Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Klahn A. Hugo' _publ_contact_author_email HKLAHN@UCV.CL _publ_section_title ; Heterobimetallic Re=Pd Complexes Bridged by eta1 :eta5-Ph2PC5H4 Ligand. Synthesis, Electronic and Crystal Structure of (CO)2P(Me3) (eta5-C5H4PPh2) Re-PdCl2 and (CO)2P(OMe)3(eta5-C5H4PPh2) Re-PdCl2. ; loop_ _publ_author_name 'Klahn A. Hugo' 'Ramiro Arratia-Perez' 'Mauricio Fuentealba' 'Maria T. Garland' 'Fernando Godoy' ; R.Ramirez-Tagle' ; 'Diego Sierra' # Attachment 'COMPLEX3_sol5.cif' data_sol5 _database_code_depnum_ccdc_archive 'CCDC 756945' #TrackingRef 'COMPLEX3_sol5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H23 Cl2 O2 P2 Pd Re, 2(C2 H3 N)' _chemical_formula_sum 'C26 H29 Cl2 N2 O2 P2 Pd Re' _chemical_formula_weight 826.95 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' Pd Pd -0.9988 1.0072 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 16.853(2) _cell_length_b 17.329(2) _cell_length_c 10.1789(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2972.8(7) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 941 _cell_measurement_theta_min 1.77 _cell_measurement_theta_max 27.76 _exptl_crystal_description Polyhedron _exptl_crystal_colour Orange _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.848 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1600 _exptl_absorpt_coefficient_mu 4.986 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.108 _exptl_absorpt_correction_T_max 0.388 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14883 _diffrn_reflns_av_R_equivalents 0.0656 _diffrn_reflns_av_sigmaI/netI 0.1090 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 28.02 _reflns_number_total 6413 _reflns_number_gt 4766 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0360P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.019(10) _refine_ls_number_reflns 6413 _refine_ls_number_parameters 330 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0969 _refine_ls_R_factor_gt 0.0692 _refine_ls_wR_factor_ref 0.1358 _refine_ls_wR_factor_gt 0.1255 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.76166(3) 0.47686(3) -0.00483(4) 0.03398(15) Uani 1 1 d . . . Pd1 Pd 0.73091(6) 0.48256(7) 0.26162(9) 0.0382(3) Uani 1 1 d . . . Cl2 Cl 0.6796(2) 0.4823(2) 0.4764(3) 0.0538(9) Uani 1 1 d . . . P1 P 0.6119(2) 0.49324(19) 0.1772(3) 0.0320(8) Uani 1 1 d . . . C2 C 0.6458(8) 0.4196(9) -0.0688(13) 0.046(4) Uani 1 1 d . . . H2 H 0.6339 0.3695 -0.0426 0.055 Uiso 1 1 calc R . . C1 C 0.6251(7) 0.4920(8) -0.0001(19) 0.048(4) Uani 1 1 d . . . C5 C 0.6609(8) 0.5506(8) -0.0748(12) 0.041(3) Uani 1 1 d . . . H5 H 0.6609 0.6024 -0.0505 0.049 Uiso 1 1 calc R . . C3 C 0.6873(8) 0.4424(11) -0.1816(13) 0.053(4) Uani 1 1 d . . . H3 H 0.7070 0.4089 -0.2452 0.063 Uiso 1 1 calc R . . O1 O 0.8178(7) 0.3250(7) 0.1154(12) 0.068(4) Uani 1 1 d . . . C6 C 0.8004(7) 0.3824(9) 0.0769(14) 0.041(3) Uani 1 1 d . . . C4 C 0.6950(9) 0.5241(10) -0.1847(13) 0.052(4) Uani 1 1 d . . . H4 H 0.7190 0.5534 -0.2502 0.063 Uiso 1 1 calc R . . P2 P 0.8820(2) 0.4715(2) -0.1242(4) 0.0431(9) Uani 1 1 d . . . O2 O 0.8525(7) 0.6081(7) 0.1304(11) 0.067(3) Uani 1 1 d . . . C7 C 0.8195(9) 0.5565(11) 0.0910(18) 0.058(4) Uani 1 1 d . . . Cl1 Cl 0.8630(2) 0.4627(3) 0.3415(4) 0.0677(13) Uani 1 1 d . . . C17 C 0.5569(7) 0.5812(7) 0.2026(13) 0.036(3) Uani 1 1 d . . . C11 C 0.5498(7) 0.4095(8) 0.2085(12) 0.037(3) Uani 1 1 d . . . C9 C 0.9639(8) 0.4326(10) -0.0394(17) 0.070(5) Uani 1 1 d . . . H9A H 1.0122 0.4515 -0.0777 0.106 Uiso 1 1 calc R . . H9B H 0.9627 0.3773 -0.0455 0.106 Uiso 1 1 calc R . . H9C H 0.9615 0.4477 0.0513 0.106 Uiso 1 1 calc R . . C10 C 0.9160(9) 0.5630(10) -0.1812(18) 0.071(6) Uani 1 1 d . . . H10A H 0.9201 0.5979 -0.1084 0.107 Uiso 1 1 calc R . . H10B H 0.8791 0.5831 -0.2443 0.107 Uiso 1 1 calc R . . H10C H 0.9672 0.5571 -0.2216 0.107 Uiso 1 1 calc R . . C12 C 0.4731(9) 0.4042(9) 0.1688(15) 0.049(4) Uani 1 1 d . . . H12 H 0.4485 0.4469 0.1313 0.059 Uiso 1 1 calc R . . C22 C 0.5753(11) 0.6295(9) 0.3085(17) 0.063(5) Uani 1 1 d . . . H22 H 0.6158 0.6161 0.3663 0.076 Uiso 1 1 calc R . . C14 C 0.4643(10) 0.2747(10) 0.2350(18) 0.057(4) Uani 1 1 d . . . H14 H 0.4349 0.2298 0.2469 0.068 Uiso 1 1 calc R . . C15 C 0.5441(11) 0.2778(11) 0.271(2) 0.077(7) Uani 1 1 d . . . H15 H 0.5697 0.2338 0.3021 0.093 Uiso 1 1 calc R . . C13 C 0.4315(9) 0.3371(9) 0.1833(17) 0.053(5) Uani 1 1 d . . . H13 H 0.3788 0.3353 0.1561 0.064 Uiso 1 1 calc R . . C16 C 0.5836(10) 0.3447(10) 0.2612(18) 0.067(5) Uani 1 1 d . . . H16 H 0.6356 0.3472 0.2911 0.080 Uiso 1 1 calc R . . C19 C 0.4612(10) 0.6725(11) 0.1337(18) 0.065(5) Uani 1 1 d . . . H19 H 0.4213 0.6868 0.0753 0.078 Uiso 1 1 calc R . . C18 C 0.5008(9) 0.6047(10) 0.1184(15) 0.052(4) Uani 1 1 d . . . H18 H 0.4885 0.5736 0.0468 0.062 Uiso 1 1 calc R . . C21 C 0.5338(13) 0.6962(11) 0.3267(18) 0.079(6) Uani 1 1 d . . . H21 H 0.5423 0.7256 0.4018 0.095 Uiso 1 1 calc R . . C20 C 0.4814(11) 0.7191(10) 0.237(2) 0.066(5) Uani 1 1 d . . . H20 H 0.4580 0.7675 0.2454 0.080 Uiso 1 1 calc R . . C23 C 0.7589(12) 0.2405(13) 0.397(2) 0.064(5) Uani 1 1 d . . . C24 C 0.7980(15) 0.2893(12) 0.497(3) 0.130(9) Uani 1 1 d . . . H24A H 0.8204 0.3340 0.4554 0.194 Uiso 1 1 calc R . . H24B H 0.8394 0.2605 0.5394 0.194 Uiso 1 1 calc R . . H24C H 0.7597 0.3053 0.5614 0.194 Uiso 1 1 calc R . . N1 N 0.7305(11) 0.2058(14) 0.321(2) 0.102(7) Uani 1 1 d . . . C26 C 0.6833(11) 0.1587(12) 0.989(3) 0.101(6) Uani 1 1 d . . . H26A H 0.7069 0.1681 1.0737 0.151 Uiso 1 1 calc R . . H26B H 0.6947 0.1068 0.9622 0.151 Uiso 1 1 calc R . . H26C H 0.6269 0.1657 0.9951 0.151 Uiso 1 1 calc R . . C25 C 0.7152(13) 0.2115(14) 0.896(3) 0.079(7) Uani 1 1 d . . . N2 N 0.7427(16) 0.250(2) 0.817(3) 0.151(11) Uani 1 1 d . . . C8 C 0.8805(11) 0.4143(12) -0.2672(18) 0.086(6) Uani 1 1 d . . . H8A H 0.8439 0.4359 -0.3294 0.130 Uiso 1 1 calc R . . H8B H 0.8642 0.3628 -0.2451 0.130 Uiso 1 1 calc R . . H8C H 0.9327 0.4129 -0.3052 0.130 Uiso 1 1 calc R . . 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 0.0317(3) 0.0430(3) 0.0272(2) 0.0044(4) 0.0005(4) -0.0034(2) Pd1 0.0321(6) 0.0537(8) 0.0289(6) 0.0034(6) -0.0018(4) -0.0044(5) Cl2 0.060(2) 0.077(3) 0.0241(19) 0.0074(19) 0.0070(15) 0.0038(19) P1 0.039(2) 0.0271(19) 0.0296(16) 0.0011(14) -0.0038(14) -0.0023(15) C2 0.044(9) 0.053(10) 0.040(8) 0.000(7) -0.026(6) -0.008(7) C1 0.032(7) 0.054(9) 0.059(9) 0.013(11) -0.019(9) 0.013(6) C5 0.060(10) 0.032(8) 0.029(7) 0.010(6) 0.002(6) 0.018(7) C3 0.038(9) 0.093(14) 0.027(7) -0.017(8) -0.010(6) 0.015(9) O1 0.065(9) 0.061(8) 0.079(8) 0.035(7) -0.008(6) 0.018(7) C6 0.019(7) 0.051(10) 0.053(9) 0.004(7) 0.000(6) -0.006(6) C4 0.066(11) 0.069(13) 0.022(7) -0.003(8) 0.006(6) -0.006(10) P2 0.042(2) 0.045(2) 0.042(2) 0.0052(19) 0.0102(16) 0.0000(19) O2 0.053(8) 0.079(9) 0.069(8) -0.020(7) 0.010(5) -0.025(7) C7 0.040(10) 0.067(13) 0.068(11) -0.017(10) 0.003(8) -0.006(9) Cl1 0.036(2) 0.118(4) 0.050(2) 0.008(3) -0.0093(17) -0.003(2) C17 0.042(8) 0.021(7) 0.045(8) 0.002(6) 0.003(6) -0.008(6) C11 0.037(8) 0.049(9) 0.025(6) -0.004(6) 0.007(5) -0.001(7) C9 0.042(9) 0.097(13) 0.072(14) 0.009(10) 0.014(7) 0.024(9) C10 0.053(10) 0.076(13) 0.085(13) 0.044(11) 0.037(9) 0.000(10) C12 0.043(10) 0.037(9) 0.067(10) -0.001(8) -0.019(8) -0.007(7) C22 0.077(13) 0.047(11) 0.065(11) -0.016(9) -0.035(9) 0.025(10) C14 0.066(12) 0.039(10) 0.065(11) -0.010(9) 0.005(9) -0.014(9) C15 0.072(14) 0.043(11) 0.117(18) 0.027(11) -0.026(12) -0.011(10) C13 0.025(9) 0.044(11) 0.091(13) -0.013(10) 0.012(8) -0.008(8) C16 0.061(11) 0.050(11) 0.089(14) 0.018(10) -0.026(9) -0.007(9) C19 0.042(12) 0.066(13) 0.087(13) 0.021(11) -0.013(8) 0.024(10) C18 0.036(10) 0.067(11) 0.053(9) -0.009(8) -0.010(6) 0.010(9) C21 0.128(19) 0.060(13) 0.049(11) -0.034(10) -0.004(11) 0.014(13) C20 0.078(14) 0.033(10) 0.089(15) -0.017(10) 0.009(11) 0.011(10) C23 0.048(12) 0.060(14) 0.084(14) 0.024(11) 0.004(10) 0.025(10) C24 0.21(3) 0.091(17) 0.087(16) -0.01(2) -0.03(2) -0.020(17) N1 0.077(14) 0.106(18) 0.123(18) 0.044(14) -0.025(12) -0.012(12) C26 0.091(14) 0.091(16) 0.121(17) 0.00(2) 0.002(19) 0.007(12) C25 0.072(15) 0.070(18) 0.094(19) -0.041(14) 0.001(13) 0.012(12) N2 0.17(3) 0.13(3) 0.15(3) 0.02(2) 0.030(19) 0.010(17) C8 0.085(14) 0.104(17) 0.070(13) -0.025(12) 0.024(11) -0.011(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 C6 1.949(16) . ? Re1 C7 1.951(18) . ? Re1 C5 2.242(12) . ? Re1 C3 2.272(13) . ? Re1 C2 2.284(13) . ? Re1 C4 2.299(14) . ? Re1 C1 2.317(12) . ? Re1 P2 2.367(4) . ? Re1 Pd1 2.7630(11) . ? Pd1 P1 2.190(4) . ? Pd1 Cl2 2.351(3) . ? Pd1 Cl1 2.394(4) . ? Pd1 C7 2.624(18) . ? P1 C17 1.803(13) . ? P1 C11 1.816(14) . ? P1 C1 1.82(2) . ? C2 C3 1.401(19) . ? C2 C1 1.48(2) . ? C1 C5 1.41(2) . ? C5 C4 1.339(17) . ? C3 C4 1.42(2) . ? O1 C6 1.108(16) . ? P2 C9 1.762(15) . ? P2 C8 1.762(18) . ? P2 C10 1.782(15) . ? O2 C7 1.126(18) . ? C17 C18 1.340(19) . ? C17 C22 1.399(19) . ? C11 C12 1.358(18) . ? C11 C16 1.37(2) . ? C12 C13 1.37(2) . ? C22 C21 1.36(2) . ? C14 C13 1.33(2) . ? C14 C15 1.40(2) . ? C15 C16 1.34(2) . ? C19 C18 1.36(2) . ? C19 C20 1.37(2) . ? C21 C20 1.33(3) . ? C23 N1 1.10(3) . ? C23 C24 1.48(3) . ? C26 C25 1.43(3) . ? C25 N2 1.14(3) . ? 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 C6 Re1 C7 102.3(7) . . ? C6 Re1 C5 150.3(5) . . ? C7 Re1 C5 97.7(6) . . ? C6 Re1 C3 107.6(6) . . ? C7 Re1 C3 149.0(8) . . ? C5 Re1 C3 58.7(5) . . ? C6 Re1 C2 92.5(5) . . ? C7 Re1 C2 151.2(6) . . ? C5 Re1 C2 60.6(6) . . ? C3 Re1 C2 35.8(5) . . ? C6 Re1 C4 143.4(6) . . ? C7 Re1 C4 113.0(7) . . ? C5 Re1 C4 34.3(5) . . ? C3 Re1 C4 36.3(5) . . ? C2 Re1 C4 60.7(6) . . ? C6 Re1 C1 114.8(5) . . ? C7 Re1 C1 113.9(6) . . ? C5 Re1 C1 35.9(5) . . ? C3 Re1 C1 59.9(6) . . ? C2 Re1 C1 37.5(5) . . ? C4 Re1 C1 59.4(6) . . ? C6 Re1 P2 84.2(4) . . ? C7 Re1 P2 81.7(5) . . ? C5 Re1 P2 120.6(3) . . ? C3 Re1 P2 93.2(4) . . ? C2 Re1 P2 124.7(4) . . ? C4 Re1 P2 91.4(4) . . ? C1 Re1 P2 150.1(5) . . ? C6 Re1 Pd1 71.0(4) . . ? C7 Re1 Pd1 65.0(5) . . ? C5 Re1 Pd1 98.6(3) . . ? C3 Re1 Pd1 133.1(4) . . ? C2 Re1 Pd1 97.7(4) . . ? C4 Re1 Pd1 132.6(4) . . ? C1 Re1 Pd1 77.8(5) . . ? P2 Re1 Pd1 131.79(10) . . ? P1 Pd1 Cl2 91.61(13) . . ? P1 Pd1 Cl1 175.39(16) . . ? Cl2 Pd1 Cl1 91.47(14) . . ? P1 Pd1 C7 102.7(4) . . ? Cl2 Pd1 C7 145.6(4) . . ? Cl1 Pd1 C7 76.5(4) . . ? P1 Pd1 Re1 77.87(10) . . ? Cl2 Pd1 Re1 169.03(10) . . ? Cl1 Pd1 Re1 98.86(11) . . ? C7 Pd1 Re1 42.4(4) . . ? C17 P1 C11 110.7(6) . . ? C17 P1 C1 102.4(6) . . ? C11 P1 C1 103.6(6) . . ? C17 P1 Pd1 119.1(4) . . ? C11 P1 Pd1 113.0(5) . . ? C1 P1 Pd1 106.0(4) . . ? C3 C2 C1 105.5(15) . . ? C3 C2 Re1 71.6(8) . . ? C1 C2 Re1 72.5(7) . . ? C5 C1 C2 104.8(15) . . ? C5 C1 P1 125.5(12) . . ? C2 C1 P1 120.6(11) . . ? C5 C1 Re1 69.2(7) . . ? C2 C1 Re1 70.1(7) . . ? P1 C1 Re1 98.2(6) . . ? C4 C5 C1 112.8(14) . . ? C4 C5 Re1 75.2(9) . . ? C1 C5 Re1 75.0(7) . . ? C2 C3 C4 110.1(14) . . ? C2 C3 Re1 72.6(7) . . ? C4 C3 Re1 72.9(8) . . ? O1 C6 Re1 173.3(14) . . ? C5 C4 C3 106.5(13) . . ? C5 C4 Re1 70.5(8) . . ? C3 C4 Re1 70.9(8) . . ? C9 P2 C8 101.6(9) . . ? C9 P2 C10 104.4(8) . . ? C8 P2 C10 103.7(9) . . ? C9 P2 Re1 115.7(5) . . ? C8 P2 Re1 115.7(6) . . ? C10 P2 Re1 114.1(6) . . ? O2 C7 Re1 170.4(17) . . ? O2 C7 Pd1 115.6(13) . . ? Re1 C7 Pd1 72.6(6) . . ? C18 C17 C22 117.9(13) . . ? C18 C17 P1 121.9(12) . . ? C22 C17 P1 120.1(11) . . ? C12 C11 C16 117.1(14) . . ? C12 C11 P1 123.4(12) . . ? C16 C11 P1 119.0(11) . . ? C11 C12 C13 121.0(15) . . ? C21 C22 C17 119.9(15) . . ? C13 C14 C15 118.4(15) . . ? C16 C15 C14 119.4(17) . . ? C14 C13 C12 121.6(15) . . ? C15 C16 C11 122.3(16) . . ? C18 C19 C20 118.3(16) . . ? C17 C18 C19 122.4(15) . . ? C20 C21 C22 120.1(16) . . ? C21 C20 C19 121.0(17) . . ? N1 C23 C24 178(3) . . ? N2 C25 C26 175(3) . . ? 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 C6 Re1 Pd1 P1 -121.1(4) . . . . ? C7 Re1 Pd1 P1 124.7(6) . . . . ? C5 Re1 Pd1 P1 30.2(4) . . . . ? C3 Re1 Pd1 P1 -24.5(6) . . . . ? C2 Re1 Pd1 P1 -31.1(4) . . . . ? C4 Re1 Pd1 P1 25.8(6) . . . . ? C1 Re1 Pd1 P1 0.8(4) . . . . ? P2 Re1 Pd1 P1 175.76(16) . . . . ? C6 Re1 Pd1 Cl2 -104.4(7) . . . . ? C7 Re1 Pd1 Cl2 141.4(8) . . . . ? C5 Re1 Pd1 Cl2 46.9(7) . . . . ? C3 Re1 Pd1 Cl2 -7.8(9) . . . . ? C2 Re1 Pd1 Cl2 -14.5(7) . . . . ? C4 Re1 Pd1 Cl2 42.4(8) . . . . ? C1 Re1 Pd1 Cl2 17.4(7) . . . . ? P2 Re1 Pd1 Cl2 -167.6(6) . . . . ? C6 Re1 Pd1 Cl1 55.6(4) . . . . ? C7 Re1 Pd1 Cl1 -58.6(6) . . . . ? C5 Re1 Pd1 Cl1 -153.1(4) . . . . ? C3 Re1 Pd1 Cl1 152.2(6) . . . . ? C2 Re1 Pd1 Cl1 145.6(4) . . . . ? C4 Re1 Pd1 Cl1 -157.5(6) . . . . ? C1 Re1 Pd1 Cl1 177.5(4) . . . . ? P2 Re1 Pd1 Cl1 -7.5(2) . . . . ? C6 Re1 Pd1 C7 114.2(7) . . . . ? C5 Re1 Pd1 C7 -94.5(7) . . . . ? C3 Re1 Pd1 C7 -149.2(9) . . . . ? C2 Re1 Pd1 C7 -155.8(7) . . . . ? C4 Re1 Pd1 C7 -99.0(8) . . . . ? C1 Re1 Pd1 C7 -123.9(7) . . . . ? P2 Re1 Pd1 C7 51.0(6) . . . . ? Cl2 Pd1 P1 C17 67.5(5) . . . . ? Cl1 Pd1 P1 C17 -160.7(19) . . . . ? C7 Pd1 P1 C17 -81.0(7) . . . . ? Re1 Pd1 P1 C17 -115.6(5) . . . . ? Cl2 Pd1 P1 C11 -65.1(5) . . . . ? Cl1 Pd1 P1 C11 67(2) . . . . ? C7 Pd1 P1 C11 146.4(6) . . . . ? Re1 Pd1 P1 C11 111.8(5) . . . . ? Cl2 Pd1 P1 C1 -177.9(5) . . . . ? Cl1 Pd1 P1 C1 -46(2) . . . . ? C7 Pd1 P1 C1 33.6(6) . . . . ? Re1 Pd1 P1 C1 -1.0(5) . . . . ? C6 Re1 C2 C3 -117.2(11) . . . . ? C7 Re1 C2 C3 121.3(15) . . . . ? C5 Re1 C2 C3 76.2(10) . . . . ? C4 Re1 C2 C3 36.7(9) . . . . ? C1 Re1 C2 C3 113.5(14) . . . . ? P2 Re1 C2 C3 -32.5(11) . . . . ? Pd1 Re1 C2 C3 171.7(9) . . . . ? C6 Re1 C2 C1 129.3(10) . . . . ? C7 Re1 C2 C1 7.8(19) . . . . ? C5 Re1 C2 C1 -37.4(9) . . . . ? C3 Re1 C2 C1 -113.5(14) . . . . ? C4 Re1 C2 C1 -76.9(10) . . . . ? P2 Re1 C2 C1 -146.0(8) . . . . ? Pd1 Re1 C2 C1 58.2(9) . . . . ? C3 C2 C1 C5 -3.7(14) . . . . ? Re1 C2 C1 C5 60.8(9) . . . . ? C3 C2 C1 P1 -152.4(9) . . . . ? Re1 C2 C1 P1 -87.9(8) . . . . ? C3 C2 C1 Re1 -64.5(9) . . . . ? C17 P1 C1 C5 56.6(12) . . . . ? C11 P1 C1 C5 171.8(11) . . . . ? Pd1 P1 C1 C5 -69.0(11) . . . . ? C17 P1 C1 C2 -161.5(10) . . . . ? C11 P1 C1 C2 -46.3(11) . . . . ? Pd1 P1 C1 C2 72.9(11) . . . . ? C17 P1 C1 Re1 126.8(5) . . . . ? C11 P1 C1 Re1 -118.0(6) . . . . ? Pd1 P1 C1 Re1 1.2(5) . . . . ? C6 Re1 C1 C5 -173.8(9) . . . . ? C7 Re1 C1 C5 68.6(11) . . . . ? C3 Re1 C1 C5 -77.1(10) . . . . ? C2 Re1 C1 C5 -115.4(15) . . . . ? C4 Re1 C1 C5 -34.9(9) . . . . ? P2 Re1 C1 C5 -48.5(13) . . . . ? Pd1 Re1 C1 C5 124.0(9) . . . . ? C6 Re1 C1 C2 -58.4(11) . . . . ? C7 Re1 C1 C2 -175.9(10) . . . . ? C5 Re1 C1 C2 115.4(15) . . . . ? C3 Re1 C1 C2 38.3(9) . . . . ? C4 Re1 C1 C2 80.6(10) . . . . ? P2 Re1 C1 C2 67.0(11) . . . . ? Pd1 Re1 C1 C2 -120.6(9) . . . . ? C6 Re1 C1 P1 61.2(8) . . . . ? C7 Re1 C1 P1 -56.3(9) . . . . ? C5 Re1 C1 P1 -124.9(11) . . . . ? C3 Re1 C1 P1 157.9(9) . . . . ? C2 Re1 C1 P1 119.6(11) . . . . ? C4 Re1 C1 P1 -159.8(9) . . . . ? P2 Re1 C1 P1 -173.4(3) . . . . ? Pd1 Re1 C1 P1 -1.0(4) . . . . ? C2 C1 C5 C4 5.0(16) . . . . ? P1 C1 C5 C4 151.6(11) . . . . ? Re1 C1 C5 C4 66.4(11) . . . . ? C2 C1 C5 Re1 -61.4(8) . . . . ? P1 C1 C5 Re1 85.2(9) . . . . ? C6 Re1 C5 C4 -107.8(13) . . . . ? C7 Re1 C5 C4 120.1(11) . . . . ? C3 Re1 C5 C4 -38.4(9) . . . . ? C2 Re1 C5 C4 -80.1(10) . . . . ? C1 Re1 C5 C4 -119.1(14) . . . . ? P2 Re1 C5 C4 35.2(11) . . . . ? Pd1 Re1 C5 C4 -174.2(9) . . . . ? C6 Re1 C5 C1 11.4(16) . . . . ? C7 Re1 C5 C1 -120.8(10) . . . . ? C3 Re1 C5 C1 80.7(10) . . . . ? C2 Re1 C5 C1 39.1(10) . . . . ? C4 Re1 C5 C1 119.1(14) . . . . ? P2 Re1 C5 C1 154.3(8) . . . . ? Pd1 Re1 C5 C1 -55.0(9) . . . . ? C1 C2 C3 C4 1.4(14) . . . . ? Re1 C2 C3 C4 -63.7(10) . . . . ? C1 C2 C3 Re1 65.1(8) . . . . ? C6 Re1 C3 C2 68.8(11) . . . . ? C7 Re1 C3 C2 -127.0(13) . . . . ? C5 Re1 C3 C2 -82.1(10) . . . . ? C4 Re1 C3 C2 -118.3(13) . . . . ? C1 Re1 C3 C2 -40.1(9) . . . . ? P2 Re1 C3 C2 153.7(9) . . . . ? Pd1 Re1 C3 C2 -11.3(13) . . . . ? C6 Re1 C3 C4 -172.9(8) . . . . ? C7 Re1 C3 C4 -8.7(16) . . . . ? C5 Re1 C3 C4 36.3(8) . . . . ? C2 Re1 C3 C4 118.3(13) . . . . ? C1 Re1 C3 C4 78.2(9) . . . . ? P2 Re1 C3 C4 -87.9(8) . . . . ? Pd1 Re1 C3 C4 107.0(9) . . . . ? C7 Re1 C6 O1 179(100) . . . . ? C5 Re1 C6 O1 48(12) . . . . ? C3 Re1 C6 O1 -9(12) . . . . ? C2 Re1 C6 O1 24(12) . . . . ? C4 Re1 C6 O1 -16(12) . . . . ? C1 Re1 C6 O1 55(12) . . . . ? P2 Re1 C6 O1 -100(12) . . . . ? Pd1 Re1 C6 O1 122(12) . . . . ? C1 C5 C4 C3 -4.1(16) . . . . ? Re1 C5 C4 C3 62.1(10) . . . . ? C1 C5 C4 Re1 -66.3(10) . . . . ? C2 C3 C4 C5 1.5(16) . . . . ? Re1 C3 C4 C5 -61.9(10) . . . . ? C2 C3 C4 Re1 63.5(9) . . . . ? C6 Re1 C4 C5 127.6(11) . . . . ? C7 Re1 C4 C5 -68.7(11) . . . . ? C3 Re1 C4 C5 116.2(13) . . . . ? C2 Re1 C4 C5 80.0(10) . . . . ? C1 Re1 C4 C5 36.5(9) . . . . ? P2 Re1 C4 C5 -150.3(9) . . . . ? Pd1 Re1 C4 C5 7.9(12) . . . . ? C6 Re1 C4 C3 11.5(13) . . . . ? C7 Re1 C4 C3 175.2(9) . . . . ? C5 Re1 C4 C3 -116.2(13) . . . . ? C2 Re1 C4 C3 -36.2(8) . . . . ? C1 Re1 C4 C3 -79.7(9) . . . . ? P2 Re1 C4 C3 93.6(8) . . . . ? Pd1 Re1 C4 C3 -108.3(8) . . . . ? C6 Re1 P2 C9 -33.2(8) . . . . ? C7 Re1 P2 C9 70.2(9) . . . . ? C5 Re1 P2 C9 164.2(8) . . . . ? C3 Re1 P2 C9 -140.6(8) . . . . ? C2 Re1 P2 C9 -122.2(8) . . . . ? C4 Re1 P2 C9 -176.8(8) . . . . ? C1 Re1 P2 C9 -165.1(9) . . . . ? Pd1 Re1 P2 C9 24.8(7) . . . . ? C6 Re1 P2 C8 85.4(9) . . . . ? C7 Re1 P2 C8 -171.2(10) . . . . ? C5 Re1 P2 C8 -77.1(9) . . . . ? C3 Re1 P2 C8 -22.0(9) . . . . ? C2 Re1 P2 C8 -3.6(9) . . . . ? C4 Re1 P2 C8 -58.2(9) . . . . ? C1 Re1 P2 C8 -46.5(11) . . . . ? Pd1 Re1 P2 C8 143.4(8) . . . . ? C6 Re1 P2 C10 -154.4(8) . . . . ? C7 Re1 P2 C10 -51.0(9) . . . . ? C5 Re1 P2 C10 43.1(8) . . . . ? C3 Re1 P2 C10 98.2(9) . . . . ? C2 Re1 P2 C10 116.6(9) . . . . ? C4 Re1 P2 C10 62.0(8) . . . . ? C1 Re1 P2 C10 73.7(10) . . . . ? Pd1 Re1 P2 C10 -96.4(7) . . . . ? C6 Re1 C7 O2 148(9) . . . . ? C5 Re1 C7 O2 -54(9) . . . . ? C3 Re1 C7 O2 -17(10) . . . . ? C2 Re1 C7 O2 -93(9) . . . . ? C4 Re1 C7 O2 -22(9) . . . . ? C1 Re1 C7 O2 -88(9) . . . . ? P2 Re1 C7 O2 66(9) . . . . ? Pd1 Re1 C7 O2 -150(9) . . . . ? C6 Re1 C7 Pd1 -62.0(5) . . . . ? C5 Re1 C7 Pd1 95.9(4) . . . . ? C3 Re1 C7 Pd1 133.5(10) . . . . ? C2 Re1 C7 Pd1 57.4(14) . . . . ? C4 Re1 C7 Pd1 127.9(4) . . . . ? C1 Re1 C7 Pd1 62.5(6) . . . . ? P2 Re1 C7 Pd1 -144.1(3) . . . . ? P1 Pd1 C7 O2 119.2(14) . . . . ? Cl2 Pd1 C7 O2 6.9(19) . . . . ? Cl1 Pd1 C7 O2 -65.4(14) . . . . ? Re1 Pd1 C7 O2 174.7(18) . . . . ? P1 Pd1 C7 Re1 -55.5(5) . . . . ? Cl2 Pd1 C7 Re1 -167.8(2) . . . . ? Cl1 Pd1 C7 Re1 119.9(5) . . . . ? C11 P1 C17 C18 -72.5(14) . . . . ? C1 P1 C17 C18 37.4(14) . . . . ? Pd1 P1 C17 C18 153.9(11) . . . . ? C11 P1 C17 C22 111.2(13) . . . . ? C1 P1 C17 C22 -138.9(13) . . . . ? Pd1 P1 C17 C22 -22.4(15) . . . . ? C17 P1 C11 C12 41.5(14) . . . . ? C1 P1 C11 C12 -67.6(13) . . . . ? Pd1 P1 C11 C12 178.1(11) . . . . ? C17 P1 C11 C16 -146.2(12) . . . . ? C1 P1 C11 C16 104.6(13) . . . . ? Pd1 P1 C11 C16 -9.7(13) . . . . ? C16 C11 C12 C13 1(2) . . . . ? P1 C11 C12 C13 173.4(12) . . . . ? C18 C17 C22 C21 3(3) . . . . ? P1 C17 C22 C21 179.6(14) . . . . ? C13 C14 C15 C16 4(3) . . . . ? C15 C14 C13 C12 -2(3) . . . . ? C11 C12 C13 C14 -1(3) . . . . ? C14 C15 C16 C11 -4(3) . . . . ? C12 C11 C16 C15 2(3) . . . . ? P1 C11 C16 C15 -171.2(16) . . . . ? C22 C17 C18 C19 -1(3) . . . . ? P1 C17 C18 C19 -177.3(13) . . . . ? C20 C19 C18 C17 2(3) . . . . ? C17 C22 C21 C20 -7(3) . . . . ? C22 C21 C20 C19 8(3) . . . . ? C18 C19 C20 C21 -5(3) . . . . ? _diffrn_measured_fraction_theta_max 0.931 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 3.111 _refine_diff_density_min -1.867 _refine_diff_density_rms 0.209 # Attachment 'COMPLEX4_MFHKDS2m.cif' data_mfhkds2m _database_code_depnum_ccdc_archive 'CCDC 756946' #TrackingRef 'COMPLEX4_MFHKDS2m.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H23 Cl2 O5 P2 Pd Re, C H2 Cl2' _chemical_formula_sum 'C23 H25 Cl4 O5 P2 Pd Re' _chemical_formula_weight 877.77 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' 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' Pd Pd -0.9988 1.0072 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 19.1773(6) _cell_length_b 13.3897(4) _cell_length_c 22.1610(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5690.5(3) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 958 _cell_measurement_theta_min 1.77 _cell_measurement_theta_max 27.77 _exptl_crystal_description Plate _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.049 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3376 _exptl_absorpt_coefficient_mu 5.403 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.2046 _exptl_absorpt_correction_T_max 0.6590 _exptl_absorpt_process_details 'Bruker XPREP' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 72639 _diffrn_reflns_av_R_equivalents 0.0733 _diffrn_reflns_av_sigmaI/netI 0.0322 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 27.89 _reflns_number_total 6555 _reflns_number_gt 5578 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics CrystalMaker _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0519P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6555 _refine_ls_number_parameters 328 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0398 _refine_ls_R_factor_gt 0.0327 _refine_ls_wR_factor_ref 0.0858 _refine_ls_wR_factor_gt 0.0826 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.017 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.311789(15) -0.00461(2) 0.195000(14) 0.02060(9) Uani 1 1 d . . . Re1 Re 0.176784(8) 0.065464(12) 0.179791(7) 0.01883(7) Uani 1 1 d . . . Cl1 Cl 0.33215(6) -0.06990(8) 0.09629(6) 0.0356(3) Uani 1 1 d . . . Cl2 Cl 0.42629(5) -0.03966(8) 0.22799(5) 0.0290(2) Uani 1 1 d . . . P2 P 0.09345(6) 0.04336(8) 0.10538(5) 0.0255(2) Uani 1 1 d . . . P1 P 0.28851(5) 0.05969(7) 0.28382(5) 0.0196(2) Uani 1 1 d . . . O1 O 0.26869(15) 0.1607(2) 0.08179(13) 0.0325(7) Uani 1 1 d . . . O2 O 0.18903(15) -0.1636(2) 0.16770(14) 0.0314(7) Uani 1 1 d . . . O3 O 0.04516(17) 0.1381(3) 0.08932(16) 0.0472(9) Uani 1 1 d . . . O4 O 0.03595(17) -0.0299(3) 0.12755(16) 0.0474(9) Uani 1 1 d . . . O5 O 0.11540(18) 0.0112(3) 0.03966(15) 0.0474(9) Uani 1 1 d . . . C1 C 0.2029(2) 0.1126(3) 0.27618(17) 0.0219(8) Uani 1 1 d . . . C2 C 0.1894(2) 0.2007(3) 0.24111(18) 0.0242(8) Uani 1 1 d . . . H2 H 0.2213 0.2509 0.2323 0.029 Uiso 1 1 calc R . . C3 C 0.1194(2) 0.1974(3) 0.22239(18) 0.0265(9) Uani 1 1 d . . . H3 H 0.0969 0.2458 0.1994 0.032 Uiso 1 1 calc R . . C4 C 0.0886(2) 0.1081(3) 0.24442(18) 0.0268(9) Uani 1 1 d . . . H4 H 0.0428 0.0877 0.2380 0.032 Uiso 1 1 calc R . . C5 C 0.1395(2) 0.0559(3) 0.27762(18) 0.0245(9) Uani 1 1 d . . . H5 H 0.1330 -0.0049 0.2971 0.029 Uiso 1 1 calc R . . C6 C 0.2359(2) 0.1196(3) 0.11699(18) 0.0250(9) Uani 1 1 d . . . C7 C 0.1889(2) -0.0770(3) 0.17034(19) 0.0216(9) Uani 1 1 d . . . C8 C 0.0749(3) 0.2204(4) 0.0545(3) 0.0528(14) Uani 1 1 d . . . H8A H 0.1077 0.2562 0.0791 0.079 Uiso 1 1 calc R . . H8B H 0.0383 0.2647 0.0421 0.079 Uiso 1 1 calc R . . H8C H 0.0981 0.1943 0.0196 0.079 Uiso 1 1 calc R . . C9 C -0.0278(3) -0.0441(5) 0.0934(3) 0.0618(17) Uani 1 1 d . . . H9A H -0.0576 0.0129 0.0988 0.093 Uiso 1 1 calc R . . H9B H -0.0513 -0.1030 0.1074 0.093 Uiso 1 1 calc R . . H9C H -0.0167 -0.0514 0.0514 0.093 Uiso 1 1 calc R . . C10 C 0.1518(3) -0.0833(4) 0.0294(2) 0.0406(11) Uani 1 1 d . . . H10A H 0.1993 -0.0775 0.0428 0.061 Uiso 1 1 calc R . . H10B H 0.1511 -0.0990 -0.0129 0.061 Uiso 1 1 calc R . . H10C H 0.1290 -0.1356 0.0515 0.061 Uiso 1 1 calc R . . C11 C 0.3459(2) 0.1608(3) 0.30565(18) 0.0230(8) Uani 1 1 d . . . C12 C 0.3488(2) 0.1961(3) 0.36484(19) 0.0296(9) Uani 1 1 d . . . H12 H 0.3201 0.1680 0.3942 0.035 Uiso 1 1 calc R . . C13 C 0.3934(2) 0.2717(3) 0.3800(2) 0.0330(10) Uani 1 1 d . . . H13 H 0.3949 0.2948 0.4195 0.040 Uiso 1 1 calc R . . C14 C 0.4364(2) 0.3139(3) 0.3369(2) 0.0314(10) Uani 1 1 d . . . H14 H 0.4673 0.3643 0.3477 0.038 Uiso 1 1 calc R . . C15 C 0.4334(2) 0.2814(3) 0.2781(2) 0.0315(10) Uani 1 1 d . . . H15 H 0.4615 0.3110 0.2489 0.038 Uiso 1 1 calc R . . C16 C 0.3885(2) 0.2041(3) 0.26224(19) 0.0267(9) Uani 1 1 d . . . H16 H 0.3869 0.1815 0.2226 0.032 Uiso 1 1 calc R . . C17 C 0.2803(2) -0.0271(3) 0.34625(18) 0.0234(8) Uani 1 1 d . . . C18 C 0.3175(2) -0.1169(3) 0.3446(2) 0.0260(9) Uani 1 1 d . . . H18 H 0.3450 -0.1321 0.3112 0.031 Uiso 1 1 calc R . . C19 C 0.3136(2) -0.1831(3) 0.3923(2) 0.0322(10) Uani 1 1 d . . . H19 H 0.3376 -0.2434 0.3907 0.039 Uiso 1 1 calc R . . C20 C 0.2739(2) -0.1595(3) 0.44237(19) 0.0337(10) Uani 1 1 d . . . H20 H 0.2723 -0.2035 0.4748 0.040 Uiso 1 1 calc R . . C21 C 0.2367(2) -0.0712(3) 0.44462(19) 0.0317(10) Uani 1 1 d . . . H21 H 0.2095 -0.0562 0.4782 0.038 Uiso 1 1 calc R . . C22 C 0.2400(2) -0.0053(3) 0.39656(19) 0.0284(9) Uani 1 1 d . . . H22 H 0.2150 0.0542 0.3980 0.034 Uiso 1 1 calc R . . C23 C 0.4820(3) 0.0789(4) 0.0904(3) 0.0559(15) Uani 1 1 d . . . H23A H 0.4800 0.0422 0.1281 0.067 Uiso 1 1 calc R . . H23B H 0.4457 0.0531 0.0642 0.067 Uiso 1 1 calc R . . Cl3 Cl 0.46631(11) 0.20574(13) 0.10457(10) 0.1000(8) Uani 1 1 d . . . Cl4 Cl 0.56282(8) 0.05964(11) 0.05672(8) 0.0642(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.01634(16) 0.02307(17) 0.02239(17) -0.00241(12) 0.00100(11) 0.00136(11) Re1 0.01534(10) 0.02167(11) 0.01948(10) -0.00149(6) -0.00046(6) 0.00014(5) Cl1 0.0288(6) 0.0456(7) 0.0323(6) -0.0154(5) 0.0045(5) 0.0028(4) Cl2 0.0174(5) 0.0300(5) 0.0395(6) 0.0008(4) -0.0005(4) 0.0031(4) P2 0.0199(5) 0.0323(6) 0.0242(6) 0.0015(4) -0.0037(4) -0.0054(4) P1 0.0166(5) 0.0230(5) 0.0194(5) -0.0008(4) -0.0001(4) -0.0010(4) O1 0.0325(17) 0.0391(17) 0.0258(16) 0.0003(13) 0.0056(13) -0.0089(14) O2 0.0325(17) 0.0267(17) 0.0348(17) -0.0041(13) -0.0017(13) 0.0053(13) O3 0.039(2) 0.051(2) 0.051(2) 0.0089(17) -0.0077(17) 0.0025(16) O4 0.0291(19) 0.075(2) 0.039(2) -0.0006(18) -0.0007(15) -0.0182(17) O5 0.038(2) 0.069(2) 0.0350(19) -0.0051(17) -0.0016(16) -0.0025(18) C1 0.021(2) 0.024(2) 0.021(2) -0.0045(15) 0.0022(16) 0.0002(15) C2 0.025(2) 0.025(2) 0.023(2) -0.0045(17) 0.0035(16) -0.0004(16) C3 0.024(2) 0.029(2) 0.027(2) -0.0061(17) -0.0012(17) 0.0078(17) C4 0.018(2) 0.034(2) 0.029(2) -0.0082(18) 0.0009(17) 0.0015(17) C5 0.020(2) 0.031(2) 0.022(2) -0.0033(16) 0.0028(17) -0.0028(16) C6 0.022(2) 0.028(2) 0.025(2) -0.0044(17) -0.0065(17) -0.0002(16) C7 0.018(2) 0.027(2) 0.020(2) 0.0018(16) -0.0008(15) 0.0014(15) C8 0.057(4) 0.042(3) 0.059(4) 0.018(3) -0.005(3) -0.003(2) C9 0.032(3) 0.086(4) 0.068(4) -0.007(3) -0.010(3) -0.023(3) C10 0.045(3) 0.044(3) 0.032(3) -0.011(2) 0.000(2) -0.005(2) C11 0.0169(19) 0.025(2) 0.027(2) 0.0003(16) -0.0013(16) 0.0033(16) C12 0.027(2) 0.033(2) 0.029(2) -0.0008(18) 0.0014(18) -0.0037(18) C13 0.030(2) 0.036(2) 0.033(2) -0.0076(19) -0.0039(19) -0.0016(19) C14 0.025(2) 0.024(2) 0.045(3) -0.0047(19) -0.005(2) -0.0013(17) C15 0.024(2) 0.028(2) 0.043(3) 0.0051(19) 0.0023(19) -0.0028(17) C16 0.028(2) 0.024(2) 0.029(2) 0.0019(17) -0.0011(18) -0.0008(16) C17 0.022(2) 0.028(2) 0.021(2) 0.0011(16) -0.0035(16) -0.0084(16) C18 0.027(2) 0.025(2) 0.025(2) -0.0031(17) -0.0048(17) -0.0049(16) C19 0.035(3) 0.028(2) 0.034(3) 0.0004(19) -0.0066(19) -0.0023(18) C20 0.034(2) 0.037(2) 0.030(2) 0.0077(19) -0.0042(19) -0.0100(19) C21 0.030(2) 0.041(3) 0.024(2) 0.0024(18) 0.0023(18) -0.0056(19) C22 0.028(2) 0.033(2) 0.025(2) -0.0001(17) -0.0029(17) -0.0019(17) C23 0.053(4) 0.051(3) 0.064(4) 0.003(3) 0.021(3) -0.006(3) Cl3 0.1176(17) 0.0576(10) 0.1247(18) 0.0151(10) 0.0641(14) 0.0215(10) Cl4 0.0367(8) 0.0757(10) 0.0802(12) -0.0116(8) 0.0036(7) 0.0092(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Pd1 P1 2.1943(10) . ? Pd1 Cl2 2.3614(10) . ? Pd1 Cl1 2.3878(12) . ? Pd1 Re1 2.7744(3) . ? Re1 C7 1.933(4) . ? Re1 C6 1.936(4) . ? Re1 C2 2.276(4) . ? Re1 C1 2.283(4) . ? Re1 C3 2.286(4) . ? Re1 C5 2.287(4) . ? Re1 C4 2.289(4) . ? Re1 P2 2.3153(11) . ? P2 O4 1.556(3) . ? P2 O5 1.576(4) . ? P2 O3 1.611(3) . ? P1 C1 1.796(4) . ? P1 C11 1.811(4) . ? P1 C17 1.814(4) . ? O1 C6 1.143(5) . ? O2 C7 1.161(5) . ? O3 C8 1.460(6) . ? O4 C9 1.450(6) . ? O5 C10 1.464(6) . ? C1 C5 1.435(5) . ? C1 C2 1.436(5) . ? C2 C3 1.406(5) . ? C3 C4 1.420(6) . ? C4 C5 1.408(6) . ? C11 C16 1.388(6) . ? C11 C12 1.395(5) . ? C12 C13 1.368(6) . ? C13 C14 1.381(6) . ? C14 C15 1.376(6) . ? C15 C16 1.392(5) . ? C17 C22 1.387(6) . ? C17 C18 1.399(6) . ? C18 C19 1.382(6) . ? C19 C20 1.382(6) . ? C20 C21 1.383(6) . ? C21 C22 1.385(6) . ? C23 Cl4 1.740(6) . ? C23 Cl3 1.753(5) . ? 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 P1 Pd1 Cl2 89.39(4) . . ? P1 Pd1 Cl1 177.06(4) . . ? Cl2 Pd1 Cl1 93.37(4) . . ? P1 Pd1 Re1 77.67(3) . . ? Cl2 Pd1 Re1 166.55(3) . . ? Cl1 Pd1 Re1 99.51(3) . . ? C7 Re1 C6 102.80(17) . . ? C7 Re1 C2 146.80(16) . . ? C6 Re1 C2 93.95(15) . . ? C7 Re1 C1 110.37(16) . . ? C6 Re1 C1 116.14(15) . . ? C2 Re1 C1 36.71(14) . . ? C7 Re1 C3 149.91(16) . . ? C6 Re1 C3 106.82(15) . . ? C2 Re1 C3 35.90(13) . . ? C1 Re1 C3 60.37(14) . . ? C7 Re1 C5 94.87(16) . . ? C6 Re1 C5 152.36(15) . . ? C2 Re1 C5 60.79(14) . . ? C1 Re1 C5 36.59(14) . . ? C3 Re1 C5 60.07(14) . . ? C7 Re1 C4 113.75(17) . . ? C6 Re1 C4 142.10(16) . . ? C2 Re1 C4 60.43(14) . . ? C1 Re1 C4 60.50(14) . . ? C3 Re1 C4 36.16(15) . . ? C5 Re1 C4 35.85(14) . . ? C7 Re1 P2 83.07(12) . . ? C6 Re1 P2 86.57(11) . . ? C2 Re1 P2 126.87(10) . . ? C1 Re1 P2 148.55(10) . . ? C3 Re1 P2 93.46(10) . . ? C5 Re1 P2 116.87(10) . . ? C4 Re1 P2 88.13(10) . . ? C7 Re1 Pd1 64.38(12) . . ? C6 Re1 Pd1 70.58(11) . . ? C2 Re1 Pd1 95.59(10) . . ? C1 Re1 Pd1 77.01(10) . . ? C3 Re1 Pd1 131.36(10) . . ? C5 Re1 Pd1 99.09(10) . . ? C4 Re1 Pd1 134.27(10) . . ? P2 Re1 Pd1 133.43(3) . . ? O4 P2 O5 108.0(2) . . ? O4 P2 O3 99.2(2) . . ? O5 P2 O3 99.47(19) . . ? O4 P2 Re1 110.18(14) . . ? O5 P2 Re1 120.58(14) . . ? O3 P2 Re1 116.97(14) . . ? C1 P1 C11 106.63(18) . . ? C1 P1 C17 104.18(19) . . ? C11 P1 C17 109.16(18) . . ? C1 P1 Pd1 104.84(13) . . ? C11 P1 Pd1 114.16(14) . . ? C17 P1 Pd1 116.78(14) . . ? C8 O3 P2 119.1(3) . . ? C9 O4 P2 121.0(4) . . ? C10 O5 P2 120.5(3) . . ? C5 C1 C2 107.1(3) . . ? C5 C1 P1 124.3(3) . . ? C2 C1 P1 122.7(3) . . ? C5 C1 Re1 71.8(2) . . ? C2 C1 Re1 71.4(2) . . ? P1 C1 Re1 100.34(17) . . ? C3 C2 C1 107.9(3) . . ? C3 C2 Re1 72.4(2) . . ? C1 C2 Re1 71.9(2) . . ? C2 C3 C4 108.8(4) . . ? C2 C3 Re1 71.7(2) . . ? C4 C3 Re1 72.0(2) . . ? C5 C4 C3 108.1(4) . . ? C5 C4 Re1 72.0(2) . . ? C3 C4 Re1 71.8(2) . . ? C4 C5 C1 108.2(4) . . ? C4 C5 Re1 72.2(2) . . ? C1 C5 Re1 71.6(2) . . ? O1 C6 Re1 173.2(4) . . ? O2 C7 Re1 172.5(4) . . ? C16 C11 C12 119.2(4) . . ? C16 C11 P1 119.0(3) . . ? C12 C11 P1 121.9(3) . . ? C13 C12 C11 120.4(4) . . ? C12 C13 C14 120.5(4) . . ? C15 C14 C13 120.0(4) . . ? C14 C15 C16 120.0(4) . . ? C11 C16 C15 120.0(4) . . ? C22 C17 C18 119.1(4) . . ? C22 C17 P1 121.8(3) . . ? C18 C17 P1 119.1(3) . . ? C19 C18 C17 120.2(4) . . ? C18 C19 C20 119.9(4) . . ? C19 C20 C21 120.6(4) . . ? C20 C21 C22 119.6(4) . . ? C21 C22 C17 120.6(4) . . ? Cl4 C23 Cl3 111.9(3) . . ? 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 P1 Pd1 Re1 C7 -118.22(14) . . . . ? Cl2 Pd1 Re1 C7 -134.35(19) . . . . ? Cl1 Pd1 Re1 C7 62.63(14) . . . . ? P1 Pd1 Re1 C6 126.34(12) . . . . ? Cl2 Pd1 Re1 C6 110.20(17) . . . . ? Cl1 Pd1 Re1 C6 -52.81(12) . . . . ? P1 Pd1 Re1 C2 34.10(11) . . . . ? Cl2 Pd1 Re1 C2 17.97(17) . . . . ? Cl1 Pd1 Re1 C2 -145.05(11) . . . . ? P1 Pd1 Re1 C1 2.23(10) . . . . ? Cl2 Pd1 Re1 C1 -13.90(16) . . . . ? Cl1 Pd1 Re1 C1 -176.92(10) . . . . ? P1 Pd1 Re1 C3 30.69(14) . . . . ? Cl2 Pd1 Re1 C3 14.55(19) . . . . ? Cl1 Pd1 Re1 C3 -148.46(14) . . . . ? P1 Pd1 Re1 C5 -27.15(10) . . . . ? Cl2 Pd1 Re1 C5 -43.29(16) . . . . ? Cl1 Pd1 Re1 C5 153.70(10) . . . . ? P1 Pd1 Re1 C4 -19.23(15) . . . . ? Cl2 Pd1 Re1 C4 -35.4(2) . . . . ? Cl1 Pd1 Re1 C4 161.62(15) . . . . ? P1 Pd1 Re1 P2 -168.56(5) . . . . ? Cl2 Pd1 Re1 P2 175.31(13) . . . . ? Cl1 Pd1 Re1 P2 12.29(5) . . . . ? C7 Re1 P2 O4 60.3(2) . . . . ? C6 Re1 P2 O4 163.6(2) . . . . ? C2 Re1 P2 O4 -104.0(2) . . . . ? C1 Re1 P2 O4 -57.9(3) . . . . ? C3 Re1 P2 O4 -89.68(19) . . . . ? C5 Re1 P2 O4 -31.7(2) . . . . ? C4 Re1 P2 O4 -53.90(19) . . . . ? Pd1 Re1 P2 O4 104.67(16) . . . . ? C7 Re1 P2 O5 -66.5(2) . . . . ? C6 Re1 P2 O5 36.8(2) . . . . ? C2 Re1 P2 O5 129.2(2) . . . . ? C1 Re1 P2 O5 175.2(2) . . . . ? C3 Re1 P2 O5 143.5(2) . . . . ? C5 Re1 P2 O5 -158.5(2) . . . . ? C4 Re1 P2 O5 179.3(2) . . . . ? Pd1 Re1 P2 O5 -22.16(18) . . . . ? C7 Re1 P2 O3 172.5(2) . . . . ? C6 Re1 P2 O3 -84.19(19) . . . . ? C2 Re1 P2 O3 8.2(2) . . . . ? C1 Re1 P2 O3 54.2(3) . . . . ? C3 Re1 P2 O3 22.48(18) . . . . ? C5 Re1 P2 O3 80.50(19) . . . . ? C4 Re1 P2 O3 58.27(19) . . . . ? Pd1 Re1 P2 O3 -143.17(15) . . . . ? Cl2 Pd1 P1 C1 173.44(14) . . . . ? Cl1 Pd1 P1 C1 13.7(8) . . . . ? Re1 Pd1 P1 C1 -2.86(13) . . . . ? Cl2 Pd1 P1 C11 57.12(14) . . . . ? Cl1 Pd1 P1 C11 -102.6(8) . . . . ? Re1 Pd1 P1 C11 -119.18(14) . . . . ? Cl2 Pd1 P1 C17 -71.88(15) . . . . ? Cl1 Pd1 P1 C17 128.4(8) . . . . ? Re1 Pd1 P1 C17 111.82(15) . . . . ? O4 P2 O3 C8 -167.4(4) . . . . ? O5 P2 O3 C8 -57.2(4) . . . . ? Re1 P2 O3 C8 74.3(4) . . . . ? O5 P2 O4 C9 -56.3(5) . . . . ? O3 P2 O4 C9 46.8(4) . . . . ? Re1 P2 O4 C9 170.1(4) . . . . ? O4 P2 O5 C10 -67.4(4) . . . . ? O3 P2 O5 C10 -170.3(3) . . . . ? Re1 P2 O5 C10 60.4(4) . . . . ? C11 P1 C1 C5 -160.2(3) . . . . ? C17 P1 C1 C5 -44.8(4) . . . . ? Pd1 P1 C1 C5 78.4(3) . . . . ? C11 P1 C1 C2 50.4(4) . . . . ? C17 P1 C1 C2 165.8(3) . . . . ? Pd1 P1 C1 C2 -71.0(3) . . . . ? C11 P1 C1 Re1 124.85(17) . . . . ? C17 P1 C1 Re1 -119.76(17) . . . . ? Pd1 P1 C1 Re1 3.45(16) . . . . ? C7 Re1 C1 C5 -69.6(3) . . . . ? C6 Re1 C1 C5 173.9(2) . . . . ? C2 Re1 C1 C5 115.9(3) . . . . ? C3 Re1 C1 C5 78.7(3) . . . . ? C4 Re1 C1 C5 36.8(2) . . . . ? P2 Re1 C1 C5 41.5(3) . . . . ? Pd1 Re1 C1 C5 -125.6(2) . . . . ? C7 Re1 C1 C2 174.5(2) . . . . ? C6 Re1 C1 C2 58.0(3) . . . . ? C3 Re1 C1 C2 -37.2(2) . . . . ? C5 Re1 C1 C2 -115.9(3) . . . . ? C4 Re1 C1 C2 -79.1(2) . . . . ? P2 Re1 C1 C2 -74.4(3) . . . . ? Pd1 Re1 C1 C2 118.5(2) . . . . ? C7 Re1 C1 P1 53.3(2) . . . . ? C6 Re1 C1 P1 -63.1(2) . . . . ? C2 Re1 C1 P1 -121.2(3) . . . . ? C3 Re1 C1 P1 -158.4(2) . . . . ? C5 Re1 C1 P1 122.9(3) . . . . ? C4 Re1 C1 P1 159.8(2) . . . . ? P2 Re1 C1 P1 164.42(8) . . . . ? Pd1 Re1 C1 P1 -2.71(13) . . . . ? C5 C1 C2 C3 0.5(4) . . . . ? P1 C1 C2 C3 154.5(3) . . . . ? Re1 C1 C2 C3 64.0(3) . . . . ? C5 C1 C2 Re1 -63.4(3) . . . . ? P1 C1 C2 Re1 90.5(3) . . . . ? C7 Re1 C2 C3 -125.7(3) . . . . ? C6 Re1 C2 C3 113.5(3) . . . . ? C1 Re1 C2 C3 -116.2(3) . . . . ? C5 Re1 C2 C3 -78.3(3) . . . . ? C4 Re1 C2 C3 -37.0(2) . . . . ? P2 Re1 C2 C3 24.9(3) . . . . ? Pd1 Re1 C2 C3 -175.6(2) . . . . ? C7 Re1 C2 C1 -9.5(4) . . . . ? C6 Re1 C2 C1 -130.2(2) . . . . ? C3 Re1 C2 C1 116.2(3) . . . . ? C5 Re1 C2 C1 37.9(2) . . . . ? C4 Re1 C2 C1 79.3(2) . . . . ? P2 Re1 C2 C1 141.08(19) . . . . ? Pd1 Re1 C2 C1 -59.4(2) . . . . ? C1 C2 C3 C4 -0.7(4) . . . . ? Re1 C2 C3 C4 62.9(3) . . . . ? C1 C2 C3 Re1 -63.6(3) . . . . ? C7 Re1 C3 C2 117.5(3) . . . . ? C6 Re1 C3 C2 -72.9(3) . . . . ? C1 Re1 C3 C2 38.1(2) . . . . ? C5 Re1 C3 C2 80.5(3) . . . . ? C4 Re1 C3 C2 117.6(4) . . . . ? P2 Re1 C3 C2 -160.3(2) . . . . ? Pd1 Re1 C3 C2 5.8(3) . . . . ? C7 Re1 C3 C4 -0.1(4) . . . . ? C6 Re1 C3 C4 169.5(2) . . . . ? C2 Re1 C3 C4 -117.6(3) . . . . ? C1 Re1 C3 C4 -79.5(2) . . . . ? C5 Re1 C3 C4 -37.1(2) . . . . ? P2 Re1 C3 C4 82.1(2) . . . . ? Pd1 Re1 C3 C4 -111.8(2) . . . . ? C2 C3 C4 C5 0.6(5) . . . . ? Re1 C3 C4 C5 63.3(3) . . . . ? C2 C3 C4 Re1 -62.6(3) . . . . ? C7 Re1 C4 C5 63.2(3) . . . . ? C6 Re1 C4 C5 -133.2(3) . . . . ? C2 Re1 C4 C5 -80.1(2) . . . . ? C1 Re1 C4 C5 -37.6(2) . . . . ? C3 Re1 C4 C5 -116.7(3) . . . . ? P2 Re1 C4 C5 144.8(2) . . . . ? Pd1 Re1 C4 C5 -13.4(3) . . . . ? C7 Re1 C4 C3 180.0(2) . . . . ? C6 Re1 C4 C3 -16.5(4) . . . . ? C2 Re1 C4 C3 36.7(2) . . . . ? C1 Re1 C4 C3 79.1(2) . . . . ? C5 Re1 C4 C3 116.7(3) . . . . ? P2 Re1 C4 C3 -98.5(2) . . . . ? Pd1 Re1 C4 C3 103.3(2) . . . . ? C3 C4 C5 C1 -0.3(4) . . . . ? Re1 C4 C5 C1 62.9(3) . . . . ? C3 C4 C5 Re1 -63.2(3) . . . . ? C2 C1 C5 C4 -0.2(4) . . . . ? P1 C1 C5 C4 -153.6(3) . . . . ? Re1 C1 C5 C4 -63.3(3) . . . . ? C2 C1 C5 Re1 63.1(3) . . . . ? P1 C1 C5 Re1 -90.3(3) . . . . ? C7 Re1 C5 C4 -124.9(3) . . . . ? C6 Re1 C5 C4 105.2(4) . . . . ? C2 Re1 C5 C4 78.9(3) . . . . ? C1 Re1 C5 C4 117.0(3) . . . . ? C3 Re1 C5 C4 37.4(2) . . . . ? P2 Re1 C5 C4 -40.2(3) . . . . ? Pd1 Re1 C5 C4 170.3(2) . . . . ? C7 Re1 C5 C1 118.1(2) . . . . ? C6 Re1 C5 C1 -11.8(4) . . . . ? C2 Re1 C5 C1 -38.0(2) . . . . ? C3 Re1 C5 C1 -79.5(2) . . . . ? C4 Re1 C5 C1 -117.0(3) . . . . ? P2 Re1 C5 C1 -157.20(19) . . . . ? Pd1 Re1 C5 C1 53.3(2) . . . . ? C7 Re1 C6 O1 179(100) . . . . ? C2 Re1 C6 O1 -30(3) . . . . ? C1 Re1 C6 O1 -60(3) . . . . ? C3 Re1 C6 O1 4(3) . . . . ? C5 Re1 C6 O1 -52(3) . . . . ? C4 Re1 C6 O1 14(3) . . . . ? P2 Re1 C6 O1 97(3) . . . . ? Pd1 Re1 C6 O1 -124(3) . . . . ? C6 Re1 C7 O2 -156(3) . . . . ? C2 Re1 C7 O2 86(3) . . . . ? C1 Re1 C7 O2 80(3) . . . . ? C3 Re1 C7 O2 14(3) . . . . ? C5 Re1 C7 O2 45(3) . . . . ? C4 Re1 C7 O2 14(3) . . . . ? P2 Re1 C7 O2 -71(3) . . . . ? Pd1 Re1 C7 O2 143(3) . . . . ? C1 P1 C11 C16 -101.6(3) . . . . ? C17 P1 C11 C16 146.4(3) . . . . ? Pd1 P1 C11 C16 13.7(4) . . . . ? C1 P1 C11 C12 78.6(4) . . . . ? C17 P1 C11 C12 -33.4(4) . . . . ? Pd1 P1 C11 C12 -166.1(3) . . . . ? C16 C11 C12 C13 -0.7(6) . . . . ? P1 C11 C12 C13 179.1(3) . . . . ? C11 C12 C13 C14 -0.1(6) . . . . ? C12 C13 C14 C15 1.3(7) . . . . ? C13 C14 C15 C16 -1.7(6) . . . . ? C12 C11 C16 C15 0.3(6) . . . . ? P1 C11 C16 C15 -179.5(3) . . . . ? C14 C15 C16 C11 0.9(6) . . . . ? C1 P1 C17 C22 -38.5(4) . . . . ? C11 P1 C17 C22 75.1(4) . . . . ? Pd1 P1 C17 C22 -153.6(3) . . . . ? C1 P1 C17 C18 143.8(3) . . . . ? C11 P1 C17 C18 -102.6(3) . . . . ? Pd1 P1 C17 C18 28.8(4) . . . . ? C22 C17 C18 C19 0.5(6) . . . . ? P1 C17 C18 C19 178.3(3) . . . . ? C17 C18 C19 C20 -1.4(6) . . . . ? C18 C19 C20 C21 1.6(6) . . . . ? C19 C20 C21 C22 -1.0(6) . . . . ? C20 C21 C22 C17 0.1(6) . . . . ? C18 C17 C22 C21 0.1(6) . . . . ? P1 C17 C22 C21 -177.6(3) . . . . ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 3.535 _refine_diff_density_min -1.065 _refine_diff_density_rms 0.173