728 0.5985 0.7511 11.00000 0.05 1.11 Q7 1 0.7320 0.3550 0.9011 11.00000 0.05 1.07 Q8 1 0.7542 0.6350 0.7551 11.00000 0.05 1.06 Q9 1 0.7904 0.1650 0.7954 11.00000 0.05 1.04 Q10 1 0.7154 0.6566 0.7599 11.00000 0.05 1.03 Q11 1 0.7522 0.2428 0.6937 11.00000 0.05 0.95 Q12 1 0.8268 0.4418 0.7003 11.00000 0.05 0.89 Q13 1 0.8996 0.4613 0.7458 11.00000 0.05 0.88 Q14 1 0.6184 0.5188 0.7675 11.00000 0.05 0.85 Q15 1 0.7637 0.1982 0.7324 11.00000 0.05 0.83 Q16 1 0.8333 0.2376 0.7572 11.00000 0.05 0.79 Q17 1 0.7237 0.5123 0.6940 11.00000 0.05 0.79 Q18 1 0.8865 0.7580 0.6157 11.00000 0.05 0.78 Q19 1 0.8219 0.3457 0.7729 11.00000 0.05 0.75 Q20 1 0.7858 0.9277 0.5277 11.00000 0.05 0.75 ; _shelx_res_checksum 72633 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 0.73747(2) 0.49451(2) 0.76277(2) 0.01527(5) Uani 1 1 d . . . . . O1 O 0.6915(3) 0.5009(3) 0.8811(2) 0.0232(6) Uani 1 1 d . . . . . Cl1 Cl 0.99210(10) 0.40630(11) 0.76264(7) 0.01993(19) Uani 1 1 d . . . . . Cl2 Cl 0.75336(12) 0.25682(11) 0.75279(8) 0.0252(2) Uani 1 1 d . . . . . O11 O 0.3143(3) 0.6340(3) 0.6690(2) 0.0203(6) Uani 1 1 d . . . . . C12 C 0.4579(4) 0.6027(4) 0.6634(3) 0.0159(7) Uani 1 1 d . . . . . N13 N 0.5115(4) 0.5569(4) 0.7441(2) 0.0176(7) Uani 1 1 d . . . . . C14 C 0.3907(4) 0.5467(5) 0.8228(3) 0.0218(8) Uani 1 1 d . . . . . C15 C 0.2599(5) 0.5996(6) 0.7663(4) 0.0310(11) Uani 1 1 d . . . . . H151 H 0.2151 0.5252 0.7716 0.067(16) Uiso 1 1 calc R U . . . H152 H 0.1862 0.6837 0.7912 0.067(16) Uiso 1 1 calc R U . . . C16 C 0.3716(5) 0.6445(5) 0.8964(3) 0.0245(9) Uani 1 1 d . . . . . H161 H 0.4599 0.6156 0.9267 0.044(10) Uiso 1 1 calc R U . . . H162 H 0.2899 0.6394 0.9450 0.044(10) Uiso 1 1 calc R U . . . H163 H 0.3526 0.7415 0.8647 0.044(10) Uiso 1 1 calc R U . . . C17 C 0.4149(5) 0.3957(5) 0.8685(4) 0.0299(10) Uani 1 1 d . . . . . H171 H 0.4344 0.3349 0.8187 0.045(10) Uiso 1 1 calc R U . . . H172 H 0.3283 0.3897 0.9118 0.045(10) Uiso 1 1 calc R U . . . H173 H 0.4976 0.3650 0.9045 0.045(10) Uiso 1 1 calc R U . . . O21 O 0.7622(3) 0.5264(3) 0.6238(2) 0.0149(5) Uani 1 1 d . . . . . C21 C 0.6836(4) 0.5904(4) 0.5521(3) 0.0136(7) Uani 1 1 d . . . . . C22 C 0.5314(4) 0.6283(4) 0.5689(3) 0.0139(7) Uani 1 1 d . . . . . C23 C 0.4520(4) 0.6881(4) 0.4907(3) 0.0197(8) Uani 1 1 d . . . . . H23 H 0.3498 0.7112 0.5006 0.026(7) Uiso 1 1 calc R U . . . C24 C 0.5205(5) 0.7134(4) 0.4009(3) 0.0196(8) Uani 1 1 d . . . . . H24 H 0.4660 0.7544 0.3489 0.026(7) Uiso 1 1 calc R U . . . C25 C 0.6696(5) 0.6787(4) 0.3864(3) 0.0203(8) Uani 1 1 d . . . . . H25 H 0.7166 0.6981 0.3244 0.026(7) Uiso 1 1 calc R U . . . C26 C 0.7514(4) 0.6162(4) 0.4607(3) 0.0160(7) Uani 1 1 d . . . . . H26 H 0.8538 0.5911 0.4491 0.026(7) Uiso 1 1 calc R U . . . P1 P 0.74027(10) 0.74119(10) 0.74869(7) 0.01306(18) Uani 1 1 d . . . . . C31 C 0.8171(4) 0.8035(4) 0.6310(3) 0.0133(7) Uani 1 1 d . . . . . C32 C 0.9528(4) 0.7159(4) 0.5928(3) 0.0152(7) Uani 1 1 d . . . . . H32 H 1.0002 0.6297 0.6290 0.032(7) Uiso 1 1 calc R U . . . C33 C 1.0168(4) 0.7538(4) 0.5040(3) 0.0183(8) Uani 1 1 d . . . . . H33 H 1.1079 0.6937 0.4789 0.032(7) Uiso 1 1 calc R U . . . C34 C 0.9480(4) 0.8811(4) 0.4504(3) 0.0188(8) Uani 1 1 d . . . . . H34 H 0.9913 0.9070 0.3884 0.032(7) Uiso 1 1 calc R U . . . C35 C 0.8165(5) 0.9690(4) 0.4884(3) 0.0197(8) Uani 1 1 d . . . . . H35 H 0.7705 1.0564 0.4528 0.032(7) Uiso 1 1 calc R U . . . C36 C 0.7516(4) 0.9310(4) 0.5775(3) 0.0177(8) Uani 1 1 d . . . . . H36 H 0.6612 0.9923 0.6026 0.032(7) Uiso 1 1 calc R U . . . C41 C 0.8478(4) 0.7694(4) 0.8295(3) 0.0157(7) Uani 1 1 d . . . . . C42 C 0.8800(4) 0.6784(5) 0.9136(3) 0.0185(8) Uani 1 1 d . . . . . H42 H 0.8533 0.5954 0.9275 0.032(7) Uiso 1 1 calc R U . . . C43 C 0.9512(5) 0.7102(5) 0.9768(3) 0.0231(9) Uani 1 1 d . . . . . H43 H 0.9733 0.6486 1.0340 0.032(7) Uiso 1 1 calc R U . . . C44 C 0.9899(5) 0.8301(5) 0.9572(3) 0.0261(10) Uani 1 1 d . . . . . H44 H 1.0392 0.8504 1.0008 0.032(7) Uiso 1 1 calc R U . . . C45 C 0.9577(5) 0.9215(5) 0.8747(4) 0.0286(10) Uani 1 1 d . . . . . H45 H 0.9838 1.0048 0.8619 0.032(7) Uiso 1 1 calc R U . . . C46 C 0.8872(5) 0.8910(5) 0.8106(3) 0.0230(9) Uani 1 1 d . . . . . H46 H 0.8657 0.9533 0.7535 0.032(7) Uiso 1 1 calc R U . . . C51 C 0.5631(4) 0.8718(4) 0.7758(3) 0.0162(7) Uani 1 1 d . . . . . C52 C 0.4587(4) 0.9085(4) 0.7139(3) 0.0157(7) Uani 1 1 d . . . . . H52 H 0.4818 0.8697 0.6554 0.034(7) Uiso 1 1 calc R U . . . C53 C 0.3213(4) 1.0015(4) 0.7376(3) 0.0192(8) Uani 1 1 d . . . . . H53 H 0.2513 1.0273 0.6947 0.034(7) Uiso 1 1 calc R U . . . C54 C 0.2860(4) 1.0569(5) 0.8240(3) 0.0215(8) Uani 1 1 d . . . . . H54 H 0.1917 1.1197 0.8403 0.034(7) Uiso 1 1 calc R U . . . C55 C 0.3868(5) 1.0210(6) 0.8852(3) 0.0300(11) Uani 1 1 d . . . . . H55 H 0.3627 1.0590 0.9441 0.034(7) Uiso 1 1 calc R U . . . C56 C 0.5251(5) 0.9287(5) 0.8616(3) 0.0260(9) Uani 1 1 d . . . . . H56 H 0.5944 0.9042 0.9047 0.034(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 0.01435(8) 0.01533(8) 0.01322(8) 0.00030(5) -0.00237(5) -0.00196(6) O1 0.0222(15) 0.0280(17) 0.0152(14) 0.0022(12) -0.0025(12) -0.0051(13) Cl1 0.0149(4) 0.0201(5) 0.0191(4) 0.0021(4) -0.0056(4) 0.0009(4) Cl2 0.0256(5) 0.0140(4) 0.0341(6) -0.0002(4) -0.0043(4) -0.0052(4) O11 0.0118(13) 0.0248(16) 0.0221(15) -0.0038(12) -0.0025(11) -0.0027(11) C12 0.0114(16) 0.0136(17) 0.0209(19) -0.0029(15) -0.0028(14) -0.0009(14) N13 0.0135(15) 0.0198(17) 0.0173(16) 0.0001(13) -0.0011(13) -0.0044(13) C14 0.0149(18) 0.029(2) 0.019(2) -0.0022(17) 0.0022(15) -0.0074(17) C15 0.016(2) 0.047(3) 0.030(2) -0.004(2) -0.0018(18) -0.011(2) C16 0.024(2) 0.026(2) 0.022(2) -0.0002(17) 0.0025(17) -0.0095(18) C17 0.029(2) 0.029(2) 0.030(2) -0.005(2) 0.011(2) -0.014(2) O21 0.0117(12) 0.0156(13) 0.0160(13) 0.0014(10) -0.0045(10) -0.0032(10) C21 0.0139(17) 0.0090(16) 0.0172(18) -0.0003(13) -0.0069(14) -0.0011(13) C22 0.0133(17) 0.0101(16) 0.0159(17) -0.0016(13) -0.0031(14) -0.0002(13) C23 0.0152(18) 0.0141(18) 0.028(2) -0.0053(16) -0.0113(16) 0.0029(15) C24 0.025(2) 0.0110(18) 0.0189(19) 0.0010(15) -0.0106(16) 0.0013(15) C25 0.027(2) 0.0146(19) 0.0175(19) 0.0000(15) -0.0061(16) -0.0040(16) C26 0.0166(18) 0.0119(17) 0.0187(19) -0.0032(14) -0.0025(15) -0.0028(14) P1 0.0126(4) 0.0124(4) 0.0115(4) -0.0007(3) -0.0033(3) -0.0004(3) C31 0.0141(17) 0.0126(17) 0.0113(16) -0.0015(13) -0.0037(13) -0.0010(14) C32 0.0144(17) 0.0141(18) 0.0147(17) 0.0002(14) -0.0029(14) -0.0021(14) C33 0.0132(17) 0.0175(19) 0.022(2) -0.0046(15) 0.0004(15) -0.0026(15) C34 0.0204(19) 0.021(2) 0.0146(18) -0.0004(15) -0.0008(15) -0.0078(16) C35 0.024(2) 0.0141(18) 0.0167(19) 0.0028(15) -0.0058(16) -0.0019(16) C36 0.0201(19) 0.0109(17) 0.0168(18) -0.0011(14) -0.0016(15) 0.0010(15) C41 0.0126(17) 0.0198(19) 0.0109(17) -0.0026(14) -0.0026(13) -0.0001(14) C42 0.0168(18) 0.021(2) 0.0151(18) -0.0010(15) -0.0050(15) -0.0022(15) C43 0.019(2) 0.030(2) 0.0125(18) -0.0070(16) -0.0033(15) 0.0042(17) C44 0.020(2) 0.035(3) 0.023(2) -0.0185(19) -0.0059(17) 0.0006(18) C45 0.028(2) 0.028(2) 0.033(3) -0.012(2) -0.002(2) -0.011(2) C46 0.024(2) 0.018(2) 0.025(2) -0.0016(17) -0.0047(17) -0.0048(17) C51 0.0145(17) 0.0151(18) 0.0158(18) -0.0028(14) -0.0018(14) -0.0005(14) C52 0.0172(18) 0.0144(18) 0.0136(17) -0.0014(14) -0.0018(14) -0.0031(14) C53 0.0150(18) 0.0150(19) 0.024(2) 0.0009(15) -0.0065(15) 0.0000(15) C54 0.0141(18) 0.020(2) 0.023(2) -0.0038(16) 0.0010(16) 0.0026(15) C55 0.025(2) 0.039(3) 0.022(2) -0.019(2) -0.0029(18) 0.002(2) C56 0.021(2) 0.034(3) 0.019(2) -0.0100(18) -0.0063(17) 0.0014(18) 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 168.16(13) . . yes O1 Re1 N13 90.29(14) . . ? O21 Re1 N13 82.54(12) . . ? O1 Re1 Cl1 97.37(11) . . ? O21 Re1 Cl1 90.63(8) . . ? Cl1 Re1 N13 171.03(10) . . yes O1 Re1 Cl2 100.93(11) . . ? O21 Re1 Cl2 88.23(9) . . ? N13 Re1 Cl2 87.59(10) . . ? Cl1 Re1 Cl2 86.39(4) . . yes O1 Re1 P1 87.26(11) . . ? O21 Re1 P1 83.94(8) . . ? N13 Re1 P1 94.54(10) . . ? Cl1 Re1 P1 90.49(3) . . ? Cl2 Re1 P1 171.54(4) . . yes C12 O11 C15 108.0(3) . . ? N13 C12 O11 115.7(4) . . ? N13 C12 C22 128.9(3) . . ? O11 C12 C22 115.4(3) . . ? C12 N13 C14 108.8(3) . . yes C12 N13 Re1 126.1(3) . . yes C14 N13 Re1 125.0(3) . . yes N13 C14 C17 111.1(4) . . ? N13 C14 C16 111.0(3) . . ? C17 C14 C16 111.8(4) . . ? N13 C14 C15 101.0(3) . . ? C17 C14 C15 111.0(4) . . ? C16 C14 C15 110.5(4) . . ? O11 C15 C14 106.5(3) . . ? O11 C15 H151 110.4 . . ? C14 C15 H151 110.4 . . ? O11 C15 H152 110.4 . . ? C14 C15 H152 110.4 . . ? H151 C15 H152 108.6 . . ? 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 139.5(3) . . yes O21 C21 C26 120.2(3) . . ? O21 C21 C22 120.0(3) . . ? C26 C21 C22 119.8(3) . . ? C21 C22 C23 118.7(4) . . ? C21 C22 C12 121.0(3) . . ? C23 C22 C12 120.4(4) . . ? C24 C23 C22 120.9(4) . . ? C24 C23 H23 119.6 . . ? C22 C23 H23 119.6 . . ? C23 C24 C25 119.5(4) . . ? C23 C24 H24 120.3 . . ? C25 C24 H24 120.3 . . ? C26 C25 C24 121.3(4) . . ? C26 C25 H25 119.3 . . ? C24 C25 H25 119.3 . . ? C25 C26 C21 119.8(4) . . ? C25 C26 H26 120.1 . . ? C21 C26 H26 120.1 . . ? C31 P1 C51 106.71(18) . . ? C31 P1 C41 103.33(18) . . ? C51 P1 C41 102.59(18) . . ? C31 P1 Re1 113.44(13) . . ? C51 P1 Re1 114.49(13) . . ? C41 P1 Re1 115.05(13) . . ? C36 C31 C32 118.5(4) . . ? C36 C31 P1 124.5(3) . . ? C32 C31 P1 117.0(3) . . ? C33 C32 C31 120.7(4) . . ? C33 C32 H32 119.6 . . ? C31 C32 H32 119.6 . . ? C32 C33 C34 120.0(4) . . ? C32 C33 H33 120.0 . . ? C34 C33 H33 120.0 . . ? C35 C34 C33 119.5(4) . . ? C35 C34 H34 120.3 . . ? C33 C34 H34 120.3 . . ? C36 C35 C34 120.6(4) . . ? C36 C35 H35 119.7 . . ? C34 C35 H35 119.7 . . ? C35 C36 C31 120.7(4) . . ? C35 C36 H36 119.7 . . ? C31 C36 H36 119.7 . . ? C46 C41 C42 119.4(4) . . ? C46 C41 P1 118.9(3) . . ? C42 C41 P1 121.4(3) . . ? C43 C42 C41 119.5(4) . . ? C43 C42 H42 120.2 . . ? C41 C42 H42 120.2 . . ? C44 C43 C42 120.5(4) . . ? C44 C43 H43 119.7 . . ? C42 C43 H43 119.7 . . ? C43 C44 C45 120.5(4) . . ? C43 C44 H44 119.7 . . ? C45 C44 H44 119.7 . . ? C44 C45 C46 119.7(4) . . ? C44 C45 H45 120.1 . . ? C46 C45 H45 120.1 . . ? C45 C46 C41 120.3(4) . . ? C45 C46 H46 119.8 . . ? C41 C46 H46 119.8 . . ? C56 C51 C52 118.4(4) . . ? C56 C51 P1 120.9(3) . . ? C52 C51 P1 120.6(3) . . ? C53 C52 C51 120.3(4) . . ? C53 C52 H52 119.8 . . ? C51 C52 H52 119.8 . . ? C52 C53 C54 120.1(4) . . ? C52 C53 H53 119.9 . . ? C54 C53 H53 119.9 . . ? C55 C54 C53 120.0(4) . . ? C55 C54 H54 120.0 . . ? C53 C54 H54 120.0 . . ? C54 C55 C56 120.1(4) . . ? C54 C55 H55 119.9 . . ? C56 C55 H55 119.9 . . ? C51 C56 C55 121.0(4) . . ? C51 C56 H56 119.5 . . ? C55 C56 H56 119.5 . . ? 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 Re1 O1 1.684(3) . yes Re1 O21 1.947(3) . yes Re1 N13 2.166(3) . yes Re1 Cl1 2.3747(11) . yes Re1 Cl2 2.4019(12) . yes Re1 P1 2.4961(11) . yes O11 C12 1.342(5) . ? O11 C15 1.431(6) . ? C12 N13 1.304(5) . ? C12 C22 1.445(6) . ? N13 C14 1.511(5) . ? C14 C17 1.514(6) . ? C14 C16 1.523(6) . ? C14 C15 1.543(6) . ? 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 1.339(4) . yes C21 C26 1.387(6) . ? C21 C22 1.412(5) . ? C22 C23 1.413(5) . ? C23 C24 1.369(6) . ? C23 H23 0.95 . ? C24 C25 1.385(6) . ? C24 H24 0.95 . ? C25 C26 1.385(5) . ? C25 H25 0.95 . ? C26 H26 0.95 . ? P1 C31 1.824(4) . yes P1 C51 1.827(4) . yes P1 C41 1.832(4) . yes C31 C36 1.392(5) . ? C31 C32 1.411(5) . ? C32 C33 1.370(6) . ? C32 H32 0.95 . ? C33 C34 1.400(6) . ? C33 H33 0.95 . ? C34 C35 1.384(6) . ? C34 H34 0.95 . ? C35 C36 1.377(6) . ? C35 H35 0.95 . ? C36 H36 0.95 . ? C41 C46 1.393(6) . ? C41 C42 1.398(5) . ? C42 C43 1.389(6) . ? C42 H42 0.95 . ? C43 C44 1.373(7) . ? C43 H43 0.95 . ? C44 C45 1.381(7) . ? C44 H44 0.95 . ? C45 C46 1.387(6) . ? C45 H45 0.95 . ? C46 H46 0.95 . ? C51 C56 1.391(6) . ? C51 C52 1.397(5) . ? C52 C53 1.389(6) . ? C52 H52 0.95 . ? C53 C54 1.392(6) . ? C53 H53 0.95 . ? C54 C55 1.365(6) . ? C54 H54 0.95 . ? C55 C56 1.392(6) . ? 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 -2.9(5) . . . . ? C15 O11 C12 C22 178.7(4) . . . . ? O11 C12 N13 C14 2.3(5) . . . . ? C22 C12 N13 C14 -179.6(4) . . . . ? O11 C12 N13 Re1 179.4(3) . . . . ? C22 C12 N13 Re1 -2.5(6) . . . . ? C12 N13 C14 C17 117.0(4) . . . . ? Re1 N13 C14 C17 -60.1(5) . . . . ? C12 N13 C14 C16 -117.9(4) . . . . ? Re1 N13 C14 C16 65.0(4) . . . . ? C12 N13 C14 C15 -0.8(5) . . . . ? Re1 N13 C14 C15 -177.9(3) . . . . ? C12 O11 C15 C14 2.2(5) . . . . ? N13 C14 C15 O11 -0.8(5) . . . . ? C17 C14 C15 O11 -118.7(4) . . . . ? C16 C14 C15 O11 116.7(4) . . . . ? Re1 O21 C21 C26 164.7(3) . . . . ? Re1 O21 C21 C22 -17.0(6) . . . . ? O21 C21 C22 C23 -176.4(3) . . . . ? C26 C21 C22 C23 2.0(6) . . . . ? O21 C21 C22 C12 1.7(6) . . . . ? C26 C21 C22 C12 -179.9(3) . . . . ? N13 C12 C22 C21 6.5(6) . . . . ? O11 C12 C22 C21 -175.4(3) . . . . ? N13 C12 C22 C23 -175.4(4) . . . . ? O11 C12 C22 C23 2.7(5) . . . . ? C21 C22 C23 C24 -2.2(6) . . . . ? C12 C22 C23 C24 179.7(4) . . . . ? C22 C23 C24 C25 0.5(6) . . . . ? C23 C24 C25 C26 1.3(6) . . . . ? C24 C25 C26 C21 -1.5(6) . . . . ? O21 C21 C26 C25 178.2(4) . . . . ? C22 C21 C26 C25 -0.2(6) . . . . ? C51 P1 C31 C36 3.1(4) . . . . ? C41 P1 C31 C36 -104.7(4) . . . . ? Re1 P1 C31 C36 130.1(3) . . . . ? C51 P1 C31 C32 -177.4(3) . . . . ? C41 P1 C31 C32 74.8(3) . . . . ? Re1 P1 C31 C32 -50.4(3) . . . . ? C36 C31 C32 C33 -1.6(6) . . . . ? P1 C31 C32 C33 178.8(3) . . . . ? C31 C32 C33 C34 0.4(6) . . . . ? C32 C33 C34 C35 1.1(6) . . . . ? C33 C34 C35 C36 -1.3(6) . . . . ? C34 C35 C36 C31 0.1(6) . . . . ? C32 C31 C36 C35 1.4(6) . . . . ? P1 C31 C36 C35 -179.1(3) . . . . ? C31 P1 C41 C46 39.1(4) . . . . ? C51 P1 C41 C46 -71.7(4) . . . . ? Re1 P1 C41 C46 163.3(3) . . . . ? C31 P1 C41 C42 -146.6(3) . . . . ? C51 P1 C41 C42 102.6(4) . . . . ? Re1 P1 C41 C42 -22.4(4) . . . . ? C46 C41 C42 C43 -0.3(6) . . . . ? P1 C41 C42 C43 -174.6(3) . . . . ? C41 C42 C43 C44 0.0(6) . . . . ? C42 C43 C44 C45 0.5(7) . . . . ? C43 C44 C45 C46 -0.7(7) . . . . ? C44 C45 C46 C41 0.5(7) . . . . ? C42 C41 C46 C45 0.0(7) . . . . ? P1 C41 C46 C45 174.4(4) . . . . ? C31 P1 C51 C56 -128.8(4) . . . . ? C41 P1 C51 C56 -20.5(4) . . . . ? Re1 P1 C51 C56 104.8(4) . . . . ? C31 P1 C51 C52 56.2(4) . . . . ? C41 P1 C51 C52 164.5(3) . . . . ? Re1 P1 C51 C52 -70.2(3) . . . . ? C56 C51 C52 C53 1.0(6) . . . . ? P1 C51 C52 C53 176.1(3) . . . . ? C51 C52 C53 C54 -1.1(6) . . . . ? C52 C53 C54 C55 0.7(7) . . . . ? C53 C54 C55 C56 -0.2(8) . . . . ? C52 C51 C56 C55 -0.6(7) . . . . ? P1 C51 C56 C55 -175.6(4) . . . . ? C54 C55 C56 C51 0.1(8) . . . . ?