Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _publ_contact_author_email braunst@chimie.u-strasbg.fr _publ_contact_author_name 'Pierre Braunstein' _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year 2003 _journal_page_first 1669 _audit_creation_date 10-05-02 _publ_contact_author_address ; Institut Le Bel, rue Blaise Pascal, 67000 STRASBOURG, FRANCE ; _publ_contact_author_phone 0390241593 _publ_contact_author_fax 0390241232 _publ_contact_letter ; ; _publ_requested_category FM _publ_section_title ; New phosphinooxazoline and related phosphinoiminolate palladium complexes; structure of unusual zwitterionic dinuclear pd(II) complex. ; _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. A.L. Spek, PLATON 98, Utrecht University, The Netherland, 1998. KappaCCD Operation Manual (1997), Nonius B.V., Delft, The Nederlands. Otwinowski, Z. & Minor, W. (1997), Methods in Enzymology, 276, 307-326. Sheldrick, G.M. (1997). SHELXL97. Program for the refinement of crystal structures. University of Gottingen. Germany. ; loop_ _publ_author_name _publ_author_address A.Apfelbacher ; Laboratoire de Chimie de coordination, UMR CNRS 7513 Universit\'e Louis Pasteur Strasbourg France ; P.Braunstein ; Laboratoire de Chimie de coordination, UMR CNRS 7513 Universit\'e Louis Pasteur Strasbourg France ; L.Brissieux ; Laboratoire de Chimie de coordination, UMR CNRS 7513 Universit\'e Louis Pasteur Strasbourg France ; R.Welter ; Laboratoire DECMET, UMR CNRS 7513 Universit\'e Louis Pasteur Strasbourg France ; data_pbr27 _database_code_CSD 200357 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H31 N2 O P Pd, 2(C H2 Cl2)' _chemical_formula_sum 'C33 H35 Cl4 N2 O P Pd' _chemical_formula_weight 754.80 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Pd Pd -0.9988 1.0072 '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' O O 0.0106 0.0060 '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' 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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' 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' _cell_length_a 9.011(3) _cell_length_b 15.511(3) _cell_length_c 23.932(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3344.9(14) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7528 _cell_measurement_theta_min 1.018 _cell_measurement_theta_max 34.972 _exptl_crystal_description prism _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.499 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1536 _exptl_absorpt_coefficient_mu 0.951 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 KappaCCD _diffrn_measurement_method '\p scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14455 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1222 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 34.97 _reflns_number_total 14454 _reflns_number_gt 10434 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON 98 (Spek, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0498P)^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 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 0.00(3) _refine_ls_number_reflns 14454 _refine_ls_number_parameters 365 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0971 _refine_ls_R_factor_gt 0.0639 _refine_ls_wR_factor_ref 0.1389 _refine_ls_wR_factor_gt 0.1277 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _refine_ls_shift/su_max 0.004 _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 P P 0.23502(10) 0.78249(6) 0.83826(4) 0.02104(17) Uani 1 1 d . . . N1 N 0.1472(3) 0.8535(2) 0.73081(12) 0.0247(6) Uani 1 1 d . . . N2 N 0.0106(4) 1.0253(2) 0.79325(13) 0.0253(6) Uani 1 1 d . . . Pd Pd 0.11166(3) 0.902322(16) 0.813131(10) 0.02053(6) Uani 1 1 d . . . O1 O 0.2364(3) 0.74452(18) 0.67695(10) 0.0291(6) Uani 1 1 d . . . C23 C 0.0821(4) 0.9466(2) 0.89146(14) 0.0236(7) Uani 1 1 d . . . C24 C 0.0771(4) 0.9026(3) 0.94213(15) 0.0301(7) Uani 1 1 d . . . H2 H 0.0944 0.8435 0.9425 0.036 Uiso 1 1 calc . . . C25 C 0.0471(6) 0.9446(3) 0.99247(17) 0.0406(10) Uani 1 1 d . . . H3 H 0.0448 0.9139 1.0258 0.049 Uiso 1 1 calc . . . C26 C 0.0211(7) 1.0318(3) 0.99205(19) 0.0522(14) Uani 1 1 d . . . H4 H -0.0002 1.0600 1.0254 0.063 Uiso 1 1 calc . . . C27 C 0.0258(7) 1.0772(3) 0.94406(19) 0.0492(13) Uani 1 1 d . . . H5 H 0.0092 1.1363 0.9448 0.059 Uiso 1 1 calc . . . C28 C 0.0556(5) 1.0360(3) 0.89262(16) 0.0312(8) Uani 1 1 d . . . C29 C 0.0623(5) 1.0834(2) 0.83857(16) 0.0332(8) Uani 1 1 d . . . H7A H -0.0003 1.1342 0.8403 0.040 Uiso 1 1 calc . . . H7B H 0.1633 1.1018 0.8312 0.040 Uiso 1 1 calc . . . C30 C 0.0508(5) 1.0634(3) 0.73800(18) 0.0367(9) Uani 1 1 d . . . H8A H 0.0174 1.0259 0.7086 0.055 Uiso 1 1 calc . . . H8B H 0.1565 1.0700 0.7357 0.055 Uiso 1 1 calc . . . H8C H 0.0042 1.1187 0.7341 0.055 Uiso 1 1 calc . . . C31 C -0.1543(5) 1.0175(3) 0.7948(2) 0.0388(10) Uani 1 1 d . . . H9A H -0.1864 0.9791 0.7657 0.058 Uiso 1 1 calc . . . H9B H -0.1981 1.0732 0.7891 0.058 Uiso 1 1 calc . . . H9C H -0.1845 0.9952 0.8304 0.058 Uiso 1 1 calc . . . C16 C 0.0715(4) 0.8613(2) 0.67686(14) 0.0274(7) Uani 1 1 d . . . C17 C -0.0876(4) 0.8284(2) 0.67671(15) 0.0283(8) Uani 1 1 d . . . C18 C -0.1678(6) 0.8288(3) 0.6275(2) 0.0421(10) Uani 1 1 d . . . H12 H -0.1250 0.8507 0.5951 0.051 Uiso 1 1 calc . . . C19 C -0.3144(6) 0.7965(4) 0.6260(2) 0.0513(13) Uani 1 1 d . . . H13 H -0.3689 0.7995 0.5931 0.062 Uiso 1 1 calc . . . C20 C -0.3760(5) 0.7609(3) 0.6723(2) 0.0485(12) Uani 1 1 d . . . H14 H -0.4711 0.7379 0.6707 0.058 Uiso 1 1 calc . . . C21 C -0.2963(5) 0.7591(3) 0.7221(2) 0.0408(10) Uani 1 1 d . . . H15 H -0.3389 0.7358 0.7541 0.049 Uiso 1 1 calc . . . C22 C -0.1536(4) 0.7919(3) 0.72395(17) 0.0308(8) Uani 1 1 d . . . H16 H -0.1006 0.7896 0.7573 0.037 Uiso 1 1 calc . . . C15 C 0.1715(5) 0.8069(3) 0.63905(15) 0.0322(8) Uani 1 1 d . . . H17A H 0.1142 0.7786 0.6101 0.039 Uiso 1 1 calc . . . H17B H 0.2476 0.8422 0.6217 0.039 Uiso 1 1 calc . . . C14 C 0.2247(4) 0.7801(2) 0.72951(14) 0.0242(7) Uani 1 1 d . . . C13 C 0.2892(4) 0.7396(2) 0.77407(15) 0.0268(7) Uani 1 1 d . . . H13A H 0.3552 0.6938 0.7705 0.032 Uiso 1 1 calc . . . C1 C 0.1291(4) 0.6991(2) 0.87504(14) 0.0258(7) Uani 1 1 d . . . C2 C -0.0244(5) 0.7045(3) 0.87790(16) 0.0331(8) Uani 1 1 d . . . H21 H -0.0712 0.7539 0.8647 0.040 Uiso 1 1 calc . . . C3 C -0.1081(6) 0.6398(3) 0.89938(18) 0.0440(11) Uani 1 1 d . . . H22 H -0.2109 0.6449 0.9004 0.053 Uiso 1 1 calc . . . C4 C -0.0405(7) 0.5663(3) 0.9196(2) 0.0513(14) Uani 1 1 d . . . H23 H -0.0976 0.5222 0.9348 0.062 Uiso 1 1 calc . . . C5 C 0.1119(8) 0.5583(3) 0.91741(19) 0.0481(12) Uani 1 1 d . . . H24 H 0.1571 0.5086 0.9308 0.058 Uiso 1 1 calc . . . C6 C 0.1981(5) 0.6243(3) 0.89524(18) 0.0354(9) Uani 1 1 d . . . H25 H 0.3008 0.6188 0.8938 0.043 Uiso 1 1 calc . . . C7 C 0.4015(4) 0.7979(2) 0.87983(13) 0.0218(6) Uani 1 1 d . . . C8 C 0.4090(4) 0.7850(2) 0.93737(14) 0.0274(7) Uani 1 1 d . . . H27 H 0.3261 0.7649 0.9565 0.033 Uiso 1 1 calc . . . C9 C 0.5390(5) 0.8017(3) 0.96637(16) 0.0325(8) Uani 1 1 d . . . H28 H 0.5422 0.7924 1.0047 0.039 Uiso 1 1 calc . . . C10 C 0.6634(5) 0.8318(3) 0.93935(19) 0.0366(9) Uani 1 1 d . . . H29 H 0.7506 0.8426 0.9589 0.044 Uiso 1 1 calc . . . C11 C 0.6554(5) 0.8457(3) 0.8822(2) 0.0396(10) Uani 1 1 d . . . H30 H 0.7382 0.8667 0.8635 0.047 Uiso 1 1 calc . . . C12 C 0.5277(4) 0.8290(3) 0.85268(15) 0.0279(7) Uani 1 1 d . . . H31 H 0.5254 0.8385 0.8143 0.033 Uiso 1 1 calc . . . C32 C 0.5256(6) 0.4639(3) 0.7837(2) 0.0519(13) Uani 1 1 d . . . H32A H 0.5956 0.4173 0.7775 0.062 Uiso 1 1 calc . . . H32B H 0.4271 0.4389 0.7860 0.062 Uiso 1 1 calc . . . Cl1 Cl 0.5676(2) 0.51468(14) 0.84765(8) 0.0828(6) Uani 1 1 d . . . Cl2 Cl 0.53257(15) 0.53526(9) 0.72667(7) 0.0585(3) Uani 1 1 d . . . Cl3 Cl -0.1094(6) 0.3636(3) 1.0039(2) 0.1040(6) Uiso 0.50 1 d PD . . C33 C -0.0668(4) 0.4461(3) 1.06710(17) 0.1040(6) Uiso 0.50 1 d PD . . Cl4 Cl -0.0668(4) 0.4461(3) 1.06710(17) 0.1040(6) Uiso 0.50 1 d P . . C34 C 0.1186(5) 0.4140(2) 1.07596(15) 0.1040(6) Uiso 0.50 1 d PD . . Cl5 Cl 0.1186(5) 0.4140(2) 1.07596(15) 0.1040(6) Uiso 0.50 1 d PD . . Cl6 Cl 0.1376(6) 0.3184(3) 1.0289(2) 0.1040(6) Uiso 0.50 1 d PD . . 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 P 0.0217(4) 0.0216(4) 0.0198(4) 0.0009(3) 0.0002(3) 0.0017(3) N1 0.0276(16) 0.0267(15) 0.0199(13) 0.0021(11) -0.0017(11) -0.0031(12) N2 0.0231(14) 0.0234(14) 0.0296(15) 0.0024(12) -0.0021(12) 0.0002(12) Pd 0.02115(10) 0.02041(10) 0.02005(9) 0.00128(10) -0.00109(10) 0.00107(10) O1 0.0330(14) 0.0347(13) 0.0197(12) -0.0040(10) 0.0001(10) -0.0001(11) C23 0.0222(18) 0.0259(16) 0.0228(15) -0.0038(12) -0.0001(12) 0.0024(13) C24 0.0335(19) 0.0298(17) 0.0269(15) -0.0030(16) -0.0003(13) 0.0044(17) C25 0.050(3) 0.047(3) 0.0247(18) -0.0007(17) 0.0032(18) 0.004(2) C26 0.077(4) 0.047(3) 0.033(2) -0.014(2) 0.006(2) 0.017(3) C27 0.080(4) 0.031(2) 0.036(2) -0.0108(17) -0.002(2) 0.015(2) C28 0.041(2) 0.0243(18) 0.0284(18) -0.0045(14) -0.0033(16) 0.0037(16) C29 0.046(2) 0.0233(18) 0.0306(18) -0.0021(14) 0.0009(16) 0.0034(15) C30 0.043(2) 0.030(2) 0.037(2) 0.0133(16) -0.0019(18) 0.0052(18) C31 0.0229(18) 0.033(2) 0.061(3) 0.0048(19) -0.0019(17) 0.0063(16) C16 0.0343(19) 0.0277(17) 0.0200(16) 0.0014(12) -0.0043(13) -0.0047(14) C17 0.033(2) 0.0198(14) 0.0326(19) 0.0002(13) -0.0070(14) 0.0027(13) C18 0.046(3) 0.038(2) 0.043(2) 0.0050(19) -0.015(2) -0.004(2) C19 0.043(3) 0.052(3) 0.059(3) -0.006(2) -0.024(2) -0.002(2) C20 0.027(2) 0.043(2) 0.075(3) -0.014(2) -0.005(2) 0.0001(19) C21 0.033(2) 0.039(2) 0.051(3) -0.013(2) 0.010(2) 0.0000(18) C22 0.0294(19) 0.0309(19) 0.0323(18) -0.0030(15) 0.0030(15) -0.0006(15) C15 0.039(2) 0.038(2) 0.0197(16) 0.0006(14) 0.0023(15) -0.0058(18) C14 0.0236(16) 0.0256(17) 0.0234(15) -0.0006(13) 0.0033(13) -0.0054(14) C13 0.0283(18) 0.0298(18) 0.0223(16) -0.0033(13) 0.0002(14) 0.0050(14) C1 0.0308(19) 0.0224(15) 0.0243(15) -0.0007(12) 0.0016(14) -0.0019(14) C2 0.030(2) 0.041(2) 0.0281(18) -0.0014(16) 0.0020(15) -0.0058(17) C3 0.043(2) 0.054(3) 0.034(2) -0.0084(19) 0.009(2) -0.020(2) C4 0.069(4) 0.040(2) 0.045(3) -0.012(2) 0.015(2) -0.029(3) C5 0.081(4) 0.0236(18) 0.040(2) 0.0014(16) 0.007(3) -0.006(3) C6 0.044(2) 0.0267(18) 0.036(2) 0.0000(15) -0.0036(18) -0.0002(17) C7 0.0223(16) 0.0216(14) 0.0215(13) 0.0011(11) 0.0013(13) 0.0033(14) C8 0.029(2) 0.0327(18) 0.0202(14) 0.0026(13) -0.0012(13) -0.0007(15) C9 0.033(2) 0.035(2) 0.0293(18) -0.0028(16) -0.0092(16) 0.0058(17) C10 0.0290(19) 0.039(2) 0.042(2) 0.0037(18) -0.0125(17) 0.0023(17) C11 0.0270(19) 0.041(2) 0.051(3) 0.014(2) 0.0004(18) -0.0044(17) C12 0.0268(18) 0.0334(19) 0.0234(16) 0.0064(14) -0.0007(14) 0.0013(15) C32 0.046(3) 0.043(3) 0.067(3) -0.010(2) -0.015(3) 0.008(2) Cl1 0.0675(10) 0.1100(14) 0.0708(10) -0.0411(10) 0.0003(8) 0.0040(10) Cl2 0.0403(6) 0.0526(8) 0.0825(10) 0.0087(7) -0.0066(7) 0.0005(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 P C13 1.744(4) . ? P C7 1.816(4) . ? P C1 1.832(4) . ? P Pd 2.2477(10) . ? N1 C14 1.335(5) . ? N1 C16 1.465(4) . ? N1 Pd 2.135(3) . ? N2 C29 1.485(5) . ? N2 C31 1.491(6) . ? N2 C30 1.493(5) . ? N2 Pd 2.166(3) . ? Pd C23 2.014(3) . ? O1 C14 1.377(4) . ? O1 C15 1.450(5) . ? C23 C24 1.392(5) . ? C23 C28 1.408(5) . ? C24 C25 1.396(6) . ? C25 C26 1.373(7) . ? C26 C27 1.348(7) . ? C27 C28 1.412(6) . ? C28 C29 1.489(6) . ? C16 C17 1.522(5) . ? C16 C15 1.530(6) . ? C17 C18 1.381(6) . ? C17 C22 1.397(5) . ? C18 C19 1.413(7) . ? C19 C20 1.355(8) . ? C20 C21 1.392(7) . ? C21 C22 1.383(6) . ? C14 C13 1.368(5) . ? C1 C2 1.387(6) . ? C1 C6 1.403(6) . ? C2 C3 1.358(6) . ? C3 C4 1.380(8) . ? C4 C5 1.379(9) . ? C5 C6 1.390(7) . ? C7 C8 1.393(5) . ? C7 C12 1.396(5) . ? C8 C9 1.386(5) . ? C9 C10 1.376(6) . ? C10 C11 1.385(6) . ? C11 C12 1.376(6) . ? C32 Cl2 1.759(6) . ? C32 Cl1 1.762(6) . ? Cl3 Cl4 2.017(6) . ? Cl3 C33 2.017(6) . ? Cl3 Cl6 2.409(7) . ? C33 Cl5 1.756(6) . ? C33 C34 1.756(6) . ? Cl4 Cl5 1.756(6) . ? Cl4 C34 1.756(6) . ? C34 Cl6 1.869(6) . ? Cl5 Cl6 1.869(6) . ? 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 C13 P C7 107.55(17) . . ? C13 P C1 107.44(18) . . ? C7 P C1 105.07(16) . . ? C13 P Pd 102.61(13) . . ? C7 P Pd 116.51(11) . . ? C1 P Pd 117.03(13) . . ? C14 N1 C16 107.1(3) . . ? C14 N1 Pd 113.7(2) . . ? C16 N1 Pd 135.5(2) . . ? C29 N2 C31 110.1(3) . . ? C29 N2 C30 109.3(3) . . ? C31 N2 C30 107.2(3) . . ? C29 N2 Pd 104.0(2) . . ? C31 N2 Pd 110.0(2) . . ? C30 N2 Pd 116.2(2) . . ? C23 Pd N1 178.62(14) . . ? C23 Pd N2 81.30(13) . . ? N1 Pd N2 99.96(12) . . ? C23 Pd P 95.64(10) . . ? N1 Pd P 83.05(9) . . ? N2 Pd P 174.08(9) . . ? C14 O1 C15 105.8(3) . . ? C24 C23 C28 117.4(3) . . ? C24 C23 Pd 130.4(3) . . ? C28 C23 Pd 112.1(3) . . ? C23 C24 C25 122.0(4) . . ? C26 C25 C24 119.1(4) . . ? C27 C26 C25 121.0(4) . . ? C26 C27 C28 120.9(4) . . ? C23 C28 C27 119.6(4) . . ? C23 C28 C29 117.5(3) . . ? C27 C28 C29 122.8(4) . . ? N2 C29 C28 108.8(3) . . ? N1 C16 C17 114.4(3) . . ? N1 C16 C15 101.6(3) . . ? C17 C16 C15 111.6(3) . . ? C18 C17 C22 118.0(4) . . ? C18 C17 C16 119.6(4) . . ? C22 C17 C16 122.3(3) . . ? C17 C18 C19 120.6(5) . . ? C20 C19 C18 120.4(5) . . ? C19 C20 C21 119.8(4) . . ? C22 C21 C20 119.9(5) . . ? C21 C22 C17 121.2(4) . . ? O1 C15 C16 103.6(3) . . ? N1 C14 C13 126.6(3) . . ? N1 C14 O1 113.7(3) . . ? C13 C14 O1 119.7(3) . . ? C14 C13 P 113.1(3) . . ? C2 C1 C6 118.3(4) . . ? C2 C1 P 120.0(3) . . ? C6 C1 P 121.2(3) . . ? C3 C2 C1 121.9(4) . . ? C2 C3 C4 119.9(5) . . ? C5 C4 C3 120.0(4) . . ? C4 C5 C6 120.3(5) . . ? C5 C6 C1 119.6(5) . . ? C8 C7 C12 118.0(3) . . ? C8 C7 P 124.3(3) . . ? C12 C7 P 117.6(2) . . ? C9 C8 C7 120.6(4) . . ? C10 C9 C8 121.1(4) . . ? C9 C10 C11 118.3(4) . . ? C12 C11 C10 121.4(4) . . ? C11 C12 C7 120.5(3) . . ? Cl2 C32 Cl1 112.6(3) . . ? Cl4 Cl3 C33 0.0(3) . . ? Cl4 Cl3 Cl6 79.8(2) . . ? C33 Cl3 Cl6 79.8(2) . . ? Cl5 C33 C34 0.0(3) . . ? Cl5 C33 Cl3 95.3(3) . . ? C34 C33 Cl3 95.3(3) . . ? Cl5 Cl4 C34 0.0(3) . . ? Cl5 Cl4 Cl3 95.3(3) . . ? C34 Cl4 Cl3 95.3(3) . . ? Cl4 C34 C33 0.0(3) . . ? Cl4 C34 Cl6 103.8(3) . . ? C33 C34 Cl6 103.8(3) . . ? Cl4 Cl5 C33 0.0(3) . . ? Cl4 Cl5 Cl6 103.8(3) . . ? C33 Cl5 Cl6 103.8(3) . . ? Cl5 Cl6 C34 0.0(3) . . ? Cl5 Cl6 Cl3 80.5(2) . . ? C34 Cl6 Cl3 80.5(2) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 34.97 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.038 _refine_diff_density_min -1.355 _refine_diff_density_rms 0.117 data_andreas _database_code_CSD 200358 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H43 Cl N3 O P Pd2, 2(C4 H8 O)' _chemical_formula_sum 'C48 H59 Cl N3 O3 P Pd2' _chemical_formula_weight 1005.20 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' Pd Pd -0.9988 1.0072 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 10.5450(10) _cell_length_b 17.3610(10) _cell_length_c 24.6940(10) _cell_angle_alpha 90.000 _cell_angle_beta 90.000 _cell_angle_gamma 90.000 _cell_volume 4520.8(5) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 24956 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description prism _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.477 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2064 _exptl_absorpt_coefficient_mu 0.934 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34396 _diffrn_reflns_av_R_equivalents 0.0441 _diffrn_reflns_av_sigmaI/netI 0.0564 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 30.04 _reflns_number_total 13096 _reflns_number_gt 10932 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ATOMS (Dowty, 1995)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0646P)^2^+0.2081P] 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(2) _refine_ls_number_reflns 13096 _refine_ls_number_parameters 473 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0556 _refine_ls_R_factor_gt 0.0413 _refine_ls_wR_factor_ref 0.1107 _refine_ls_wR_factor_gt 0.1031 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.033 _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 -0.00710(2) -0.735869(14) -0.147501(11) 0.02587(7) Uani 1 1 d . . . Pd2 Pd 0.23263(3) -0.915199(14) -0.091853(11) 0.02737(7) Uani 1 1 d . . . Cl Cl 0.02371(10) -0.87498(6) -0.06091(4) 0.0439(2) Uani 1 1 d . . . P P 0.12567(8) -0.81795(5) -0.18789(4) 0.02371(18) Uani 1 1 d . . . O O 0.3675(3) -0.72746(15) -0.08492(12) 0.0385(6) Uani 1 1 d . . . N1 N 0.1602(3) -0.70622(17) -0.10285(12) 0.0294(7) Uani 1 1 d . . . N2 N -0.1546(3) -0.67773(18) -0.10134(14) 0.0360(8) Uani 1 1 d . . . N3 N 0.2105(3) -1.02871(18) -0.05806(13) 0.0344(7) Uani 1 1 d . . . C1 C 0.0773(3) -0.9176(2) -0.20031(14) 0.0263(7) Uani 1 1 d . . . C28 C -0.2712(4) -0.7390(2) -0.17409(19) 0.0411(9) Uani 1 1 d . . . C13 C 0.2621(3) -0.81984(19) -0.14232(14) 0.0277(7) Uani 1 1 d . . . H13 H 0.3436 -0.8243 -0.1628 0.033 Uiso 1 1 calc . . . C40 C 0.2367(5) -1.0271(2) 0.00010(16) 0.0445(10) Uani 1 1 d . . . H40A H 0.3209 -1.0049 0.0064 0.067 Uiso 1 1 calc . . . H40B H 0.2341 -1.0796 0.0145 0.067 Uiso 1 1 calc . . . H40C H 0.1725 -0.9956 0.0184 0.067 Uiso 1 1 calc . . . C8 C 0.2527(4) -0.7171(2) -0.25681(15) 0.0334(8) Uani 1 1 d . . . H8 H 0.2680 -0.6883 -0.2248 0.040 Uiso 1 1 calc . . . C24 C -0.1486(4) -0.7620(2) -0.25464(17) 0.0361(9) Uani 1 1 d . . . H24 H -0.0700 -0.7713 -0.2723 0.043 Uiso 1 1 calc . . . C10 C 0.2728(4) -0.7307(3) -0.35263(17) 0.0444(10) Uani 1 1 d . . . H10 H 0.3013 -0.7111 -0.3864 0.053 Uiso 1 1 calc . . . C32 C 0.4112(4) -0.9489(2) -0.10094(15) 0.0293(8) Uani 1 1 d . . . C2 C 0.1682(4) -0.9719(2) -0.21518(16) 0.0324(8) Uani 1 1 d . . . H2 H 0.2548 -0.9571 -0.2174 0.039 Uiso 1 1 calc . . . C5 C -0.0845(4) -1.0147(2) -0.20771(18) 0.0369(9) Uani 1 1 d . . . H5 H -0.1708 -1.0298 -0.2048 0.044 Uiso 1 1 calc . . . C7 C 0.1872(3) -0.7872(2) -0.25346(14) 0.0270(7) Uani 1 1 d . . . C37 C 0.4260(4) -1.0298(2) -0.09350(17) 0.0347(8) Uani 1 1 d . . . C17 C 0.1497(4) -0.5655(2) -0.08046(15) 0.0315(8) Uani 1 1 d . . . C27 C -0.3821(4) -0.7369(3) -0.2039(2) 0.0505(12) Uani 1 1 d . . . H27 H -0.4612 -0.7293 -0.1863 0.061 Uiso 1 1 calc . . . C33 C 0.5202(4) -0.9055(2) -0.10690(16) 0.0355(8) Uani 1 1 d . . . H33 H 0.5130 -0.8513 -0.1110 0.043 Uiso 1 1 calc . . . C11 C 0.2101(4) -0.7995(3) -0.35069(17) 0.0444(10) Uani 1 1 d . . . H11 H 0.1965 -0.8281 -0.3830 0.053 Uiso 1 1 calc . . . C39 C 0.0852(5) -1.0623(3) -0.0678(2) 0.0480(11) Uani 1 1 d . . . H39A H 0.0670 -1.0615 -0.1067 0.072 Uiso 1 1 calc . . . H39B H 0.0208 -1.0323 -0.0485 0.072 Uiso 1 1 calc . . . H39C H 0.0840 -1.1156 -0.0548 0.072 Uiso 1 1 calc . . . C22 C 0.1551(4) -0.5414(2) -0.13418(16) 0.0388(9) Uani 1 1 d . . . H22 H 0.1853 -0.5752 -0.1615 0.047 Uiso 1 1 calc . . . C16 C 0.1970(4) -0.6456(2) -0.06426(16) 0.0369(9) Uani 1 1 d . . . H16 H 0.1629 -0.6588 -0.0276 0.044 Uiso 1 1 calc . . . C6 C -0.0487(4) -0.9391(2) -0.19653(16) 0.0313(8) Uani 1 1 d . . . H6 H -0.1109 -0.9023 -0.1863 0.038 Uiso 1 1 calc . . . C12 C 0.1663(4) -0.8274(2) -0.30153(16) 0.0360(9) Uani 1 1 d . . . H12 H 0.1213 -0.8748 -0.3006 0.043 Uiso 1 1 calc . . . C30 C -0.1783(4) -0.5976(2) -0.11861(18) 0.0394(9) Uani 1 1 d . . . H30A H -0.1037 -0.5659 -0.1105 0.059 Uiso 1 1 calc . . . H30B H -0.2520 -0.5772 -0.0992 0.059 Uiso 1 1 calc . . . H30C H -0.1948 -0.5964 -0.1577 0.059 Uiso 1 1 calc . . . C14 C 0.2582(4) -0.74991(19) -0.10991(15) 0.0285(7) Uani 1 1 d . . . C23 C -0.1519(4) -0.7520(2) -0.19876(17) 0.0318(8) Uani 1 1 d . . . C38 C 0.3075(4) -1.0752(2) -0.08665(18) 0.0414(9) Uani 1 1 d . . . H38A H 0.2748 -1.0908 -0.1226 0.050 Uiso 1 1 calc . . . H38B H 0.3258 -1.1225 -0.0656 0.050 Uiso 1 1 calc . . . C20 C 0.0727(4) -0.4179(2) -0.10890(19) 0.0436(10) Uani 1 1 d . . . H20 H 0.0461 -0.3676 -0.1188 0.052 Uiso 1 1 calc . . . C18 C 0.1064(4) -0.5145(2) -0.04106(17) 0.0394(9) Uani 1 1 d . . . H18 H 0.1036 -0.5302 -0.0042 0.047 Uiso 1 1 calc . . . C9 C 0.2951(4) -0.6894(2) -0.30575(18) 0.0386(9) Uani 1 1 d . . . H9 H 0.3398 -0.6420 -0.3073 0.046 Uiso 1 1 calc . . . C36 C 0.5468(4) -1.0630(2) -0.09392(19) 0.0421(10) Uani 1 1 d . . . H36 H 0.5553 -1.1171 -0.0894 0.051 Uiso 1 1 calc . . . C25 C -0.2594(5) -0.7586(2) -0.2845(2) 0.0494(11) Uani 1 1 d . . . H25 H -0.2555 -0.7650 -0.3227 0.059 Uiso 1 1 calc . . . C21 C 0.1158(5) -0.4671(3) -0.14735(19) 0.0457(10) Uani 1 1 d . . . H21 H 0.1193 -0.4506 -0.1840 0.055 Uiso 1 1 calc . . . C15 C 0.3411(5) -0.6518(2) -0.0632(2) 0.0465(11) Uani 1 1 d . . . H15A H 0.3802 -0.6113 -0.0859 0.056 Uiso 1 1 calc . . . H15B H 0.3736 -0.6470 -0.0258 0.056 Uiso 1 1 calc . . . C4 C 0.0084(5) -1.0683(2) -0.22335(17) 0.0397(9) Uani 1 1 d . . . H4 H -0.0155 -1.1197 -0.2317 0.048 Uiso 1 1 calc . . . C29 C -0.2676(4) -0.7253(3) -0.1139(2) 0.0462(10) Uani 1 1 d . . . H29A H -0.3456 -0.6982 -0.1022 0.055 Uiso 1 1 calc . . . H29B H -0.2628 -0.7750 -0.0945 0.055 Uiso 1 1 calc . . . C3 C 0.1343(4) -1.0467(2) -0.22661(17) 0.0385(9) Uani 1 1 d . . . H3 H 0.1970 -1.0832 -0.2367 0.046 Uiso 1 1 calc . . . C35 C 0.6532(4) -1.0186(3) -0.10076(18) 0.0456(11) Uani 1 1 d . . . H35 H 0.7346 -1.0420 -0.1012 0.055 Uiso 1 1 calc . . . C34 C 0.6417(4) -0.9393(3) -0.10702(18) 0.0424(10) Uani 1 1 d . . . H34 H 0.7151 -0.9081 -0.1113 0.051 Uiso 1 1 calc . . . C31 C -0.1315(5) -0.6777(3) -0.04134(19) 0.0486(11) Uani 1 1 d . . . H31A H -0.0594 -0.6441 -0.0330 0.073 Uiso 1 1 calc . . . H31B H -0.1126 -0.7303 -0.0293 0.073 Uiso 1 1 calc . . . H31C H -0.2073 -0.6588 -0.0226 0.073 Uiso 1 1 calc . . . C19 C 0.0673(4) -0.4407(2) -0.05545(19) 0.0417(10) Uani 1 1 d . . . H19 H 0.0370 -0.4062 -0.0286 0.050 Uiso 1 1 calc . . . C26 C -0.3772(5) -0.7458(3) -0.2599(3) 0.0587(14) Uani 1 1 d . . . H26 H -0.4524 -0.7433 -0.2810 0.070 Uiso 1 1 calc . . . O1 O 0.4933(8) -0.4212(4) -0.1987(3) 0.158(3) Uiso 1 1 d D . . C41 C 0.4287(8) -0.4456(4) -0.2448(3) 0.102(2) Uiso 1 1 d D . . H41A H 0.4838 -0.4412 -0.2771 0.123 Uiso 1 1 calc . . . H41B H 0.3520 -0.4138 -0.2506 0.123 Uiso 1 1 calc . . . C42 C 0.3921(7) -0.5300(3) -0.2349(3) 0.093(2) Uiso 1 1 d D . . H42A H 0.3083 -0.5348 -0.2172 0.111 Uiso 1 1 calc . . . H42B H 0.3927 -0.5605 -0.2688 0.111 Uiso 1 1 calc . . . C43 C 0.5009(9) -0.5530(5) -0.1969(4) 0.149(4) Uiso 1 1 d D . . H43A H 0.5685 -0.5793 -0.2176 0.179 Uiso 1 1 calc . . . H43B H 0.4693 -0.5888 -0.1688 0.179 Uiso 1 1 calc . . . C44 C 0.5540(9) -0.4799(5) -0.1702(4) 0.127(3) Uiso 1 1 d D . . H44A H 0.5326 -0.4780 -0.1312 0.152 Uiso 1 1 calc . . . H44B H 0.6472 -0.4767 -0.1744 0.152 Uiso 1 1 calc . . . O2 O 0.5067(5) -1.2560(3) -0.0257(2) 0.1098(17) Uiso 1 1 d D . . C45 C 0.4135(5) -1.2566(4) 0.0141(2) 0.0737(17) Uiso 1 1 d D . . H45A H 0.3705 -1.2060 0.0159 0.088 Uiso 1 1 calc . . . H45B H 0.4513 -1.2678 0.0499 0.088 Uiso 1 1 calc . . . C46 C 0.3186(7) -1.3199(4) -0.0017(3) 0.098(2) Uiso 1 1 d D . . H46A H 0.2355 -1.2967 -0.0107 0.118 Uiso 1 1 calc . . . H46B H 0.3067 -1.3561 0.0289 0.118 Uiso 1 1 calc . . . C48 C 0.4745(7) -1.3045(4) -0.0683(2) 0.094(2) Uiso 1 1 d D . . H48A H 0.5510 -1.3326 -0.0807 0.113 Uiso 1 1 calc . . . H48B H 0.4426 -1.2734 -0.0990 0.113 Uiso 1 1 calc . . . C47 C 0.3724(7) -1.3628(4) -0.0511(3) 0.110(3) Uiso 1 1 d D . . H47A H 0.4096 -1.4131 -0.0410 0.132 Uiso 1 1 calc . . . H47B H 0.3076 -1.3703 -0.0796 0.132 Uiso 1 1 calc . . . 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 0.02784(12) 0.02347(12) 0.02630(13) -0.00185(10) 0.00078(11) 0.00114(11) Pd2 0.03174(13) 0.02493(12) 0.02545(13) 0.00257(11) 0.00060(11) 0.00082(11) Cl 0.0444(6) 0.0442(5) 0.0429(6) 0.0075(4) 0.0175(5) 0.0072(4) P 0.0255(4) 0.0226(4) 0.0230(4) -0.0002(3) 0.0004(3) -0.0013(3) O 0.0411(14) 0.0350(14) 0.0395(16) -0.0036(13) -0.0151(13) -0.0021(12) N1 0.0366(16) 0.0275(14) 0.0240(16) -0.0013(12) -0.0055(13) 0.0016(13) N2 0.0411(18) 0.0307(15) 0.036(2) 0.0003(14) 0.0092(14) 0.0052(14) N3 0.0444(19) 0.0294(15) 0.0295(16) 0.0022(13) 0.0016(14) -0.0018(14) C1 0.0345(17) 0.0213(15) 0.0231(16) -0.0012(14) -0.0005(13) -0.0025(14) C28 0.0319(18) 0.0310(18) 0.061(3) -0.0069(19) 0.0056(19) -0.0022(17) C13 0.0297(16) 0.0289(15) 0.0246(16) 0.0022(14) -0.0035(14) -0.0002(14) C40 0.061(3) 0.0395(19) 0.033(2) 0.0113(17) 0.004(2) -0.001(2) C8 0.035(2) 0.0300(17) 0.0350(19) 0.0035(15) 0.0006(16) -0.0013(16) C24 0.038(2) 0.0283(18) 0.042(2) -0.0034(17) -0.0078(17) 0.0047(17) C10 0.041(2) 0.059(3) 0.033(2) 0.013(2) 0.0075(19) -0.005(2) C32 0.0325(18) 0.0311(18) 0.0244(19) 0.0008(15) -0.0005(14) 0.0055(15) C2 0.0355(19) 0.0301(18) 0.032(2) -0.0006(15) 0.0018(16) 0.0008(15) C5 0.041(2) 0.033(2) 0.037(2) 0.0022(17) -0.0019(17) -0.0035(17) C7 0.0259(16) 0.0302(17) 0.0249(17) 0.0059(14) 0.0021(13) 0.0014(14) C37 0.051(2) 0.0274(17) 0.0255(18) -0.0016(16) 0.0034(18) 0.0061(16) C17 0.041(2) 0.0237(16) 0.0295(19) -0.0030(14) -0.0072(15) -0.0029(15) C27 0.0263(18) 0.040(2) 0.085(4) -0.011(2) -0.001(2) 0.0016(18) C33 0.036(2) 0.0373(19) 0.0329(19) 0.0049(15) -0.0012(16) 0.0041(17) C11 0.054(3) 0.056(3) 0.0235(19) 0.0004(19) 0.0040(19) -0.010(2) C39 0.050(3) 0.039(2) 0.055(3) 0.011(2) -0.003(2) -0.013(2) C22 0.056(3) 0.0328(19) 0.028(2) -0.0015(16) -0.0024(18) 0.0069(19) C16 0.058(3) 0.0300(18) 0.0225(18) -0.0008(15) -0.0060(17) 0.0036(18) C6 0.0330(18) 0.0317(18) 0.0294(19) 0.0042(15) 0.0008(15) -0.0016(15) C12 0.037(2) 0.040(2) 0.031(2) -0.0044(17) 0.0015(17) -0.0089(17) C30 0.043(2) 0.036(2) 0.039(2) -0.0052(18) 0.0025(18) 0.0093(18) C14 0.0313(17) 0.0244(17) 0.0299(17) 0.0052(13) -0.0092(14) -0.0034(14) C23 0.0305(17) 0.0220(17) 0.043(2) -0.0003(15) -0.0065(16) 0.0020(14) C38 0.058(3) 0.0255(17) 0.041(2) 0.0035(18) 0.004(2) 0.0034(17) C20 0.049(2) 0.0310(19) 0.051(3) -0.0013(19) -0.009(2) 0.0079(19) C18 0.052(2) 0.033(2) 0.033(2) 0.0004(17) -0.0018(19) -0.0002(19) C9 0.037(2) 0.036(2) 0.043(2) 0.0131(18) 0.0056(17) -0.0040(16) C36 0.053(2) 0.036(2) 0.037(2) -0.0036(18) 0.005(2) 0.0167(18) C25 0.051(3) 0.042(2) 0.055(3) -0.008(2) -0.021(2) 0.009(2) C21 0.061(3) 0.044(2) 0.032(2) 0.0051(19) -0.004(2) 0.001(2) C15 0.058(3) 0.032(2) 0.050(3) -0.0051(19) -0.029(2) -0.001(2) C4 0.053(2) 0.0286(18) 0.037(2) -0.0018(15) 0.000(2) -0.0084(19) C29 0.036(2) 0.046(2) 0.056(3) -0.005(2) 0.015(2) 0.001(2) C3 0.048(2) 0.0345(19) 0.033(2) -0.0081(17) 0.0019(18) 0.0042(18) C35 0.043(2) 0.057(3) 0.037(2) 0.000(2) 0.0083(19) 0.024(2) C34 0.037(2) 0.052(2) 0.039(2) -0.0008(19) 0.0034(17) 0.0062(19) C31 0.061(3) 0.048(2) 0.036(2) 0.002(2) 0.011(2) 0.007(2) C19 0.049(2) 0.034(2) 0.042(2) -0.0071(18) 0.0047(19) 0.0003(18) C26 0.043(2) 0.044(3) 0.088(4) -0.018(3) -0.026(3) 0.005(2) _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 C23 2.003(4) . ? Pd1 N1 2.143(3) . ? Pd1 N2 2.176(3) . ? Pd1 P 2.2329(9) . ? Pd2 C32 1.984(4) . ? Pd2 C13 2.095(3) . ? Pd2 N3 2.153(3) . ? Pd2 Cl 2.4342(11) . ? P C7 1.824(4) . ? P C13 1.827(4) . ? P C1 1.829(4) . ? O C14 1.364(4) . ? O C15 1.446(5) . ? N1 C14 1.294(5) . ? N1 C16 1.472(5) . ? N2 C30 1.477(5) . ? N2 C29 1.483(6) . ? N2 C31 1.501(6) . ? N3 C40 1.463(5) . ? N3 C39 1.465(6) . ? N3 C38 1.482(5) . ? C1 C6 1.384(5) . ? C1 C2 1.394(5) . ? C28 C27 1.382(6) . ? C28 C23 1.416(6) . ? C28 C29 1.505(6) . ? C13 C14 1.455(5) . ? C8 C9 1.376(5) . ? C8 C7 1.401(5) . ? C24 C25 1.383(6) . ? C24 C23 1.391(6) . ? C10 C11 1.366(6) . ? C10 C9 1.381(6) . ? C32 C33 1.382(6) . ? C32 C37 1.425(5) . ? C2 C3 1.376(5) . ? C5 C6 1.392(5) . ? C5 C4 1.405(6) . ? C7 C12 1.395(5) . ? C37 C36 1.398(6) . ? C37 C38 1.486(6) . ? C17 C18 1.392(6) . ? C17 C22 1.392(5) . ? C17 C16 1.530(5) . ? C27 C26 1.392(8) . ? C33 C34 1.408(6) . ? C11 C12 1.386(6) . ? C22 C21 1.394(6) . ? C16 C15 1.523(6) . ? C20 C21 1.355(6) . ? C20 C19 1.379(6) . ? C18 C19 1.393(6) . ? C36 C35 1.371(7) . ? C25 C26 1.402(7) . ? C4 C3 1.382(6) . ? C35 C34 1.391(7) . ? O1 C41 1.392(2) . ? O1 C44 1.394(2) . ? C41 C42 1.536(2) . ? C42 C43 1.536(2) . ? C43 C44 1.536(2) . ? O2 C45 1.389(2) . ? O2 C48 1.390(2) . ? C45 C46 1.535(2) . ? C46 C47 1.539(2) . ? C48 C47 1.537(2) . ? 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 C23 Pd1 N1 170.48(14) . . ? C23 Pd1 N2 81.45(15) . . ? N1 Pd1 N2 101.97(13) . . ? C23 Pd1 P 96.10(11) . . ? N1 Pd1 P 82.35(9) . . ? N2 Pd1 P 167.95(9) . . ? C32 Pd2 C13 91.43(15) . . ? C32 Pd2 N3 82.91(14) . . ? C13 Pd2 N3 165.90(13) . . ? C32 Pd2 Cl 168.19(11) . . ? C13 Pd2 Cl 95.42(10) . . ? N3 Pd2 Cl 92.46(9) . . ? C7 P C13 105.76(16) . . ? C7 P C1 103.13(16) . . ? C13 P C1 107.81(16) . . ? C7 P Pd1 115.64(12) . . ? C13 P Pd1 103.31(12) . . ? C1 P Pd1 120.25(12) . . ? C14 O C15 105.3(3) . . ? C14 N1 C16 107.2(3) . . ? C14 N1 Pd1 116.6(2) . . ? C16 N1 Pd1 136.2(3) . . ? C30 N2 C29 109.1(3) . . ? C30 N2 C31 108.2(3) . . ? C29 N2 C31 109.7(3) . . ? C30 N2 Pd1 114.0(3) . . ? C29 N2 Pd1 101.9(2) . . ? C31 N2 Pd1 113.6(3) . . ? C40 N3 C39 109.9(3) . . ? C40 N3 C38 110.4(3) . . ? C39 N3 C38 109.1(3) . . ? C40 N3 Pd2 110.0(2) . . ? C39 N3 Pd2 113.5(3) . . ? C38 N3 Pd2 103.8(2) . . ? C6 C1 C2 119.7(3) . . ? C6 C1 P 120.8(3) . . ? C2 C1 P 119.5(3) . . ? C27 C28 C23 121.8(4) . . ? C27 C28 C29 122.8(4) . . ? C23 C28 C29 115.3(4) . . ? C14 C13 P 107.6(2) . . ? C14 C13 Pd2 109.1(2) . . ? P C13 Pd2 105.28(17) . . ? C9 C8 C7 121.0(4) . . ? C25 C24 C23 120.2(4) . . ? C11 C10 C9 120.4(4) . . ? C33 C32 C37 117.4(3) . . ? C33 C32 Pd2 129.8(3) . . ? C37 C32 Pd2 112.3(3) . . ? C3 C2 C1 120.9(4) . . ? C6 C5 C4 119.3(4) . . ? C12 C7 C8 117.5(3) . . ? C12 C7 P 123.5(3) . . ? C8 C7 P 118.8(3) . . ? C36 C37 C32 120.3(4) . . ? C36 C37 C38 123.3(3) . . ? C32 C37 C38 116.4(3) . . ? C18 C17 C22 119.2(3) . . ? C18 C17 C16 120.1(3) . . ? C22 C17 C16 120.6(3) . . ? C28 C27 C26 119.6(4) . . ? C32 C33 C34 122.0(4) . . ? C10 C11 C12 119.8(4) . . ? C17 C22 C21 119.3(4) . . ? N1 C16 C15 102.9(3) . . ? N1 C16 C17 113.2(3) . . ? C15 C16 C17 113.2(4) . . ? C1 C6 C5 120.1(4) . . ? C11 C12 C7 121.2(4) . . ? N1 C14 O 116.5(3) . . ? N1 C14 C13 125.9(3) . . ? O C14 C13 117.6(3) . . ? C24 C23 C28 118.0(4) . . ? C24 C23 Pd1 128.7(3) . . ? C28 C23 Pd1 112.5(3) . . ? N3 C38 C37 110.2(3) . . ? C21 C20 C19 120.3(4) . . ? C17 C18 C19 120.3(4) . . ? C8 C9 C10 120.0(4) . . ? C35 C36 C37 121.0(4) . . ? C24 C25 C26 121.6(4) . . ? C20 C21 C22 121.3(4) . . ? O C15 C16 104.5(3) . . ? C3 C4 C5 120.4(3) . . ? N2 C29 C28 108.4(3) . . ? C2 C3 C4 119.6(4) . . ? C36 C35 C34 119.9(4) . . ? C35 C34 C33 119.4(4) . . ? C20 C19 C18 119.7(4) . . ? C27 C26 C25 118.8(4) . . ? C41 O1 C44 114.6(7) . . ? O1 C41 C42 106.5(6) . . ? C43 C42 C41 99.0(6) . . ? C42 C43 C44 108.7(6) . . ? O1 C44 C43 102.7(7) . . ? C45 O2 C48 111.0(5) . . ? O2 C45 C46 106.7(5) . . ? C45 C46 C47 107.9(5) . . ? O2 C48 C47 111.1(6) . . ? C48 C47 C46 99.2(5) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 30.04 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.250 _refine_diff_density_min -0.740 _refine_diff_density_rms 0.110 data_bris4 _database_code_CSD 200359 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H20 Cl2 N O P Pd, C H2 Cl2' _chemical_formula_sum 'C23 H22 Cl4 N O P Pd' _chemical_formula_weight 607.59 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 8.541(5) _cell_length_b 13.825(5) _cell_length_c 20.676(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2441.4(18) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 35245 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.653 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1216 _exptl_absorpt_coefficient_mu 1.280 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _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 '\p scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5580 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0873 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.58 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5579 _reflns_number_gt 4479 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ATOMS V6 (Dowty, 2002)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0000P)^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 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 -0.03(3) _refine_ls_number_reflns 5579 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0464 _refine_ls_R_factor_gt 0.0307 _refine_ls_wR_factor_ref 0.0698 _refine_ls_wR_factor_gt 0.0635 _refine_ls_goodness_of_fit_ref 0.754 _refine_ls_restrained_S_all 0.754 _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 Pd Pd 1.05569(3) 0.212543(18) -0.110080(12) 0.02447(7) Uani 1 1 d . . . P P 0.83051(11) 0.27133(6) -0.14504(4) 0.0250(2) Uani 1 1 d . . . Cl1 Cl 1.29035(11) 0.15113(7) -0.06572(5) 0.0363(2) Uani 1 1 d . . . Cl2 Cl 1.18570(11) 0.29982(7) -0.18756(4) 0.0366(2) Uani 1 1 d . . . Cl3 Cl 0.54386(18) -0.14338(10) -0.06282(6) 0.0680(4) Uani 1 1 d . . . Cl4 Cl 0.55334(16) -0.02717(10) -0.18027(6) 0.0685(4) Uani 1 1 d . . . N N 0.9165(4) 0.1404(2) -0.04651(13) 0.0270(7) Uani 1 1 d . . . O O 0.6834(3) 0.10783(17) -0.00198(12) 0.0341(6) Uani 1 1 d . . . C17 C 0.9900(4) -0.0333(2) -0.04513(17) 0.0275(8) Uani 1 1 d . . . C1 C 0.8216(4) 0.4002(2) -0.15465(17) 0.0279(8) Uani 1 1 d . . . C16 C 0.9489(5) 0.0553(2) -0.00513(16) 0.0287(8) Uani 1 1 d . . . H11 H 1.0351 0.0702 0.0245 0.034 Uiso 1 1 calc . . . C7 C 0.7487(4) 0.2140(3) -0.21595(16) 0.0270(7) Uani 1 1 d . . . C14 C 0.7705(5) 0.1607(3) -0.04237(17) 0.0287(8) Uani 1 1 d . . . C12 C 0.8274(5) 0.1380(3) -0.24463(17) 0.0309(8) Uani 1 1 d . . . H14 H 0.9258 0.1201 -0.2295 0.037 Uiso 1 1 calc . . . C13 C 0.6946(4) 0.2399(2) -0.07943(17) 0.0296(8) Uani 1 1 d . . . H15A H 0.6763 0.2955 -0.0518 0.036 Uiso 1 1 calc . . . H15B H 0.5951 0.2186 -0.0969 0.036 Uiso 1 1 calc . . . C3 C 0.8669(4) 0.5575(3) -0.1084(2) 0.0385(9) Uani 1 1 d . . . H16 H 0.8942 0.5957 -0.0731 0.046 Uiso 1 1 calc . . . C11 C 0.7601(5) 0.0880(3) -0.29625(19) 0.0389(10) Uani 1 1 d . . . H17 H 0.8120 0.0360 -0.3150 0.047 Uiso 1 1 calc . . . C18 C 0.9380(5) -0.0452(2) -0.10825(18) 0.0356(8) Uani 1 1 d . . . H18 H 0.8763 0.0022 -0.1273 0.043 Uiso 1 1 calc . . . C8 C 0.6020(5) 0.2409(3) -0.23875(19) 0.0365(10) Uani 1 1 d . . . H19 H 0.5473 0.2908 -0.2188 0.044 Uiso 1 1 calc . . . C22 C 1.0801(5) -0.1044(3) -0.01742(18) 0.0370(10) Uani 1 1 d . . . H20 H 1.1147 -0.0972 0.0250 0.044 Uiso 1 1 calc . . . C4 C 0.8323(5) 0.6004(3) -0.1668(2) 0.0386(10) Uani 1 1 d . . . H21 H 0.8359 0.6673 -0.1708 0.046 Uiso 1 1 calc . . . C20 C 1.0689(5) -0.1977(3) -0.1144(2) 0.0497(11) Uani 1 1 d . . . H22 H 1.0961 -0.2527 -0.1377 0.060 Uiso 1 1 calc . . . C5 C 0.7927(5) 0.5449(3) -0.2189(2) 0.0386(10) Uani 1 1 d . . . H23 H 0.7681 0.5743 -0.2581 0.046 Uiso 1 1 calc . . . C15 C 0.7944(5) 0.0468(3) 0.03327(18) 0.0362(10) Uani 1 1 d . . . H24A H 0.7586 -0.0197 0.0345 0.043 Uiso 1 1 calc . . . H24B H 0.8080 0.0698 0.0772 0.043 Uiso 1 1 calc . . . C6 C 0.7890(5) 0.4437(3) -0.21366(18) 0.0334(9) Uani 1 1 d . . . H26 H 0.7649 0.4060 -0.2495 0.040 Uiso 1 1 calc . . . C9 C 0.5379(5) 0.1932(3) -0.2911(2) 0.0432(10) Uani 1 1 d . . . H28 H 0.4416 0.2128 -0.3075 0.052 Uiso 1 1 calc . . . C2 C 0.8613(4) 0.4581(3) -0.10186(18) 0.0329(9) Uani 1 1 d . . . H29 H 0.8841 0.4297 -0.0622 0.040 Uiso 1 1 calc . . . C10 C 0.6163(6) 0.1165(3) -0.31904(19) 0.0477(12) Uani 1 1 d . . . H2 H 0.5713 0.0839 -0.3537 0.057 Uiso 1 1 calc . . . C21 C 1.1202(6) -0.1870(3) -0.0520(2) 0.0483(12) Uani 1 1 d . . . H1 H 1.1814 -0.2347 -0.0329 0.058 Uiso 1 1 calc . . . C23 C 0.4399(6) -0.0700(3) -0.1170(2) 0.0601(12) Uani 1 1 d . . . H3A H 0.3530 -0.1068 -0.1346 0.072 Uiso 1 1 calc . . . H3B H 0.3968 -0.0154 -0.0935 0.072 Uiso 1 1 calc . . . C19 C 0.9774(5) -0.1275(3) -0.1431(2) 0.0473(11) Uani 1 1 d . . . H5 H 0.9424 -0.1352 -0.1853 0.057 Uiso 1 1 calc . . . 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 Pd 0.02442(13) 0.02364(12) 0.02536(12) -0.00034(12) 0.00188(12) 0.00006(12) P 0.0255(5) 0.0235(5) 0.0262(4) 0.0010(4) 0.0019(4) 0.0005(4) Cl1 0.0285(5) 0.0422(6) 0.0381(5) 0.0033(5) -0.0019(4) 0.0043(4) Cl2 0.0335(5) 0.0409(6) 0.0355(5) 0.0088(4) 0.0081(4) -0.0026(5) Cl3 0.0737(9) 0.0805(9) 0.0498(7) 0.0197(6) -0.0072(7) -0.0023(9) Cl4 0.0521(7) 0.0932(10) 0.0603(7) 0.0334(7) -0.0099(7) -0.0209(8) N 0.0290(18) 0.0226(15) 0.0293(16) -0.0032(12) 0.0024(13) -0.0004(14) O 0.0332(15) 0.0339(14) 0.0352(14) 0.0078(12) 0.0072(13) -0.0038(13) C17 0.030(2) 0.0230(18) 0.0290(19) 0.0003(15) 0.0013(15) -0.0066(15) C1 0.028(2) 0.0245(18) 0.031(2) 0.0021(15) 0.0030(17) -0.0005(16) C16 0.034(2) 0.0241(17) 0.0279(17) 0.0038(14) -0.0028(19) 0.0024(18) C7 0.0280(19) 0.0245(17) 0.0285(17) 0.0016(17) 0.0033(15) -0.0027(17) C14 0.032(2) 0.026(2) 0.0277(19) 0.0004(16) 0.0035(16) -0.0007(17) C12 0.030(2) 0.0297(19) 0.033(2) 0.0014(17) 0.0019(17) -0.0019(18) C13 0.032(2) 0.0253(19) 0.0312(18) -0.0015(15) 0.0074(16) 0.0028(16) C3 0.039(2) 0.034(2) 0.043(2) -0.011(2) 0.003(2) -0.0061(17) C11 0.043(3) 0.039(2) 0.035(2) -0.0120(19) 0.0082(19) -0.006(2) C18 0.039(2) 0.0342(19) 0.0334(19) -0.0025(17) -0.006(2) -0.0027(19) C8 0.035(2) 0.031(2) 0.044(2) 0.0000(18) 0.0002(17) -0.0017(17) C22 0.043(3) 0.031(2) 0.037(2) 0.0031(17) -0.001(2) 0.0017(19) C4 0.030(2) 0.0222(19) 0.064(3) 0.000(2) 0.001(2) -0.0018(17) C20 0.049(3) 0.031(2) 0.069(3) -0.017(2) 0.017(3) -0.010(2) C5 0.034(2) 0.032(2) 0.049(2) 0.0145(19) -0.0039(19) 0.0023(18) C15 0.044(3) 0.033(2) 0.031(2) 0.0057(17) 0.0064(19) 0.0029(19) C6 0.032(2) 0.030(2) 0.038(2) -0.0009(17) -0.0046(18) -0.0013(18) C9 0.039(3) 0.042(2) 0.049(2) 0.0024(19) -0.008(2) -0.010(2) C2 0.035(2) 0.0322(19) 0.032(2) 0.0025(17) 0.0024(17) -0.0011(17) C10 0.058(3) 0.053(3) 0.032(2) -0.008(2) 0.000(2) -0.023(2) C21 0.050(3) 0.028(2) 0.067(3) 0.006(2) 0.013(2) 0.0040(18) C23 0.058(3) 0.054(3) 0.068(3) 0.020(2) 0.011(3) 0.007(3) C19 0.054(3) 0.048(3) 0.040(2) -0.014(2) 0.002(2) -0.012(2) _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 Pd N 2.034(3) . ? Pd P 2.2095(14) . ? Pd Cl2 2.2924(10) . ? Pd Cl1 2.3620(14) . ? P C1 1.794(4) . ? P C7 1.807(4) . ? P C13 1.837(4) . ? Cl3 C23 1.752(5) . ? Cl4 C23 1.732(5) . ? N C14 1.281(5) . ? N C16 1.480(4) . ? O C14 1.336(4) . ? O C15 1.464(4) . ? C17 C22 1.373(5) . ? C17 C18 1.388(5) . ? C17 C16 1.519(5) . ? C1 C6 1.388(5) . ? C1 C2 1.395(5) . ? C16 C15 1.544(6) . ? C7 C12 1.382(5) . ? C7 C8 1.389(5) . ? C14 C13 1.486(5) . ? C12 C11 1.396(5) . ? C3 C4 1.378(6) . ? C3 C2 1.381(5) . ? C11 C10 1.373(6) . ? C18 C19 1.387(5) . ? C8 C9 1.380(5) . ? C22 C21 1.390(6) . ? C4 C5 1.365(6) . ? C20 C21 1.371(6) . ? C20 C19 1.379(6) . ? C5 C6 1.404(5) . ? C9 C10 1.381(6) . ? 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 N Pd P 83.28(9) . . ? N Pd Cl2 173.20(9) . . ? P Pd Cl2 89.97(5) . . ? N Pd Cl1 93.95(10) . . ? P Pd Cl1 176.25(3) . . ? Cl2 Pd Cl1 92.84(5) . . ? C1 P C7 109.20(17) . . ? C1 P C13 106.82(16) . . ? C7 P C13 104.55(16) . . ? C1 P Pd 116.01(13) . . ? C7 P Pd 116.15(12) . . ? C13 P Pd 102.79(13) . . ? C14 N C16 108.5(3) . . ? C14 N Pd 120.3(3) . . ? C16 N Pd 130.8(2) . . ? C14 O C15 105.4(3) . . ? C22 C17 C18 119.1(3) . . ? C22 C17 C16 118.7(3) . . ? C18 C17 C16 122.3(3) . . ? C6 C1 C2 119.2(3) . . ? C6 C1 P 122.4(3) . . ? C2 C1 P 118.2(3) . . ? N C16 C17 111.7(3) . . ? N C16 C15 101.4(3) . . ? C17 C16 C15 114.6(3) . . ? C12 C7 C8 119.8(3) . . ? C12 C7 P 119.6(3) . . ? C8 C7 P 120.5(3) . . ? N C14 O 117.7(3) . . ? N C14 C13 123.5(3) . . ? O C14 C13 118.9(3) . . ? C7 C12 C11 120.3(4) . . ? C14 C13 P 106.2(3) . . ? C4 C3 C2 120.4(4) . . ? C10 C11 C12 119.3(4) . . ? C19 C18 C17 120.5(4) . . ? C9 C8 C7 119.8(4) . . ? C17 C22 C21 120.7(4) . . ? C5 C4 C3 120.2(3) . . ? C21 C20 C19 120.6(4) . . ? C4 C5 C6 120.3(4) . . ? O C15 C16 104.7(3) . . ? C1 C6 C5 119.7(4) . . ? C8 C9 C10 120.2(4) . . ? C3 C2 C1 120.1(4) . . ? C11 C10 C9 120.7(4) . . ? C20 C21 C22 119.7(4) . . ? Cl4 C23 Cl3 113.4(3) . . ? C20 C19 C18 119.5(4) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.641 _refine_diff_density_min -0.677 _refine_diff_density_rms 0.077 data_st889 _database_code_CSD 200360 _audit_creation_date 10-05-02 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H37 Cl2 N3 O Pd3' _chemical_formula_sum 'C27 H37 Cl2 N3 O Pd3' _chemical_formula_weight 809.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Pd Pd -0.9988 1.0072 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.540(5) _cell_length_b 12.370(5) _cell_length_c 13.327(5) _cell_angle_alpha 84.288(5) _cell_angle_beta 82.088(5) _cell_angle_gamma 70.423(5) _cell_volume 1465.3(11) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 10248 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description prism _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.835 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 800 _exptl_absorpt_coefficient_mu 2.028 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 KappaCCD _diffrn_measurement_method '\p scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6671 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0924 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6670 _reflns_number_gt 5146 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ATOMS (Dowty, 1995)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0000P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6670 _refine_ls_number_parameters 329 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0542 _refine_ls_R_factor_gt 0.0360 _refine_ls_wR_factor_ref 0.0991 _refine_ls_wR_factor_gt 0.0917 _refine_ls_goodness_of_fit_ref 0.946 _refine_ls_restrained_S_all 0.946 _refine_ls_shift/su_max 0.027 _refine_ls_shift/su_mean 0.002 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 C19 C 1.1992(5) -0.4037(4) 0.1527(3) 0.0236(9) Uani 1 1 d . . . C20 C 1.3504(5) -0.4541(4) 0.1238(3) 0.0257(10) Uani 1 1 d . . . H20 H 1.3821 -0.5042 0.0715 0.031 Uiso 1 1 calc . . . C21 C 1.4565(5) -0.4299(4) 0.1733(4) 0.0329(11) Uani 1 1 d . . . H21 H 1.5582 -0.4636 0.1536 0.039 Uiso 1 1 calc . . . C22 C 1.4090(5) -0.3557(4) 0.2515(3) 0.0288(10) Uani 1 1 d . . . H22 H 1.4792 -0.3391 0.2839 0.035 Uiso 1 1 calc . . . C23 C 1.2582(6) -0.3060(4) 0.2820(4) 0.0348(12) Uani 1 1 d . . . H23 H 1.2274 -0.2576 0.3356 0.042 Uiso 1 1 calc . . . C24 C 1.1525(5) -0.3283(4) 0.2326(3) 0.0277(10) Uani 1 1 d . . . C25 C 0.9868(6) -0.2821(4) 0.2633(4) 0.0362(12) Uani 1 1 d . . . H25A H 0.9575 -0.3312 0.3176 0.043 Uiso 1 1 calc . . . H25B H 0.9598 -0.2055 0.2873 0.043 Uiso 1 1 calc . . . C27 C 0.7558(6) -0.2800(5) 0.2077(4) 0.0468(15) Uani 1 1 d . . . H27A H 0.7606 -0.3486 0.2495 0.070 Uiso 1 1 calc . . . H27B H 0.7045 -0.2780 0.1501 0.070 Uiso 1 1 calc . . . H27C H 0.7027 -0.2140 0.2463 0.070 Uiso 1 1 calc . . . C26 C 0.9053(7) -0.1718(4) 0.1080(4) 0.0474(15) Uani 1 1 d . . . H26A H 1.0056 -0.1731 0.0848 0.071 Uiso 1 1 calc . . . H26B H 0.8550 -0.1058 0.1472 0.071 Uiso 1 1 calc . . . H26C H 0.8525 -0.1677 0.0507 0.071 Uiso 1 1 calc . . . C1 C 0.8344(5) -0.2353(4) 0.5468(3) 0.0227(9) Uani 1 1 d . . . C2 C 0.9486(5) -0.1873(4) 0.5203(3) 0.0258(10) Uani 1 1 d . . . H2 H 0.9389 -0.1289 0.4694 0.031 Uiso 1 1 calc . . . C3 C 1.0769(5) -0.2269(4) 0.5699(4) 0.0306(11) Uani 1 1 d . . . H3 H 1.1531 -0.1951 0.5518 0.037 Uiso 1 1 calc . . . C4 C 1.0922(5) -0.3133(4) 0.6461(4) 0.0317(11) Uani 1 1 d . . . H4 H 1.1787 -0.3393 0.6787 0.038 Uiso 1 1 calc . . . C5 C 0.9801(5) -0.3611(4) 0.6739(3) 0.0281(10) Uani 1 1 d . . . H5 H 0.9905 -0.4189 0.7253 0.034 Uiso 1 1 calc . . . C6 C 0.8518(5) -0.3222(4) 0.6247(3) 0.0226(9) Uani 1 1 d . . . C7 C 0.7221(5) -0.3662(4) 0.6514(3) 0.0269(10) Uani 1 1 d . . . H7A H 0.7578 -0.4471 0.6726 0.032 Uiso 1 1 calc . . . H7B H 0.6558 -0.3249 0.7071 0.032 Uiso 1 1 calc . . . C9 C 0.4872(5) -0.3554(4) 0.5937(4) 0.0318(11) Uani 1 1 d . . . H9A H 0.4337 -0.2951 0.6384 0.048 Uiso 1 1 calc . . . H9B H 0.4949 -0.4285 0.6287 0.048 Uiso 1 1 calc . . . H9C H 0.4345 -0.3467 0.5354 0.048 Uiso 1 1 calc . . . C8 C 0.7201(6) -0.4423(4) 0.4912(4) 0.0339(11) Uani 1 1 d . . . H8A H 0.8189 -0.4392 0.4693 0.051 Uiso 1 1 calc . . . H8B H 0.6666 -0.4328 0.4332 0.051 Uiso 1 1 calc . . . H8C H 0.7271 -0.5154 0.5261 0.051 Uiso 1 1 calc . . . C10 C 0.5948(5) 0.1001(4) 0.2257(3) 0.0239(9) Uani 1 1 d . . . C11 C 0.7348(5) 0.1110(4) 0.2319(3) 0.0252(10) Uani 1 1 d . . . H11 H 0.7923 0.0698 0.2827 0.030 Uiso 1 1 calc . . . C12 C 0.7870(5) 0.1826(4) 0.1628(4) 0.0322(11) Uani 1 1 d . . . H12 H 0.8793 0.1905 0.1678 0.039 Uiso 1 1 calc . . . C13 C 0.7031(6) 0.2436(4) 0.0849(4) 0.0353(12) Uani 1 1 d . . . H13 H 0.7394 0.2917 0.0383 0.042 Uiso 1 1 calc . . . C14 C 0.5661(6) 0.2319(4) 0.0779(3) 0.0331(11) Uani 1 1 d . . . H14 H 0.5106 0.2710 0.0255 0.040 Uiso 1 1 calc . . . C15 C 0.5105(5) 0.1621(4) 0.1485(3) 0.0243(9) Uani 1 1 d . . . C16 C 0.3581(5) 0.1495(4) 0.1501(3) 0.0284(10) Uani 1 1 d . . . H16A H 0.2829 0.2116 0.1858 0.034 Uiso 1 1 calc . . . H16B H 0.3337 0.1538 0.0812 0.034 Uiso 1 1 calc . . . C17 C 0.2025(5) 0.0435(5) 0.2398(4) 0.0356(12) Uani 1 1 d . . . H17A H 0.1616 0.1021 0.2878 0.053 Uiso 1 1 calc . . . H17B H 0.2020 -0.0292 0.2722 0.053 Uiso 1 1 calc . . . H17C H 0.1429 0.0617 0.1841 0.053 Uiso 1 1 calc . . . C18 C 0.4184(5) -0.0539(4) 0.1286(3) 0.0307(11) Uani 1 1 d . . . H18A H 0.5195 -0.0593 0.1031 0.046 Uiso 1 1 calc . . . H18B H 0.3581 -0.0357 0.0733 0.046 Uiso 1 1 calc . . . H18C H 0.4168 -0.1260 0.1620 0.046 Uiso 1 1 calc . . . N2 N 0.3582(4) 0.0372(3) 0.2016(3) 0.0235(8) Uani 1 1 d . . . N1 N 0.6396(4) -0.3492(3) 0.5605(3) 0.0220(8) Uani 1 1 d . . . N3 N 0.9095(4) -0.2788(3) 0.1726(3) 0.0311(9) Uani 1 1 d . . . Pd3 Pd 1.03257(4) -0.41834(3) 0.08850(2) 0.02330(10) Uani 1 1 d . . . Pd1 Pd 0.64392(4) -0.19360(3) 0.48816(2) 0.01941(9) Uani 1 1 d . . . Pd2 Pd 0.50386(4) -0.00141(3) 0.31392(2) 0.02023(9) Uani 1 1 d . . . Cl2 Cl 1.17778(14) -0.57541(11) -0.00302(10) 0.0404(3) Uani 1 1 d . . . Cl1 Cl 0.39911(12) -0.13778(10) 0.41988(8) 0.0275(2) Uani 1 1 d . . . O1 O 0.6672(3) -0.0494(3) 0.4092(2) 0.0226(6) Uani 1 1 d D . . H37 H 0.654(6) 0.007(3) 0.456(3) 0.044(15) Uiso 1 1 d 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 C19 0.027(2) 0.026(2) 0.021(2) 0.0002(18) -0.0041(18) -0.0126(19) C20 0.023(2) 0.028(2) 0.021(2) 0.0035(19) -0.0015(18) -0.0044(19) C21 0.021(2) 0.042(3) 0.035(3) 0.010(2) -0.004(2) -0.014(2) C22 0.029(3) 0.036(3) 0.031(2) 0.003(2) -0.013(2) -0.020(2) C23 0.047(3) 0.033(3) 0.030(3) -0.005(2) -0.011(2) -0.017(2) C24 0.032(3) 0.027(2) 0.026(2) 0.0000(19) -0.005(2) -0.011(2) C25 0.034(3) 0.044(3) 0.030(3) -0.018(2) -0.004(2) -0.007(2) C27 0.026(3) 0.064(4) 0.047(3) -0.033(3) 0.002(2) -0.005(3) C26 0.057(4) 0.023(3) 0.053(4) -0.005(2) -0.020(3) 0.005(3) C1 0.024(2) 0.028(2) 0.017(2) -0.0006(18) -0.0010(17) -0.0094(19) C2 0.027(2) 0.032(3) 0.021(2) -0.0019(19) 0.0003(18) -0.014(2) C3 0.020(2) 0.045(3) 0.030(3) -0.009(2) -0.0006(19) -0.014(2) C4 0.016(2) 0.041(3) 0.035(3) -0.009(2) -0.009(2) -0.002(2) C5 0.026(2) 0.028(2) 0.027(2) 0.0014(19) -0.012(2) -0.003(2) C6 0.022(2) 0.022(2) 0.023(2) -0.0055(18) -0.0003(17) -0.0050(18) C7 0.029(3) 0.021(2) 0.028(2) 0.0001(19) -0.001(2) -0.006(2) C9 0.028(3) 0.028(3) 0.043(3) 0.001(2) -0.003(2) -0.016(2) C8 0.041(3) 0.028(3) 0.035(3) -0.008(2) -0.005(2) -0.013(2) C10 0.025(2) 0.021(2) 0.021(2) -0.0051(18) -0.0009(18) -0.0009(18) C11 0.025(2) 0.020(2) 0.027(2) 0.0019(18) -0.0052(19) -0.0030(18) C12 0.027(3) 0.031(3) 0.036(3) 0.001(2) 0.002(2) -0.009(2) C13 0.040(3) 0.030(3) 0.033(3) 0.007(2) 0.003(2) -0.012(2) C14 0.043(3) 0.025(2) 0.023(2) 0.0054(19) -0.007(2) -0.001(2) C15 0.026(2) 0.022(2) 0.022(2) -0.0029(18) -0.0072(18) -0.0002(19) C16 0.031(3) 0.024(2) 0.026(2) -0.0020(19) -0.008(2) -0.002(2) C17 0.020(2) 0.046(3) 0.039(3) -0.005(2) -0.009(2) -0.006(2) C18 0.037(3) 0.031(3) 0.024(2) -0.007(2) -0.009(2) -0.007(2) N2 0.0216(19) 0.027(2) 0.0210(18) -0.0053(15) -0.0063(15) -0.0045(16) N1 0.0219(19) 0.0221(19) 0.0230(19) -0.0018(15) -0.0015(15) -0.0086(15) N3 0.024(2) 0.032(2) 0.035(2) -0.0149(18) -0.0058(17) -0.0011(17) Pd3 0.02123(19) 0.02375(19) 0.02351(18) -0.00544(14) -0.00336(14) -0.00399(14) Pd1 0.01989(18) 0.02040(17) 0.01984(17) -0.00091(13) -0.00405(13) -0.00839(14) Pd2 0.02081(18) 0.02208(18) 0.01789(17) -0.00139(13) -0.00467(13) -0.00606(14) Cl2 0.0279(6) 0.0417(7) 0.0492(8) -0.0230(6) -0.0091(6) -0.0007(5) Cl1 0.0272(6) 0.0325(6) 0.0290(6) 0.0019(5) -0.0093(5) -0.0167(5) O1 0.0260(17) 0.0253(16) 0.0191(15) 0.0020(13) -0.0083(13) -0.0105(14) _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 C19 C20 1.382(6) . ? C19 C24 1.411(6) . ? C19 Pd3 1.972(4) . ? C20 C21 1.405(6) . ? C21 C22 1.384(7) . ? C22 C23 1.381(7) . ? C23 C24 1.389(6) . ? C24 C25 1.502(7) . ? C25 N3 1.491(6) . ? C27 N3 1.481(6) . ? C26 N3 1.497(7) . ? C1 C2 1.397(6) . ? C1 C6 1.403(6) . ? C1 Pd1 1.965(4) . ? C2 C3 1.390(6) . ? C3 C4 1.384(7) . ? C4 C5 1.379(7) . ? C5 C6 1.387(6) . ? C6 C7 1.498(6) . ? C7 N1 1.494(6) . ? C9 N1 1.485(6) . ? C8 N1 1.481(6) . ? C10 C15 1.397(6) . ? C10 C11 1.400(6) . ? C10 Pd2 1.967(5) . ? C11 C12 1.374(6) . ? C12 C13 1.398(7) . ? C13 C14 1.380(7) . ? C14 C15 1.385(7) . ? C15 C16 1.510(6) . ? C16 N2 1.487(6) . ? C17 N2 1.481(6) . ? C18 N2 1.475(5) . ? N2 Pd2 2.095(3) . ? N1 Pd1 2.076(4) . ? N3 Pd3 2.068(4) . ? Pd3 Cl2 2.3205(13) . ? Pd3 Cl2 2.4661(16) 2_745 ? Pd1 O1 2.041(3) . ? Pd1 Cl1 2.4776(16) . ? Pd1 Pd2 3.2335(9) . ? Pd2 O1 2.041(3) . ? Pd2 Cl1 2.4708(13) . ? Cl2 Pd3 2.4661(16) 2_745 ? 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 C20 C19 C24 119.4(4) . . ? C20 C19 Pd3 126.8(3) . . ? C24 C19 Pd3 113.8(3) . . ? C19 C20 C21 120.2(4) . . ? C22 C21 C20 119.7(4) . . ? C23 C22 C21 120.6(4) . . ? C22 C23 C24 120.1(4) . . ? C23 C24 C19 120.0(4) . . ? C23 C24 C25 123.7(4) . . ? C19 C24 C25 116.2(4) . . ? N3 C25 C24 107.8(4) . . ? C2 C1 C6 118.6(4) . . ? C2 C1 Pd1 127.3(3) . . ? C6 C1 Pd1 114.1(3) . . ? C3 C2 C1 119.9(4) . . ? C4 C3 C2 120.5(4) . . ? C5 C4 C3 120.4(4) . . ? C4 C5 C6 119.6(4) . . ? C5 C6 C1 121.0(4) . . ? C5 C6 C7 123.6(4) . . ? C1 C6 C7 115.4(4) . . ? N1 C7 C6 109.0(4) . . ? C15 C10 C11 119.2(4) . . ? C15 C10 Pd2 114.7(3) . . ? C11 C10 Pd2 126.0(3) . . ? C12 C11 C10 119.9(4) . . ? C11 C12 C13 120.8(4) . . ? C14 C13 C12 119.4(4) . . ? C13 C14 C15 120.4(4) . . ? C14 C15 C10 120.3(4) . . ? C14 C15 C16 123.9(4) . . ? C10 C15 C16 115.8(4) . . ? N2 C16 C15 109.7(4) . . ? C18 N2 C17 108.3(3) . . ? C18 N2 C16 109.8(3) . . ? C17 N2 C16 109.3(4) . . ? C18 N2 Pd2 107.4(3) . . ? C17 N2 Pd2 114.5(3) . . ? C16 N2 Pd2 107.5(3) . . ? C8 N1 C9 108.8(3) . . ? C8 N1 C7 109.1(3) . . ? C9 N1 C7 109.0(3) . . ? C8 N1 Pd1 108.8(3) . . ? C9 N1 Pd1 114.6(3) . . ? C7 N1 Pd1 106.5(2) . . ? C27 N3 C25 108.4(4) . . ? C27 N3 C26 110.6(4) . . ? C25 N3 C26 109.0(4) . . ? C27 N3 Pd3 112.2(3) . . ? C25 N3 Pd3 108.6(3) . . ? C26 N3 Pd3 108.0(3) . . ? C19 Pd3 N3 82.57(17) . . ? C19 Pd3 Cl2 95.47(13) . . ? N3 Pd3 Cl2 178.02(11) . . ? C19 Pd3 Cl2 176.39(13) . 2_745 ? N3 Pd3 Cl2 95.78(11) . 2_745 ? Cl2 Pd3 Cl2 86.19(5) . 2_745 ? C1 Pd1 O1 94.85(15) . . ? C1 Pd1 N1 82.32(16) . . ? O1 Pd1 N1 174.42(13) . . ? C1 Pd1 Cl1 177.97(12) . . ? O1 Pd1 Cl1 85.43(8) . . ? N1 Pd1 Cl1 97.57(10) . . ? C1 Pd1 Pd2 131.52(13) . . ? O1 Pd1 Pd2 37.62(8) . . ? N1 Pd1 Pd2 143.88(10) . . ? Cl1 Pd1 Pd2 49.11(3) . . ? C10 Pd2 O1 93.92(15) . . ? C10 Pd2 N2 82.87(16) . . ? O1 Pd2 N2 172.54(13) . . ? C10 Pd2 Cl1 176.95(12) . . ? O1 Pd2 Cl1 85.60(9) . . ? N2 Pd2 Cl1 97.24(11) . . ? C10 Pd2 Pd1 129.62(13) . . ? O1 Pd2 Pd1 37.62(8) . . ? N2 Pd2 Pd1 142.93(10) . . ? Cl1 Pd2 Pd1 49.29(4) . . ? Pd3 Cl2 Pd3 93.81(5) . 2_745 ? Pd2 Cl1 Pd1 81.60(4) . . ? Pd1 O1 Pd2 104.76(13) . . ? 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 C24 C19 C20 C21 -0.4(7) . . . . ? Pd3 C19 C20 C21 176.1(3) . . . . ? C19 C20 C21 C22 0.3(7) . . . . ? C20 C21 C22 C23 0.6(7) . . . . ? C21 C22 C23 C24 -1.4(8) . . . . ? C22 C23 C24 C19 1.3(7) . . . . ? C22 C23 C24 C25 177.4(5) . . . . ? C20 C19 C24 C23 -0.4(7) . . . . ? Pd3 C19 C24 C23 -177.3(4) . . . . ? C20 C19 C24 C25 -176.7(4) . . . . ? Pd3 C19 C24 C25 6.3(5) . . . . ? C23 C24 C25 N3 155.7(4) . . . . ? C19 C24 C25 N3 -28.1(6) . . . . ? C6 C1 C2 C3 0.8(6) . . . . ? Pd1 C1 C2 C3 179.8(3) . . . . ? C1 C2 C3 C4 -0.4(7) . . . . ? C2 C3 C4 C5 -0.2(7) . . . . ? C3 C4 C5 C6 0.2(7) . . . . ? C4 C5 C6 C1 0.2(7) . . . . ? C4 C5 C6 C7 -178.2(4) . . . . ? C2 C1 C6 C5 -0.8(6) . . . . ? Pd1 C1 C6 C5 -179.9(3) . . . . ? C2 C1 C6 C7 177.8(4) . . . . ? Pd1 C1 C6 C7 -1.3(5) . . . . ? C5 C6 C7 N1 -154.8(4) . . . . ? C1 C6 C7 N1 26.7(5) . . . . ? C15 C10 C11 C12 0.4(6) . . . . ? Pd2 C10 C11 C12 177.7(3) . . . . ? C10 C11 C12 C13 -1.1(7) . . . . ? C11 C12 C13 C14 0.2(8) . . . . ? C12 C13 C14 C15 1.3(7) . . . . ? C13 C14 C15 C10 -2.0(7) . . . . ? C13 C14 C15 C16 176.4(4) . . . . ? C11 C10 C15 C14 1.1(6) . . . . ? Pd2 C10 C15 C14 -176.5(3) . . . . ? C11 C10 C15 C16 -177.4(4) . . . . ? Pd2 C10 C15 C16 5.0(5) . . . . ? C14 C15 C16 N2 155.5(4) . . . . ? C10 C15 C16 N2 -26.0(5) . . . . ? C15 C16 N2 C18 -84.0(4) . . . . ? C15 C16 N2 C17 157.3(4) . . . . ? C15 C16 N2 Pd2 32.5(4) . . . . ? C6 C7 N1 C8 79.9(4) . . . . ? C6 C7 N1 C9 -161.4(3) . . . . ? C6 C7 N1 Pd1 -37.2(4) . . . . ? C24 C25 N3 C27 157.3(4) . . . . ? C24 C25 N3 C26 -82.2(5) . . . . ? C24 C25 N3 Pd3 35.2(5) . . . . ? C20 C19 Pd3 N3 -165.1(4) . . . . ? C24 C19 Pd3 N3 11.6(3) . . . . ? C20 C19 Pd3 Cl2 15.1(4) . . . . ? C24 C19 Pd3 Cl2 -168.2(3) . . . . ? C20 C19 Pd3 Cl2 -102(2) . . . 2_745 ? C24 C19 Pd3 Cl2 75(2) . . . 2_745 ? C27 N3 Pd3 C19 -146.5(4) . . . . ? C25 N3 Pd3 C19 -26.6(3) . . . . ? C26 N3 Pd3 C19 91.4(3) . . . . ? C27 N3 Pd3 Cl2 -140(4) . . . . ? C25 N3 Pd3 Cl2 -20(4) . . . . ? C26 N3 Pd3 Cl2 98(4) . . . . ? C27 N3 Pd3 Cl2 36.8(4) . . . 2_745 ? C25 N3 Pd3 Cl2 156.6(3) . . . 2_745 ? C26 N3 Pd3 Cl2 -85.3(3) . . . 2_745 ? C2 C1 Pd1 O1 -10.6(4) . . . . ? C6 C1 Pd1 O1 168.4(3) . . . . ? C2 C1 Pd1 N1 164.6(4) . . . . ? C6 C1 Pd1 N1 -16.4(3) . . . . ? C2 C1 Pd1 Cl1 -108(4) . . . . ? C6 C1 Pd1 Cl1 71(4) . . . . ? C2 C1 Pd1 Pd2 -1.2(5) . . . . ? C6 C1 Pd1 Pd2 177.8(2) . . . . ? C8 N1 Pd1 C1 -87.5(3) . . . . ? C9 N1 Pd1 C1 150.5(3) . . . . ? C7 N1 Pd1 C1 29.9(3) . . . . ? C8 N1 Pd1 O1 -27.7(14) . . . . ? C9 N1 Pd1 O1 -149.6(11) . . . . ? C7 N1 Pd1 O1 89.7(12) . . . . ? C8 N1 Pd1 Cl1 94.5(3) . . . . ? C9 N1 Pd1 Cl1 -27.4(3) . . . . ? C7 N1 Pd1 Cl1 -148.1(2) . . . . ? C8 N1 Pd1 Pd2 74.3(3) . . . . ? C9 N1 Pd1 Pd2 -47.7(4) . . . . ? C7 N1 Pd1 Pd2 -168.35(19) . . . . ? C15 C10 Pd2 O1 -175.5(3) . . . . ? C11 C10 Pd2 O1 7.1(4) . . . . ? C15 C10 Pd2 N2 11.2(3) . . . . ? C11 C10 Pd2 N2 -166.1(4) . . . . ? C15 C10 Pd2 Cl1 104(2) . . . . ? C11 C10 Pd2 Cl1 -74(3) . . . . ? C15 C10 Pd2 Pd1 171.4(2) . . . . ? C11 C10 Pd2 Pd1 -6.0(4) . . . . ? C18 N2 Pd2 C10 93.5(3) . . . . ? C17 N2 Pd2 C10 -146.2(3) . . . . ? C16 N2 Pd2 C10 -24.6(3) . . . . ? C18 N2 Pd2 O1 28.5(11) . . . . ? C17 N2 Pd2 O1 148.8(9) . . . . ? C16 N2 Pd2 O1 -89.6(10) . . . . ? C18 N2 Pd2 Cl1 -83.4(3) . . . . ? C17 N2 Pd2 Cl1 36.9(3) . . . . ? C16 N2 Pd2 Cl1 158.5(2) . . . . ? C18 N2 Pd2 Pd1 -60.7(3) . . . . ? C17 N2 Pd2 Pd1 59.6(4) . . . . ? C16 N2 Pd2 Pd1 -178.86(19) . . . . ? C1 Pd1 Pd2 C10 6.3(2) . . . . ? O1 Pd1 Pd2 C10 21.8(2) . . . . ? N1 Pd1 Pd2 C10 -149.3(2) . . . . ? Cl1 Pd1 Pd2 C10 -176.27(15) . . . . ? C1 Pd1 Pd2 O1 -15.5(2) . . . . ? N1 Pd1 Pd2 O1 -171.0(2) . . . . ? Cl1 Pd1 Pd2 O1 161.97(14) . . . . ? C1 Pd1 Pd2 N2 152.2(2) . . . . ? O1 Pd1 Pd2 N2 167.7(2) . . . . ? N1 Pd1 Pd2 N2 -3.3(2) . . . . ? Cl1 Pd1 Pd2 N2 -30.32(17) . . . . ? C1 Pd1 Pd2 Cl1 -177.44(16) . . . . ? O1 Pd1 Pd2 Cl1 -161.97(14) . . . . ? N1 Pd1 Pd2 Cl1 27.01(17) . . . . ? C19 Pd3 Cl2 Pd3 -176.79(13) . . . 2_745 ? N3 Pd3 Cl2 Pd3 176(4) . . . 2_745 ? Cl2 Pd3 Cl2 Pd3 0.0 2_745 . . 2_745 ? C10 Pd2 Cl1 Pd1 70(2) . . . . ? O1 Pd2 Cl1 Pd1 -10.92(9) . . . . ? N2 Pd2 Cl1 Pd1 162.13(10) . . . . ? C1 Pd1 Cl1 Pd2 109(4) . . . . ? O1 Pd1 Cl1 Pd2 10.93(8) . . . . ? N1 Pd1 Cl1 Pd2 -164.33(10) . . . . ? C1 Pd1 O1 Pd2 168.44(16) . . . . ? N1 Pd1 O1 Pd2 109.1(12) . . . . ? Cl1 Pd1 O1 Pd2 -13.58(11) . . . . ? C10 Pd2 O1 Pd1 -163.36(16) . . . . ? N2 Pd2 O1 Pd1 -99.1(10) . . . . ? Cl1 Pd2 O1 Pd1 13.61(11) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.766 _refine_diff_density_min -1.197 _refine_diff_density_rms 0.138 data_wel4 _database_code_CSD 200361 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H23 Cl N O P Pd' _chemical_formula_sum 'C23 H23 Cl N O P Pd' _chemical_formula_weight 502.24 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.998(5) _cell_length_b 8.647(5) _cell_length_c 12.017(5) _cell_angle_alpha 90.00 _cell_angle_beta 107.690(5) _cell_angle_gamma 90.00 _cell_volume 1088.8(9) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6402 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description prism _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.532 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 508 _exptl_absorpt_coefficient_mu 1.062 # Absorption correction _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.862 _exptl_absorpt_correction_T_max 0.900 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _diffrn_reflns_av_R_equivalents 0.028 _diffrn_ambient_temperature 173(2) _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 '\p scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5518 _diffrn_reflns_av_sigmaI/netI 0.0723 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 29.96 _reflns_number_total 5517 _reflns_number_gt 5076 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON 98 (Spek, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0375P)^2^+0.1665P] 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 -0.02(2) _refine_ls_number_reflns 5517 _refine_ls_number_parameters 253 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0323 _refine_ls_R_factor_gt 0.0277 _refine_ls_wR_factor_ref 0.0771 _refine_ls_wR_factor_gt 0.0737 _refine_ls_goodness_of_fit_ref 0.807 _refine_ls_restrained_S_all 0.807 _refine_ls_shift/su_max 0.005 _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 Pd Pd 1.001492(17) 0.18529(3) 0.668903(15) 0.02044(6) Uani 1 1 d . . . P P 0.84676(7) 0.33102(10) 0.69130(6) 0.02125(15) Uani 1 1 d . . . Cl Cl 1.18478(7) 0.04689(10) 0.66000(7) 0.02918(16) Uani 1 1 d . . . C13 C 0.8875(3) 0.5230(4) 0.6448(3) 0.0255(6) Uani 1 1 d . . . H5A H 0.8498 0.5362 0.5612 0.031 Uiso 1 1 calc . . . H5B H 0.8568 0.6047 0.6846 0.031 Uiso 1 1 calc . . . O O 1.0873(2) 0.6638(3) 0.6852(2) 0.0312(5) Uani 1 1 d . . . N N 1.0992(2) 0.4035(3) 0.6978(2) 0.0256(6) Uani 1 1 d . . . C7 C 0.8563(3) 0.3601(4) 0.8437(3) 0.0251(6) Uani 1 1 d . . . C17 C 1.3007(3) 0.4187(4) 0.8609(3) 0.0317(7) Uani 1 1 d . . . C18 C 1.2406(3) 0.4406(5) 0.9456(3) 0.0409(8) Uani 1 1 d . . . H11 H 1.1559 0.4727 0.9237 0.049 Uiso 1 1 calc . . . C16 C 1.2354(3) 0.4532(4) 0.7339(3) 0.0300(7) Uani 1 1 d . . . H16 H 1.2805 0.4015 0.6854 0.036 Uiso 1 1 calc . . . C1 C 0.6773(3) 0.3029(4) 0.6189(3) 0.0256(6) Uani 1 1 d . . . C12 C 0.9391(3) 0.2667(4) 0.9287(3) 0.0308(7) Uani 1 1 d . . . H13 H 0.9881 0.1917 0.9071 0.037 Uiso 1 1 calc . . . C6 C 0.6042(3) 0.2290(4) 0.6794(3) 0.0335(8) Uani 1 1 d . . . H19 H 0.6426 0.1953 0.7556 0.040 Uiso 1 1 calc . . . C4 C 0.4176(3) 0.2562(5) 0.5148(4) 0.0426(9) Uani 1 1 d . . . H21 H 0.3303 0.2432 0.4805 0.051 Uiso 1 1 calc . . . C19 C 1.3052(5) 0.4152(6) 1.0626(4) 0.0538(11) Uani 1 1 d . . . H10 H 1.2638 0.4307 1.1186 0.065 Uiso 1 1 calc . . . C15 C 1.2222(3) 0.6285(5) 0.7048(4) 0.0387(8) Uani 1 1 d . . . H3A H 1.2755 0.6890 0.7692 0.046 Uiso 1 1 calc . . . H3B H 1.2467 0.6506 0.6354 0.046 Uiso 1 1 calc . . . C9 C 0.7912(4) 0.4900(5) 0.9940(4) 0.0436(9) Uani 1 1 d . . . H16 H 0.7421 0.5648 1.0160 0.052 Uiso 1 1 calc . . . C10 C 0.8729(4) 0.3968(5) 1.0775(3) 0.0408(9) Uani 1 1 d . . . H15 H 0.8777 0.4082 1.1557 0.049 Uiso 1 1 calc . . . C3 C 0.4897(4) 0.3262(5) 0.4535(3) 0.0433(9) Uani 1 1 d . . . H22 H 0.4509 0.3587 0.3771 0.052 Uiso 1 1 calc . . . C5 C 0.4754(3) 0.2054(5) 0.6274(4) 0.0395(9) Uani 1 1 d . . . H20 H 0.4275 0.1551 0.6682 0.047 Uiso 1 1 calc . . . C11 C 0.9478(4) 0.2867(5) 1.0458(3) 0.0416(9) Uani 1 1 d . . . H14 H 1.0038 0.2262 1.1027 0.050 Uiso 1 1 calc . . . C2 C 0.6200(3) 0.3490(5) 0.5046(3) 0.0339(7) Uani 1 1 d . . . H23 H 0.6684 0.3948 0.4622 0.041 Uiso 1 1 calc . . . C8 C 0.7829(3) 0.4710(4) 0.8768(3) 0.0360(8) Uani 1 1 d . . . H17 H 0.7278 0.5330 0.8203 0.043 Uiso 1 1 calc . . . C22 C 1.4251(4) 0.3699(8) 0.8963(4) 0.0616(15) Uani 1 1 d . . . H7 H 1.4670 0.3533 0.8408 0.074 Uiso 1 1 calc . . . C20 C 1.4304(5) 0.3671(8) 1.0959(4) 0.0696(16) Uani 1 1 d . . . H9 H 1.4738 0.3501 1.1743 0.083 Uiso 1 1 calc . . . C14 C 1.0297(3) 0.5259(4) 0.6773(2) 0.0249(6) Uani 1 1 d . . . C23 C 0.8876(3) -0.0067(4) 0.6339(3) 0.0313(7) Uani 1 1 d . . . H1A H 0.8792 -0.0476 0.7055 0.047 Uiso 1 1 calc . . . H1B H 0.9251 -0.0835 0.5968 0.047 Uiso 1 1 calc . . . H1C H 0.8048 0.0207 0.5829 0.047 Uiso 1 1 calc . . . C21 C 1.4898(5) 0.3449(10) 1.0136(4) 0.086(2) Uani 1 1 d . . . H8 H 1.5745 0.3127 1.0358 0.104 Uiso 1 1 calc . . . 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 Pd 0.01797(9) 0.02174(10) 0.02263(9) -0.00144(9) 0.00772(6) -0.00113(10) P 0.0178(3) 0.0237(4) 0.0228(3) -0.0006(3) 0.0069(3) -0.0003(3) Cl 0.0261(4) 0.0298(4) 0.0367(4) 0.0001(3) 0.0171(3) 0.0021(3) C13 0.0233(14) 0.0245(16) 0.0276(14) 0.0008(11) 0.0062(11) 0.0016(12) O 0.0286(10) 0.0208(14) 0.0441(11) 0.0004(10) 0.0111(9) -0.0045(10) N 0.0200(12) 0.0255(15) 0.0330(13) -0.0055(10) 0.0107(10) -0.0061(10) C7 0.0236(14) 0.0258(16) 0.0274(14) -0.0030(11) 0.0100(11) -0.0041(12) C17 0.0244(15) 0.0313(18) 0.0394(17) -0.0067(13) 0.0099(13) -0.0056(13) C18 0.0339(19) 0.049(2) 0.0412(19) -0.0066(17) 0.0133(15) -0.0017(18) C16 0.0216(15) 0.0338(19) 0.0364(17) -0.0061(13) 0.0115(13) -0.0071(14) C1 0.0194(14) 0.0259(17) 0.0317(15) -0.0014(11) 0.0083(12) -0.0012(12) C12 0.0315(17) 0.0345(19) 0.0276(15) 0.0022(13) 0.0105(13) 0.0031(14) C6 0.0266(16) 0.035(2) 0.0400(17) 0.0006(13) 0.0123(13) -0.0028(13) C4 0.0213(16) 0.037(2) 0.063(2) -0.0061(17) 0.0025(16) -0.0062(15) C19 0.057(3) 0.068(3) 0.039(2) -0.009(2) 0.0181(19) -0.008(2) C15 0.0272(17) 0.0331(19) 0.058(2) 0.0004(16) 0.0164(16) -0.0068(14) C9 0.053(2) 0.042(2) 0.043(2) -0.0153(17) 0.0255(19) -0.0066(18) C10 0.051(2) 0.046(2) 0.0296(17) -0.0076(14) 0.0183(16) -0.0146(18) C3 0.0351(19) 0.041(2) 0.0418(19) 0.0046(17) -0.0056(15) -0.0057(18) C5 0.0271(15) 0.039(3) 0.057(2) -0.0019(19) 0.0188(14) -0.0061(17) C11 0.046(2) 0.052(3) 0.0263(17) 0.0041(15) 0.0109(16) -0.0038(18) C2 0.0305(17) 0.038(2) 0.0318(16) -0.0013(14) 0.0075(13) -0.0079(16) C8 0.0367(19) 0.038(2) 0.0357(17) -0.0032(14) 0.0140(15) 0.0041(16) C22 0.0279(19) 0.112(5) 0.044(2) 0.000(2) 0.0107(17) 0.009(2) C20 0.052(3) 0.113(5) 0.035(2) 0.002(3) -0.0001(19) -0.009(3) C14 0.0275(15) 0.0246(17) 0.0240(14) -0.0017(11) 0.0097(11) -0.0028(13) C23 0.0214(15) 0.0229(16) 0.0478(19) -0.0053(13) 0.0077(14) -0.0055(12) C21 0.036(2) 0.169(7) 0.049(3) 0.014(4) 0.005(2) 0.013(4) _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 Pd C23 2.046(3) . ? Pd N 2.147(3) . ? Pd P 2.1988(11) . ? Pd Cl 2.3746(12) . ? P C1 1.817(3) . ? P C7 1.820(3) . ? P C13 1.849(4) . ? C13 C14 1.493(4) . ? O C14 1.340(4) . ? O C15 1.461(4) . ? N C14 1.285(4) . ? N C16 1.490(4) . ? C7 C8 1.387(5) . ? C7 C12 1.400(5) . ? C17 C22 1.370(5) . ? C17 C18 1.384(5) . ? C17 C16 1.507(5) . ? C18 C19 1.386(6) . ? C16 C15 1.553(5) . ? C1 C2 1.384(5) . ? C1 C6 1.393(5) . ? C12 C11 1.391(5) . ? C6 C5 1.379(5) . ? C4 C3 1.375(6) . ? C4 C5 1.381(6) . ? C19 C20 1.377(7) . ? C9 C10 1.385(6) . ? C9 C8 1.394(5) . ? C10 C11 1.385(6) . ? C3 C2 1.392(5) . ? C22 C21 1.389(6) . ? C20 C21 1.355(7) . ? 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 C23 Pd N 172.76(13) . . ? C23 Pd P 92.40(11) . . ? N Pd P 81.06(8) . . ? C23 Pd Cl 93.26(11) . . ? N Pd Cl 93.44(8) . . ? P Pd Cl 173.50(3) . . ? C1 P C7 103.73(14) . . ? C1 P C13 106.41(15) . . ? C7 P C13 103.59(15) . . ? C1 P Pd 125.73(11) . . ? C7 P Pd 113.09(11) . . ? C13 P Pd 102.12(11) . . ? C14 C13 P 105.5(2) . . ? C14 O C15 105.1(3) . . ? C14 N C16 107.7(3) . . ? C14 N Pd 117.0(2) . . ? C16 N Pd 135.2(2) . . ? C8 C7 C12 119.7(3) . . ? C8 C7 P 121.5(2) . . ? C12 C7 P 118.7(2) . . ? C22 C17 C18 118.0(4) . . ? C22 C17 C16 119.9(3) . . ? C18 C17 C16 122.0(3) . . ? C17 C18 C19 120.8(4) . . ? N C16 C17 111.4(3) . . ? N C16 C15 101.5(3) . . ? C17 C16 C15 113.9(3) . . ? C2 C1 C6 119.3(3) . . ? C2 C1 P 121.9(2) . . ? C6 C1 P 118.8(2) . . ? C11 C12 C7 119.7(3) . . ? C5 C6 C1 120.5(3) . . ? C3 C4 C5 119.8(3) . . ? C20 C19 C18 120.1(4) . . ? O C15 C16 105.1(3) . . ? C10 C9 C8 119.5(4) . . ? C9 C10 C11 120.7(3) . . ? C4 C3 C2 120.6(4) . . ? C6 C5 C4 120.1(3) . . ? C10 C11 C12 120.0(4) . . ? C1 C2 C3 119.7(3) . . ? C7 C8 C9 120.4(4) . . ? C17 C22 C21 121.2(4) . . ? C21 C20 C19 119.5(4) . . ? N C14 O 118.6(3) . . ? N C14 C13 123.4(3) . . ? O C14 C13 118.0(3) . . ? C20 C21 C22 120.4(5) . . ? 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 C23 Pd P C1 -29.43(17) . . . . ? N Pd P C1 147.44(15) . . . . ? Cl Pd P C1 179.9(3) . . . . ? C23 Pd P C7 99.22(15) . . . . ? N Pd P C7 -83.92(13) . . . . ? Cl Pd P C7 -51.5(3) . . . . ? C23 Pd P C13 -150.12(15) . . . . ? N Pd P C13 26.74(13) . . . . ? Cl Pd P C13 59.2(3) . . . . ? C1 P C13 C14 -164.9(2) . . . . ? C7 P C13 C14 86.1(2) . . . . ? Pd P C13 C14 -31.6(2) . . . . ? C23 Pd N C14 3.6(12) . . . . ? P Pd N C14 -22.1(2) . . . . ? Cl Pd N C14 161.4(2) . . . . ? C23 Pd N C16 -173.7(10) . . . . ? P Pd N C16 160.6(3) . . . . ? Cl Pd N C16 -15.9(3) . . . . ? C1 P C7 C8 -53.2(3) . . . . ? C13 P C7 C8 57.8(3) . . . . ? Pd P C7 C8 167.6(3) . . . . ? C1 P C7 C12 126.2(3) . . . . ? C13 P C7 C12 -122.8(3) . . . . ? Pd P C7 C12 -13.0(3) . . . . ? C22 C17 C18 C19 0.6(7) . . . . ? C16 C17 C18 C19 -176.8(4) . . . . ? C14 N C16 C17 111.1(3) . . . . ? Pd N C16 C17 -71.5(4) . . . . ? C14 N C16 C15 -10.5(3) . . . . ? Pd N C16 C15 166.9(2) . . . . ? C22 C17 C16 N 142.5(4) . . . . ? C18 C17 C16 N -40.2(5) . . . . ? C22 C17 C16 C15 -103.5(5) . . . . ? C18 C17 C16 C15 73.8(5) . . . . ? C7 P C1 C2 148.5(3) . . . . ? C13 P C1 C2 39.6(3) . . . . ? Pd P C1 C2 -79.2(3) . . . . ? C7 P C1 C6 -33.4(3) . . . . ? C13 P C1 C6 -142.3(3) . . . . ? Pd P C1 C6 98.9(3) . . . . ? C8 C7 C12 C11 -0.5(5) . . . . ? P C7 C12 C11 -179.9(3) . . . . ? C2 C1 C6 C5 -1.7(6) . . . . ? P C1 C6 C5 -179.9(3) . . . . ? C17 C18 C19 C20 -0.2(8) . . . . ? C14 O C15 C16 -12.2(3) . . . . ? N C16 C15 O 13.6(3) . . . . ? C17 C16 C15 O -106.2(3) . . . . ? C8 C9 C10 C11 1.0(6) . . . . ? C5 C4 C3 C2 -1.2(7) . . . . ? C1 C6 C5 C4 -0.5(6) . . . . ? C3 C4 C5 C6 2.0(7) . . . . ? C9 C10 C11 C12 -1.4(6) . . . . ? C7 C12 C11 C10 1.1(6) . . . . ? C6 C1 C2 C3 2.5(6) . . . . ? P C1 C2 C3 -179.4(3) . . . . ? C4 C3 C2 C1 -1.1(7) . . . . ? C12 C7 C8 C9 0.0(5) . . . . ? P C7 C8 C9 179.4(3) . . . . ? C10 C9 C8 C7 -0.3(6) . . . . ? C18 C17 C22 C21 -0.8(9) . . . . ? C16 C17 C22 C21 176.6(6) . . . . ? C18 C19 C20 C21 0.0(10) . . . . ? C16 N C14 O 3.3(4) . . . . ? Pd N C14 O -174.6(2) . . . . ? C16 N C14 C13 -176.8(3) . . . . ? Pd N C14 C13 5.3(4) . . . . ? C15 O C14 N 6.1(4) . . . . ? C15 O C14 C13 -173.8(3) . . . . ? P C13 C14 N 19.1(3) . . . . ? P C13 C14 O -161.0(2) . . . . ? C19 C20 C21 C22 -0.2(12) . . . . ? C17 C22 C21 C20 0.6(12) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 29.96 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.421 _refine_diff_density_min -0.845 _refine_diff_density_rms 0.115