Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_pdbu _database_code_CSD 185527 _audit_creation_date 04-02-02 _journal_coden_Cambridge 182 loop_ _publ_author_name 'Le Floch, Pascal' 'Doux, Marjolaine' 'Melaimi, Mohand' 'Mezailles, N.' 'Ricard, Louis' _publ_contact_author_name 'Dr Pascal Le Floch' _publ_contact_author_address ; Dpt of Chemistry CNRS Ecole Polytechnique Palaiseau Cedex 91128 FRANCE ; _publ_contact_author_email LEFLOCH@POLY.POLYTECHNIQUE.FR _publ_requested_journal 'Chemical Communications' _publ_section_title ; A s4, l5-Phosphinine Palladium Complex: A New Type of Phosphorus Ligand and Catalyst. Application to the Pd-Catalyzed Formation of Arylboronic Esters ; _publ_requested_coeditor_name ? _publ_contact_letter ; Please consider this CIF submission for publication as a new structure paper in Chem. Comm.. The figures, chemical structure diagram (scheme), Transfert of Copyright Agreement form and structure factors will be sent on receipt of your acknowledgement letter ; #=============================================================================== _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C. & Guagliardi, A. (1993) J. Appl. Cryst. 26, 343-350. Sheldrick, G.M. SHELXL97. Program for crystal structure refinement. University of Gottingen, Germany, 1997. Sluis, P. v.d., Spek, A.L. (1990). Acta Cryst. A46, 194-201. Spek, A.L. (1990). Acta Cryst. A46, C-34. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H42 Cl3 P3 Pd S2' _chemical_formula_weight 964.62 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' '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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Orthorhombic' _symmetry_space_group_name_H-M 'Pna21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 19.482(5) _cell_length_b 24.081(5) _cell_length_c 9.337(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4380(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150.0(10) _cell_measurement_reflns_used 251 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 20.0 _exptl_crystal_description 'plate' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.463 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1968 _exptl_absorpt_coefficient_mu 0.844 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8493 _exptl_absorpt_correction_T_max 0.9751 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(10) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'KappaCCD' _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 24182 _diffrn_reflns_av_R_equivalents 0.1142 _diffrn_reflns_av_sigmaI/netI 0.0732 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 4.04 _diffrn_reflns_theta_max 21.96 _reflns_number_total 5292 _reflns_number_gt 4122 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0467P)^2^+4.0242P] 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 mixed _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 0.01(4) _refine_ls_number_reflns 5292 _refine_ls_number_parameters 497 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0698 _refine_ls_R_factor_gt 0.0475 _refine_ls_wR_factor_ref 0.1106 _refine_ls_wR_factor_gt 0.1015 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.002 _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 1.24461(3) 1.82662(2) 1.64492(7) 0.03513(19) Uani 1 1 d . . . Cl1 Cl 1.18387(12) 1.82960(9) 1.8656(2) 0.0517(6) Uani 1 1 d . . . S1 S 1.22994(12) 1.73160(8) 1.6167(2) 0.0494(6) Uani 1 1 d . . . S2 S 1.25724(11) 1.92230(6) 1.6428(3) 0.0407(5) Uani 1 1 d . . . P1 P 1.31845(10) 1.82270(8) 1.4698(2) 0.0316(5) Uani 1 1 d . . . P2 P 1.24844(11) 1.71719(8) 1.4052(2) 0.0340(5) Uani 1 1 d . . . P3 P 1.27318(11) 1.93760(8) 1.4315(2) 0.0352(5) Uani 1 1 d . . . C1 C 1.3054(3) 1.7689(3) 1.3448(8) 0.0276(18) Uani 1 1 d . . . C2 C 1.3377(3) 1.7743(3) 1.2119(8) 0.0272(18) Uani 1 1 d . . . C3 C 1.3649(3) 1.8256(3) 1.1609(10) 0.034(2) Uani 1 1 d . . . H3 H 1.3925 1.8250 1.0771 0.040 Uiso 1 1 calc R . . C4 C 1.3532(4) 1.8773(3) 1.2278(9) 0.0314(19) Uani 1 1 d . . . C5 C 1.3225(4) 1.8827(3) 1.3622(8) 0.0319(19) Uani 1 1 d . . . C6 C 1.1692(4) 1.7181(3) 1.3079(9) 0.037(2) Uani 1 1 d . . . C7 C 1.1170(5) 1.6810(3) 1.3453(10) 0.045(2) Uani 1 1 d . . . H7 H 1.1245 1.6548 1.4198 0.054 Uiso 1 1 calc R . . C8 C 1.0558(5) 1.6820(3) 1.2763(11) 0.053(3) Uani 1 1 d . . . H8 H 1.0211 1.6561 1.3012 0.064 Uiso 1 1 calc R . . C9 C 1.0436(4) 1.7206(4) 1.1698(11) 0.054(3) Uani 1 1 d . . . H9 H 1.0004 1.7215 1.1225 0.065 Uiso 1 1 calc R . . C10 C 1.0934(4) 1.7574(3) 1.1331(12) 0.053(2) Uani 1 1 d . . . H10 H 1.0843 1.7844 1.0613 0.063 Uiso 1 1 calc R . . C11 C 1.1566(4) 1.7564(3) 1.1977(9) 0.041(2) Uani 1 1 d . . . H11 H 1.1916 1.7814 1.1681 0.049 Uiso 1 1 calc R . . C12 C 1.2795(4) 1.6473(3) 1.3865(9) 0.037(2) Uani 1 1 d . . . C13 C 1.2586(4) 1.6142(3) 1.2723(9) 0.039(2) Uani 1 1 d . . . H13 H 1.2270 1.6277 1.2031 0.047 Uiso 1 1 calc R . . C14 C 1.2851(5) 1.5608(3) 1.2623(12) 0.060(3) Uani 1 1 d . . . H14 H 1.2721 1.5383 1.1832 0.072 Uiso 1 1 calc R . . C15 C 1.3289(5) 1.5395(4) 1.3608(12) 0.063(3) Uani 1 1 d . . . H15 H 1.3452 1.5025 1.3512 0.076 Uiso 1 1 calc R . . C16 C 1.3499(5) 1.5723(4) 1.4772(12) 0.069(3) Uani 1 1 d . . . H16 H 1.3807 1.5580 1.5470 0.083 Uiso 1 1 calc R . . C17 C 1.3246(5) 1.6263(3) 1.4882(10) 0.055(3) Uani 1 1 d . . . H17 H 1.3384 1.6491 1.5661 0.066 Uiso 1 1 calc R . . C18 C 1.3495(4) 1.7255(3) 1.1174(10) 0.033(2) Uani 1 1 d . . . C19 C 1.3175(5) 1.7196(3) 0.9882(9) 0.043(2) Uani 1 1 d . . . H19 H 1.2849 1.7464 0.9576 0.052 Uiso 1 1 calc R . . C20 C 1.3326(5) 1.6743(4) 0.9015(11) 0.067(3) Uani 1 1 d . . . H20 H 1.3105 1.6703 0.8114 0.080 Uiso 1 1 calc R . . C21 C 1.3793(6) 1.6355(4) 0.9464(13) 0.068(3) Uani 1 1 d . . . H21 H 1.3893 1.6043 0.8878 0.081 Uiso 1 1 calc R . . C22 C 1.4109(5) 1.6417(4) 1.0725(12) 0.063(3) Uani 1 1 d . . . H22 H 1.4438 1.6150 1.1029 0.075 Uiso 1 1 calc R . . C23 C 1.3961(4) 1.6859(3) 1.1574(12) 0.047(2) Uani 1 1 d . . . H23 H 1.4187 1.6894 1.2470 0.057 Uiso 1 1 calc R . . C24 C 1.3755(4) 1.9273(3) 1.1469(11) 0.0348(18) Uani 1 1 d . . . C25 C 1.3475(4) 1.9393(3) 1.0109(10) 0.046(2) Uani 1 1 d . . . H25 H 1.3141 1.9153 0.9701 0.055 Uiso 1 1 calc R . . C26 C 1.3691(5) 1.9861(4) 0.9369(11) 0.061(3) Uani 1 1 d . . . H26 H 1.3498 1.9947 0.8461 0.074 Uiso 1 1 calc R . . C27 C 1.4184(5) 2.0202(4) 0.9949(12) 0.061(3) Uani 1 1 d . . . H27 H 1.4334 2.0516 0.9423 0.074 Uiso 1 1 calc R . . C28 C 1.4466(4) 2.0098(3) 1.1280(13) 0.056(2) Uani 1 1 d . . . H28 H 1.4799 2.0340 1.1682 0.067 Uiso 1 1 calc R . . C29 C 1.4247(4) 1.9627(3) 1.2009(10) 0.041(2) Uani 1 1 d . . . H29 H 1.4445 1.9545 1.2915 0.049 Uiso 1 1 calc R . . C30 C 1.3115(4) 2.0062(3) 1.4196(9) 0.035(2) Uani 1 1 d . . . C31 C 1.2899(5) 2.0443(3) 1.3216(11) 0.055(3) Uani 1 1 d . . . H31 H 1.2551 2.0350 1.2544 0.066 Uiso 1 1 calc R . . C32 C 1.3195(6) 2.0973(4) 1.3212(15) 0.083(4) Uani 1 1 d . . . H32 H 1.3054 2.1240 1.2523 0.099 Uiso 1 1 calc R . . C33 C 1.3692(6) 2.1107(5) 1.4213(17) 0.084(4) Uani 1 1 d . . . H33 H 1.3873 2.1473 1.4244 0.101 Uiso 1 1 calc R . . C34 C 1.3923(5) 2.0719(5) 1.5150(13) 0.071(3) Uani 1 1 d . . . H34 H 1.4284 2.0808 1.5795 0.085 Uiso 1 1 calc R . . C35 C 1.3636(4) 2.0196(3) 1.5167(9) 0.050(2) Uani 1 1 d . . . H35 H 1.3791 1.9927 1.5838 0.060 Uiso 1 1 calc R . . C36 C 1.1931(4) 1.9429(3) 1.3403(9) 0.035(2) Uani 1 1 d . . . C37 C 1.1805(4) 1.9178(3) 1.2092(9) 0.040(2) Uani 1 1 d . . . H37 H 1.2156 1.8961 1.1660 0.048 Uiso 1 1 calc R . . C38 C 1.1193(4) 1.9235(3) 1.1407(13) 0.050(2) Uani 1 1 d . . . H38 H 1.1124 1.9055 1.0513 0.060 Uiso 1 1 calc R . . C39 C 1.0677(4) 1.9546(3) 1.1984(10) 0.051(3) Uani 1 1 d . . . H39 H 1.0252 1.9588 1.1497 0.061 Uiso 1 1 calc R . . C40 C 1.0789(5) 1.9799(3) 1.3301(10) 0.051(2) Uani 1 1 d . . . H40 H 1.0435 2.0014 1.3731 0.061 Uiso 1 1 calc R . . C41 C 1.1400(4) 1.9741(3) 1.3972(9) 0.046(2) Uani 1 1 d . . . H41 H 1.1467 1.9920 1.4867 0.055 Uiso 1 1 calc R . . C42 C 1.4020(4) 1.8071(4) 1.5472(10) 0.051(2) Uani 1 1 d . . . H42A H 1.4006 1.7689 1.5860 0.061 Uiso 1 1 calc R . . H42B H 1.4365 1.8076 1.4693 0.061 Uiso 1 1 calc R . . C43 C 1.4256(5) 1.8442(4) 1.6606(17) 0.102(4) Uani 1 1 d . . . H43A H 1.3907 1.8449 1.7376 0.122 Uiso 1 1 calc R . . H43B H 1.4293 1.8823 1.6213 0.122 Uiso 1 1 calc R . . C44 C 1.4929(9) 1.8283(6) 1.724(2) 0.183(10) Uani 1 1 d . . . H44A H 1.5283 1.8346 1.6497 0.220 Uiso 1 1 calc R . . H44B H 1.5025 1.8548 1.8026 0.220 Uiso 1 1 calc R . . C45 C 1.5029(8) 1.7767(6) 1.7767(17) 0.147(7) Uani 1 1 d . . . H45A H 1.5487 1.7636 1.7497 0.221 Uiso 1 1 calc R . . H45B H 1.4681 1.7516 1.7373 0.221 Uiso 1 1 calc R . . H45C H 1.4990 1.7776 1.8813 0.221 Uiso 1 1 calc R . . Cl2 Cl 1.0222(2) 1.83236(14) 1.4608(4) 0.1227(13) Uani 1 1 d . . . Cl3 Cl 1.0265(2) 1.91447(16) 1.6900(4) 0.1342(15) Uani 1 1 d . . . C46 C 1.0672(5) 1.8608(4) 1.6037(13) 0.079(3) Uani 1 1 d . . . H46A H 1.0765 1.8310 1.6742 0.095 Uiso 1 1 calc R . . H46B H 1.1120 1.8744 1.5680 0.095 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 Pd1 0.0575(4) 0.0231(3) 0.0247(3) -0.0010(4) 0.0023(4) 0.0010(3) Cl1 0.0730(16) 0.0493(14) 0.0328(13) 0.0023(11) 0.0102(12) 0.0074(11) S1 0.0936(17) 0.0232(10) 0.0313(16) -0.0009(10) 0.0090(13) -0.0070(10) S2 0.0732(13) 0.0203(9) 0.0286(10) -0.0030(13) 0.0046(13) 0.0012(9) P1 0.0427(13) 0.0254(11) 0.0267(12) -0.0038(10) -0.0026(10) 0.0007(9) P2 0.0527(13) 0.0209(11) 0.0284(12) -0.0010(9) 0.0031(11) -0.0016(9) P3 0.0532(14) 0.0212(11) 0.0313(13) -0.0012(10) 0.0009(11) -0.0004(9) C1 0.027(4) 0.023(4) 0.033(5) -0.007(4) -0.002(4) 0.004(3) C2 0.030(4) 0.025(4) 0.026(4) -0.001(4) 0.000(4) 0.000(3) C3 0.033(4) 0.030(4) 0.038(6) 0.001(5) 0.013(5) -0.002(3) C4 0.024(4) 0.037(5) 0.033(5) 0.000(4) -0.003(4) -0.001(4) C5 0.044(5) 0.024(4) 0.028(5) -0.004(4) 0.001(4) -0.005(4) C6 0.042(5) 0.024(5) 0.043(6) 0.002(4) 0.013(4) -0.002(4) C7 0.057(6) 0.031(5) 0.047(6) 0.000(4) 0.015(5) -0.009(4) C8 0.048(6) 0.043(6) 0.069(7) 0.002(6) 0.016(5) -0.008(5) C9 0.036(5) 0.058(6) 0.067(8) -0.013(6) 0.014(5) -0.005(4) C10 0.044(5) 0.060(6) 0.054(6) 0.011(6) 0.009(6) -0.004(4) C11 0.040(5) 0.038(5) 0.046(6) 0.005(5) 0.006(4) -0.010(4) C12 0.060(5) 0.021(4) 0.030(5) -0.002(4) -0.011(4) 0.015(4) C13 0.053(5) 0.026(5) 0.037(5) -0.002(4) -0.008(4) -0.003(4) C14 0.068(6) 0.033(5) 0.078(7) -0.011(5) -0.010(6) 0.009(5) C15 0.080(7) 0.030(5) 0.080(8) -0.011(6) -0.011(7) 0.013(5) C16 0.096(8) 0.040(6) 0.072(8) 0.008(6) -0.017(6) 0.023(5) C17 0.089(7) 0.037(5) 0.039(6) -0.011(5) -0.017(6) 0.012(5) C18 0.041(4) 0.021(4) 0.036(6) -0.009(4) 0.014(5) -0.001(3) C19 0.069(6) 0.038(5) 0.023(5) -0.009(5) -0.007(5) 0.011(4) C20 0.089(8) 0.054(6) 0.057(7) -0.017(6) -0.018(6) -0.002(6) C21 0.096(8) 0.040(6) 0.068(8) -0.019(6) 0.022(7) 0.017(6) C22 0.072(7) 0.039(6) 0.077(8) 0.005(6) -0.002(6) 0.013(5) C23 0.055(5) 0.033(5) 0.054(6) -0.016(5) -0.005(6) 0.012(4) C24 0.047(4) 0.023(4) 0.035(5) 0.002(5) 0.005(6) 0.002(3) C25 0.054(6) 0.036(5) 0.048(7) -0.003(5) 0.014(5) -0.009(4) C26 0.080(7) 0.057(7) 0.047(6) -0.002(6) 0.007(6) -0.003(6) C27 0.068(7) 0.043(6) 0.073(8) 0.012(6) 0.030(6) 0.003(5) C28 0.052(5) 0.033(5) 0.081(8) -0.007(6) 0.007(7) -0.004(4) C29 0.037(5) 0.036(5) 0.050(6) 0.004(4) 0.006(4) -0.001(4) C30 0.038(5) 0.030(5) 0.036(5) -0.010(4) 0.008(4) -0.002(4) C31 0.057(6) 0.032(5) 0.076(7) 0.019(5) 0.000(6) 0.006(5) C32 0.069(7) 0.046(7) 0.133(12) 0.062(7) 0.033(8) 0.014(6) C33 0.067(8) 0.047(7) 0.138(13) -0.027(8) 0.030(9) -0.013(6) C34 0.069(7) 0.064(8) 0.080(8) -0.014(7) 0.008(6) -0.019(6) C35 0.061(6) 0.038(6) 0.051(6) -0.007(5) 0.002(5) -0.010(4) C36 0.047(5) 0.017(4) 0.043(6) -0.003(4) 0.012(4) -0.003(4) C37 0.040(5) 0.030(5) 0.050(6) -0.005(4) 0.009(5) -0.001(4) C38 0.058(6) 0.038(5) 0.053(6) -0.005(6) 0.006(7) 0.001(4) C39 0.046(5) 0.044(6) 0.063(7) 0.004(5) -0.011(5) -0.009(4) C40 0.049(6) 0.039(5) 0.065(7) -0.003(5) 0.011(5) 0.010(4) C41 0.046(6) 0.037(5) 0.054(7) -0.005(5) -0.006(5) -0.001(4) C42 0.060(6) 0.043(6) 0.049(6) -0.025(5) -0.010(5) 0.001(4) C43 0.092(8) 0.067(7) 0.146(13) -0.022(9) -0.065(10) 0.018(6) C44 0.194(17) 0.092(12) 0.26(3) -0.043(14) -0.141(18) 0.007(11) C45 0.197(16) 0.092(11) 0.154(15) -0.026(11) -0.097(13) 0.040(10) Cl2 0.160(3) 0.115(3) 0.093(3) 0.010(2) -0.047(3) -0.017(2) Cl3 0.150(3) 0.138(3) 0.115(3) -0.009(2) 0.039(3) 0.058(3) C46 0.071(7) 0.074(7) 0.093(10) -0.009(7) -0.010(6) 0.008(5) _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 2.180(2) . ? Pd1 S2 2.3173(17) . ? Pd1 S1 2.321(2) . ? Pd1 Cl1 2.377(3) . ? S1 P2 2.037(3) . ? S2 P3 2.031(4) . ? P1 C5 1.761(7) . ? P1 C1 1.762(7) . ? P1 C42 1.820(8) . ? P2 C1 1.760(7) . ? P2 C6 1.791(8) . ? P2 C12 1.797(7) . ? P3 C5 1.758(8) . ? P3 C36 1.783(9) . ? P3 C30 1.816(7) . ? C1 C2 1.397(10) . ? C2 C3 1.426(9) . ? C2 C18 1.489(10) . ? C3 C4 1.411(10) . ? C4 C5 1.396(11) . ? C4 C24 1.486(10) . ? C6 C7 1.399(11) . ? C6 C11 1.404(11) . ? C7 C8 1.356(12) . ? C8 C9 1.381(12) . ? C9 C10 1.358(11) . ? C10 C11 1.371(11) . ? C12 C17 1.388(11) . ? C12 C13 1.392(10) . ? C13 C14 1.389(10) . ? C14 C15 1.355(12) . ? C15 C16 1.405(13) . ? C16 C17 1.396(11) . ? C18 C19 1.365(11) . ? C18 C23 1.368(10) . ? C19 C20 1.389(11) . ? C20 C21 1.370(13) . ? C21 C22 1.337(14) . ? C22 C23 1.358(12) . ? C24 C29 1.378(10) . ? C24 C25 1.411(12) . ? C25 C26 1.389(12) . ? C26 C27 1.373(12) . ? C27 C28 1.381(13) . ? C28 C29 1.390(11) . ? C30 C31 1.363(11) . ? C30 C35 1.398(11) . ? C31 C32 1.400(13) . ? C32 C33 1.384(16) . ? C33 C34 1.357(15) . ? C34 C35 1.378(12) . ? C36 C41 1.384(11) . ? C36 C37 1.386(11) . ? C37 C38 1.360(11) . ? C38 C39 1.365(11) . ? C39 C40 1.391(12) . ? C40 C41 1.353(11) . ? C42 C43 1.459(14) . ? C43 C44 1.488(17) . ? C44 C45 1.350(17) . ? Cl2 C46 1.737(11) . ? Cl3 C46 1.717(10) . ? 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 S2 88.09(8) . . ? P1 Pd1 S1 87.32(8) . . ? S2 Pd1 S1 172.92(10) . . ? P1 Pd1 Cl1 168.52(9) . . ? S2 Pd1 Cl1 91.73(9) . . ? S1 Pd1 Cl1 93.84(8) . . ? P2 S1 Pd1 104.86(10) . . ? P3 S2 Pd1 101.82(11) . . ? C5 P1 C1 103.4(4) . . ? C5 P1 C42 110.8(4) . . ? C1 P1 C42 103.9(3) . . ? C5 P1 Pd1 115.0(3) . . ? C1 P1 Pd1 115.7(3) . . ? C42 P1 Pd1 107.5(3) . . ? C1 P2 C6 111.8(4) . . ? C1 P2 C12 114.8(4) . . ? C6 P2 C12 104.6(4) . . ? C1 P2 S1 107.6(3) . . ? C6 P2 S1 109.7(3) . . ? C12 P2 S1 108.3(3) . . ? C5 P3 C36 110.9(4) . . ? C5 P3 C30 115.9(3) . . ? C36 P3 C30 105.5(4) . . ? C5 P3 S2 107.7(3) . . ? C36 P3 S2 110.1(3) . . ? C30 P3 S2 106.7(3) . . ? C2 C1 P2 129.4(5) . . ? C2 C1 P1 117.0(5) . . ? P2 C1 P1 113.5(4) . . ? C1 C2 C3 123.1(7) . . ? C1 C2 C18 121.4(6) . . ? C3 C2 C18 115.4(7) . . ? C4 C3 C2 123.8(8) . . ? C5 C4 C3 123.3(7) . . ? C5 C4 C24 120.4(7) . . ? C3 C4 C24 116.3(7) . . ? C4 C5 P3 129.4(6) . . ? C4 C5 P1 117.1(6) . . ? P3 C5 P1 112.5(4) . . ? C7 C6 C11 118.4(8) . . ? C7 C6 P2 119.5(7) . . ? C11 C6 P2 122.1(6) . . ? C8 C7 C6 120.6(8) . . ? C7 C8 C9 120.4(8) . . ? C10 C9 C8 119.8(9) . . ? C9 C10 C11 121.3(9) . . ? C10 C11 C6 119.4(7) . . ? C17 C12 C13 120.1(7) . . ? C17 C12 P2 119.1(6) . . ? C13 C12 P2 120.8(6) . . ? C14 C13 C12 118.2(8) . . ? C15 C14 C13 122.6(9) . . ? C14 C15 C16 119.7(8) . . ? C17 C16 C15 118.5(9) . . ? C12 C17 C16 120.8(8) . . ? C19 C18 C23 118.1(8) . . ? C19 C18 C2 122.4(7) . . ? C23 C18 C2 119.4(8) . . ? C18 C19 C20 120.0(8) . . ? C21 C20 C19 119.8(9) . . ? C22 C21 C20 120.0(9) . . ? C21 C22 C23 120.2(9) . . ? C22 C23 C18 121.9(10) . . ? C29 C24 C25 118.1(7) . . ? C29 C24 C4 121.2(8) . . ? C25 C24 C4 120.7(7) . . ? C26 C25 C24 119.8(8) . . ? C27 C26 C25 120.0(10) . . ? C26 C27 C28 121.7(9) . . ? C27 C28 C29 117.8(8) . . ? C24 C29 C28 122.6(9) . . ? C31 C30 C35 120.3(7) . . ? C31 C30 P3 121.8(6) . . ? C35 C30 P3 118.0(6) . . ? C30 C31 C32 119.3(9) . . ? C33 C32 C31 119.9(10) . . ? C34 C33 C32 120.5(10) . . ? C33 C34 C35 120.1(10) . . ? C34 C35 C30 119.9(9) . . ? C41 C36 C37 116.4(8) . . ? C41 C36 P3 120.6(7) . . ? C37 C36 P3 123.0(6) . . ? C38 C37 C36 121.7(8) . . ? C37 C38 C39 121.0(10) . . ? C38 C39 C40 118.3(9) . . ? C41 C40 C39 120.1(8) . . ? C40 C41 C36 122.4(8) . . ? C43 C42 P1 116.4(6) . . ? C42 C43 C44 114.2(10) . . ? C45 C44 C43 120.5(15) . . ? Cl3 C46 Cl2 115.2(6) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 21.96 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.603 _refine_diff_density_min -0.419 _refine_diff_density_rms 0.067