# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1457 #======================================================================= data_global #======================================================================= _audit_creation_date 14-01-99 # 1. SUBMISSION DETAILS _publ_contact_author_name # Name of author for correspondance ;Prof. Jean Fischer ; _publ_contact_author_address # Address of author for correspondance ;Laboratoire de Cristallochimie et de Chimie Structurale Universite Louis Pasteur 4, rue Blaise Pascal 67070 Strasbourg cedex France ; _publ_contact_author_phone '+33 (0)3 88 41 60 58' _publ_contact_author_fax '+33 (0)3 88 41 53 63' _publ_contact_author_email fischer@chimie.u-strasbg.fr _publ_requested_journal 'Dalton' _publ_contact_letter ; ; _publ_requested_category FM #======================================================================= # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #======================================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; Heterobimetallic Alkoxysilyl Cationuc Complexes: Insvestigation into the Displacement of a mu2-eta2-Si-O-Bridge by Functional Phosphine Ligands ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Blin Joel' ;Laboratoire de Chimie de Coordination Universite Louis Pasteur 4, rue Blaise Pascal 67070 Strasbourg cedex France ; 'Braunstein Pierre' ;Laboratoire de Chimie de Coordination Universite Louis Pasteur 4, rue Blaise Pascal 67070 Strasbourg cedex France ; 'Fischer Jean' ;Laboratoire de Cristallochimie et de Chimie Structurale Universite Louis Pasteur 4, rue Blaise Pascal 67070 Strasbourg cedex France ; 'Kickelbick Guido' ;Institut fur Anorganische Chemie Technische Hochschule Wien Getreidemarkt 9/153 1060 Wien Austria ; 'Knorr Michael' ;Laboratoire de Chimie de Coordination Universite Louis Pasteur 4, rue Blaise Pascal 67070 Strasbourg cedex France ; 'Morise Xavier' ;Laboratoire de Chimie de Coordination Universite Louis Pasteur 4, rue Blaise Pascal 67070 Strasbourg cedex France ; 'Wirth Tobias' ;Laboratoire de Chimie de Coordination Universite Louis Pasteur 4, rue Blaise Pascal 67070 Strasbourg cedex France ; # 4. TEXT _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_exptl_prep ; ? ; _publ_section_exptl_refinement ; ? ; _publ_section_references ; Burla, M.C., Camalli, M., Cascarano, G.,Giacovazzo, C., Polidori, G., Spagna, R. &Viterbo, D. (1989). SIR. J. Appl. Cryst. 22, 389-393. OpenMoleN, Interactive Intelligent Structure solution (1997) Nonius B.V., Delft, The Netherlands. North, A.C.T., Phillips, D.C., Mathews, F.S. (1968). Acta Cryst., A24, 351-359. ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ? ; #======================================================================= # If more than one structure is reported, sections 5-10 should be filled in # per structure. For each data set, replace the ? in the data_? line below # by a unique identifier. data_st17 #======================================================================= # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C51 H47 Cl F6 O P4 Pd' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C51 H47 Cl F6 O P4 Pd' _chemical_formula_weight 1055.68 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1 H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1 Cl ? 0.132 0.159 International_Tables_Vol_IV_Table_2.3.1 F ? 0.014 0.010 International_Tables_Vol_IV_Table_2.3.1 O ? 0.008 0.006 International_Tables_Vol_IV_Table_2.3.1 P ? 0.090 0.095 International_Tables_Vol_IV_Table_2.3.1 Pd ? -1.177 1.007 International_Tables_Vol_IV_Table_2.3.1 #======================================================================= # 6. CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' -x,1/2+y,1/2-z -x,-y,-z +x,1/2-y,1/2+z _cell_length_a 11.500(3) _cell_length_b 20.814(6) _cell_length_c 21.055(6) _cell_angle_alpha 90 _cell_angle_beta 97.92(2) _cell_angle_gamma 90 _cell_volume 4991(4) _cell_formula_units_Z 4 _cell_measurement_temperature 294 _cell_measurement_reflns_used 24 _cell_measurement_theta_min 18.0 _cell_measurement_theta_max 19.5 _cell_special_details ; ? ; _exptl_crystal_description prism _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.40 _exptl_crystal_density_method 'none' _exptl_crystal_F_000 2152 _exptl_absorpt_coefficient_mu 0.612 _exptl_absorpt_correction_type psi_scan_(North,_Phillips,_Mathews,_1968) _exptl_absorpt_correction_T_min 0.9752 _exptl_absorpt_correction_T_max 1.0000 #======================================================================= # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 294 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Enraf_Nonius_CAD4 _diffrn_measurement_method \q/2\q _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 1 1 6 2 1 2 3 1 2 _diffrn_reflns_number 15846 _diffrn_reflns_av_R_equivalents 0.017 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 30.41 _reflns_number_total 15568 _reflns_number_gt 8137 _reflns_threshold_expression >3.0\s(I) _computing_data_collection 'CAD4_(Enraf-Nonius,_1994)' _computing_cell_refinement CAD4_(Enraf-Nonius,_1994) _computing_data_reduction 'process_OpenMoleN_(_1997)' _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement LSFM_OpenMoleN_(_1997) _computing_molecular_graphics ? _computing_publication_material CIFGEN_IN_OpenMoleN_(_1997) #======================================================================= # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme '4Fo^2^/(\s^2^(Fo^2^) + 0.0064 Fo^4^)' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 8137 _refine_ls_number_parameters 542 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.127 _refine_ls_R_factor_gt 0.051 _refine_ls_wR_factor_all 0.139 _refine_ls_wR_factor_ref 0.080 _refine_ls_goodness_of_fit_all 2.681 _refine_ls_goodness_of_fit_ref 1.528 _refine_ls_shift/su_max 0.018 _refine_ls_shift/esd_mean 0.001 _refine_diff_density_max 1.257 _refine_diff_density_min -0.138 #======================================================================= # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol PD 0.13343(3) 0.24595(1) 0.43553(1) 0.0403(1) Uani ? ? Pd CL -0.0157(1) 0.21605(6) 0.49433(7) 0.0758(6) Uani ? ? Cl P1 0.16619(9) 0.14255(5) 0.40672(5) 0.0439(5) Uani ? ? P C1 0.2266(5) 0.0879(2) 0.4697(2) 0.063(3) Uani ? ? C C2 0.1513(7) 0.0505(4) 0.4990(3) 0.103(5) Uani ? ? C C3 0.1929(9) 0.0128(4) 0.5500(4) 0.131(6) Uani ? ? C C4 0.3118(9) 0.0100(5) 0.5688(4) 0.143(7) Uani ? ? C C5 0.3817(8) 0.0449(6) 0.5422(5) 0.159(7) Uani ? ? C C6 0.3415(6) 0.0837(5) 0.4912(4) 0.123(6) Uani ? ? C C7 0.0485(4) 0.1007(2) 0.3579(2) 0.050(2) Uani ? ? C C8 -0.0646(4) 0.1248(3) 0.3494(3) 0.067(3) Uani ? ? C C9 -0.1515(5) 0.0920(3) 0.3108(3) 0.085(4) Uani ? ? C C10 -0.1288(6) 0.0376(3) 0.2818(3) 0.091(4) Uani ? ? C C11 -0.0172(6) 0.0128(3) 0.2891(3) 0.098(4) Uani ? ? C C12 0.0714(5) 0.0454(3) 0.3266(3) 0.076(3) Uani ? ? C C13 0.2759(4) 0.1630(2) 0.3545(2) 0.058(2) Uani ? ? C P2 0.27890(9) 0.24946(5) 0.37344(6) 0.0490(5) Uani ? ? P C14 0.4273(4) 0.2658(3) 0.4101(3) 0.062(3) Uani ? ? C C15 0.4474(4) 0.3061(3) 0.4619(3) 0.067(3) Uani ? ? C C16 0.5630(5) 0.3164(3) 0.4910(3) 0.091(4) Uani ? ? C C17 0.6504(5) 0.2847(4) 0.4706(4) 0.100(5) Uani ? ? C C18 0.6346(5) 0.2470(4) 0.4167(5) 0.112(5) Uani ? ? C C19 0.5193(5) 0.2365(3) 0.3875(4) 0.094(4) Uani ? ? C C20 0.2488(4) 0.2928(2) 0.2989(2) 0.060(2) Uani ? ? C C21 0.3325(5) 0.3323(3) 0.2758(3) 0.085(3) Uani ? ? C C22 0.2995(7) 0.3678(3) 0.2191(3) 0.107(4) Uani ? ? C C23 0.1906(9) 0.3632(4) 0.1866(4) 0.115(6) Uani ? ? C C24 0.1077(8) 0.3241(4) 0.2095(4) 0.114(5) Uani ? ? C C25 0.1383(6) 0.2886(3) 0.2651(3) 0.079(4) Uani ? ? C P3 0.09313(9) 0.35543(5) 0.45498(5) 0.0410(5) Uani ? ? P C26 0.2001(3) 0.4180(2) 0.4472(2) 0.044(2) Uani ? ? C C27 0.2311(4) 0.4304(2) 0.3863(2) 0.055(2) Uani ? ? C C28 0.3151(4) 0.4756(3) 0.3779(3) 0.067(3) Uani ? ? C C29 0.3672(5) 0.5103(3) 0.4293(3) 0.077(3) Uani ? ? C C30 0.3352(5) 0.5002(3) 0.4897(3) 0.079(3) Uani ? ? C C31 0.2529(4) 0.4537(2) 0.4982(2) 0.060(3) Uani ? ? C C32 -0.0345(4) 0.3814(2) 0.4008(2) 0.049(2) Uani ? ? C C33 -0.1017(5) 0.3356(3) 0.3657(3) 0.083(4) Uani ? ? C C34 -0.1952(7) 0.3548(4) 0.3208(4) 0.118(5) Uani ? ? C C35 -0.2269(6) 0.4188(3) 0.3161(4) 0.099(4) Uani ? ? C C36 -0.1599(5) 0.4638(3) 0.3504(3) 0.078(3) Uani ? ? C C37 -0.0650(5) 0.4455(2) 0.3922(3) 0.062(3) Uani ? ? C C38 0.0595(4) 0.3633(2) 0.5363(2) 0.046(2) Uani ? ? C C39 0.1420(4) 0.3393(2) 0.5853(2) 0.058(2) Uani ? ? C C40 0.1192(6) 0.3413(3) 0.6473(3) 0.076(3) Uani ? ? C C41 0.0173(6) 0.3672(3) 0.6621(3) 0.087(4) Uani ? ? C C42 -0.0644(5) 0.3913(3) 0.6143(3) 0.091(3) Uani ? ? C C43 -0.0445(4) 0.3898(2) 0.5514(2) 0.062(3) Uani ? ? C O1 0.2394(3) 0.3137(2) 0.5659(2) 0.065(2) Uani ? ? O C44 0.3200(7) 0.2803(4) 0.6100(4) 0.116(5) Uani ? ? C P 0.4698(1) 0.06462(8) 0.24856(8) 0.0750(8) Uani ? ? P F1 0.4299(4) 0.1382(2) 0.2450(2) 0.110(3) Uani ? ? F F2 0.3451(4) 0.0491(2) 0.2658(2) 0.146(3) Uani ? ? F F3 0.5881(3) 0.0840(3) 0.2263(3) 0.159(3) Uani ? ? F F4 0.4222(4) 0.0538(3) 0.1779(2) 0.153(4) Uani ? ? F F5 0.5170(5) 0.0804(3) 0.3191(2) 0.151(4) Uani ? ? F F6 0.5097(5) -0.0050(2) 0.2511(3) 0.195(4) Uani ? ? F C45 0.7266(5) 0.1626(3) 0.6212(2) 0.245(7) Uiso ? ? C C46 0.7819(5) 0.2194(3) 0.6260(2) 0.155(4) Uiso ? ? C C47 0.7389(5) 0.2646(3) 0.6617(2) 0.221(6) Uiso ? ? C C48 0.6451(5) 0.2543(3) 0.6947(2) 0.190(6) Uiso ? ? C C49 0.5895(5) 0.1949(3) 0.6888(2) 0.235(7) Uiso ? ? C C50 0.6302(5) 0.1490(3) 0.6520(2) 0.211(6) Uiso ? ? C C51 0.7711(5) 0.1112(3) 0.5807(2) 0.260(7) Uiso ? ? C H1 0.0697 0.0510 0.4837 0.1388 Uiso calc C2 H H2 0.1406 -0.0111 0.5721 0.1820 Uiso calc C3 H H3 0.3424 -0.0185 0.6022 0.2057 Uiso calc C4 H H4 0.4632 0.0442 0.5578 0.2220 Uiso calc C5 H H5 0.3958 0.1080 0.4709 0.1741 Uiso calc C6 H H6 -0.0823 0.1635 0.3699 0.0898 Uiso calc C8 H H7 -0.2292 0.1086 0.3048 0.1144 Uiso calc C9 H H8 -0.1904 0.0157 0.2557 0.1242 Uiso calc C10 H H9 -0.0012 -0.0263 0.2687 0.1316 Uiso calc C11 H H10 0.1494 0.0294 0.3307 0.0988 Uiso calc C12 H H11 0.2498 0.1543 0.3105 0.0744 Uiso calc C13 H H12 0.3493 0.1425 0.3670 0.0744 Uiso calc C13 H H13 0.3837 0.3267 0.4779 0.0897 Uiso calc C15 H H14 0.5785 0.3461 0.5254 0.1254 Uiso calc C16 H H15 0.7268 0.2881 0.4941 0.1525 Uiso calc C17 H H16 0.6995 0.2288 0.3998 0.1731 Uiso calc C18 H H17 0.5051 0.2086 0.3516 0.1345 Uiso calc C19 H H18 0.4101 0.3350 0.2979 0.1071 Uiso calc C21 H H19 0.3551 0.3955 0.2037 0.1413 Uiso calc C22 H H20 0.1704 0.3866 0.1479 0.1577 Uiso calc C23 H H21 0.0302 0.3216 0.1871 0.1557 Uiso calc C24 H H22 0.0819 0.2611 0.2799 0.1032 Uiso calc C25 H H23 0.1937 0.4072 0.3503 0.0718 Uiso calc C27 H H24 0.3367 0.4827 0.3365 0.0869 Uiso calc C28 H H25 0.4254 0.5414 0.4236 0.1011 Uiso calc C29 H H26 0.3698 0.5252 0.5252 0.1041 Uiso calc C30 H H27 0.2326 0.4463 0.5398 0.0779 Uiso calc C31 H H28 -0.0844 0.2913 0.3722 0.1175 Uiso calc C33 H H29 -0.2371 0.3240 0.2933 0.1683 Uiso calc C34 H H30 -0.2959 0.4314 0.2887 0.1373 Uiso calc C35 H H31 -0.1793 0.5080 0.3452 0.1042 Uiso calc C36 H H32 -0.0186 0.4773 0.4161 0.0838 Uiso calc C37 H H33 0.1751 0.3245 0.6805 0.1053 Uiso calc C40 H H34 0.0029 0.3686 0.7054 0.1158 Uiso calc C41 H H35 -0.1353 0.4092 0.6248 0.1137 Uiso calc C42 H H36 -0.1012 0.4066 0.5185 0.0789 Uiso calc C43 H H37 0.3831 0.2654 0.5891 0.1573 Uiso calc C44 H H38 0.3495 0.3081 0.6442 0.1573 Uiso calc C44 H H39 0.2820 0.2446 0.6264 0.1573 Uiso calc C44 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol PD 0.0385(1) 0.0370(1) 0.0460(1) -0.0024(1) 0.0118(1) -0.0044(1) Pd CL 0.0774(6) 0.0597(7) 0.0941(7) -0.0116(5) 0.0516(5) -0.0047(6) Cl P1 0.0435(5) 0.0407(5) 0.0478(5) -0.0012(4) 0.0060(4) -0.0050(5) P C1 0.071(3) 0.063(3) 0.056(3) 0.019(2) -0.004(2) -0.010(2) C C2 0.114(5) 0.126(5) 0.077(4) 0.003(4) 0.000(4) 0.045(3) C C3 0.198(9) 0.134(6) 0.084(4) 0.014(6) 0.004(5) 0.049(4) C C4 0.191(7) 0.193(8) 0.080(5) 0.090(6) -0.019(5) 0.017(5) C C5 0.113(6) 0.24(1) 0.150(7) 0.047(6) -0.022(5) 0.069(7) C C6 0.079(4) 0.183(8) 0.128(6) 0.029(5) -0.026(4) 0.035(6) C C7 0.054(2) 0.049(2) 0.047(2) -0.011(2) 0.002(2) 0.003(2) C C8 0.060(3) 0.069(3) 0.073(3) -0.010(2) -0.010(3) 0.006(3) C C9 0.066(3) 0.105(4) 0.088(4) -0.031(3) -0.009(3) 0.013(3) C C10 0.100(4) 0.119(4) 0.064(3) -0.060(3) -0.001(3) -0.005(3) C C11 0.136(5) 0.100(4) 0.069(3) -0.060(3) 0.020(3) -0.027(3) C C12 0.081(3) 0.067(3) 0.081(3) -0.016(3) 0.011(3) -0.020(3) C C13 0.055(2) 0.054(2) 0.067(2) -0.007(2) 0.022(2) -0.018(2) C P2 0.0428(5) 0.0516(6) 0.0532(5) -0.0088(5) 0.0156(4) -0.0122(5) P C14 0.047(2) 0.068(3) 0.075(3) -0.013(2) 0.015(2) -0.015(2) C C15 0.055(3) 0.071(3) 0.078(3) -0.004(2) 0.000(2) -0.019(3) C C16 0.064(3) 0.101(4) 0.116(5) -0.015(3) -0.018(3) -0.036(4) C C17 0.043(3) 0.143(6) 0.162(7) -0.015(4) 0.001(4) -0.036(6) C C18 0.045(3) 0.148(6) 0.208(7) -0.014(3) 0.022(4) -0.083(5) C C19 0.046(2) 0.131(5) 0.138(5) -0.013(3) 0.028(3) -0.061(4) C C20 0.072(3) 0.053(2) 0.056(2) -0.004(2) 0.023(2) -0.010(2) C C21 0.097(4) 0.078(4) 0.081(3) -0.006(3) 0.041(3) 0.000(3) C C22 0.165(5) 0.070(4) 0.105(4) -0.008(4) 0.069(3) 0.015(3) C C23 0.184(7) 0.093(5) 0.087(5) 0.020(5) 0.022(5) 0.013(4) C C24 0.141(6) 0.132(6) 0.080(4) 0.019(5) -0.009(5) 0.005(5) C C25 0.090(4) 0.075(4) 0.072(3) -0.002(3) 0.007(3) 0.003(3) C P3 0.0431(5) 0.0376(5) 0.0425(5) 0.0006(4) 0.0086(4) -0.0023(4) P C26 0.042(2) 0.039(2) 0.051(2) 0.000(2) 0.007(2) -0.002(2) C C27 0.062(2) 0.052(2) 0.053(2) -0.005(2) 0.009(2) 0.000(2) C C28 0.061(3) 0.068(3) 0.073(3) -0.013(2) 0.016(2) 0.012(3) C C29 0.067(3) 0.067(3) 0.101(4) -0.021(2) 0.015(3) 0.009(3) C C30 0.078(3) 0.073(3) 0.086(4) -0.024(3) -0.002(3) -0.017(3) C C31 0.063(3) 0.059(3) 0.059(3) -0.008(2) 0.010(2) -0.006(2) C C32 0.048(2) 0.048(2) 0.052(2) -0.002(2) 0.005(2) 0.005(2) C C33 0.081(3) 0.060(3) 0.116(5) 0.002(3) -0.038(3) -0.004(3) C C34 0.118(5) 0.087(5) 0.158(6) 0.003(4) -0.072(4) -0.009(5) C C35 0.084(4) 0.092(4) 0.126(5) 0.011(3) -0.040(4) 0.020(4) C C36 0.083(3) 0.065(3) 0.088(4) 0.025(3) 0.000(3) 0.012(3) C C37 0.070(3) 0.050(2) 0.069(3) 0.008(2) -0.006(3) -0.003(2) C C38 0.056(2) 0.042(2) 0.040(2) -0.000(2) 0.013(2) -0.003(2) C C39 0.074(3) 0.054(2) 0.048(2) -0.001(2) 0.015(2) -0.003(2) C C40 0.116(4) 0.082(4) 0.046(3) 0.007(4) 0.014(3) 0.006(3) C C41 0.126(4) 0.094(4) 0.055(3) 0.013(4) 0.040(3) -0.004(3) C C42 0.111(3) 0.071(3) 0.095(3) 0.015(3) 0.064(2) -0.007(3) C C43 0.069(3) 0.049(2) 0.069(3) 0.003(2) 0.027(2) -0.005(2) C O1 0.068(2) 0.082(2) 0.049(2) 0.019(2) 0.004(2) 0.008(2) O C44 0.121(5) 0.146(6) 0.088(4) 0.055(4) -0.013(4) 0.025(4) C P 0.0545(7) 0.0875(9) 0.0883(9) 0.0034(7) 0.0131(7) -0.0333(7) P F1 0.132(3) 0.099(3) 0.101(2) 0.010(2) 0.039(2) 0.001(2) F F2 0.124(2) 0.115(3) 0.220(4) -0.032(2) 0.101(2) -0.065(3) F F3 0.076(2) 0.192(4) 0.276(5) -0.040(3) 0.071(2) -0.119(3) F F4 0.136(4) 0.260(5) 0.101(3) -0.031(4) 0.013(3) -0.086(3) F F5 0.188(4) 0.182(4) 0.100(3) 0.085(3) -0.035(3) -0.035(3) F F6 0.265(5) 0.115(3) 0.243(5) 0.091(3) 0.122(3) -0.007(3) F # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag PD CL 2.333(1) . . ? PD P1 2.281(1) . . ? PD P2 2.262(1) . . ? PD P3 2.372(1) . . ? P1 C1 1.812(6) . . ? P1 C7 1.806(5) . . ? P1 C13 1.834(5) . . ? C1 C2 1.37(1) . . ? C1 C6 1.339(9) . . ? C2 C3 1.36(1) . . ? C3 C4 1.37(2) . . ? C4 C5 1.27(2) . . ? C5 C6 1.37(1) . . ? C7 C8 1.383(7) . . ? C7 C12 1.369(7) . . ? C8 C9 1.379(8) . . ? C9 C10 1.33(1) . . ? C10 C11 1.37(1) . . ? C11 C12 1.379(9) . . ? C13 P2 1.843(5) . . ? P2 C14 1.805(5) . . ? P2 C20 1.802(6) . . ? C14 C15 1.370(7) . . ? C14 C19 1.362(8) . . ? C15 C16 1.402(8) . . ? C16 C17 1.32(1) . . ? C17 C18 1.37(1) . . ? C18 C19 1.40(1) . . ? C20 C21 1.402(8) . . ? C20 C25 1.371(8) . . ? C21 C22 1.41(1) . . ? C22 C23 1.35(1) . . ? C23 C24 1.39(1) . . ? C24 C25 1.39(1) . . ? P3 C26 1.813(4) . . ? P3 C32 1.813(5) . . ? P3 C38 1.814(4) . . ? C26 C27 1.402(7) . . ? C26 C31 1.377(7) . . ? C27 C28 1.377(7) . . ? C28 C29 1.369(8) . . ? C29 C30 1.388(9) . . ? C30 C31 1.383(8) . . ? C32 C33 1.376(7) . . ? C32 C37 1.385(7) . . ? C33 C34 1.390(9) . . ? C34 C35 1.38(1) . . ? C35 C36 1.36(1) . . ? C36 C37 1.360(8) . . ? C38 C39 1.395(7) . . ? C38 C43 1.393(7) . . ? C39 C40 1.366(7) . . ? C39 O1 1.353(6) . . ? C40 C41 1.365(9) . . ? C41 C42 1.37(1) . . ? C42 C43 1.376(8) . . ? O1 C44 1.403(7) . . ? P F1 1.597(5) . . ? P F2 1.560(5) . . ? P F3 1.553(5) . . ? P F4 1.529(5) . . ? P F5 1.545(5) . . ? P F6 1.519(5) . . ? F1 F2 2.167(6) . . ? F1 F5 2.109(7) . . ? F2 F4 2.161(7) . . ? F3 F4 2.131(7) . . ? F3 F6 2.157(9) . . ? F4 F6 2.111(9) . . ? C45 C46 1.340(7) . . ? C45 C50 1.388(8) . . ? C45 C51 1.500(8) . . ? C46 C47 1.3399 . . ? C47 C48 1.3784 . . ? C48 C49 1.3881 . . ? C49 C50 1.3547 . . ? 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag CL PD P1 92.86(5) . . . ? CL PD P2 166.26(5) . . . ? CL PD P3 89.38(5) . . . ? P1 PD P2 73.40(4) . . . ? P1 PD P3 174.52(4) . . . ? P2 PD P3 104.26(4) . . . ? C1 P1 C7 107.1(2) . . . ? C1 P1 C13 111.0(3) . . . ? C7 P1 C13 107.1(2) . . . ? P1 C1 C2 118.9(5) . . . ? P1 C1 C6 123.3(6) . . . ? C2 C1 C6 117.8(7) . . . ? C1 C2 C3 120.4(8) . . . ? C2 C3 C4 118(1) . . . ? C3 C4 C5 121(1) . . . ? C4 C5 C6 121(1) . . . ? C1 C6 C5 120(1) . . . ? P1 C7 C8 121.1(4) . . . ? P1 C7 C12 120.1(4) . . . ? C8 C7 C12 118.8(5) . . . ? C7 C8 C9 119.3(6) . . . ? C8 C9 C10 121.3(7) . . . ? C9 C10 C11 120.6(6) . . . ? C10 C11 C12 119.0(7) . . . ? C7 C12 C11 120.9(7) . . . ? P1 C13 P2 95.2(2) . . . ? C13 P2 C14 105.3(2) . . . ? C13 P2 C20 107.7(2) . . . ? C14 P2 C20 109.6(3) . . . ? P2 C14 C15 120.1(4) . . . ? P2 C14 C19 120.1(5) . . . ? C15 C14 C19 119.8(5) . . . ? C14 C15 C16 119.2(6) . . . ? C15 C16 C17 119.9(7) . . . ? C16 C17 C18 122.3(7) . . . ? C17 C18 C19 117.6(7) . . . ? C14 C19 C18 120.7(7) . . . ? P2 C20 C21 122.5(5) . . . ? P2 C20 C25 118.2(4) . . . ? C21 C20 C25 119.2(6) . . . ? C20 C21 C22 119.0(7) . . . ? C21 C22 C23 121.0(8) . . . ? C22 C23 C24 120.1(8) . . . ? C23 C24 C25 119.9(8) . . . ? C20 C25 C24 120.9(7) . . . ? C26 P3 C32 103.3(2) . . . ? C26 P3 C38 104.8(2) . . . ? C32 P3 C38 107.9(2) . . . ? P3 C26 C27 118.4(3) . . . ? P3 C26 C31 123.4(4) . . . ? C27 C26 C31 118.2(4) . . . ? C26 C27 C28 121.1(5) . . . ? C27 C28 C29 119.8(5) . . . ? C28 C29 C30 120.2(5) . . . ? C29 C30 C31 119.7(5) . . . ? C26 C31 C30 121.0(5) . . . ? P3 C32 C33 118.5(4) . . . ? P3 C32 C37 122.5(4) . . . ? C33 C32 C37 118.9(5) . . . ? C32 C33 C34 119.4(6) . . . ? C33 C34 C35 119.9(7) . . . ? C34 C35 C36 120.1(6) . . . ? C35 C36 C37 119.9(6) . . . ? C32 C37 C36 121.4(5) . . . ? P3 C38 C39 117.0(3) . . . ? P3 C38 C43 123.5(4) . . . ? C39 C38 C43 119.4(4) . . . ? C38 C39 C40 119.7(5) . . . ? C38 C39 O1 115.1(4) . . . ? C40 C39 O1 125.2(5) . . . ? C39 C40 C41 121.0(6) . . . ? C40 C41 C42 119.9(5) . . . ? C41 C42 C43 120.6(6) . . . ? C38 C43 C42 119.4(6) . . . ? C39 O1 C44 119.6(5) . . . ? F1 P F2 86.7(3) . . . ? F1 P F3 89.7(3) . . . ? F1 P F4 91.9(3) . . . ? F1 P F5 84.3(3) . . . ? F1 P F6 178.8(3) . . . ? F2 P F3 174.7(4) . . . ? F2 P F4 88.8(3) . . . ? F2 P F5 91.9(4) . . . ? F2 P F6 94.4(3) . . . ? F3 P F4 87.5(3) . . . ? F3 P F5 91.6(4) . . . ? F3 P F6 89.2(4) . . . ? F4 P F5 176.2(4) . . . ? F4 P F6 87.7(4) . . . ? F5 P F6 96.0(4) . . . ? P F1 F2 45.9(2) . . . ? P F1 F5 46.8(2) . . . ? F2 F1 F5 62.9(3) . . . ? P F2 F1 47.4(2) . . . ? P F2 F4 45.0(2) . . . ? F1 F2 F4 62.6(2) . . . ? P F3 F4 45.8(2) . . . ? P F3 F6 44.8(2) . . . ? F4 F3 F6 59.0(3) . . . ? P F4 F2 46.2(2) . . . ? P F4 F3 46.7(2) . . . ? P F4 F6 46.0(2) . . . ? F2 F4 F3 92.9(3) . . . ? F2 F4 F6 63.8(3) . . . ? F3 F4 F6 61.1(3) . . . ? P F5 F1 48.9(2) . . . ? P F6 F3 46.0(2) . . . ? P F6 F4 46.4(2) . . . ? F3 F6 F4 59.9(3) . . . ? C46 C45 C50 123.1(6) . . . ? C46 C45 C51 118.5(6) . . . ? C50 C45 C51 118.5(5) . . . ? C45 C46 C47 117.0(3) . . . ? C46 C47 C48 123.23 . . . ? C47 C48 C49 118.46 . . . ? C48 C49 C50 119.19 . . . ? C45 C50 C49 119.0(3) . . . ? #======================================================================= data_st18 #======================================================================= # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C54 H54 Cl8 O3 P4 Pd2' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C54 H54 Cl8 O3 P4 Pd2' _chemical_formula_weight 1371.35 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1 H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1 Cl ? 0.132 0.159 International_Tables_Vol_IV_Table_2.3.1 O ? 0.008 0.006 International_Tables_Vol_IV_Table_2.3.1 P ? 0.090 0.095 International_Tables_Vol_IV_Table_2.3.1 Pd ? -1.177 1.007 International_Tables_Vol_IV_Table_2.3.1 #======================================================================= # 6. CRYSTAL DATA _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 41' _symmetry_space_group_name_Hall ' P 4w' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' -x,-y,1/2+z -y,+x,1/4+z +y,-x,3/4+z _cell_length_a 21.171(6) _cell_length_b 21.171(6) _cell_length_c 14.309(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 6413(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173 _cell_measurement_reflns_used 24 _cell_measurement_theta_min 18.0 _cell_measurement_theta_max 19.5 _cell_special_details ; ? ; _exptl_crystal_description prism _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.59 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.42 _exptl_crystal_density_method 'none' _exptl_crystal_F_000 2760 _exptl_absorpt_coefficient_mu 1.031 _exptl_absorpt_correction_type psi_scan_(North,_Phillips,_Mathews,_1968) _exptl_absorpt_correction_T_min 0.8930 _exptl_absorpt_correction_T_max 1.0000 #======================================================================= # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Enraf_Nonius_CAD4 _diffrn_measurement_method \q/2\q _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 1 1 -2 2 3 -4 3 1 -1 _diffrn_reflns_number 9185 _diffrn_reflns_av_R_equivalents 0.022 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 29.98 _reflns_number_total 8052 _reflns_number_gt 7145 _reflns_threshold_expression >3.0\s(I) _computing_data_collection 'CAD4_(Enraf-Nonius,_1994)' _computing_cell_refinement CAD4_(Enraf-Nonius,_1994) _computing_data_reduction 'process_OpenMoleN_(_1997)' _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement LSFM_OpenMoleN_(_1997) _computing_molecular_graphics ? _computing_publication_material CIFGEN_IN_OpenMoleN_(_1997) #======================================================================= # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme '4Fo^2^/(\s^2^(Fo^2^) + 0.0064 Fo^4^)' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack -0.19(2) _refine_ls_number_reflns 7145 _refine_ls_number_parameters 639 _refine_ls_number_restraints 1 _refine_ls_number_constraints 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_R_factor_all 0.046 _refine_ls_R_factor_gt 0.036 _refine_ls_wR_factor_all 0.073 _refine_ls_wR_factor_ref 0.054 _refine_ls_goodness_of_fit_all 1.607 _refine_ls_goodness_of_fit_ref 1.181 _refine_ls_shift/su_max 0.008 _refine_ls_shift/esd_mean 0.000 _refine_diff_density_max 1.189 _refine_diff_density_min -0.266 #======================================================================= # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol PD1 0.28237(2) -0.01420(2) 0.2947 0.0187(1) Uani ? ? Pd PD2 0.38812(2) 0.06542(2) 0.40115(3) 0.0189(1) Uani ? ? Pd CL1 0.21953(6) -0.11090(6) 0.2844(1) 0.0305(6) Uani ? ? Cl CL2 0.45754(6) 0.06883(8) 0.53606(9) 0.0322(6) Uani ? ? Cl C1 0.3325(2) 0.0643(2) 0.2903(3) 0.020(2) Uani ? ? C O1 0.3299(2) 0.1024(2) 0.2304(3) 0.031(2) Uani ? ? O P1 0.36603(6) -0.06188(6) 0.21437(9) 0.0205(5) Uani ? ? P C2 0.3458(2) -0.0876(3) 0.0969(3) 0.025(2) Uani ? ? C C3 0.3191(3) -0.1473(3) 0.0835(4) 0.039(3) Uani ? ? C C4 0.3003(4) -0.1662(4) -0.0033(5) 0.048(3) Uani ? ? C C5 0.3072(3) -0.1261(4) -0.0793(5) 0.044(3) Uani ? ? C C6 0.3328(3) -0.0681(4) -0.0665(5) 0.046(3) Uani ? ? C C7 0.3517(3) -0.0482(3) 0.0209(4) 0.040(3) Uani ? ? C C8 0.3999(2) -0.1307(2) 0.2701(4) 0.025(2) Uani ? ? C C9 0.3760(3) -0.1527(3) 0.3554(4) 0.031(2) Uani ? ? C C10 0.4045(3) -0.2040(3) 0.3988(5) 0.039(3) Uani ? ? C C11 0.4560(3) -0.2330(3) 0.3592(6) 0.044(3) Uani ? ? C C12 0.4790(3) -0.2117(3) 0.2768(6) 0.047(3) Uani ? ? C C13 0.4511(3) -0.1616(3) 0.2300(5) 0.038(3) Uani ? ? C C14 0.4346(2) -0.0101(3) 0.1956(3) 0.023(2) Uani ? ? C P2 0.46611(6) 0.02441(6) 0.30303(9) 0.0202(5) Uani ? ? P C15 0.5175(2) 0.0876(3) 0.2613(4) 0.025(2) Uani ? ? C C16 0.5293(3) 0.1387(3) 0.3221(5) 0.042(3) Uani ? ? C C17 0.5684(4) 0.1868(3) 0.2923(6) 0.050(4) Uani ? ? C C18 0.5948(3) 0.1859(3) 0.2027(6) 0.049(3) Uani ? ? C C19 0.5825(3) 0.1367(3) 0.1438(5) 0.046(3) Uani ? ? C C20 0.5442(3) 0.0878(3) 0.1724(4) 0.035(3) Uani ? ? C C21 0.5203(2) -0.0354(3) 0.3468(3) 0.024(2) Uani ? ? C C22 0.5076(3) -0.0665(3) 0.4295(4) 0.030(2) Uani ? ? C C23 0.5487(3) -0.1127(3) 0.4630(4) 0.040(3) Uani ? ? C C24 0.6029(3) -0.1277(3) 0.4120(5) 0.042(3) Uani ? ? C C25 0.6160(3) -0.0973(3) 0.3290(5) 0.043(3) Uani ? ? C C26 0.5748(2) -0.0518(3) 0.2971(4) 0.031(2) Uani ? ? C P3 0.20394(6) 0.04755(6) 0.36519(9) 0.0186(5) Uani ? ? P C27 0.1454(2) 0.0740(2) 0.2799(4) 0.023(2) Uani ? ? C C28 0.1134(3) 0.1320(3) 0.2868(4) 0.030(2) Uani ? ? C C29 0.0700(3) 0.1491(3) 0.2201(5) 0.035(3) Uani ? ? C C30 0.0567(3) 0.1086(3) 0.1465(5) 0.037(3) Uani ? ? C C31 0.0873(3) 0.0506(3) 0.1385(4) 0.036(3) Uani ? ? C C32 0.1322(3) 0.0337(3) 0.2049(4) 0.027(2) Uani ? ? C C33 0.1584(2) 0.0137(2) 0.4601(4) 0.023(2) Uani ? ? C C34 0.1073(3) 0.0463(3) 0.4980(4) 0.034(3) Uani ? ? C C35 0.0741(3) 0.0209(3) 0.5743(5) 0.039(3) Uani ? ? C C36 0.0926(3) -0.0345(3) 0.6128(4) 0.040(3) Uani ? ? C C37 0.1433(3) -0.0669(3) 0.5759(4) 0.034(3) Uani ? ? C C38 0.1754(3) -0.0445(3) 0.4984(4) 0.028(2) Uani ? ? C C39 0.2326(2) 0.1230(2) 0.4133(3) 0.021(2) Uani ? ? C P4 0.30609(6) 0.11621(6) 0.48032(9) 0.0201(5) Uani ? ? P C40 0.3216(3) 0.1979(2) 0.5132(4) 0.029(2) Uani ? ? C C41 0.2824(3) 0.2481(3) 0.4902(5) 0.039(3) Uani ? ? C C42 0.2993(3) 0.3094(3) 0.5108(6) 0.048(4) Uani ? ? C C43 0.3536(4) 0.3231(3) 0.5546(8) 0.052(4) Uani ? ? C C44 0.3957(5) 0.2729(4) 0.579(1) 0.086(6) Uani ? ? C C45 0.3783(3) 0.2111(4) 0.5585(8) 0.062(4) Uani ? ? C C46 0.2814(3) 0.0761(3) 0.5868(3) 0.025(2) Uani ? ? C C47 0.2342(3) 0.0999(3) 0.6428(4) 0.032(3) Uani ? ? C C48 0.2141(3) 0.0656(4) 0.7196(5) 0.043(3) Uani ? ? C C49 0.2413(3) 0.0103(4) 0.7426(4) 0.041(3) Uani ? ? C C50 0.2897(3) -0.0156(3) 0.6871(5) 0.035(3) Uani ? ? C C51 0.3094(2) 0.0186(3) 0.6094(4) 0.027(2) Uani ? ? C C52 0.4118(6) 0.2253(6) 0.185(1) 0.097(8) Uani ? ? C CL3 0.3805(3) 0.2549(3) 0.2865(4) 0.179(4) Uani ? ? Cl CL4 0.4239(4) 0.2816(3) 0.0994(5) 0.198(5) Uani ? ? Cl C53 0.2717(7) 0.2455(6) 0.779(1) 0.112(9) Uani ? ? C CL5 0.3227(2) 0.2975(2) 0.8290(3) 0.107(2) Uani ? ? Cl CL6 0.1951(2) 0.2586(1) 0.7942(3) 0.104(2) Uani ? ? Cl C54 0.2264(4) 0.1448(5) 0.0727(6) 0.059(5) Uani ? ? C CL7 0.2587(1) 0.2148(1) 0.0536(2) 0.097(2) Uani ? ? Cl CL8 0.2218(1) 0.0967(1) -0.0339(2) 0.086(2) Uani ? ? Cl O2 0.2853(5) 0.4248(4) 0.2840(8) 0.121(7) Uani ? ? O O3 0.3821(6) 0.4648(6) 0.382(2) 0.29(1) Uani ? ? O H1 0.3139 -0.1749 0.1353 0.0518 Uiso calc C3 H H2 0.2824 -0.2070 -0.0117 0.0628 Uiso calc C4 H H3 0.2942 -0.1393 -0.1398 0.0618 Uiso calc C5 H H4 0.3377 -0.0407 -0.1185 0.0675 Uiso calc C6 H H5 0.3689 -0.0071 0.0287 0.0540 Uiso calc C7 H H6 0.3405 -0.1327 0.3833 0.0400 Uiso calc C9 H H7 0.3882 -0.2191 0.4565 0.0505 Uiso calc C10 H H8 0.4753 -0.2679 0.3895 0.0595 Uiso calc C11 H H9 0.5151 -0.2315 0.2505 0.0612 Uiso calc C12 H H10 0.4668 -0.1486 0.1709 0.0489 Uiso calc C13 H H11 0.4222 0.0233 0.1552 0.0313 Uiso calc C14 H H12 0.4671 -0.0342 0.1668 0.0313 Uiso calc C14 H H13 0.5107 0.1400 0.3825 0.0549 Uiso calc C16 H H14 0.5775 0.2210 0.3331 0.0672 Uiso calc C17 H H15 0.6212 0.2196 0.1828 0.0634 Uiso calc C18 H H16 0.6005 0.1361 0.0830 0.0609 Uiso calc C19 H H17 0.5359 0.0538 0.1309 0.0460 Uiso calc C20 H H18 0.4706 -0.0563 0.4639 0.0399 Uiso calc C22 H H19 0.5398 -0.1338 0.5201 0.0528 Uiso calc C23 H H20 0.6310 -0.1591 0.4348 0.0551 Uiso calc C24 H H21 0.6529 -0.1076 0.2943 0.0574 Uiso calc C25 H H22 0.5837 -0.0309 0.2397 0.0422 Uiso calc C26 H H23 0.1218 0.1595 0.3378 0.0391 Uiso calc C28 H H24 0.0491 0.1887 0.2244 0.0460 Uiso calc C29 H H25 0.0263 0.1206 0.1010 0.0492 Uiso calc C30 H H26 0.0777 0.0229 0.0883 0.0469 Uiso calc C31 H H27 0.1539 -0.0053 0.1993 0.0359 Uiso calc C32 H H28 0.0949 0.0858 0.4723 0.0440 Uiso calc C34 H H29 0.0385 0.0426 0.5988 0.0521 Uiso calc C35 H H30 0.0707 -0.0510 0.6654 0.0544 Uiso calc C36 H H31 0.1563 -0.1054 0.6041 0.0449 Uiso calc C37 H H32 0.2087 -0.0685 0.4716 0.0360 Uiso calc C38 H H33 0.2009 0.1396 0.4533 0.0278 Uiso calc C39 H H34 0.2396 0.1513 0.3629 0.0278 Uiso calc C39 H H35 0.2433 0.2401 0.4598 0.0528 Uiso calc C41 H H36 0.2718 0.3428 0.4936 0.0641 Uiso calc C42 H H37 0.3639 0.3656 0.5696 0.0780 Uiso calc C43 H H38 0.4350 0.2816 0.6077 0.1256 Uiso calc C44 H H39 0.4054 0.1773 0.5760 0.0886 Uiso calc C45 H H40 0.2155 0.1396 0.6289 0.0450 Uiso calc C47 H H41 0.1805 0.0814 0.7568 0.0608 Uiso calc C48 H H42 0.2277 -0.0116 0.7970 0.0613 Uiso calc C49 H H43 0.3083 -0.0551 0.7022 0.0466 Uiso calc C50 H H44 0.3425 0.0025 0.5713 0.0368 Uiso calc C51 H H45 0.3836 0.1943 0.1612 0.1262 Uiso calc C52 H H46 0.4512 0.2061 0.1993 0.1262 Uiso calc C52 H H47 0.2807 0.2048 0.8037 0.1513 Uiso calc C53 H H48 0.2795 0.2456 0.7136 0.1513 Uiso calc C53 H H49 0.1848 0.1509 0.0963 0.0883 Uiso calc C54 H H50 0.2510 0.1230 0.1178 0.0883 Uiso calc C54 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol PD1 0.0175(1) 0.0214(1) 0.0175(1) 0.0003(1) 0.0013(1) -0.0009(1) Pd PD2 0.0174(1) 0.0285(2) 0.0137(1) 0.0027(1) -0.0004(1) 0.0001(1) Pd CL1 0.0278(5) 0.0279(5) 0.0367(6) -0.0052(5) 0.0010(5) -0.0052(5) Cl CL2 0.0293(6) 0.0545(8) 0.0210(5) 0.0063(6) -0.0074(5) -0.0018(5) Cl C1 0.017(2) 0.024(2) 0.019(2) 0.001(2) -0.002(2) -0.001(2) C O1 0.034(2) 0.035(2) 0.024(2) -0.002(2) -0.006(2) 0.005(2) O P1 0.0201(5) 0.0236(6) 0.0180(5) 0.0002(5) 0.0026(4) -0.0007(4) P C2 0.020(2) 0.036(3) 0.021(2) -0.000(2) -0.001(2) -0.003(2) C C3 0.051(3) 0.039(3) 0.029(3) -0.008(3) -0.002(3) -0.004(2) C C4 0.053(4) 0.052(4) 0.040(3) -0.008(3) -0.006(3) -0.014(3) C C5 0.039(3) 0.075(4) 0.028(3) -0.004(3) -0.003(2) -0.009(3) C C6 0.045(3) 0.085(5) 0.025(2) -0.022(3) -0.011(3) 0.006(3) C C7 0.048(3) 0.048(3) 0.028(2) -0.014(3) -0.012(2) 0.008(2) C C8 0.024(2) 0.028(2) 0.025(2) 0.004(2) -0.002(2) -0.003(2) C C9 0.031(3) 0.035(3) 0.026(2) -0.002(2) -0.004(2) 0.001(2) C C10 0.045(3) 0.037(3) 0.034(3) -0.001(3) -0.009(3) 0.007(3) C C11 0.044(3) 0.033(3) 0.060(4) 0.006(3) -0.013(3) 0.009(3) C C12 0.043(3) 0.041(3) 0.057(4) 0.021(2) -0.005(3) -0.002(3) C C13 0.035(3) 0.040(3) 0.037(3) 0.005(3) 0.004(2) -0.000(3) C C14 0.020(2) 0.034(2) 0.018(2) 0.001(2) 0.003(2) 0.001(2) C P2 0.0184(5) 0.0286(6) 0.0158(4) 0.0014(5) 0.0013(4) 0.0005(4) P C15 0.021(2) 0.034(3) 0.022(2) -0.004(2) 0.005(2) 0.003(2) C C16 0.049(3) 0.045(3) 0.032(3) -0.011(3) 0.002(3) -0.003(3) C C17 0.064(4) 0.037(3) 0.055(4) -0.016(3) 0.000(4) -0.009(3) C C18 0.044(3) 0.048(3) 0.054(4) -0.015(3) 0.004(3) 0.017(3) C C19 0.047(3) 0.053(3) 0.040(3) -0.011(3) 0.008(3) 0.014(3) C C20 0.032(3) 0.046(3) 0.028(2) -0.005(3) 0.004(2) 0.005(2) C C21 0.020(2) 0.033(2) 0.020(2) 0.003(2) 0.001(2) 0.001(2) C C22 0.032(3) 0.037(3) 0.023(2) 0.009(2) 0.003(2) 0.006(2) C C23 0.050(3) 0.040(3) 0.031(3) 0.007(3) -0.004(3) 0.012(2) C C24 0.033(3) 0.041(3) 0.054(4) 0.016(2) -0.004(3) 0.007(3) C C25 0.033(3) 0.046(3) 0.053(4) 0.012(3) 0.011(3) 0.008(3) C C26 0.023(2) 0.042(3) 0.032(2) 0.004(2) 0.008(2) 0.006(2) C P3 0.0167(5) 0.0209(5) 0.0185(5) 0.0006(4) 0.0001(4) 0.0004(4) P C27 0.017(2) 0.028(2) 0.026(2) -0.000(2) 0.001(2) 0.003(2) C C28 0.032(2) 0.029(2) 0.029(2) 0.001(2) -0.004(2) -0.001(2) C C29 0.030(3) 0.029(3) 0.047(3) 0.009(2) -0.007(2) 0.006(2) C C30 0.031(3) 0.044(3) 0.038(3) 0.000(2) -0.013(2) 0.010(3) C C31 0.039(3) 0.039(3) 0.031(3) -0.003(2) -0.012(2) 0.002(2) C C32 0.032(2) 0.025(2) 0.026(2) -0.000(2) -0.006(2) -0.002(2) C C33 0.024(2) 0.027(2) 0.019(2) -0.006(2) 0.001(2) -0.001(2) C C34 0.030(3) 0.033(3) 0.038(3) 0.006(2) 0.008(2) 0.004(2) C C35 0.031(3) 0.046(3) 0.043(3) -0.000(3) 0.014(2) 0.001(3) C C36 0.049(3) 0.052(3) 0.025(2) -0.020(3) 0.008(2) 0.004(2) C C37 0.041(3) 0.037(3) 0.026(2) -0.009(2) -0.003(2) 0.007(2) C C38 0.030(2) 0.029(2) 0.024(2) -0.003(2) -0.001(2) 0.002(2) C C39 0.020(2) 0.024(2) 0.020(2) 0.004(2) -0.000(2) -0.000(2) C P4 0.0189(5) 0.0255(6) 0.0169(4) 0.0012(5) -0.0002(4) -0.0025(4) P C40 0.029(2) 0.027(2) 0.030(2) -0.002(2) -0.001(2) -0.008(2) C C41 0.032(3) 0.033(3) 0.058(4) -0.001(2) -0.008(3) -0.007(3) C C42 0.050(4) 0.033(3) 0.065(4) 0.009(3) -0.014(3) -0.010(3) C C43 0.051(4) 0.027(3) 0.102(6) -0.002(3) -0.014(4) -0.016(4) C C44 0.072(5) 0.055(4) 0.163(9) 0.010(4) -0.064(5) -0.035(5) C C45 0.050(3) 0.044(4) 0.111(6) 0.002(3) -0.048(3) -0.012(4) C C46 0.029(2) 0.030(2) 0.017(2) -0.002(2) 0.003(2) -0.001(2) C C47 0.027(2) 0.053(3) 0.023(2) 0.004(2) 0.006(2) 0.001(2) C C48 0.040(3) 0.072(4) 0.028(3) 0.012(3) 0.013(2) 0.003(3) C C49 0.036(3) 0.081(5) 0.025(2) -0.008(3) 0.003(2) 0.015(3) C C50 0.029(3) 0.046(3) 0.032(3) -0.002(2) -0.001(2) 0.012(2) C C51 0.022(2) 0.040(3) 0.023(2) -0.002(2) -0.000(2) 0.004(2) C C52 0.108(8) 0.092(7) 0.090(8) -0.015(7) 0.004(7) 0.012(7) C CL3 0.271(6) 0.171(4) 0.123(3) -0.031(4) 0.080(3) -0.044(3) Cl CL4 0.272(6) 0.176(4) 0.161(5) -0.045(4) 0.053(4) 0.050(4) Cl C53 0.13(1) 0.074(6) 0.15(1) 0.005(7) -0.02(1) -0.035(8) C CL5 0.099(2) 0.127(2) 0.096(2) -0.004(2) -0.004(2) -0.021(2) Cl CL6 0.121(2) 0.074(1) 0.125(2) -0.022(1) -0.053(2) 0.016(2) Cl C54 0.052(4) 0.117(7) 0.035(3) -0.013(5) -0.005(3) 0.015(4) C CL7 0.101(2) 0.090(2) 0.100(2) -0.003(1) 0.034(2) -0.026(2) Cl CL8 0.094(2) 0.086(2) 0.080(2) -0.016(1) -0.002(2) -0.010(1) Cl O2 0.165(8) 0.108(5) 0.099(7) -0.049(5) 0.010(7) -0.016(6) O O3 0.178(8) 0.254(9) 0.55(3) 0.137(6) 0.08(1) 0.25(1) O # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag PD1 CL1 2.446(1) . . ? PD1 C1 1.973(5) . . ? PD1 P1 2.340(1) . . ? PD1 P3 2.342(1) . . ? PD2 CL2 2.427(1) . . ? PD2 C1 1.976(5) . . ? PD2 P2 2.335(1) . . ? PD2 P4 2.336(1) . . ? C1 O1 1.178(6) . . ? P1 C2 1.818(5) . . ? P1 C8 1.809(6) . . ? P1 C14 1.838(6) . . ? C2 C3 1.397(9) . . ? C2 C7 1.376(9) . . ? C3 C4 1.36(1) . . ? C4 C5 1.39(1) . . ? C5 C6 1.36(1) . . ? C6 C7 1.378(9) . . ? C8 C9 1.402(8) . . ? C8 C13 1.389(8) . . ? C9 C10 1.388(9) . . ? C10 C11 1.37(1) . . ? C11 C12 1.35(1) . . ? C12 C13 1.39(1) . . ? C14 P2 1.828(6) . . ? P2 C15 1.824(6) . . ? P2 C21 1.819(6) . . ? C15 C16 1.410(9) . . ? C15 C20 1.393(8) . . ? C16 C17 1.38(1) . . ? C17 C18 1.40(1) . . ? C18 C19 1.36(1) . . ? C19 C20 1.377(9) . . ? C21 C22 1.380(8) . . ? C21 C26 1.401(7) . . ? C22 C23 1.393(8) . . ? C23 C24 1.40(1) . . ? C24 C25 1.38(1) . . ? C25 C26 1.378(9) . . ? P3 C27 1.827(5) . . ? P3 C33 1.813(5) . . ? P3 C39 1.842(5) . . ? C27 C28 1.406(8) . . ? C27 C32 1.399(8) . . ? C28 C29 1.372(8) . . ? C29 C30 1.39(1) . . ? C30 C31 1.39(1) . . ? C31 C32 1.389(8) . . ? C33 C34 1.395(8) . . ? C33 C38 1.395(8) . . ? C34 C35 1.405(9) . . ? C35 C36 1.35(1) . . ? C36 C37 1.38(1) . . ? C37 C38 1.384(8) . . ? C39 P4 1.833(5) . . ? P4 C40 1.822(6) . . ? P4 C46 1.821(5) . . ? C40 C41 1.387(9) . . ? C40 C45 1.393(9) . . ? C41 C42 1.38(1) . . ? C42 C43 1.34(1) . . ? C43 C44 1.43(1) . . ? C44 C45 1.39(1) . . ? C46 C47 1.376(8) . . ? C46 C51 1.393(8) . . ? C47 C48 1.384(9) . . ? C48 C49 1.35(1) . . ? C49 C50 1.41(1) . . ? C50 C51 1.391(8) . . ? C52 CL3 1.71(2) . . ? C52 CL4 1.73(2) . . ? C53 CL5 1.70(2) . . ? C53 CL6 1.66(2) . . ? C54 CL7 1.66(1) . . ? C54 CL8 1.84(1) . . ? 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag CL1 PD1 C1 174.7(2) . . . ? CL1 PD1 P1 91.21(5) . . . ? CL1 PD1 P3 96.17(5) . . . ? C1 PD1 P1 86.6(1) . . . ? C1 PD1 P3 85.7(1) . . . ? P1 PD1 P3 171.50(5) . . . ? CL2 PD2 C1 178.8(2) . . . ? CL2 PD2 P2 93.51(5) . . . ? CL2 PD2 P4 92.91(5) . . . ? C1 PD2 P2 86.2(1) . . . ? C1 PD2 P4 87.2(1) . . . ? P2 PD2 P4 171.36(5) . . . ? C2 P1 C8 105.0(3) . . . ? C2 P1 C14 103.3(2) . . . ? C8 P1 C14 103.4(3) . . . ? P1 C2 C3 119.6(4) . . . ? P1 C2 C7 121.9(5) . . . ? C3 C2 C7 118.4(5) . . . ? C2 C3 C4 120.6(7) . . . ? C3 C4 C5 120.2(7) . . . ? C4 C5 C6 119.3(6) . . . ? C5 C6 C7 121.1(7) . . . ? C2 C7 C6 120.4(7) . . . ? P1 C8 C9 120.5(4) . . . ? P1 C8 C13 120.5(5) . . . ? C9 C8 C13 119.0(6) . . . ? C8 C9 C10 119.5(6) . . . ? C9 C10 C11 120.6(7) . . . ? C10 C11 C12 119.8(6) . . . ? C11 C12 C13 121.5(7) . . . ? C8 C13 C12 119.5(6) . . . ? P1 C14 P2 113.8(3) . . . ? C14 P2 C15 103.6(3) . . . ? C14 P2 C21 104.0(3) . . . ? C15 P2 C21 104.3(3) . . . ? P2 C15 C16 117.8(4) . . . ? P2 C15 C20 122.9(5) . . . ? C16 C15 C20 119.3(6) . . . ? C15 C16 C17 118.8(7) . . . ? C16 C17 C18 120.8(7) . . . ? C17 C18 C19 120.1(6) . . . ? C18 C19 C20 120.2(7) . . . ? C15 C20 C19 120.8(7) . . . ? P2 C21 C22 120.3(4) . . . ? P2 C21 C26 121.1(4) . . . ? C22 C21 C26 118.5(5) . . . ? C21 C22 C23 120.6(6) . . . ? C22 C23 C24 119.5(6) . . . ? C23 C24 C25 120.6(6) . . . ? C24 C25 C26 119.0(6) . . . ? C21 C26 C25 121.8(6) . . . ? C27 P3 C33 105.2(2) . . . ? C27 P3 C39 102.0(2) . . . ? C33 P3 C39 103.8(2) . . . ? P3 C27 C28 123.2(4) . . . ? P3 C27 C32 117.5(4) . . . ? C28 C27 C32 119.3(5) . . . ? C27 C28 C29 120.2(6) . . . ? C28 C29 C30 120.1(6) . . . ? C29 C30 C31 120.8(6) . . . ? C30 C31 C32 119.3(6) . . . ? C27 C32 C31 120.3(5) . . . ? P3 C33 C34 120.5(4) . . . ? P3 C33 C38 120.5(4) . . . ? C34 C33 C38 119.0(5) . . . ? C33 C34 C35 120.0(6) . . . ? C34 C35 C36 120.2(6) . . . ? C35 C36 C37 120.1(6) . . . ? C36 C37 C38 121.2(6) . . . ? C33 C38 C37 119.4(6) . . . ? P3 C39 P4 114.0(3) . . . ? C39 P4 C40 102.3(3) . . . ? C39 P4 C46 103.3(2) . . . ? C40 P4 C46 106.1(3) . . . ? P4 C40 C41 123.9(5) . . . ? P4 C40 C45 117.7(5) . . . ? C41 C40 C45 118.2(6) . . . ? C40 C41 C42 121.0(6) . . . ? C41 C42 C43 121.8(7) . . . ? C42 C43 C44 119.0(7) . . . ? C43 C44 C45 119.1(8) . . . ? C40 C45 C44 120.8(8) . . . ? P4 C46 C47 121.7(5) . . . ? P4 C46 C51 118.6(4) . . . ? C47 C46 C51 119.6(5) . . . ? C46 C47 C48 119.5(6) . . . ? C47 C48 C49 121.3(6) . . . ? C48 C49 C50 120.8(6) . . . ? C49 C50 C51 117.9(6) . . . ? C46 C51 C50 120.8(6) . . . ? CL3 C52 CL4 113.9(9) . . . ? CL5 C53 CL6 117.2(9) . . . ? CL7 C54 CL8 112.3(5) . . . ?