Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Prof Gabor Besenyei' _publ_contact_author_address ; Institute of Chemistry Chemical Research Center Hungarian Academy of Sciences PO Box 17 Budapest 1525 HUNGARY ; _publ_contact_author_email BESENYEI@CHEMRES.HU _publ_section_title ; N-benzoylimido complexes of palladium. Synthesis, structural characterisation and structure-reactivity relationship ; loop_ _publ_author_name 'Gabor Besenyei' 'Sandor Holly' 'G. Keresztury' 'A. Nagy' 'I. Papai' 'Laszlo Parkanyi' ; G.Szalontai ; data_bes _database_code_depnum_ccdc_archive 'CCDC 232756' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C232 H200 Cl8 N8 O4 P16 Pd8' _chemical_formula_weight 1198.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 43 21 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y+1/2, x+1/2, z+3/4' '-x, -y, z+1/2' 'y+1/2, -x+1/2, z+1/4' 'x+1/2, -y+1/2, -z+1/4' 'y, x, -z' '-x+1/2, y+1/2, -z+3/4' '-y, -x, -z+1/2' _cell_length_a 15.011(7) _cell_length_b 15.011(7) _cell_length_c 25.622(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5773(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 16.04 _cell_measurement_theta_max 16.43 _exptl_crystal_description block _exptl_crystal_colour 'brownish red' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.379 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2424 _exptl_absorpt_coefficient_mu 0.865 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.8656 _exptl_absorpt_correction_T_max 1.0000 _exptl_special_details ? _diffrn_ambient_temperature 293(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 'Enraf-Nonius CAD4' _diffrn_measurement_method \w--2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 21 _diffrn_reflns_number 22041 _diffrn_reflns_av_R_equivalents 0.0731 _diffrn_reflns_av_sigmaI/netI 0.1127 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 2.74 _diffrn_reflns_theta_max 31.98 _reflns_number_total 9952 _reflns_number_gt 5652 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 Express' _computing_cell_refinement 'CAD4 Express' _computing_data_reduction 'XCAD4 (Harms 1996)' _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^)+(0.0438P)^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 -0.01(3) _refine_ls_number_reflns 9952 _refine_ls_number_parameters 356 _refine_ls_number_restraints 392 _refine_ls_R_factor_all 0.0926 _refine_ls_R_factor_gt 0.0440 _refine_ls_wR_factor_ref 0.1036 _refine_ls_wR_factor_gt 0.0898 _refine_ls_goodness_of_fit_ref 0.904 _refine_ls_restrained_S_all 0.945 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.001 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 0.268015(19) 0.361946(19) 0.047011(11) 0.03230(7) Uani 1 1 d . . . Cl1 Cl 0.13961(8) 0.35222(9) 0.09823(4) 0.0554(3) Uani 1 1 d . . . P1 P 0.20304(7) 0.46462(7) -0.00824(4) 0.0364(2) Uani 1 1 d . . . P2 P 0.35605(7) 0.27321(7) 0.10174(3) 0.03717(19) Uani 1 1 d . . . O1 O 0.4884(6) 0.4353(7) -0.0409(3) 0.063(2) Uani 0.50 1 d PD . . N1 N 0.37281(19) 0.37281(19) 0.0000 0.0361(10) Uani 1 2 d SD . . N2 N 0.4781(8) 0.7832(7) 0.1663(4) 0.083(2) Uani 0.50 1 d PU . . C1 C 0.2533(3) 0.4665(3) -0.07337(15) 0.0407(9) Uani 1 1 d . . . H1A H 0.2147 0.4998 -0.0966 0.053 Uiso 1 1 d R . . H1B H 0.3096 0.4979 -0.0714 0.053 Uiso 1 1 d R . . C3 C 0.4351(3) 0.4351(3) 0.0000 0.0437(14) Uani 1 2 d SD . . C4 C 0.4474(15) 0.5108(12) 0.0347(6) 0.0633(11) Uani 0.50 1 d PDU . . C5 C 0.5018(7) 0.5789(6) 0.0201(4) 0.0638(11) Uani 0.50 1 d PDU . . H5 H 0.5316 0.5778 -0.0117 0.083 Uiso 0.50 1 calc PR . . C6 C 0.5118(7) 0.6519(7) 0.0552(4) 0.0641(11) Uani 0.50 1 d PDU . . H6 H 0.5438 0.7022 0.0453 0.083 Uiso 0.50 1 calc PR . . C7 C 0.4748(7) 0.6472(7) 0.1022(4) 0.0639(10) Uani 0.50 1 d PDU . . C8 C 0.4255(7) 0.5788(6) 0.1188(4) 0.0632(11) Uani 0.50 1 d PDU . . H8 H 0.4029 0.5771 0.1525 0.082 Uiso 0.50 1 calc PR . . C9 C 0.4090(7) 0.5089(6) 0.0827(4) 0.0629(11) Uani 0.50 1 d PDU . . H9 H 0.3720 0.4618 0.0920 0.082 Uiso 0.50 1 calc PR . . C10 C 0.4787(8) 0.7253(7) 0.1384(4) 0.0651(11) Uani 0.50 1 d PU . . C1P C 0.0837(3) 0.4605(3) -0.02124(16) 0.0461(9) Uani 1 1 d U . . C2P C 0.0402(4) 0.5347(4) -0.0389(2) 0.0719(14) Uani 1 1 d U . . H2P H 0.0695 0.5891 -0.0414 0.093 Uiso 1 1 calc R . . C3P C -0.0489(4) 0.5268(5) -0.0528(3) 0.0890(17) Uani 1 1 d U . . H3P H -0.0799 0.5771 -0.0637 0.116 Uiso 1 1 calc R . . C4P C -0.0916(4) 0.4475(5) -0.0510(2) 0.0839(16) Uani 1 1 d U . . H4P H -0.1508 0.4435 -0.0615 0.109 Uiso 1 1 calc R . . C5P C -0.0486(3) 0.3747(5) -0.0339(2) 0.0693(14) Uani 1 1 d U . . H5P H -0.0785 0.3206 -0.0321 0.090 Uiso 1 1 calc R . . C6P C 0.0399(3) 0.3796(3) -0.01905(16) 0.0508(11) Uani 1 1 d U . . H6P H 0.0696 0.3288 -0.0077 0.066 Uiso 1 1 calc R . . C7P C 0.2209(3) 0.5762(3) 0.01768(16) 0.0490(10) Uani 1 1 d U . . C8P C 0.1873(4) 0.5931(4) 0.0670(2) 0.0793(16) Uani 1 1 d U . . H8P H 0.1559 0.5489 0.0845 0.103 Uiso 1 1 calc R . . C9P C 0.1998(5) 0.6735(4) 0.0900(3) 0.0929(18) Uani 1 1 d U . . H9P H 0.1760 0.6841 0.1229 0.121 Uiso 1 1 calc R . . C10P C 0.2469(5) 0.7390(4) 0.0654(3) 0.0878(17) Uani 1 1 d U . . H10P H 0.2563 0.7936 0.0816 0.114 Uiso 1 1 calc R . . C11P C 0.2801(5) 0.7229(4) 0.0162(2) 0.0825(16) Uani 1 1 d U . . H11P H 0.3117 0.7670 -0.0013 0.107 Uiso 1 1 calc R . . C12P C 0.2668(4) 0.6428(3) -0.0065(2) 0.0668(12) Uani 1 1 d U . . H12P H 0.2898 0.6328 -0.0397 0.087 Uiso 1 1 calc R . . C13P C 0.3818(3) 0.3281(3) 0.16323(18) 0.0514(11) Uani 1 1 d U . . C14P C 0.4606(4) 0.3142(4) 0.1899(2) 0.0621(13) Uani 1 1 d U . . H14P H 0.5035 0.2759 0.1764 0.081 Uiso 1 1 calc R . . C15P C 0.4754(4) 0.3578(4) 0.2371(2) 0.0727(14) Uani 1 1 d U . . H15P H 0.5282 0.3483 0.2551 0.095 Uiso 1 1 calc R . . C16P C 0.4134(5) 0.4141(5) 0.2568(3) 0.0907(18) Uani 1 1 d U . . H16P H 0.4239 0.4426 0.2884 0.118 Uiso 1 1 calc R . . C17P C 0.3374(5) 0.4289(5) 0.2314(2) 0.0915(18) Uani 1 1 d U . . H17P H 0.2956 0.4680 0.2453 0.119 Uiso 1 1 calc R . . C18P C 0.3200(4) 0.3863(4) 0.1840(2) 0.0763(16) Uani 1 1 d U . . H18P H 0.2668 0.3971 0.1665 0.099 Uiso 1 1 calc R . . C19P C 0.3141(3) 0.1644(3) 0.12172(16) 0.0498(11) Uani 1 1 d U . . C20P C 0.3698(4) 0.1056(3) 0.14992(19) 0.0668(13) Uani 1 1 d U . . H20P H 0.4284 0.1208 0.1576 0.087 Uiso 1 1 calc R . . C21P C 0.3344(5) 0.0240(4) 0.1659(2) 0.0845(16) Uani 1 1 d U . . H21P H 0.3696 -0.0162 0.1843 0.110 Uiso 1 1 calc R . . C22P C 0.2474(5) 0.0031(4) 0.1543(2) 0.0848(17) Uani 1 1 d U . . H22P H 0.2242 -0.0508 0.1661 0.110 Uiso 1 1 calc R . . C23P C 0.1943(5) 0.0583(4) 0.1263(2) 0.0807(17) Uani 1 1 d U . . H23P H 0.1360 0.0420 0.1186 0.105 Uiso 1 1 calc R . . C24P C 0.2283(4) 0.1398(3) 0.10932(18) 0.0600(10) Uani 1 1 d U . . H24P H 0.1928 0.1777 0.0895 0.078 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 0.03241(14) 0.03608(15) 0.02841(11) 0.00382(12) 0.00051(12) -0.00320(11) Cl1 0.0437(5) 0.0782(8) 0.0444(5) 0.0133(5) 0.0127(5) -0.0027(6) P1 0.0361(5) 0.0384(5) 0.0346(5) 0.0058(4) 0.0024(4) 0.0006(4) P2 0.0434(5) 0.0405(5) 0.0276(4) -0.0006(4) -0.0061(4) -0.0004(4) O1 0.069(7) 0.058(5) 0.061(5) 0.004(4) 0.029(5) -0.009(4) N1 0.0363(14) 0.0363(14) 0.036(2) 0.0005(14) -0.0005(14) -0.0043(19) N2 0.107(4) 0.064(4) 0.077(4) -0.015(3) -0.021(4) -0.005(4) C1 0.045(2) 0.039(2) 0.038(2) 0.0124(17) -0.0012(17) 0.0003(17) C3 0.0388(19) 0.0388(19) 0.053(4) 0.0000(19) 0.0000(19) -0.005(2) C4 0.0730(19) 0.0530(17) 0.0638(19) -0.0066(16) -0.0106(16) -0.0104(16) C5 0.0735(19) 0.0534(17) 0.0644(18) -0.0065(16) -0.0100(16) -0.0108(16) C6 0.0743(19) 0.0534(17) 0.0648(18) -0.0066(15) -0.0105(16) -0.0108(15) C7 0.0745(18) 0.0531(16) 0.0641(18) -0.0071(15) -0.0118(15) -0.0102(15) C8 0.0734(19) 0.0528(17) 0.0633(18) -0.0071(15) -0.0114(16) -0.0103(15) C9 0.0728(19) 0.0527(17) 0.0633(18) -0.0069(16) -0.0111(16) -0.0107(16) C10 0.076(2) 0.0536(18) 0.0651(19) -0.0074(17) -0.0125(17) -0.0097(17) C1P 0.039(2) 0.062(2) 0.038(2) 0.0042(19) 0.0031(17) 0.0048(18) C2P 0.059(3) 0.079(3) 0.078(3) 0.030(3) -0.001(2) 0.012(2) C3P 0.068(3) 0.107(4) 0.092(4) 0.036(3) -0.007(3) 0.022(3) C4P 0.055(3) 0.120(4) 0.077(3) 0.018(3) -0.002(3) -0.002(3) C5P 0.046(2) 0.101(3) 0.061(3) 0.003(3) 0.000(2) -0.011(2) C6P 0.042(2) 0.067(3) 0.043(2) 0.0048(19) 0.0023(17) -0.0023(19) C7P 0.059(2) 0.042(2) 0.045(2) 0.0047(18) 0.0026(19) -0.0003(19) C8P 0.105(4) 0.060(3) 0.072(3) -0.010(2) 0.024(3) -0.012(3) C9P 0.125(4) 0.078(3) 0.076(3) -0.015(3) 0.024(3) -0.006(3) C10P 0.121(4) 0.063(3) 0.079(3) -0.011(3) 0.005(3) -0.011(3) C11P 0.115(4) 0.060(3) 0.073(3) 0.002(3) 0.005(3) -0.021(3) C12P 0.090(3) 0.053(2) 0.058(2) -0.001(2) 0.008(2) -0.015(2) C13P 0.061(3) 0.050(2) 0.044(2) -0.0074(18) -0.0134(19) -0.0022(19) C14P 0.063(3) 0.065(3) 0.059(3) -0.014(2) -0.017(2) 0.010(2) C15P 0.083(3) 0.081(3) 0.054(3) -0.012(3) -0.028(2) 0.003(3) C16P 0.104(4) 0.101(4) 0.067(3) -0.028(3) -0.018(3) 0.001(3) C17P 0.092(4) 0.108(4) 0.075(3) -0.036(3) -0.007(3) 0.018(3) C18P 0.076(3) 0.097(4) 0.056(3) -0.030(3) -0.012(2) 0.025(3) C19P 0.070(3) 0.046(2) 0.034(2) -0.0001(16) 0.0006(19) -0.010(2) C20P 0.098(3) 0.053(2) 0.050(2) 0.009(2) -0.010(3) -0.010(3) C21P 0.126(4) 0.066(3) 0.061(3) 0.017(3) -0.006(3) -0.004(3) C22P 0.125(4) 0.064(3) 0.066(3) 0.009(3) 0.015(3) -0.020(3) C23P 0.094(4) 0.076(3) 0.072(3) -0.009(3) 0.020(3) -0.026(3) C24P 0.069(3) 0.055(2) 0.056(2) -0.003(2) 0.012(2) -0.015(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 N1 1.988(3) . ? Pd1 P1 2.3088(13) . ? Pd1 Cl1 2.3365(13) . ? Pd1 P2 2.3423(12) . ? Pd1 Pd1 3.1273(9) 6 ? P1 C1P 1.823(4) . ? P1 C1 1.831(4) . ? P1 C7P 1.822(5) . ? P2 C13P 1.819(4) . ? P2 C19P 1.824(5) . ? P2 C1 1.835(4) 6 ? O1 C4 0.414(15) 6 ? O1 C9 1.183(12) 6 ? O1 C3 1.319(4) . ? O1 C5 1.768(12) 6 ? N1 C3 1.321(6) . ? N1 Pd1 1.988(3) 6 ? N2 C10 1.126(13) . ? C1 P2 1.835(4) 6 ? C1 H1A 0.9701 . ? C1 H1B 0.9701 . ? C3 O1 1.319(4) 6 ? C3 C4 1.454(17) . ? C3 C4 1.454(17) 6 ? C4 O1 0.414(15) 6 ? C4 C9 1.360(11) . ? C4 C5 1.360(11) . ? C5 C6 1.425(11) . ? C5 H5 0.9300 . ? C6 C7 1.329(10) . ? C6 H6 0.9300 . ? C7 C8 1.333(10) . ? C7 C10 1.496(15) . ? C8 C9 1.420(11) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C1P C2P 1.369(7) . ? C1P C6P 1.383(6) . ? C2P C3P 1.389(8) . ? C2P H2P 0.9300 . ? C3P C4P 1.352(9) . ? C3P H3P 0.9300 . ? C4P C5P 1.342(9) . ? C4P H4P 0.9300 . ? C5P C6P 1.383(7) . ? C5P H5P 0.9300 . ? C6P H6P 0.9300 . ? C7P C12P 1.363(7) . ? C7P C8P 1.383(7) . ? C8P C9P 1.356(8) . ? C8P H8P 0.9300 . ? C9P C10P 1.365(9) . ? C9P H9P 0.9300 . ? C10P C11P 1.376(9) . ? C10P H10P 0.9300 . ? C11P C12P 1.351(7) . ? C11P H11P 0.9300 . ? C12P H12P 0.9300 . ? C13P C14P 1.382(7) . ? C13P C18P 1.382(7) . ? C14P C15P 1.392(7) . ? C14P H14P 0.9300 . ? C15P C16P 1.355(9) . ? C15P H15P 0.9300 . ? C16P C17P 1.332(9) . ? C16P H16P 0.9300 . ? C17P C18P 1.396(7) . ? C17P H17P 0.9300 . ? C18P H18P 0.9300 . ? C19P C24P 1.377(7) . ? C19P C20P 1.414(7) . ? C20P C21P 1.397(8) . ? C20P H20P 0.9300 . ? C21P C22P 1.376(9) . ? C21P H21P 0.9300 . ? C22P C23P 1.355(9) . ? C22P H22P 0.9300 . ? C23P C24P 1.396(8) . ? C23P H23P 0.9300 . ? C24P H24P 0.9300 . ? 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 N1 Pd1 P1 84.72(4) . . ? N1 Pd1 Cl1 176.62(4) . . ? P1 Pd1 Cl1 92.16(4) . . ? N1 Pd1 P2 87.88(4) . . ? P1 Pd1 P2 170.05(4) . . ? Cl1 Pd1 P2 95.37(5) . . ? N1 Pd1 Pd1 38.13(9) . 6 ? P1 Pd1 Pd1 91.09(4) . 6 ? Cl1 Pd1 Pd1 140.94(3) . 6 ? P2 Pd1 Pd1 87.16(4) . 6 ? C1P P1 C1 103.80(19) . . ? C1P P1 C7P 104.0(2) . . ? C1 P1 C7P 104.94(19) . . ? C1P P1 Pd1 120.28(15) . . ? C1 P1 Pd1 113.27(13) . . ? C7P P1 Pd1 109.16(15) . . ? C13P P2 C19P 103.6(2) . . ? C13P P2 C1 103.0(2) . 6 ? C19P P2 C1 106.1(2) . 6 ? C13P P2 Pd1 112.39(16) . . ? C19P P2 Pd1 118.86(17) . . ? C1 P2 Pd1 111.43(13) 6 . ? C4 O1 C9 107(3) 6 6 ? C4 O1 C3 101(3) 6 . ? C9 O1 C3 151.3(8) 6 . ? C4 O1 C5 9(5) 6 6 ? C9 O1 C5 105.1(7) 6 6 ? C3 O1 C5 103.2(6) . 6 ? C3 N1 Pd1 128.14(9) . . ? C3 N1 Pd1 128.13(9) . 6 ? Pd1 N1 Pd1 103.73(18) . 6 ? P1 C1 P2 114.5(2) . 6 ? P1 C1 H1A 108.8 . . ? P2 C1 H1A 108.6 6 . ? P1 C1 H1B 108.6 . . ? P2 C1 H1B 108.6 6 . ? H1A C1 H1B 107.6 . . ? N1 C3 O1 115.5(4) . 6 ? N1 C3 O1 115.5(4) . . ? O1 C3 O1 128.9(8) 6 . ? N1 C3 C4 130.0(5) . . ? O1 C3 C4 16.3(6) 6 . ? O1 C3 C4 113.9(6) . . ? N1 C3 C4 130.0(5) . 6 ? O1 C3 C4 113.9(6) 6 6 ? O1 C3 C4 16.3(6) . 6 ? C4 C3 C4 100.0(10) . 6 ? O1 C4 C9 56(2) 6 . ? O1 C4 C5 168(7) 6 . ? C9 C4 C5 121.2(13) . . ? O1 C4 C3 63(2) 6 . ? C9 C4 C3 118.9(9) . . ? C5 C4 C3 119.8(9) . . ? C4 C5 C6 118.0(10) . . ? C4 C5 H5 121.0 . . ? C6 C5 H5 121.0 . . ? C7 C6 C5 119.1(9) . . ? C7 C6 H6 120.4 . . ? C5 C6 H6 120.4 . . ? C6 C7 C8 124.1(10) . . ? C6 C7 C10 120.2(8) . . ? C8 C7 C10 115.3(8) . . ? C7 C8 C9 117.3(10) . . ? C7 C8 H8 121.3 . . ? C9 C8 H8 121.3 . . ? C4 C9 C8 120.0(10) . . ? C4 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? N2 C10 C7 177.1(13) . . ? C2P C1P C6P 120.0(4) . . ? C2P C1P P1 120.1(4) . . ? C6P C1P P1 119.4(4) . . ? C1P C2P C3P 118.4(6) . . ? C1P C2P H2P 120.8 . . ? C3P C2P H2P 120.8 . . ? C4P C3P C2P 121.5(6) . . ? C4P C3P H3P 119.3 . . ? C2P C3P H3P 119.3 . . ? C5P C4P C3P 120.0(6) . . ? C5P C4P H4P 120.0 . . ? C3P C4P H4P 120.0 . . ? C4P C5P C6P 120.6(6) . . ? C4P C5P H5P 119.7 . . ? C6P C5P H5P 119.7 . . ? C5P C6P C1P 119.5(5) . . ? C5P C6P H6P 120.3 . . ? C1P C6P H6P 120.3 . . ? C12P C7P C8P 117.7(5) . . ? C12P C7P P1 125.6(4) . . ? C8P C7P P1 116.6(4) . . ? C9P C8P C7P 120.7(6) . . ? C9P C8P H8P 119.7 . . ? C7P C8P H8P 119.7 . . ? C8P C9P C10P 120.8(6) . . ? C8P C9P H9P 119.6 . . ? C10P C9P H9P 119.6 . . ? C9P C10P C11P 119.0(6) . . ? C9P C10P H10P 120.5 . . ? C11P C10P H10P 120.5 . . ? C12P C11P C10P 119.8(6) . . ? C12P C11P H11P 120.1 . . ? C10P C11P H11P 120.1 . . ? C11P C12P C7P 122.1(5) . . ? C11P C12P H12P 118.9 . . ? C7P C12P H12P 118.9 . . ? C14P C13P C18P 118.6(4) . . ? C14P C13P P2 122.8(4) . . ? C18P C13P P2 118.5(4) . . ? C13P C14P C15P 119.7(5) . . ? C13P C14P H14P 120.2 . . ? C15P C14P H14P 120.2 . . ? C16P C15P C14P 120.5(5) . . ? C16P C15P H15P 119.7 . . ? C14P C15P H15P 119.7 . . ? C17P C16P C15P 120.6(6) . . ? C17P C16P H16P 119.7 . . ? C15P C16P H16P 119.7 . . ? C16P C17P C18P 120.7(6) . . ? C16P C17P H17P 119.7 . . ? C18P C17P H17P 119.7 . . ? C13P C18P C17P 119.9(5) . . ? C13P C18P H18P 120.1 . . ? C17P C18P H18P 120.1 . . ? C24P C19P C20P 120.3(5) . . ? C24P C19P P2 119.8(4) . . ? C20P C19P P2 119.9(4) . . ? C21P C20P C19P 118.2(6) . . ? C21P C20P H20P 120.9 . . ? C19P C20P H20P 120.9 . . ? C22P C21P C20P 119.9(6) . . ? C22P C21P H21P 120.1 . . ? C20P C21P H21P 120.1 . . ? C23P C22P C21P 122.2(6) . . ? C23P C22P H22P 118.9 . . ? C21P C22P H22P 118.9 . . ? C22P C23P C24P 119.1(6) . . ? C22P C23P H23P 120.4 . . ? C24P C23P H23P 120.4 . . ? C19P C24P C23P 120.3(6) . . ? C19P C24P H24P 119.9 . . ? C23P C24P H24P 119.9 . . ? 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 N1 Pd1 P1 C1P 146.37(19) . . . . ? Cl1 Pd1 P1 C1P -32.34(17) . . . . ? P2 Pd1 P1 C1P -171.5(2) . . . . ? Pd1 Pd1 P1 C1P 108.72(17) 6 . . . ? N1 Pd1 P1 C1 22.89(17) . . . . ? Cl1 Pd1 P1 C1 -155.82(15) . . . . ? P2 Pd1 P1 C1 65.0(3) . . . . ? Pd1 Pd1 P1 C1 -14.76(15) 6 . . . ? N1 Pd1 P1 C7P -93.63(18) . . . . ? Cl1 Pd1 P1 C7P 87.66(16) . . . . ? P2 Pd1 P1 C7P -51.5(3) . . . . ? Pd1 Pd1 P1 C7P -131.27(16) 6 . . . ? N1 Pd1 P2 C13P 111.2(2) . . . . ? P1 Pd1 P2 C13P 69.3(3) . . . . ? Cl1 Pd1 P2 C13P -69.74(18) . . . . ? Pd1 Pd1 P2 C13P 149.34(18) 6 . . . ? N1 Pd1 P2 C19P -127.63(19) . . . . ? P1 Pd1 P2 C19P -169.5(2) . . . . ? Cl1 Pd1 P2 C19P 51.45(17) . . . . ? Pd1 Pd1 P2 C19P -89.46(17) 6 . . . ? N1 Pd1 P2 C1 -3.87(16) . . . 6 ? P1 Pd1 P2 C1 -45.8(3) . . . 6 ? Cl1 Pd1 P2 C1 175.21(14) . . . 6 ? Pd1 Pd1 P2 C1 34.30(14) 6 . . 6 ? P1 Pd1 N1 C3 81.45(3) . . . . ? Cl1 Pd1 N1 C3 103.8(16) . . . . ? P2 Pd1 N1 C3 -91.90(3) . . . . ? Pd1 Pd1 N1 C3 180.0 6 . . . ? P1 Pd1 N1 Pd1 -98.55(3) . . . 6 ? Cl1 Pd1 N1 Pd1 -76.2(16) . . . 6 ? P2 Pd1 N1 Pd1 88.10(3) . . . 6 ? C1P P1 C1 P2 -87.3(3) . . . 6 ? C7P P1 C1 P2 163.8(2) . . . 6 ? Pd1 P1 C1 P2 44.8(3) . . . 6 ? Pd1 N1 C3 O1 11.4(7) . . . 6 ? Pd1 N1 C3 O1 -168.6(7) 6 . . 6 ? Pd1 N1 C3 O1 -168.6(7) . . . . ? Pd1 N1 C3 O1 11.4(7) 6 . . . ? Pd1 N1 C3 C4 2.5(13) . . . . ? Pd1 N1 C3 C4 -177.5(13) 6 . . . ? Pd1 N1 C3 C4 -177.5(13) . . . 6 ? Pd1 N1 C3 C4 2.5(13) 6 . . 6 ? C4 O1 C3 N1 -155(5) 6 . . . ? C9 O1 C3 N1 7(3) 6 . . . ? C5 O1 C3 N1 -163.9(5) 6 . . . ? C4 O1 C3 O1 25(5) 6 . . 6 ? C9 O1 C3 O1 -173(3) 6 . . 6 ? C5 O1 C3 O1 16.1(5) 6 . . 6 ? C4 O1 C3 C4 32(7) 6 . . . ? C9 O1 C3 C4 -165.5(18) 6 . . . ? C5 O1 C3 C4 23(2) 6 . . . ? C9 O1 C3 C4 162(8) 6 . . 6 ? C5 O1 C3 C4 -9(5) 6 . . 6 ? N1 C3 C4 O1 30(6) . . . 6 ? O1 C3 C4 O1 -159(5) . . . 6 ? C4 C3 C4 O1 -150(6) 6 . . 6 ? N1 C3 C4 C9 21(3) . . . . ? O1 C3 C4 C9 -8(4) 6 . . . ? O1 C3 C4 C9 -167.3(11) . . . . ? C4 C3 C4 C9 -159(3) 6 . . . ? N1 C3 C4 C5 -163.3(12) . . . . ? O1 C3 C4 C5 167(7) 6 . . . ? O1 C3 C4 C5 8(3) . . . . ? C4 C3 C4 C5 16.7(12) 6 . . . ? O1 C4 C5 C6 -80(17) 6 . . . ? C9 C4 C5 C6 -5(3) . . . . ? C3 C4 C5 C6 179.8(14) . . . . ? C4 C5 C6 C7 6(2) . . . . ? C5 C6 C7 C8 -2.3(18) . . . . ? C5 C6 C7 C10 -175.6(10) . . . . ? C6 C7 C8 C9 -2.7(18) . . . . ? C10 C7 C8 C9 170.9(10) . . . . ? O1 C4 C9 C8 166(5) 6 . . . ? C5 C4 C9 C8 0(3) . . . . ? C3 C4 C9 C8 175.3(14) . . . . ? C7 C8 C9 C4 4(2) . . . . ? C6 C7 C10 N2 143(24) . . . . ? C8 C7 C10 N2 -30(25) . . . . ? C1 P1 C1P C2P -73.7(4) . . . . ? C7P P1 C1P C2P 35.9(5) . . . . ? Pd1 P1 C1P C2P 158.4(4) . . . . ? C1 P1 C1P C6P 98.8(4) . . . . ? C7P P1 C1P C6P -151.6(3) . . . . ? Pd1 P1 C1P C6P -29.1(4) . . . . ? C6P C1P C2P C3P 1.8(8) . . . . ? P1 C1P C2P C3P 174.2(5) . . . . ? C1P C2P C3P C4P -2.2(10) . . . . ? C2P C3P C4P C5P 1.9(11) . . . . ? C3P C4P C5P C6P -1.1(10) . . . . ? C4P C5P C6P C1P 0.7(8) . . . . ? C2P C1P C6P C5P -1.1(7) . . . . ? P1 C1P C6P C5P -173.6(4) . . . . ? C1P P1 C7P C12P -112.2(5) . . . . ? C1 P1 C7P C12P -3.5(5) . . . . ? Pd1 P1 C7P C12P 118.2(5) . . . . ? C1P P1 C7P C8P 70.2(5) . . . . ? C1 P1 C7P C8P 179.0(4) . . . . ? Pd1 P1 C7P C8P -59.3(5) . . . . ? C12P C7P C8P C9P 0.3(9) . . . . ? P1 C7P C8P C9P 178.0(6) . . . . ? C7P C8P C9P C10P -1.0(12) . . . . ? C8P C9P C10P C11P 1.3(12) . . . . ? C9P C10P C11P C12P -0.9(11) . . . . ? C10P C11P C12P C7P 0.1(10) . . . . ? C8P C7P C12P C11P 0.2(9) . . . . ? P1 C7P C12P C11P -177.4(5) . . . . ? C19P P2 C13P C14P 82.5(5) . . . . ? C1 P2 C13P C14P -27.8(5) 6 . . . ? Pd1 P2 C13P C14P -147.9(4) . . . . ? C19P P2 C13P C18P -97.7(5) . . . . ? C1 P2 C13P C18P 151.9(5) 6 . . . ? Pd1 P2 C13P C18P 31.9(5) . . . . ? C18P C13P C14P C15P 0.9(9) . . . . ? P2 C13P C14P C15P -179.4(4) . . . . ? C13P C14P C15P C16P -0.4(9) . . . . ? C14P C15P C16P C17P -0.3(11) . . . . ? C15P C16P C17P C18P 0.4(12) . . . . ? C14P C13P C18P C17P -0.8(10) . . . . ? P2 C13P C18P C17P 179.5(5) . . . . ? C16P C17P C18P C13P 0.1(11) . . . . ? C13P P2 C19P C24P 118.5(4) . . . . ? C1 P2 C19P C24P -133.4(4) 6 . . . ? Pd1 P2 C19P C24P -7.0(4) . . . . ? C13P P2 C19P C20P -61.4(4) . . . . ? C1 P2 C19P C20P 46.7(4) 6 . . . ? Pd1 P2 C19P C20P 173.0(3) . . . . ? C24P C19P C20P C21P -1.9(8) . . . . ? P2 C19P C20P C21P 178.1(4) . . . . ? C19P C20P C21P C22P -0.4(9) . . . . ? C20P C21P C22P C23P 1.8(10) . . . . ? C21P C22P C23P C24P -1.1(10) . . . . ? C20P C19P C24P C23P 2.7(7) . . . . ? P2 C19P C24P C23P -177.3(4) . . . . ? C22P C23P C24P C19P -1.2(8) . . . . ? _diffrn_reflns_theta_full 31.98 _refine_diff_density_max 0.470 _refine_diff_density_min -0.949 _refine_diff_density_rms 0.098 # ============================ 3C ========================= data_3c _database_code_depnum_ccdc_archive 'CCDC 232757' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C57 H48 Br Cl2 N O P4 Pd2' _chemical_formula_weight 1250.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 41 21 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y+1/2, x+1/2, z+1/4' '-x, -y, z+1/2' 'y+1/2, -x+1/2, z+3/4' 'x+1/2, -y+1/2, -z+3/4' 'y, x, -z' '-x+1/2, y+1/2, -z+1/4' '-y, -x, -z+1/2' _cell_length_a 15.079(1) _cell_length_b 15.079(1) _cell_length_c 25.970(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5905.0(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 30.70 _cell_measurement_theta_max 36.38 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.407 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2504 _exptl_absorpt_coefficient_mu 7.846 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.6526 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius CAD4' _diffrn_measurement_method \w--2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 2 _diffrn_reflns_number 13245 _diffrn_reflns_av_R_equivalents 0.0888 _diffrn_reflns_av_sigmaI/netI 0.1041 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 4.48 _diffrn_reflns_theta_max 75.49 _reflns_number_total 6031 _reflns_number_gt 5118 _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^)+(0.1004P)^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(2) _refine_ls_number_reflns 6031 _refine_ls_number_parameters 284 _refine_ls_number_restraints 34 _refine_ls_R_factor_all 0.0690 _refine_ls_R_factor_gt 0.0610 _refine_ls_wR_factor_ref 0.1564 _refine_ls_wR_factor_gt 0.1501 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.310 _refine_ls_shift/su_max 0.033 _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 Pd1 Pd 0.14212(4) 0.23639(3) 0.046720(19) 0.04275(18) Uani 1 1 d . . . Br1 Br -0.2327(2) -0.0258(4) 0.13626(15) 0.1319(12) Uani 0.50 1 d PU . . Cl1 Cl 0.14947(18) 0.36379(14) 0.09795(8) 0.0669(5) Uani 1 1 d . . . P1 P 0.22914(13) 0.14869(13) 0.10093(7) 0.0458(4) Uani 1 1 d . . . P3 P 0.04009(14) 0.29960(13) -0.00872(8) 0.0465(4) Uani 1 1 d . . . O1 O 0.0674(12) 0.0245(11) -0.0425(4) 0.088(5) Uani 0.50 1 d PDU . . N1 N 0.1336(4) 0.1336(4) 0.0000 0.0493(19) Uani 1 2 d SD . . C1 C 0.2495(5) 0.0399(6) 0.0732(3) 0.0502(17) Uani 1 1 d . . . H1A H 0.1935 0.0083 0.0714 0.065 Uiso 1 1 calc R . . H1B H 0.2881 0.0072 0.0962 0.065 Uiso 1 1 calc R . . C3 C 0.0722(4) 0.0722(4) 0.0000 0.071(4) Uani 1 2 d SD . . C4 C -0.0040(7) 0.0482(11) 0.0286(5) 0.080(8) Uani 0.50 1 d PGD . . C5 C -0.0729(10) -0.0064(12) 0.0124(5) 0.094(8) Uani 0.50 1 d PG . . H5 H -0.0738 -0.0277 -0.0212 0.122 Uiso 0.50 1 calc PR . . C6 C -0.1404(9) -0.0291(12) 0.0464(6) 0.140(15) Uani 0.50 1 d PG . . H6 H -0.1865 -0.0655 0.0355 0.182 Uiso 0.50 1 calc PR . . C7 C -0.1390(8) 0.0028(12) 0.0966(6) 0.084(6) Uani 0.50 1 d PGU . . C8 C -0.0701(9) 0.0573(11) 0.1128(5) 0.094(8) Uani 0.50 1 d PG . . H8 H -0.0692 0.0786 0.1464 0.123 Uiso 0.50 1 calc PR . . C9 C -0.0026(8) 0.0800(10) 0.0788(6) 0.081(7) Uani 0.50 1 d PG . . H9 H 0.0434 0.1165 0.0897 0.105 Uiso 0.50 1 calc PR . . C1P C 0.3373(3) 0.1894(4) 0.1209(2) 0.057(2) Uani 1 1 d G . . C2P C 0.3606(5) 0.2759(4) 0.1085(3) 0.075(3) Uani 1 1 d G . . H2P H 0.3218 0.3112 0.0896 0.098 Uiso 1 1 calc R . . C3P C 0.4419(5) 0.3098(5) 0.1243(3) 0.100(5) Uani 1 1 d G . . H3P H 0.4576 0.3677 0.1160 0.130 Uiso 1 1 calc R . . C4P C 0.4999(4) 0.2570(7) 0.1524(4) 0.104(4) Uani 1 1 d GU . . H4P H 0.5543 0.2796 0.1630 0.136 Uiso 1 1 calc R . . C5P C 0.4766(5) 0.1704(7) 0.1648(3) 0.110(5) Uani 1 1 d G . . H5P H 0.5153 0.1351 0.1837 0.143 Uiso 1 1 calc R . . C6P C 0.3952(5) 0.1366(5) 0.1490(3) 0.084(3) Uani 1 1 d G . . H6P H 0.3796 0.0787 0.1573 0.109 Uiso 1 1 calc R . . C7P C 0.1737(4) 0.1216(4) 0.1617(2) 0.0552(19) Uani 1 1 d G . . C8P C 0.1865(5) 0.0413(4) 0.1870(3) 0.074(3) Uani 1 1 d G . . H8P H 0.2247 -0.0008 0.1732 0.097 Uiso 1 1 calc R . . C9P C 0.1420(6) 0.0241(5) 0.2327(3) 0.088(4) Uani 1 1 d G . . H9P H 0.1505 -0.0296 0.2496 0.115 Uiso 1 1 calc R . . C10P C 0.0847(7) 0.0871(6) 0.2533(3) 0.093(4) Uani 1 1 d G . . H10P H 0.0550 0.0755 0.2839 0.121 Uiso 1 1 calc R . . C11P C 0.0720(7) 0.1674(6) 0.2280(3) 0.108(5) Uani 1 1 d G . . H11P H 0.0337 0.2095 0.2418 0.140 Uiso 1 1 calc R . . C12P C 0.1165(6) 0.1846(4) 0.1822(3) 0.088(4) Uani 1 1 d G . . H12P H 0.1080 0.2383 0.1653 0.114 Uiso 1 1 calc R . . C13P C -0.0696(3) 0.2788(5) 0.0172(3) 0.062(2) Uani 1 1 d G . . C14P C -0.1362(4) 0.2348(6) -0.0096(2) 0.080(3) Uani 1 1 d G . . H14P H -0.1263 0.2160 -0.0432 0.104 Uiso 1 1 calc R . . C15P C -0.2175(4) 0.2189(8) 0.0138(3) 0.105(5) Uani 1 1 d G . . H15P H -0.2621 0.1895 -0.0041 0.137 Uiso 1 1 calc R . . C16P C -0.2323(4) 0.2470(9) 0.0641(3) 0.113(5) Uani 1 1 d G . . H16P H -0.2867 0.2364 0.0798 0.146 Uiso 1 1 calc R . . C17P C -0.1657(6) 0.2910(9) 0.0909(3) 0.128(7) Uani 1 1 d G . . H17P H -0.1756 0.3098 0.1245 0.166 Uiso 1 1 calc R . . C18P C -0.0844(5) 0.3069(7) 0.0674(3) 0.101(4) Uani 1 1 d GU . . H18P H -0.0399 0.3364 0.0854 0.131 Uiso 1 1 calc R . . C19P C 0.0432(4) 0.4177(3) -0.0220(3) 0.061(2) Uani 1 1 d G . . C20P C -0.0320(4) 0.4611(5) -0.0400(3) 0.084(3) Uani 1 1 d G . . H20P H -0.0854 0.4307 -0.0427 0.110 Uiso 1 1 calc R . . C21P C -0.0273(5) 0.5500(5) -0.0539(4) 0.115(6) Uani 1 1 d G . . H21P H -0.0776 0.5791 -0.0659 0.149 Uiso 1 1 calc R . . C22P C 0.0526(6) 0.5955(3) -0.0497(4) 0.098(4) Uani 1 1 d G . . H22P H 0.0557 0.6550 -0.0590 0.127 Uiso 1 1 calc R . . C23P C 0.1277(5) 0.5521(4) -0.0317(3) 0.091(4) Uani 1 1 d G . . H23P H 0.1812 0.5825 -0.0290 0.118 Uiso 1 1 calc R . . C24P C 0.1230(4) 0.4632(4) -0.0178(3) 0.067(2) Uani 1 1 d G . . H24P H 0.1733 0.4341 -0.0058 0.087 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 0.0457(3) 0.0405(3) 0.0420(3) 0.0001(2) -0.0047(2) -0.0043(2) Br1 0.0789(15) 0.196(2) 0.1207(18) 0.0693(18) -0.0045(14) -0.0405(16) Cl1 0.0905(15) 0.0511(10) 0.0591(10) -0.0109(8) -0.0147(11) -0.0059(11) P1 0.0480(9) 0.0464(9) 0.0430(8) 0.0070(7) -0.0026(7) -0.0046(7) P3 0.0468(10) 0.0441(9) 0.0485(9) 0.0005(7) -0.0070(8) 0.0010(7) O1 0.088(7) 0.076(7) 0.099(7) -0.020(6) -0.029(6) -0.015(6) N1 0.049(3) 0.049(3) 0.049(4) 0.004(3) -0.004(3) 0.000(4) C1 0.043(4) 0.057(4) 0.050(4) 0.009(3) -0.003(3) -0.001(3) C3 0.047(4) 0.047(4) 0.118(12) 0.014(5) -0.014(5) -0.004(5) C4 0.039(9) 0.060(11) 0.14(2) 0.007(12) -0.036(11) -0.013(8) C5 0.089(17) 0.098(18) 0.094(17) 0.012(14) -0.019(14) -0.025(14) C6 0.079(17) 0.12(2) 0.22(4) 0.02(3) -0.03(2) -0.061(18) C7 0.074(8) 0.096(8) 0.083(8) 0.007(7) -0.006(6) -0.006(7) C8 0.032(8) 0.096(17) 0.16(2) 0.005(17) 0.009(11) -0.013(9) C9 0.078(14) 0.054(10) 0.112(17) 0.008(11) -0.049(14) -0.017(9) C1P 0.052(5) 0.071(6) 0.048(4) 0.001(4) 0.000(3) -0.011(4) C2P 0.061(5) 0.083(7) 0.081(6) -0.013(5) 0.010(5) -0.022(5) C3P 0.085(8) 0.114(11) 0.102(9) -0.030(8) 0.015(7) -0.045(8) C4P 0.088(6) 0.122(7) 0.103(6) -0.014(6) -0.005(5) -0.023(6) C5P 0.078(8) 0.165(16) 0.086(8) 0.007(9) -0.031(7) -0.007(9) C6P 0.063(6) 0.125(10) 0.063(5) 0.012(6) -0.019(5) -0.009(7) C7P 0.050(4) 0.065(5) 0.050(4) 0.000(3) 0.004(3) -0.009(3) C8P 0.082(7) 0.076(6) 0.066(5) 0.019(5) 0.010(5) 0.011(5) C9P 0.102(9) 0.090(8) 0.073(7) 0.027(6) 0.020(6) -0.003(7) C10P 0.108(10) 0.104(10) 0.067(6) 0.011(6) 0.029(7) 0.011(8) C11P 0.137(14) 0.101(10) 0.085(8) 0.014(7) 0.056(9) 0.025(9) C12P 0.104(9) 0.086(8) 0.074(6) 0.005(6) 0.033(6) 0.013(7) C13P 0.062(5) 0.063(5) 0.061(5) -0.010(4) -0.007(4) 0.008(4) C14P 0.061(5) 0.099(8) 0.079(6) -0.008(6) -0.001(5) -0.019(5) C15P 0.051(6) 0.156(14) 0.109(10) -0.024(10) -0.006(6) -0.030(7) C16P 0.065(7) 0.185(18) 0.088(8) -0.008(10) 0.016(6) -0.013(9) C17P 0.090(10) 0.21(2) 0.086(8) -0.024(11) 0.030(7) -0.024(12) C18P 0.092(6) 0.121(7) 0.090(6) -0.013(6) 0.001(5) -0.010(6) C19P 0.084(6) 0.049(4) 0.049(4) -0.001(3) -0.007(4) 0.004(4) C20P 0.081(7) 0.064(6) 0.108(9) 0.002(6) -0.035(7) 0.017(5) C21P 0.153(15) 0.070(7) 0.122(11) 0.012(8) -0.046(11) 0.030(8) C22P 0.128(12) 0.054(6) 0.112(10) 0.005(6) -0.023(9) -0.006(7) C23P 0.132(11) 0.057(6) 0.084(7) 0.011(5) -0.022(7) -0.014(7) C24P 0.099(7) 0.042(4) 0.059(5) 0.001(3) -0.007(4) -0.009(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 Pd1 N1 1.972(5) . ? Pd1 P3 2.313(2) . ? Pd1 P1 2.3350(19) . ? Pd1 Cl1 2.339(2) . ? Pd1 Pd1 3.1512(11) 6 ? Br1 C7 1.801(9) . ? P1 C1P 1.817(5) . ? P1 C1 1.817(9) . ? P1 C7P 1.832(5) . ? P3 C13P 1.813(5) . ? P3 C19P 1.814(5) . ? P3 C1 1.837(8) 6 ? O1 C4 0.632(18) 6 ? O1 C9 1.045(11) 6 ? O1 C3 1.3206(9) . ? N1 C3 1.310(7) . ? N1 Pd1 1.972(5) 6 ? C1 P3 1.836(8) 6 ? C3 O1 1.3206(9) 6 ? C3 C4 1.416(7) . ? C4 O1 0.632(18) 6 ? C4 C5 1.3900 . ? C4 C9 1.3900 . ? C5 C6 1.3900 . ? C6 C7 1.3900 . ? C7 C8 1.3900 . ? C8 C9 1.3900 . ? C1P C2P 1.3900 . ? C1P C6P 1.3900 . ? C2P C3P 1.3900 . ? C3P C4P 1.3900 . ? C4P C5P 1.3900 . ? C5P C6P 1.3900 . ? C7P C8P 1.3900 . ? C7P C12P 1.3900 . ? C8P C9P 1.3900 . ? C9P C10P 1.3900 . ? C10P C11P 1.3900 . ? C11P C12P 1.3900 . ? C13P C14P 1.3900 . ? C13P C18P 1.3900 . ? C14P C15P 1.3900 . ? C15P C16P 1.3900 . ? C16P C17P 1.3900 . ? C17P C18P 1.3900 . ? C19P C20P 1.3900 . ? C19P C24P 1.3900 . ? C20P C21P 1.3900 . ? C21P C22P 1.3900 . ? C22P C23P 1.3900 . ? C23P C24P 1.3900 . ? 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 N1 Pd1 P3 84.13(6) . . ? N1 Pd1 P1 87.85(5) . . ? P3 Pd1 P1 169.29(7) . . ? N1 Pd1 Cl1 176.50(8) . . ? P3 Pd1 Cl1 92.70(8) . . ? P1 Pd1 Cl1 95.48(8) . . ? N1 Pd1 Pd1 36.98(18) . 6 ? P3 Pd1 Pd1 90.38(6) . 6 ? P1 Pd1 Pd1 87.44(5) . 6 ? Cl1 Pd1 Pd1 141.91(7) . 6 ? C1P P1 C1 105.4(3) . . ? C1P P1 C7P 103.8(3) . . ? C1 P1 C7P 102.6(3) . . ? C1P P1 Pd1 119.0(2) . . ? C1 P1 Pd1 111.5(3) . . ? C7P P1 Pd1 112.9(2) . . ? C13P P3 C19P 105.3(4) . . ? C13P P3 C1 105.4(3) . 6 ? C19P P3 C1 103.4(3) . 6 ? C13P P3 Pd1 107.7(3) . . ? C19P P3 Pd1 120.4(2) . . ? C1 P3 Pd1 113.5(3) 6 . ? C4 O1 C9 109.5(19) 6 6 ? C4 O1 C3 85.2(10) 6 . ? C9 O1 C3 163(2) 6 . ? C3 N1 Pd1 126.98(18) . . ? C3 N1 Pd1 126.97(18) . 6 ? Pd1 N1 Pd1 106.0(4) . 6 ? P1 C1 P3 115.5(4) . 6 ? N1 C3 O1 115.1(7) . . ? N1 C3 O1 115.1(7) . 6 ? O1 C3 O1 129.8(14) . 6 ? N1 C3 C4 139.0(7) . . ? O1 C3 C4 104.7(11) . . ? O1 C3 C4 26.4(8) 6 . ? O1 C4 C5 162.3(16) 6 . ? O1 C4 C9 45.1(11) 6 . ? C5 C4 C9 120.0 . . ? O1 C4 C3 68.4(6) 6 . ? C5 C4 C3 126.8(10) . . ? C9 C4 C3 113.1(10) . . ? C6 C5 C4 120.0 . . ? C7 C6 C5 120.0 . . ? C6 C7 C8 120.0 . . ? C6 C7 Br1 116.3(9) . . ? C8 C7 Br1 123.6(9) . . ? C9 C8 C7 120.0 . . ? C8 C9 C4 120.0 . . ? C2P C1P C6P 120.0 . . ? C2P C1P P1 118.6(4) . . ? C6P C1P P1 121.4(4) . . ? C3P C2P C1P 120.0 . . ? C4P C3P C2P 120.0 . . ? C3P C4P C5P 120.0 . . ? C6P C5P C4P 120.0 . . ? C5P C6P C1P 120.0 . . ? C8P C7P C12P 120.0 . . ? C8P C7P P1 122.5(4) . . ? C12P C7P P1 117.5(4) . . ? C7P C8P C9P 120.0 . . ? C10P C9P C8P 120.0 . . ? C9P C10P C11P 120.0 . . ? C10P C11P C12P 120.0 . . ? C11P C12P C7P 120.0 . . ? C14P C13P C18P 120.0 . . ? C14P C13P P3 123.8(4) . . ? C18P C13P P3 116.2(4) . . ? C15P C14P C13P 120.0 . . ? C14P C15P C16P 120.0 . . ? C17P C16P C15P 120.0 . . ? C16P C17P C18P 120.0 . . ? C17P C18P C13P 120.0 . . ? C20P C19P C24P 120.0 . . ? C20P C19P P3 120.3(4) . . ? C24P C19P P3 119.5(4) . . ? C21P C20P C19P 120.0 . . ? C20P C21P C22P 120.0 . . ? C21P C22P C23P 120.0 . . ? C22P C23P C24P 120.0 . . ? C23P C24P C19P 120.0 . . ? 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 N1 Pd1 P1 C1P 126.2(3) . . . . ? P3 Pd1 P1 C1P 167.7(4) . . . . ? Cl1 Pd1 P1 C1P -52.7(3) . . . . ? Pd1 Pd1 P1 C1P 89.2(3) 6 . . . ? N1 Pd1 P1 C1 3.2(3) . . . . ? P3 Pd1 P1 C1 44.6(5) . . . . ? Cl1 Pd1 P1 C1 -175.7(3) . . . . ? Pd1 Pd1 P1 C1 -33.8(3) 6 . . . ? N1 Pd1 P1 C7P -111.7(3) . . . . ? P3 Pd1 P1 C7P -70.3(5) . . . . ? Cl1 Pd1 P1 C7P 69.4(3) . . . . ? Pd1 Pd1 P1 C7P -148.7(2) 6 . . . ? N1 Pd1 P3 C13P 93.9(3) . . . . ? P1 Pd1 P3 C13P 52.3(5) . . . . ? Cl1 Pd1 P3 C13P -87.6(3) . . . . ? Pd1 Pd1 P3 C13P 130.4(3) 6 . . . ? N1 Pd1 P3 C19P -145.6(3) . . . . ? P1 Pd1 P3 C19P 172.8(4) . . . . ? Cl1 Pd1 P3 C19P 32.9(3) . . . . ? Pd1 Pd1 P3 C19P -109.1(3) 6 . . . ? N1 Pd1 P3 C1 -22.4(3) . . . 6 ? P1 Pd1 P3 C1 -64.1(5) . . . 6 ? Cl1 Pd1 P3 C1 156.1(3) . . . 6 ? Pd1 Pd1 P3 C1 14.1(3) 6 . . 6 ? P3 Pd1 N1 C3 -81.50(6) . . . . ? P1 Pd1 N1 C3 91.40(5) . . . . ? Cl1 Pd1 N1 C3 -106(3) . . . . ? Pd1 Pd1 N1 C3 180.0 6 . . . ? P3 Pd1 N1 Pd1 98.50(6) . . . 6 ? P1 Pd1 N1 Pd1 -88.60(5) . . . 6 ? Cl1 Pd1 N1 Pd1 74(3) . . . 6 ? C1P P1 C1 P3 -75.0(5) . . . 6 ? C7P P1 C1 P3 176.6(4) . . . 6 ? Pd1 P1 C1 P3 55.5(5) . . . 6 ? Pd1 N1 C3 O1 162.8(10) . . . . ? Pd1 N1 C3 O1 -17.2(10) 6 . . . ? Pd1 N1 C3 O1 -17.2(10) . . . 6 ? Pd1 N1 C3 O1 162.8(10) 6 . . 6 ? Pd1 N1 C3 C4 -2.8(10) . . . . ? Pd1 N1 C3 C4 177.2(10) 6 . . . ? C4 O1 C3 N1 159(2) 6 . . . ? C9 O1 C3 N1 6(12) 6 . . . ? C4 O1 C3 O1 -21(2) 6 . . 6 ? C9 O1 C3 O1 -174(12) 6 . . 6 ? C4 O1 C3 C4 -31(3) 6 . . . ? C9 O1 C3 C4 176(11) 6 . . . ? N1 C3 C4 O1 -30(3) . . . 6 ? O1 C3 C4 O1 163.1(19) . . . 6 ? N1 C3 C4 C5 160.3(8) . . . . ? O1 C3 C4 C5 -6.3(17) . . . . ? O1 C3 C4 C5 -169(3) 6 . . . ? N1 C3 C4 C9 -24.1(15) . . . . ? O1 C3 C4 C9 169.3(11) . . . . ? O1 C3 C4 C9 6(2) 6 . . . ? O1 C4 C5 C6 29(9) 6 . . . ? C9 C4 C5 C6 0.0 . . . . ? C3 C4 C5 C6 175.3(16) . . . . ? C4 C5 C6 C7 0.0 . . . . ? C5 C6 C7 C8 0.0 . . . . ? C5 C6 C7 Br1 176.7(14) . . . . ? C6 C7 C8 C9 0.0 . . . . ? Br1 C7 C8 C9 -176.5(14) . . . . ? C7 C8 C9 C4 0.0 . . . . ? O1 C4 C9 C8 -168(4) 6 . . . ? C5 C4 C9 C8 0.0 . . . . ? C3 C4 C9 C8 -175.9(14) . . . . ? C1 P1 C1P C2P 133.8(4) . . . . ? C7P P1 C1P C2P -118.7(4) . . . . ? Pd1 P1 C1P C2P 7.8(5) . . . . ? C1 P1 C1P C6P -47.8(5) . . . . ? C7P P1 C1P C6P 59.7(5) . . . . ? Pd1 P1 C1P C6P -173.8(3) . . . . ? C6P C1P C2P C3P 0.0 . . . . ? P1 C1P C2P C3P 178.4(5) . . . . ? C1P C2P C3P C4P 0.0 . . . . ? C2P C3P C4P C5P 0.0 . . . . ? C3P C4P C5P C6P 0.0 . . . . ? C4P C5P C6P C1P 0.0 . . . . ? C2P C1P C6P C5P 0.0 . . . . ? P1 C1P C6P C5P -178.4(5) . . . . ? C1P P1 C7P C8P -83.5(5) . . . . ? C1 P1 C7P C8P 26.1(6) . . . . ? Pd1 P1 C7P C8P 146.3(4) . . . . ? C1P P1 C7P C12P 97.1(5) . . . . ? C1 P1 C7P C12P -153.3(5) . . . . ? Pd1 P1 C7P C12P -33.1(5) . . . . ? C12P C7P C8P C9P 0.0 . . . . ? P1 C7P C8P C9P -179.4(6) . . . . ? C7P C8P C9P C10P 0.0 . . . . ? C8P C9P C10P C11P 0.0 . . . . ? C9P C10P C11P C12P 0.0 . . . . ? C10P C11P C12P C7P 0.0 . . . . ? C8P C7P C12P C11P 0.0 . . . . ? P1 C7P C12P C11P 179.4(6) . . . . ? C19P P3 C13P C14P 107.9(6) . . . . ? C1 P3 C13P C14P -1.1(6) 6 . . . ? Pd1 P3 C13P C14P -122.5(5) . . . . ? C19P P3 C13P C18P -74.3(5) . . . . ? C1 P3 C13P C18P 176.7(5) 6 . . . ? Pd1 P3 C13P C18P 55.3(5) . . . . ? C18P C13P C14P C15P 0.0 . . . . ? P3 C13P C14P C15P 177.7(7) . . . . ? C13P C14P C15P C16P 0.0 . . . . ? C14P C15P C16P C17P 0.0 . . . . ? C15P C16P C17P C18P 0.0 . . . . ? C16P C17P C18P C13P 0.0 . . . . ? C14P C13P C18P C17P 0.0 . . . . ? P3 C13P C18P C17P -177.9(6) . . . . ? C13P P3 C19P C20P -36.3(5) . . . . ? C1 P3 C19P C20P 74.1(5) 6 . . . ? Pd1 P3 C19P C20P -158.1(3) . . . . ? C13P P3 C19P C24P 148.7(4) . . . . ? C1 P3 C19P C24P -100.9(5) 6 . . . ? Pd1 P3 C19P C24P 27.0(5) . . . . ? C24P C19P C20P C21P 0.0 . . . . ? P3 C19P C20P C21P -174.9(6) . . . . ? C19P C20P C21P C22P 0.0 . . . . ? C20P C21P C22P C23P 0.0 . . . . ? C21P C22P C23P C24P 0.0 . . . . ? C22P C23P C24P C19P 0.0 . . . . ? C20P C19P C24P C23P 0.0 . . . . ? P3 C19P C24P C23P 175.0(6) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 75.49 _refine_diff_density_max 1.330 _refine_diff_density_min -1.147 _refine_diff_density_rms 0.111 data_3e _database_code_depnum_ccdc_archive 'CCDC 232758' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C57 H49 Cl2 N O P4 Pd2' _chemical_formula_weight 1171.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'P 41' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y, x, z+1/4' 'y, -x, z+3/4' _cell_length_a 21.247(3) _cell_length_b 21.247(3) _cell_length_c 14.214(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6416.7(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 25.02 _cell_measurement_theta_max 28.38 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.213 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2368 _exptl_absorpt_coefficient_mu 6.485 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.8267 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type 'CU k\a' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius CAD4' _diffrn_measurement_method \w--2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 2 _diffrn_reflns_number 14586 _diffrn_reflns_av_R_equivalents 0.0290 _diffrn_reflns_av_sigmaI/netI 0.0964 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 75.04 _reflns_number_total 12907 _reflns_number_gt 8537 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 Express' _computing_cell_refinement 'CAD4 Express' _computing_data_reduction 'XCAD4 (Harms 1996)' _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^)+(0.0598P)^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 -0.019(9) _refine_ls_number_reflns 12907 _refine_ls_number_parameters 607 _refine_ls_number_restraints 619 _refine_ls_R_factor_all 0.0933 _refine_ls_R_factor_gt 0.0513 _refine_ls_wR_factor_ref 0.1211 _refine_ls_wR_factor_gt 0.1079 _refine_ls_goodness_of_fit_ref 0.912 _refine_ls_restrained_S_all 0.897 _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 Pd1 Pd 0.11184(2) 0.43246(2) 0.21081(4) 0.04284(13) Uani 1 1 d . . . Pd2 Pd 0.21813(2) 0.51073(2) 0.09567(3) 0.04084(12) Uani 1 1 d . . . Cl1 Cl 0.04766(8) 0.42594(10) 0.34442(15) 0.0644(5) Uani 1 1 d . . . Cl2 Cl 0.27894(8) 0.60258(8) 0.09063(17) 0.0618(5) Uani 1 1 d . . . P1 P 0.19349(9) 0.38549(10) 0.29097(14) 0.0513(5) Uani 1 1 d . . . P2 P 0.03460(8) 0.47473(9) 0.11428(13) 0.0455(4) Uani 1 1 d . . . P3 P 0.13425(8) 0.56166(9) 0.02343(13) 0.0447(4) Uani 1 1 d . . . P4 P 0.29550(8) 0.45052(8) 0.16988(13) 0.0412(4) Uani 1 1 d . . . O1 O 0.1390(4) 0.3311(3) 0.0768(6) 0.107(2) Uani 1 1 d . . . N1 N 0.1660(2) 0.4326(2) 0.0970(4) 0.0412(12) Uani 1 1 d . . . C1 C 0.2654(3) 0.3774(3) 0.2202(6) 0.0476(17) Uani 1 1 d . . . H1A H 0.2980 0.3591 0.2594 0.062 Uiso 1 1 calc R . . H1B H 0.2571 0.3481 0.1693 0.062 Uiso 1 1 calc R . . C2 C 0.0662(3) 0.5097(3) 0.0064(5) 0.0487(18) Uani 1 1 d . . . H2A H 0.0330 0.5336 -0.0239 0.063 Uiso 1 1 calc R . . H2B H 0.0782 0.4761 -0.0361 0.063 Uiso 1 1 calc R . . C3 C 0.1697(4) 0.3811(4) 0.0485(6) 0.064(2) Uani 1 1 d . . . C4 C 0.2067(4) 0.3715(4) -0.0374(7) 0.072(2) Uani 1 1 d D . . C5 C 0.2291(5) 0.4205(5) -0.0911(8) 0.098(4) Uani 1 1 d D . . H5 H 0.2226 0.4617 -0.0715 0.128 Uiso 1 1 calc R . . C6 C 0.2627(6) 0.4083(7) -0.1782(9) 0.121(4) Uani 1 1 d DU . . H6 H 0.2769 0.4414 -0.2154 0.157 Uiso 1 1 calc R . . C7 C 0.2729(7) 0.3488(7) -0.2037(11) 0.137(5) Uani 1 1 d DU . . H7 H 0.2962 0.3409 -0.2578 0.178 Uiso 1 1 calc R . . C8 C 0.2506(7) 0.2996(8) -0.1536(10) 0.154(6) Uani 1 1 d DU . . H8 H 0.2596 0.2588 -0.1732 0.200 Uiso 1 1 calc R . . C9 C 0.2132(6) 0.3093(5) -0.0708(8) 0.112(4) Uani 1 1 d DU . . H9 H 0.1938 0.2757 -0.0403 0.146 Uiso 1 1 calc R . . C1P C 0.1772(4) 0.3070(4) 0.3308(8) 0.080(3) Uani 1 1 d U . . C2P C 0.1885(8) 0.2570(6) 0.2811(11) 0.159(6) Uani 1 1 d U . . H2P H 0.2091 0.2633 0.2242 0.207 Uiso 1 1 calc R . . C3P C 0.1731(11) 0.1947(7) 0.3036(17) 0.218(9) Uani 1 1 d U . . H3P H 0.1800 0.1617 0.2620 0.284 Uiso 1 1 calc R . . C4P C 0.1487(10) 0.1862(10) 0.3858(19) 0.216(9) Uani 1 1 d U . . H4P H 0.1361 0.1459 0.4029 0.280 Uiso 1 1 calc R . . C5P C 0.1406(10) 0.2355(9) 0.4500(16) 0.211(9) Uani 1 1 d U . . H5P H 0.1273 0.2277 0.5113 0.274 Uiso 1 1 calc R . . C6P C 0.1531(7) 0.2977(6) 0.4189(12) 0.158(6) Uani 1 1 d U . . H6P H 0.1451 0.3318 0.4581 0.205 Uiso 1 1 calc R . . C7P C 0.2186(4) 0.4279(5) 0.3973(5) 0.067(2) Uani 1 1 d U . . C8P C 0.2681(4) 0.4037(6) 0.4540(7) 0.099(3) Uani 1 1 d U . . H8P H 0.2885 0.3665 0.4380 0.128 Uiso 1 1 calc R . . C9P C 0.2850(6) 0.4371(8) 0.5339(9) 0.128(5) Uani 1 1 d U . . H9P H 0.3154 0.4207 0.5740 0.167 Uiso 1 1 calc R . . C10P C 0.2576(6) 0.4944(8) 0.5551(8) 0.130(5) Uani 1 1 d U . . H10P H 0.2704 0.5169 0.6078 0.170 Uiso 1 1 calc R . . C11P C 0.2119(4) 0.5172(6) 0.4984(7) 0.097(3) Uani 1 1 d U . . H11P H 0.1935 0.5559 0.5118 0.126 Uiso 1 1 calc R . . C12P C 0.1921(4) 0.4833(5) 0.4206(6) 0.076(3) Uani 1 1 d U . . H12P H 0.1598 0.4992 0.3835 0.098 Uiso 1 1 calc R . . C13P C -0.0160(3) 0.4117(4) 0.0703(5) 0.054(2) Uani 1 1 d U . . C14P C -0.0220(5) 0.3570(5) 0.1206(8) 0.091(3) Uani 1 1 d U . . H14P H -0.0007 0.3532 0.1775 0.118 Uiso 1 1 calc R . . C15P C -0.0575(6) 0.3087(5) 0.0906(10) 0.113(4) Uani 1 1 d U . . H15P H -0.0603 0.2716 0.1251 0.148 Uiso 1 1 calc R . . C16P C -0.0889(6) 0.3157(6) 0.0087(10) 0.114(4) Uani 1 1 d U . . H16P H -0.1141 0.2828 -0.0122 0.148 Uiso 1 1 calc R . . C17P C -0.0854(5) 0.3680(5) -0.0439(9) 0.099(3) Uani 1 1 d U . . H17P H -0.1076 0.3710 -0.1001 0.129 Uiso 1 1 calc R . . C18P C -0.0488(4) 0.4166(5) -0.0135(6) 0.073(2) Uani 1 1 d U . . H18P H -0.0458 0.4532 -0.0492 0.095 Uiso 1 1 calc R . . C19P C -0.0187(3) 0.5348(4) 0.1603(6) 0.0521(18) Uani 1 1 d U . . C20P C -0.0729(4) 0.5524(5) 0.1121(7) 0.077(3) Uani 1 1 d U . . H20P H -0.0827 0.5341 0.0544 0.100 Uiso 1 1 calc R . . C21P C -0.1123(4) 0.5972(5) 0.1511(8) 0.091(3) Uani 1 1 d U . . H21P H -0.1488 0.6088 0.1195 0.118 Uiso 1 1 calc R . . C22P C -0.0987(4) 0.6243(5) 0.2335(8) 0.078(3) Uani 1 1 d U . . H22P H -0.1256 0.6547 0.2578 0.102 Uiso 1 1 calc R . . C23P C -0.0460(4) 0.6081(4) 0.2823(7) 0.072(2) Uani 1 1 d U . . H23P H -0.0376 0.6264 0.3404 0.094 Uiso 1 1 calc R . . C24P C -0.0053(4) 0.5644(4) 0.2447(5) 0.062(2) Uani 1 1 d U . . H24P H 0.0316 0.5545 0.2766 0.080 Uiso 1 1 calc R . . C25P C 0.1515(3) 0.5909(4) -0.0937(6) 0.056(2) Uani 1 1 d U . . C26P C 0.1824(4) 0.6485(5) -0.1014(7) 0.081(3) Uani 1 1 d U . . H26P H 0.1909 0.6723 -0.0480 0.105 Uiso 1 1 calc R . . C27P C 0.2001(5) 0.6700(6) -0.1886(9) 0.109(4) Uani 1 1 d U . . H27P H 0.2212 0.7082 -0.1938 0.142 Uiso 1 1 calc R . . C28P C 0.1873(5) 0.6363(7) -0.2672(7) 0.111(4) Uani 1 1 d U . . H28P H 0.1989 0.6518 -0.3260 0.144 Uiso 1 1 calc R . . C29P C 0.1571(5) 0.5791(7) -0.2600(7) 0.104(4) Uani 1 1 d U . . H29P H 0.1486 0.5555 -0.3136 0.135 Uiso 1 1 calc R . . C30P C 0.1398(4) 0.5572(5) -0.1730(5) 0.077(3) Uani 1 1 d U . . H30P H 0.1196 0.5185 -0.1683 0.100 Uiso 1 1 calc R . . C31P C 0.1033(3) 0.6291(3) 0.0851(6) 0.0500(17) Uani 1 1 d U . . C32P C 0.0519(4) 0.6624(4) 0.0465(8) 0.083(3) Uani 1 1 d U . . H32P H 0.0357 0.6499 -0.0114 0.107 Uiso 1 1 calc R . . C33P C 0.0251(6) 0.7124(5) 0.0918(11) 0.112(4) Uani 1 1 d U . . H33P H -0.0099 0.7330 0.0673 0.145 Uiso 1 1 calc R . . C34P C 0.0516(6) 0.7307(5) 0.1737(11) 0.112(4) Uani 1 1 d U . . H34P H 0.0334 0.7644 0.2056 0.146 Uiso 1 1 calc R . . C35P C 0.1056(5) 0.7018(5) 0.2143(9) 0.095(3) Uani 1 1 d U . . H35P H 0.1239 0.7171 0.2691 0.124 Uiso 1 1 calc R . . C36P C 0.1297(4) 0.6487(4) 0.1675(6) 0.068(2) Uani 1 1 d U . . H36P H 0.1638 0.6270 0.1928 0.089 Uiso 1 1 calc R . . C37P C 0.3399(3) 0.4869(3) 0.2644(5) 0.0477(17) Uani 1 1 d U . . C38P C 0.3198(4) 0.5432(4) 0.3044(6) 0.062(2) Uani 1 1 d U . . H38P H 0.2857 0.5648 0.2789 0.081 Uiso 1 1 calc R . . C39P C 0.3506(5) 0.5670(4) 0.3820(7) 0.083(3) Uani 1 1 d U . . H39P H 0.3360 0.6037 0.4103 0.108 Uiso 1 1 calc R . . C40P C 0.4027(5) 0.5373(6) 0.4178(7) 0.087(3) Uani 1 1 d U . . H40P H 0.4243 0.5547 0.4684 0.113 Uiso 1 1 calc R . . C41P C 0.4221(4) 0.4833(5) 0.3798(7) 0.087(3) Uani 1 1 d U . . H41P H 0.4566 0.4628 0.4059 0.113 Uiso 1 1 calc R . . C42P C 0.3924(4) 0.4570(4) 0.3030(6) 0.066(2) Uani 1 1 d U . . H42P H 0.4073 0.4197 0.2770 0.086 Uiso 1 1 calc R . . C43P C 0.3553(3) 0.4243(3) 0.0878(6) 0.0475(16) Uani 1 1 d U . . C44P C 0.3715(3) 0.4633(4) 0.0160(6) 0.056(2) Uani 1 1 d U . . H44P H 0.3516 0.5021 0.0104 0.073 Uiso 1 1 calc R . . C45P C 0.4168(4) 0.4467(4) -0.0487(7) 0.078(3) Uani 1 1 d U . . H45P H 0.4276 0.4744 -0.0968 0.102 Uiso 1 1 calc R . . C46P C 0.4460(4) 0.3888(5) -0.0420(8) 0.085(3) Uani 1 1 d U . . H46P H 0.4766 0.3776 -0.0856 0.111 Uiso 1 1 calc R . . C47P C 0.4301(4) 0.3477(5) 0.0289(8) 0.084(3) Uani 1 1 d U . . H47P H 0.4493 0.3084 0.0332 0.109 Uiso 1 1 calc R . . C48P C 0.3842(3) 0.3661(4) 0.0947(7) 0.068(2) Uani 1 1 d U . . H48P H 0.3733 0.3390 0.1434 0.089 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 0.0337(3) 0.0552(3) 0.0396(3) 0.0011(2) 0.0029(2) -0.0006(2) Pd2 0.0326(2) 0.0456(3) 0.0444(3) 0.0007(2) 0.0002(2) -0.0009(2) Cl1 0.0512(10) 0.0929(14) 0.0491(11) 0.0080(11) 0.0145(10) 0.0042(10) Cl2 0.0527(10) 0.0523(10) 0.0802(13) 0.0080(11) -0.0061(10) -0.0132(8) P1 0.0366(10) 0.0655(13) 0.0519(12) 0.0138(10) 0.0050(9) 0.0061(9) P2 0.0321(8) 0.0620(11) 0.0425(11) -0.0003(9) 0.0009(8) -0.0015(8) P3 0.0362(9) 0.0525(11) 0.0454(11) 0.0042(9) -0.0018(8) -0.0006(8) P4 0.0320(8) 0.0476(10) 0.0441(10) -0.0001(8) 0.0009(7) 0.0022(7) O1 0.143(6) 0.068(4) 0.111(6) -0.013(4) 0.026(5) -0.024(4) N1 0.040(3) 0.043(3) 0.040(3) -0.001(3) 0.003(3) 0.003(2) C1 0.039(4) 0.047(4) 0.057(4) 0.004(4) -0.001(4) 0.002(3) C2 0.040(4) 0.060(5) 0.047(4) -0.005(4) -0.007(3) -0.003(3) C3 0.057(5) 0.066(5) 0.068(6) -0.016(5) -0.007(4) -0.004(4) C4 0.052(5) 0.100(7) 0.062(6) -0.018(6) -0.001(5) 0.017(5) C5 0.088(7) 0.097(8) 0.110(9) -0.044(7) 0.028(6) -0.043(6) C6 0.120(7) 0.132(8) 0.110(8) -0.027(6) 0.030(6) -0.038(6) C7 0.120(11) 0.171(16) 0.121(12) -0.016(11) 0.039(9) 0.043(11) C8 0.173(14) 0.177(14) 0.113(11) -0.035(11) 0.031(11) 0.090(12) C9 0.145(10) 0.106(9) 0.086(8) -0.012(7) -0.008(7) 0.060(8) C1P 0.060(5) 0.068(6) 0.113(9) 0.035(6) 0.025(5) 0.006(4) C2P 0.238(15) 0.087(9) 0.152(12) 0.025(9) 0.068(11) -0.060(10) C3P 0.31(2) 0.090(10) 0.26(2) 0.041(12) 0.074(17) -0.071(12) C4P 0.203(16) 0.134(14) 0.31(3) 0.082(16) 0.106(17) -0.041(13) C5P 0.229(16) 0.156(15) 0.25(2) 0.082(15) 0.136(15) 0.001(15) C6P 0.191(13) 0.096(9) 0.187(14) 0.062(10) 0.084(12) 0.002(9) C7P 0.042(4) 0.122(8) 0.037(4) 0.008(5) 0.004(3) 0.006(5) C8P 0.064(6) 0.172(10) 0.061(6) 0.007(7) -0.004(5) 0.020(6) C9P 0.075(8) 0.234(16) 0.076(8) -0.015(9) -0.031(6) 0.029(9) C10P 0.071(7) 0.250(16) 0.071(8) -0.035(9) -0.012(6) 0.000(9) C11P 0.058(6) 0.166(10) 0.068(6) -0.028(7) 0.001(5) -0.015(6) C12P 0.047(5) 0.127(8) 0.054(5) -0.020(5) -0.005(4) -0.014(5) C13P 0.039(4) 0.079(5) 0.044(5) -0.009(4) -0.005(3) -0.002(4) C14P 0.109(8) 0.078(6) 0.085(8) 0.012(6) -0.024(6) -0.020(6) C15P 0.136(10) 0.090(7) 0.114(9) 0.001(7) -0.053(8) -0.040(7) C16P 0.106(9) 0.105(9) 0.131(11) -0.038(8) -0.007(8) -0.046(7) C17P 0.114(8) 0.098(8) 0.085(7) -0.018(7) -0.019(6) -0.048(6) C18P 0.072(6) 0.088(6) 0.059(6) -0.011(5) -0.004(5) -0.016(5) C19P 0.032(4) 0.065(5) 0.060(5) 0.004(4) -0.003(3) -0.006(3) C20P 0.046(4) 0.116(8) 0.068(6) -0.016(5) -0.013(4) 0.016(5) C21P 0.051(5) 0.122(9) 0.100(9) 0.003(7) -0.014(5) 0.011(6) C22P 0.053(5) 0.091(7) 0.091(8) -0.012(6) 0.014(5) 0.016(5) C23P 0.063(5) 0.088(6) 0.066(6) -0.021(5) 0.000(5) 0.009(5) C24P 0.049(4) 0.087(6) 0.050(5) -0.004(4) -0.007(4) 0.012(4) C25P 0.044(4) 0.075(5) 0.049(5) 0.008(4) -0.001(4) -0.003(4) C26P 0.087(7) 0.090(7) 0.066(6) 0.023(5) 0.000(5) -0.012(6) C27P 0.105(8) 0.136(10) 0.086(8) 0.051(7) 0.009(7) -0.032(7) C28P 0.100(8) 0.191(13) 0.042(6) 0.042(7) -0.013(5) -0.022(8) C29P 0.081(7) 0.180(12) 0.051(6) 0.002(7) 0.009(5) -0.045(7) C30P 0.081(6) 0.118(8) 0.031(5) -0.004(5) 0.005(4) -0.033(5) C31P 0.041(4) 0.058(4) 0.051(5) 0.004(4) 0.000(3) -0.001(3) C32P 0.067(6) 0.076(6) 0.105(8) 0.006(6) -0.012(5) 0.009(5) C33P 0.092(8) 0.096(8) 0.146(11) -0.006(9) 0.018(9) 0.044(7) C34P 0.100(9) 0.074(7) 0.162(13) -0.030(8) 0.046(9) 0.002(6) C35P 0.100(8) 0.093(7) 0.092(8) -0.012(7) 0.007(7) -0.013(6) C36P 0.073(6) 0.066(5) 0.066(6) -0.008(5) 0.006(5) 0.001(4) C37P 0.049(4) 0.041(4) 0.053(5) 0.007(3) -0.001(3) 0.005(3) C38P 0.064(5) 0.060(5) 0.062(5) -0.024(4) -0.003(4) -0.002(4) C39P 0.099(8) 0.064(6) 0.085(7) -0.024(5) 0.006(6) -0.009(5) C40P 0.085(7) 0.110(8) 0.065(6) -0.006(6) -0.011(6) -0.027(6) C41P 0.065(6) 0.111(8) 0.085(7) -0.019(6) -0.035(5) -0.011(6) C42P 0.060(5) 0.064(5) 0.075(6) -0.010(4) -0.009(4) 0.008(4) C43P 0.044(4) 0.045(4) 0.054(4) -0.010(4) -0.006(4) -0.004(3) C44P 0.045(4) 0.058(5) 0.065(5) 0.001(4) 0.016(4) -0.005(3) C45P 0.088(6) 0.067(6) 0.080(7) -0.003(5) 0.034(5) -0.006(5) C46P 0.072(6) 0.086(6) 0.097(7) -0.024(6) 0.046(6) -0.013(5) C47P 0.071(6) 0.072(6) 0.108(8) -0.008(6) 0.023(6) 0.025(5) C48P 0.058(5) 0.058(5) 0.088(6) -0.002(5) 0.025(5) 0.011(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 Pd1 N1 1.986(6) . ? Pd1 P1 2.303(2) . ? Pd1 P2 2.3200(19) . ? Pd1 Cl1 2.3421(19) . ? Pd1 Pd2 3.2471(8) . ? Pd2 N1 1.994(5) . ? Pd2 P3 2.3243(18) . ? Pd2 P4 2.3347(18) . ? Pd2 Cl2 2.3416(18) . ? P1 C1P 1.795(9) . ? P1 C1 1.837(7) . ? P1 C7P 1.838(9) . ? P2 C13P 1.828(8) . ? P2 C19P 1.828(8) . ? P2 C2 1.832(7) . ? P3 C31P 1.803(8) . ? P3 C25P 1.814(8) . ? P3 C2 1.835(7) . ? P4 C43P 1.814(7) . ? P4 C37P 1.814(8) . ? P4 C1 1.826(7) . ? O1 C3 1.311(10) . ? N1 C3 1.296(9) . ? C3 C4 1.467(12) . ? C4 C5 1.375(10) . ? C4 C9 1.412(10) . ? C5 C6 1.452(12) . ? C6 C7 1.333(12) . ? C7 C8 1.350(12) . ? C8 C9 1.435(13) . ? C1P C2P 1.298(16) . ? C1P C6P 1.367(16) . ? C2P C3P 1.400(17) . ? C3P C4P 1.29(3) . ? C4P C5P 1.40(3) . ? C5P C6P 1.418(18) . ? C7P C12P 1.345(12) . ? C7P C8P 1.422(12) . ? C8P C9P 1.386(16) . ? C9P C10P 1.382(18) . ? C10P C11P 1.352(15) . ? C11P C12P 1.385(12) . ? C13P C14P 1.370(12) . ? C13P C18P 1.384(11) . ? C14P C15P 1.344(12) . ? C15P C16P 1.350(16) . ? C16P C17P 1.340(15) . ? C17P C18P 1.364(11) . ? C19P C24P 1.384(10) . ? C19P C20P 1.391(10) . ? C20P C21P 1.384(12) . ? C21P C22P 1.335(13) . ? C22P C23P 1.361(12) . ? C23P C24P 1.377(10) . ? C25P C30P 1.359(11) . ? C25P C26P 1.394(11) . ? C26P C27P 1.373(13) . ? C27P C28P 1.354(16) . ? C28P C29P 1.379(15) . ? C29P C30P 1.371(12) . ? C31P C36P 1.365(11) . ? C31P C32P 1.412(10) . ? C32P C33P 1.367(13) . ? C33P C34P 1.350(17) . ? C34P C35P 1.424(16) . ? C35P C36P 1.405(13) . ? C37P C38P 1.393(10) . ? C37P C42P 1.397(10) . ? C38P C39P 1.379(11) . ? C39P C40P 1.371(13) . ? C40P C41P 1.333(13) . ? C41P C42P 1.379(11) . ? C43P C44P 1.359(10) . ? C43P C48P 1.383(9) . ? C44P C45P 1.377(10) . ? C45P C46P 1.381(12) . ? C46P C47P 1.376(13) . ? C47P C48P 1.407(11) . ? 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 N1 Pd1 P1 88.10(16) . . ? N1 Pd1 P2 85.86(16) . . ? P1 Pd1 P2 173.32(7) . . ? N1 Pd1 Cl1 176.71(16) . . ? P1 Pd1 Cl1 90.68(7) . . ? P2 Pd1 Cl1 95.20(7) . . ? N1 Pd1 Pd2 35.42(15) . . ? P1 Pd1 Pd2 86.98(5) . . ? P2 Pd1 Pd2 89.75(5) . . ? Cl1 Pd1 Pd2 147.55(6) . . ? N1 Pd2 P3 88.05(16) . . ? N1 Pd2 P4 86.02(16) . . ? P3 Pd2 P4 174.04(7) . . ? N1 Pd2 Cl2 178.78(19) . . ? P3 Pd2 Cl2 91.24(7) . . ? P4 Pd2 Cl2 94.70(6) . . ? N1 Pd2 Pd1 35.24(17) . . ? P3 Pd2 Pd1 85.86(5) . . ? P4 Pd2 Pd1 88.93(5) . . ? Cl2 Pd2 Pd1 145.69(6) . . ? C1P P1 C1 104.3(4) . . ? C1P P1 C7P 104.6(5) . . ? C1 P1 C7P 104.8(4) . . ? C1P P1 Pd1 114.4(3) . . ? C1 P1 Pd1 113.3(2) . . ? C7P P1 Pd1 114.4(3) . . ? C13P P2 C19P 105.6(3) . . ? C13P P2 C2 103.1(3) . . ? C19P P2 C2 104.1(3) . . ? C13P P2 Pd1 109.5(3) . . ? C19P P2 Pd1 119.8(3) . . ? C2 P2 Pd1 113.2(2) . . ? C31P P3 C25P 104.3(4) . . ? C31P P3 C2 104.7(3) . . ? C25P P3 C2 104.1(3) . . ? C31P P3 Pd2 115.8(3) . . ? C25P P3 Pd2 114.2(3) . . ? C2 P3 Pd2 112.5(2) . . ? C43P P4 C37P 104.1(3) . . ? C43P P4 C1 103.7(3) . . ? C37P P4 C1 104.7(3) . . ? C43P P4 Pd2 111.8(3) . . ? C37P P4 Pd2 117.9(2) . . ? C1 P4 Pd2 113.4(2) . . ? C3 N1 Pd1 117.8(5) . . ? C3 N1 Pd2 131.6(5) . . ? Pd1 N1 Pd2 109.3(3) . . ? P4 C1 P1 115.2(4) . . ? P2 C2 P3 115.0(4) . . ? N1 C3 O1 119.5(8) . . ? N1 C3 C4 126.3(8) . . ? O1 C3 C4 114.2(8) . . ? C5 C4 C9 119.2(10) . . ? C5 C4 C3 122.8(8) . . ? C9 C4 C3 117.5(9) . . ? C4 C5 C6 120.6(10) . . ? C7 C6 C5 118.7(12) . . ? C6 C7 C8 122.3(14) . . ? C7 C8 C9 121.0(13) . . ? C4 C9 C8 117.6(12) . . ? C2P C1P C6P 116.7(11) . . ? C2P C1P P1 123.5(9) . . ? C6P C1P P1 119.7(10) . . ? C1P C2P C3P 127.3(15) . . ? C4P C3P C2P 116(2) . . ? C3P C4P C5P 122.3(19) . . ? C4P C5P C6P 118.1(18) . . ? C1P C6P C5P 119.4(15) . . ? C12P C7P C8P 119.0(9) . . ? C12P C7P P1 120.7(6) . . ? C8P C7P P1 120.2(8) . . ? C9P C8P C7P 118.1(11) . . ? C10P C9P C8P 121.4(12) . . ? C11P C10P C9P 119.2(12) . . ? C10P C11P C12P 120.5(12) . . ? C7P C12P C11P 121.7(10) . . ? C14P C13P C18P 117.8(8) . . ? C14P C13P P2 119.8(6) . . ? C18P C13P P2 122.3(7) . . ? C15P C14P C13P 122.3(10) . . ? C14P C15P C16P 117.8(11) . . ? C17P C16P C15P 123.1(11) . . ? C16P C17P C18P 118.8(11) . . ? C17P C18P C13P 120.1(10) . . ? C24P C19P C20P 118.4(8) . . ? C24P C19P P2 120.0(6) . . ? C20P C19P P2 121.6(7) . . ? C21P C20P C19P 119.1(9) . . ? C22P C21P C20P 121.2(9) . . ? C21P C22P C23P 121.1(9) . . ? C22P C23P C24P 119.3(9) . . ? C23P C24P C19P 120.9(8) . . ? C30P C25P C26P 118.9(8) . . ? C30P C25P P3 123.0(7) . . ? C26P C25P P3 117.9(7) . . ? C27P C26P C25P 119.5(10) . . ? C28P C27P C26P 121.0(11) . . ? C27P C28P C29P 119.8(10) . . ? C30P C29P C28P 119.5(10) . . ? C25P C30P C29P 121.4(9) . . ? C36P C31P C32P 119.9(8) . . ? C36P C31P P3 120.7(6) . . ? C32P C31P P3 119.4(7) . . ? C33P C32P C31P 121.9(10) . . ? C34P C33P C32P 117.2(11) . . ? C33P C34P C35P 124.1(11) . . ? C36P C35P C34P 116.7(11) . . ? C31P C36P C35P 120.1(9) . . ? C38P C37P C42P 118.4(7) . . ? C38P C37P P4 120.6(6) . . ? C42P C37P P4 120.8(6) . . ? C39P C38P C37P 119.7(8) . . ? C40P C39P C38P 120.7(9) . . ? C41P C40P C39P 119.7(9) . . ? C40P C41P C42P 121.9(10) . . ? C41P C42P C37P 119.4(8) . . ? C44P C43P C48P 119.1(7) . . ? C44P C43P P4 118.2(5) . . ? C48P C43P P4 122.7(6) . . ? C43P C44P C45P 121.5(8) . . ? C44P C45P C46P 119.7(9) . . ? C47P C46P C45P 120.4(8) . . ? C46P C47P C48P 118.7(8) . . ? C43P C48P C47P 120.6(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P1 Pd1 Pd2 N1 91.0(3) . . . . ? P2 Pd1 Pd2 N1 -83.2(3) . . . . ? Cl1 Pd1 Pd2 N1 177.5(3) . . . . ? N1 Pd1 Pd2 P3 92.5(3) . . . . ? P1 Pd1 Pd2 P3 -176.54(8) . . . . ? P2 Pd1 Pd2 P3 9.30(7) . . . . ? Cl1 Pd1 Pd2 P3 -90.03(11) . . . . ? N1 Pd1 Pd2 P4 -84.6(3) . . . . ? P1 Pd1 Pd2 P4 6.37(7) . . . . ? P2 Pd1 Pd2 P4 -167.80(7) . . . . ? Cl1 Pd1 Pd2 P4 92.87(11) . . . . ? N1 Pd1 Pd2 Cl2 178.6(3) . . . . ? P1 Pd1 Pd2 Cl2 -90.42(11) . . . . ? P2 Pd1 Pd2 Cl2 95.41(10) . . . . ? Cl1 Pd1 Pd2 Cl2 -3.92(14) . . . . ? N1 Pd1 P1 C1P -115.0(5) . . . . ? P2 Pd1 P1 C1P -89.6(8) . . . . ? Cl1 Pd1 P1 C1P 61.9(4) . . . . ? Pd2 Pd1 P1 C1P -150.4(4) . . . . ? N1 Pd1 P1 C1 4.4(3) . . . . ? P2 Pd1 P1 C1 29.8(7) . . . . ? Cl1 Pd1 P1 C1 -178.7(3) . . . . ? Pd2 Pd1 P1 C1 -31.1(2) . . . . ? N1 Pd1 P1 C7P 124.4(3) . . . . ? P2 Pd1 P1 C7P 149.8(7) . . . . ? Cl1 Pd1 P1 C7P -58.7(3) . . . . ? Pd2 Pd1 P1 C7P 89.0(3) . . . . ? N1 Pd1 P2 C13P 95.4(3) . . . . ? P1 Pd1 P2 C13P 69.9(7) . . . . ? Cl1 Pd1 P2 C13P -81.5(3) . . . . ? Pd2 Pd1 P2 C13P 130.6(3) . . . . ? N1 Pd1 P2 C19P -142.4(3) . . . . ? P1 Pd1 P2 C19P -167.8(6) . . . . ? Cl1 Pd1 P2 C19P 40.7(3) . . . . ? Pd2 Pd1 P2 C19P -107.1(3) . . . . ? N1 Pd1 P2 C2 -19.0(3) . . . . ? P1 Pd1 P2 C2 -44.5(7) . . . . ? Cl1 Pd1 P2 C2 164.1(3) . . . . ? Pd2 Pd1 P2 C2 16.2(3) . . . . ? N1 Pd2 P3 C31P 121.4(3) . . . . ? P4 Pd2 P3 C31P 115.3(7) . . . . ? Cl2 Pd2 P3 C31P -59.6(3) . . . . ? Pd1 Pd2 P3 C31P 86.2(3) . . . . ? N1 Pd2 P3 C25P -117.4(3) . . . . ? P4 Pd2 P3 C25P -123.4(7) . . . . ? Cl2 Pd2 P3 C25P 61.6(3) . . . . ? Pd1 Pd2 P3 C25P -152.6(3) . . . . ? N1 Pd2 P3 C2 1.0(3) . . . . ? P4 Pd2 P3 C2 -5.0(8) . . . . ? Cl2 Pd2 P3 C2 180.0(3) . . . . ? Pd1 Pd2 P3 C2 -34.2(3) . . . . ? N1 Pd2 P4 C43P 100.3(3) . . . . ? P3 Pd2 P4 C43P 106.3(7) . . . . ? Cl2 Pd2 P4 C43P -78.7(2) . . . . ? Pd1 Pd2 P4 C43P 135.4(2) . . . . ? N1 Pd2 P4 C37P -139.2(3) . . . . ? P3 Pd2 P4 C37P -133.2(7) . . . . ? Cl2 Pd2 P4 C37P 41.8(3) . . . . ? Pd1 Pd2 P4 C37P -104.1(3) . . . . ? N1 Pd2 P4 C1 -16.4(3) . . . . ? P3 Pd2 P4 C1 -10.4(8) . . . . ? Cl2 Pd2 P4 C1 164.5(3) . . . . ? Pd1 Pd2 P4 C1 18.7(3) . . . . ? P1 Pd1 N1 C3 81.4(5) . . . . ? P2 Pd1 N1 C3 -95.7(6) . . . . ? Cl1 Pd1 N1 C3 13(3) . . . . ? Pd2 Pd1 N1 C3 168.9(7) . . . . ? P1 Pd1 N1 Pd2 -87.5(2) . . . . ? P2 Pd1 N1 Pd2 95.4(2) . . . . ? Cl1 Pd1 N1 Pd2 -156(3) . . . . ? P3 Pd2 N1 C3 107.6(7) . . . . ? P4 Pd2 N1 C3 -73.0(7) . . . . ? Cl2 Pd2 N1 C3 53(7) . . . . ? Pd1 Pd2 N1 C3 -166.8(9) . . . . ? P3 Pd2 N1 Pd1 -85.6(2) . . . . ? P4 Pd2 N1 Pd1 93.8(2) . . . . ? Cl2 Pd2 N1 Pd1 -140(7) . . . . ? C43P P4 C1 P1 -169.2(4) . . . . ? C37P P4 C1 P1 82.0(5) . . . . ? Pd2 P4 C1 P1 -47.8(5) . . . . ? C1P P1 C1 P4 -179.2(5) . . . . ? C7P P1 C1 P4 -69.6(5) . . . . ? Pd1 P1 C1 P4 55.8(5) . . . . ? C13P P2 C2 P3 -165.2(4) . . . . ? C19P P2 C2 P3 84.7(4) . . . . ? Pd1 P2 C2 P3 -46.9(5) . . . . ? C31P P3 C2 P2 -68.2(5) . . . . ? C25P P3 C2 P2 -177.5(4) . . . . ? Pd2 P3 C2 P2 58.3(4) . . . . ? Pd1 N1 C3 O1 -1.4(10) . . . . ? Pd2 N1 C3 O1 164.5(6) . . . . ? Pd1 N1 C3 C4 179.9(6) . . . . ? Pd2 N1 C3 C4 -14.2(13) . . . . ? N1 C3 C4 C5 -18.0(14) . . . . ? O1 C3 C4 C5 163.3(9) . . . . ? N1 C3 C4 C9 169.4(9) . . . . ? O1 C3 C4 C9 -9.4(12) . . . . ? C9 C4 C5 C6 -4.2(16) . . . . ? C3 C4 C5 C6 -176.7(9) . . . . ? C4 C5 C6 C7 -1.7(19) . . . . ? C5 C6 C7 C8 3(2) . . . . ? C6 C7 C8 C9 1(3) . . . . ? C5 C4 C9 C8 8.4(16) . . . . ? C3 C4 C9 C8 -178.6(10) . . . . ? C7 C8 C9 C4 -7(2) . . . . ? C1 P1 C1P C2P -34.7(13) . . . . ? C7P P1 C1P C2P -144.4(13) . . . . ? Pd1 P1 C1P C2P 89.7(12) . . . . ? C1 P1 C1P C6P 143.5(11) . . . . ? C7P P1 C1P C6P 33.8(11) . . . . ? Pd1 P1 C1P C6P -92.1(11) . . . . ? C6P C1P C2P C3P 7(3) . . . . ? P1 C1P C2P C3P -174.9(16) . . . . ? C1P C2P C3P C4P -5(3) . . . . ? C2P C3P C4P C5P -3(4) . . . . ? C3P C4P C5P C6P 7(4) . . . . ? C2P C1P C6P C5P -1(2) . . . . ? P1 C1P C6P C5P -179.8(14) . . . . ? C4P C5P C6P C1P -5(3) . . . . ? C1P P1 C7P C12P -129.2(8) . . . . ? C1 P1 C7P C12P 121.4(7) . . . . ? Pd1 P1 C7P C12P -3.3(8) . . . . ? C1P P1 C7P C8P 53.4(8) . . . . ? C1 P1 C7P C8P -56.0(8) . . . . ? Pd1 P1 C7P C8P 179.3(6) . . . . ? C12P C7P C8P C9P 3.0(15) . . . . ? P1 C7P C8P C9P -179.5(9) . . . . ? C7P C8P C9P C10P -4.0(19) . . . . ? C8P C9P C10P C11P 2(2) . . . . ? C9P C10P C11P C12P 0.8(19) . . . . ? C8P C7P C12P C11P -0.1(14) . . . . ? P1 C7P C12P C11P -177.6(7) . . . . ? C10P C11P C12P C7P -1.9(16) . . . . ? C19P P2 C13P C14P -104.9(8) . . . . ? C2 P2 C13P C14P 146.2(7) . . . . ? Pd1 P2 C13P C14P 25.5(8) . . . . ? C19P P2 C13P C18P 75.7(7) . . . . ? C2 P2 C13P C18P -33.2(7) . . . . ? Pd1 P2 C13P C18P -154.0(6) . . . . ? C18P C13P C14P C15P 0.9(15) . . . . ? P2 C13P C14P C15P -178.6(10) . . . . ? C13P C14P C15P C16P -1.2(19) . . . . ? C14P C15P C16P C17P 1(2) . . . . ? C15P C16P C17P C18P 0(2) . . . . ? C16P C17P C18P C13P -0.1(16) . . . . ? C14P C13P C18P C17P -0.2(13) . . . . ? P2 C13P C18P C17P 179.3(8) . . . . ? C13P P2 C19P C24P 137.5(6) . . . . ? C2 P2 C19P C24P -114.3(7) . . . . ? Pd1 P2 C19P C24P 13.4(7) . . . . ? C13P P2 C19P C20P -42.9(8) . . . . ? C2 P2 C19P C20P 65.3(7) . . . . ? Pd1 P2 C19P C20P -167.0(6) . . . . ? C24P C19P C20P C21P -1.7(13) . . . . ? P2 C19P C20P C21P 178.7(7) . . . . ? C19P C20P C21P C22P 0.7(16) . . . . ? C20P C21P C22P C23P -0.8(17) . . . . ? C21P C22P C23P C24P 1.8(15) . . . . ? C22P C23P C24P C19P -2.8(14) . . . . ? C20P C19P C24P C23P 2.7(13) . . . . ? P2 C19P C24P C23P -177.7(7) . . . . ? C31P P3 C25P C30P -139.7(7) . . . . ? C2 P3 C25P C30P -30.2(8) . . . . ? Pd2 P3 C25P C30P 92.9(7) . . . . ? C31P P3 C25P C26P 45.1(7) . . . . ? C2 P3 C25P C26P 154.7(7) . . . . ? Pd2 P3 C25P C26P -82.2(7) . . . . ? C30P C25P C26P C27P 0.1(14) . . . . ? P3 C25P C26P C27P 175.4(8) . . . . ? C25P C26P C27P C28P 0.9(17) . . . . ? C26P C27P C28P C29P -1.2(19) . . . . ? C27P C28P C29P C30P 0.7(18) . . . . ? C26P C25P C30P C29P -0.6(14) . . . . ? P3 C25P C30P C29P -175.8(8) . . . . ? C28P C29P C30P C25P 0.3(16) . . . . ? C25P P3 C31P C36P -124.7(7) . . . . ? C2 P3 C31P C36P 126.2(6) . . . . ? Pd2 P3 C31P C36P 1.7(7) . . . . ? C25P P3 C31P C32P 54.3(7) . . . . ? C2 P3 C31P C32P -54.8(7) . . . . ? Pd2 P3 C31P C32P -179.3(5) . . . . ? C36P C31P C32P C33P -3.4(14) . . . . ? P3 C31P C32P C33P 177.6(8) . . . . ? C31P C32P C33P C34P 2.8(17) . . . . ? C32P C33P C34P C35P 1(2) . . . . ? C33P C34P C35P C36P -3.6(18) . . . . ? C32P C31P C36P C35P 0.4(12) . . . . ? P3 C31P C36P C35P 179.3(7) . . . . ? C34P C35P C36P C31P 2.9(14) . . . . ? C43P P4 C37P C38P 137.8(7) . . . . ? C1 P4 C37P C38P -113.7(7) . . . . ? Pd2 P4 C37P C38P 13.3(7) . . . . ? C43P P4 C37P C42P -46.6(7) . . . . ? C1 P4 C37P C42P 61.9(7) . . . . ? Pd2 P4 C37P C42P -171.0(6) . . . . ? C42P C37P C38P C39P -2.0(12) . . . . ? P4 C37P C38P C39P 173.8(7) . . . . ? C37P C38P C39P C40P 2.9(14) . . . . ? C38P C39P C40P C41P -2.9(15) . . . . ? C39P C40P C41P C42P 2.0(16) . . . . ? C40P C41P C42P C37P -1.2(15) . . . . ? C38P C37P C42P C41P 1.1(12) . . . . ? P4 C37P C42P C41P -174.7(7) . . . . ? C37P P4 C43P C44P -93.3(6) . . . . ? C1 P4 C43P C44P 157.4(6) . . . . ? Pd2 P4 C43P C44P 34.9(6) . . . . ? C37P P4 C43P C48P 87.5(7) . . . . ? C1 P4 C43P C48P -21.7(7) . . . . ? Pd2 P4 C43P C48P -144.2(6) . . . . ? C48P C43P C44P C45P -1.2(12) . . . . ? P4 C43P C44P C45P 179.6(7) . . . . ? C43P C44P C45P C46P 1.0(14) . . . . ? C44P C45P C46P C47P 0.1(16) . . . . ? C45P C46P C47P C48P -0.8(15) . . . . ? C44P C43P C48P C47P 0.4(13) . . . . ? P4 C43P C48P C47P 179.5(7) . . . . ? C46P C47P C48P C43P 0.6(14) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 75.04 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.402 _refine_diff_density_min -0.763 _refine_diff_density_rms 0.076 # =============================== 3F =============================== data_3f _database_code_depnum_ccdc_archive 'CCDC 232759' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H51 Cl2 N O2 P4 Pd2' _chemical_formula_weight 1201.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 43' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y, x, z+3/4' 'y, -x, z+1/4' _cell_length_a 21.224(5) _cell_length_b 21.224(5) _cell_length_c 14.230(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6410(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 13.93 _cell_measurement_theta_max 15.63 _exptl_crystal_description block _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.245 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2432 _exptl_absorpt_coefficient_mu 0.780 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.9938 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.710730 _diffrn_radiation_type 'MO k\a' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius CAD4' _diffrn_measurement_method \w--2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 6 _diffrn_reflns_number 24367 _diffrn_reflns_av_R_equivalents 0.0178 _diffrn_reflns_av_sigmaI/netI 0.1138 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.58 _diffrn_reflns_theta_max 31.97 _reflns_number_total 22018 _reflns_number_gt 12729 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 Express' _computing_cell_refinement 'CAD4 Express' _computing_data_reduction 'XCAD4 (Harms 1996)' _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^)+(0.0738P)^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 -0.07(2) _refine_ls_number_reflns 22018 _refine_ls_number_parameters 623 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.1150 _refine_ls_R_factor_gt 0.0542 _refine_ls_wR_factor_ref 0.1318 _refine_ls_wR_factor_gt 0.1176 _refine_ls_goodness_of_fit_ref 0.903 _refine_ls_restrained_S_all 0.903 _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 0.007089(16) 0.718021(15) 0.21474(2) 0.03323(8) Uani 1 1 d . . . Pd2 Pd -0.070557(17) 0.611116(15) 0.32958(2) 0.03294(8) Uani 1 1 d . . . Cl1 Cl 0.09916(6) 0.77825(6) 0.20951(12) 0.0534(3) Uani 1 1 d . . . Cl2 Cl -0.07638(7) 0.54586(6) 0.46268(9) 0.0536(3) Uani 1 1 d . . . P1 P 0.05882(6) 0.63441(6) 0.14359(8) 0.0361(3) Uani 1 1 d . . . P3 P -0.11473(6) 0.69421(6) 0.41171(8) 0.0357(3) Uani 1 1 d . . . P4 P -0.02816(6) 0.53408(5) 0.23197(8) 0.0353(3) Uani 1 1 d . . . P2 P -0.05255(6) 0.79649(5) 0.28775(8) 0.0322(2) Uani 1 1 d . . . C1 C 0.0075(3) 0.5660(2) 0.1241(3) 0.0398(11) Uani 1 1 d . . . H1A H 0.0318 0.5330 0.0941 0.052 Uiso 1 1 calc R . . H1B H -0.0260 0.5780 0.0812 0.052 Uiso 1 1 calc R . . C2 C -0.1251(2) 0.7665(2) 0.3408(3) 0.0380(10) Uani 1 1 d . . . H2A H -0.1552 0.7578 0.2912 0.049 Uiso 1 1 calc R . . H2B H -0.1429 0.7991 0.3805 0.049 Uiso 1 1 calc R . . N1 N -0.07133(18) 0.66589(16) 0.2152(3) 0.0350(8) Uani 1 1 d . . . C3 C -0.1248(3) 0.6670(2) 0.1680(4) 0.0462(12) Uani 1 1 d . . . O1 O -0.1723(2) 0.6344(3) 0.1982(4) 0.0782(14) Uani 1 1 d . . . C4 C -0.1355(3) 0.7030(2) 0.0804(4) 0.0482(12) Uani 1 1 d . . . C5 C -0.1955(3) 0.7101(3) 0.0478(4) 0.0572(14) Uani 1 1 d . . . H5 H -0.2284 0.6946 0.0843 0.074 Uiso 1 1 calc R . . C6 C -0.2104(3) 0.7394(3) -0.0376(5) 0.0645(15) Uani 1 1 d . . . H6 H -0.2521 0.7438 -0.0569 0.084 Uiso 1 1 calc R . . C7 C -0.1602(3) 0.7619(3) -0.0936(4) 0.0601(15) Uani 1 1 d . . . C8 C -0.1007(3) 0.7567(3) -0.0629(4) 0.0640(17) Uani 1 1 d . . . H8 H -0.0678 0.7727 -0.0991 0.083 Uiso 1 1 calc R . . C9 C -0.0871(3) 0.7266(3) 0.0258(4) 0.0561(14) Uani 1 1 d . . . H9 H -0.0457 0.7231 0.0464 0.073 Uiso 1 1 calc R . . O2 O -0.1686(3) 0.7873(3) -0.1795(4) 0.0887(16) Uani 1 1 d . . . C10 C -0.2285(5) 0.7852(6) -0.2228(7) 0.113(3) Uani 1 1 d . . . H10A H -0.2361 0.7435 -0.2466 0.158 Uiso 1 1 calc R . . H10B H -0.2298 0.8149 -0.2737 0.158 Uiso 1 1 calc R . . H10C H -0.2604 0.7957 -0.1775 0.158 Uiso 1 1 calc R . . C1P C 0.0895(3) 0.6523(2) 0.0273(4) 0.0450(12) Uani 1 1 d . . . C2P C 0.0544(3) 0.6430(3) -0.0530(4) 0.0603(15) Uani 1 1 d . . . H2P H 0.0142 0.6256 -0.0498 0.078 Uiso 1 1 calc R . . C3P C 0.0810(4) 0.6604(3) -0.1405(4) 0.081(2) Uani 1 1 d . . . H3P H 0.0593 0.6515 -0.1958 0.105 Uiso 1 1 calc R . . C4P C 0.1366(4) 0.6893(4) -0.1448(5) 0.086(2) Uani 1 1 d . . . H4P H 0.1515 0.7039 -0.2022 0.111 Uiso 1 1 calc R . . C5P C 0.1723(4) 0.6978(4) -0.0647(5) 0.084(2) Uani 1 1 d . . . H5P H 0.2121 0.7159 -0.0691 0.109 Uiso 1 1 calc R . . C6P C 0.1495(3) 0.6796(3) 0.0210(5) 0.0629(16) Uani 1 1 d . . . H6P H 0.1736 0.6854 0.0749 0.082 Uiso 1 1 calc R . . C7P C 0.1266(2) 0.6037(2) 0.2061(4) 0.0451(11) Uani 1 1 d . . . C8P C 0.1484(3) 0.6308(3) 0.2883(4) 0.0543(13) Uani 1 1 d . . . H8P H 0.1281 0.6661 0.3127 0.071 Uiso 1 1 calc R . . C9P C 0.1995(3) 0.6062(4) 0.3339(5) 0.0710(18) Uani 1 1 d . . . H9P H 0.2134 0.6252 0.3891 0.092 Uiso 1 1 calc R . . C10P C 0.2299(4) 0.5561(4) 0.3021(7) 0.085(2) Uani 1 1 d . . . H10P H 0.2635 0.5395 0.3358 0.110 Uiso 1 1 calc R . . C11P C 0.2111(3) 0.5283(4) 0.2172(8) 0.092(3) Uani 1 1 d . . . H11P H 0.2336 0.4944 0.1928 0.120 Uiso 1 1 calc R . . C12P C 0.1583(3) 0.5515(3) 0.1689(5) 0.0635(16) Uani 1 1 d . . . H12P H 0.1448 0.5327 0.1135 0.083 Uiso 1 1 calc R . . C13P C -0.0804(2) 0.8540(2) 0.2031(4) 0.0386(10) Uani 1 1 d . . . C14P C -0.1381(3) 0.8844(3) 0.2108(5) 0.0566(14) Uani 1 1 d . . . H14P H -0.1654 0.8747 0.2598 0.074 Uiso 1 1 calc R . . C15P C -0.1548(3) 0.9300(3) 0.1434(5) 0.0705(19) Uani 1 1 d . . . H15P H -0.1933 0.9507 0.1480 0.092 Uiso 1 1 calc R . . C16P C -0.1149(3) 0.9439(3) 0.0720(6) 0.074(2) Uani 1 1 d . . . H16P H -0.1263 0.9743 0.0281 0.096 Uiso 1 1 calc R . . C17P C -0.0590(3) 0.9142(3) 0.0636(5) 0.0664(17) Uani 1 1 d . . . H17P H -0.0325 0.9241 0.0138 0.086 Uiso 1 1 calc R . . C18P C -0.0409(3) 0.8693(3) 0.1283(4) 0.0499(13) Uani 1 1 d . . . H18P H -0.0022 0.8491 0.1219 0.065 Uiso 1 1 calc R . . C19P C -0.0171(2) 0.8434(2) 0.3814(3) 0.0357(10) Uani 1 1 d . . . C20P C -0.0500(3) 0.8955(2) 0.4161(4) 0.0497(13) Uani 1 1 d . . . H20P H -0.0879 0.9075 0.3885 0.065 Uiso 1 1 calc R . . C21P C -0.0265(3) 0.9290(3) 0.4911(4) 0.0604(15) Uani 1 1 d . . . H21P H -0.0488 0.9632 0.5150 0.078 Uiso 1 1 calc R . . C22P C 0.0299(3) 0.9118(3) 0.5301(4) 0.0617(16) Uani 1 1 d . . . H22P H 0.0462 0.9343 0.5806 0.080 Uiso 1 1 calc R . . C23P C 0.0621(3) 0.8618(3) 0.4953(4) 0.0621(16) Uani 1 1 d . . . H23P H 0.1006 0.8509 0.5221 0.081 Uiso 1 1 calc R . . C24P C 0.0394(2) 0.8267(3) 0.4214(4) 0.0474(12) Uani 1 1 d . . . H24P H 0.0620 0.7923 0.3988 0.062 Uiso 1 1 calc R . . C25P C -0.0689(3) 0.7187(2) 0.5130(3) 0.0452(12) Uani 1 1 d . . . C26P C -0.0897(3) 0.7677(3) 0.5719(4) 0.0544(13) Uani 1 1 d . . . H26P H -0.1277 0.7880 0.5601 0.071 Uiso 1 1 calc R . . C27P C -0.0528(4) 0.7850(3) 0.6476(5) 0.071(2) Uani 1 1 d . . . H27P H -0.0666 0.8172 0.6870 0.093 Uiso 1 1 calc R . . C28P C 0.0028(4) 0.7565(3) 0.6660(4) 0.075(2) Uani 1 1 d . . . H28P H 0.0262 0.7686 0.7183 0.098 Uiso 1 1 calc R . . C29P C 0.0251(4) 0.7096(3) 0.6080(5) 0.0689(18) Uani 1 1 d . . . H29P H 0.0636 0.6904 0.6202 0.090 Uiso 1 1 calc R . . C30P C -0.0107(3) 0.6915(2) 0.5312(4) 0.0525(14) Uani 1 1 d . . . H30P H 0.0046 0.6606 0.4910 0.068 Uiso 1 1 calc R . . C31P C -0.1930(3) 0.6815(2) 0.4590(5) 0.0557(14) Uani 1 1 d . . . C32P C -0.2473(3) 0.6969(5) 0.4110(7) 0.101(3) Uani 1 1 d . . . H32P H -0.2447 0.7150 0.3516 0.131 Uiso 1 1 calc R . . C33P C -0.3059(4) 0.6855(6) 0.4513(9) 0.123(4) Uani 1 1 d . . . H33P H -0.3423 0.6987 0.4208 0.159 Uiso 1 1 calc R . . C34P C -0.3099(5) 0.6555(5) 0.5343(9) 0.118(3) Uani 1 1 d U . . H34P H -0.3494 0.6445 0.5573 0.154 Uiso 1 1 calc R . . C35P C -0.2577(5) 0.6408(5) 0.5858(9) 0.119(4) Uani 1 1 d U . . H35P H -0.2615 0.6247 0.6463 0.155 Uiso 1 1 calc R . . C36P C -0.1997(4) 0.6502(4) 0.5465(6) 0.082(2) Uani 1 1 d . . . H36P H -0.1640 0.6358 0.5777 0.107 Uiso 1 1 calc R . . C37P C 0.0321(2) 0.4808(2) 0.2782(3) 0.0401(10) Uani 1 1 d . . . C38P C 0.0628(3) 0.4949(3) 0.3599(4) 0.0477(12) Uani 1 1 d . . . H38P H 0.0521 0.5313 0.3926 0.062 Uiso 1 1 calc R . . C39P C 0.1098(3) 0.4558(3) 0.3950(4) 0.0630(16) Uani 1 1 d . . . H39P H 0.1312 0.4660 0.4500 0.082 Uiso 1 1 calc R . . C40P C 0.1239(3) 0.4017(3) 0.3466(5) 0.0615(16) Uani 1 1 d . . . H40P H 0.1559 0.3757 0.3687 0.080 Uiso 1 1 calc R . . C41P C 0.0927(4) 0.3853(3) 0.2680(5) 0.0688(18) Uani 1 1 d . . . H41P H 0.1013 0.3472 0.2383 0.089 Uiso 1 1 calc R . . C42P C 0.0474(3) 0.4260(3) 0.2315(4) 0.0587(15) Uani 1 1 d . . . H42P H 0.0274 0.4162 0.1753 0.076 Uiso 1 1 calc R . . C43P C -0.0889(3) 0.4826(2) 0.1860(3) 0.0456(12) Uani 1 1 d . . . C44P C -0.1434(4) 0.4725(4) 0.2414(5) 0.079(2) Uani 1 1 d . . . H44P H -0.1466 0.4908 0.3006 0.103 Uiso 1 1 calc R . . C45P C -0.1912(4) 0.4357(4) 0.2077(7) 0.091(2) Uani 1 1 d . . . H45P H -0.2271 0.4293 0.2438 0.118 Uiso 1 1 calc R . . C46P C -0.1862(4) 0.4084(4) 0.1209(7) 0.085(2) Uani 1 1 d . . . H46P H -0.2192 0.3839 0.0983 0.111 Uiso 1 1 calc R . . C47P C -0.1348(4) 0.4163(3) 0.0683(5) 0.0709(18) Uani 1 1 d . . . H47P H -0.1318 0.3963 0.0103 0.092 Uiso 1 1 calc R . . C48P C -0.0864(3) 0.4537(3) 0.0993(4) 0.0590(15) Uani 1 1 d . . . H48P H -0.0513 0.4597 0.0612 0.077 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 0.04046(18) 0.02826(16) 0.03097(16) 0.00043(14) 0.00328(14) -0.00086(14) Pd2 0.04576(19) 0.02963(16) 0.02344(13) 0.00168(13) 0.00024(14) 0.00014(14) Cl1 0.0497(7) 0.0452(6) 0.0652(8) -0.0020(6) 0.0110(7) -0.0115(5) Cl2 0.0793(9) 0.0479(7) 0.0336(6) 0.0138(6) 0.0045(6) 0.0035(6) P1 0.0446(7) 0.0343(6) 0.0294(6) -0.0012(5) 0.0043(5) 0.0017(5) P3 0.0451(7) 0.0322(6) 0.0297(6) 0.0015(5) 0.0047(5) 0.0019(5) P4 0.0520(7) 0.0288(5) 0.0252(6) -0.0007(4) 0.0007(5) -0.0011(5) P2 0.0376(6) 0.0275(5) 0.0315(5) 0.0013(4) -0.0001(5) 0.0010(4) C1 0.058(3) 0.033(2) 0.029(2) -0.0028(18) 0.001(2) 0.002(2) C2 0.042(2) 0.038(2) 0.034(2) 0.0009(19) 0.005(2) 0.0036(19) N1 0.050(2) 0.0283(17) 0.0268(17) 0.0042(15) -0.0021(17) -0.0057(15) C3 0.056(3) 0.044(3) 0.038(3) 0.005(2) -0.001(2) -0.002(2) O1 0.064(3) 0.100(4) 0.071(3) 0.032(3) -0.008(2) -0.024(2) C4 0.068(3) 0.044(3) 0.033(2) 0.003(2) -0.001(3) -0.002(2) C5 0.057(3) 0.073(4) 0.041(3) 0.007(3) -0.003(3) 0.004(3) C6 0.062(4) 0.074(4) 0.057(4) -0.003(3) -0.012(3) 0.008(3) C7 0.076(4) 0.058(3) 0.046(3) 0.012(3) -0.007(3) -0.008(3) C8 0.075(4) 0.065(4) 0.052(4) 0.011(3) -0.010(3) -0.025(3) C9 0.055(3) 0.057(3) 0.056(4) 0.005(3) -0.011(3) -0.005(3) O2 0.100(4) 0.107(4) 0.060(3) 0.039(3) -0.026(3) -0.016(3) C10 0.112(7) 0.151(9) 0.075(6) 0.041(6) -0.038(5) -0.016(6) C1P 0.059(3) 0.037(2) 0.038(3) 0.002(2) 0.011(2) -0.002(2) C2P 0.084(4) 0.066(4) 0.031(3) 0.006(2) 0.003(3) -0.018(3) C3P 0.134(7) 0.078(5) 0.030(3) 0.001(3) 0.008(3) -0.035(5) C4P 0.123(7) 0.085(5) 0.048(4) 0.007(3) 0.027(4) -0.016(5) C5P 0.094(5) 0.098(6) 0.060(4) 0.001(4) 0.029(4) -0.024(4) C6P 0.069(4) 0.071(4) 0.049(3) 0.001(3) 0.013(3) -0.008(3) C7P 0.048(3) 0.044(3) 0.043(3) -0.003(2) 0.004(2) -0.003(2) C8P 0.052(3) 0.065(4) 0.046(3) 0.004(3) -0.002(3) 0.001(3) C9P 0.065(4) 0.093(5) 0.055(4) 0.017(4) -0.008(3) -0.003(4) C10P 0.067(4) 0.099(6) 0.087(6) 0.022(5) -0.017(4) 0.000(4) C11P 0.067(4) 0.064(4) 0.145(8) 0.018(5) 0.018(5) 0.031(3) C12P 0.056(3) 0.061(4) 0.073(4) -0.002(3) 0.003(3) 0.020(3) C13P 0.040(2) 0.033(2) 0.043(3) 0.006(2) -0.007(2) -0.0006(18) C14P 0.053(3) 0.054(3) 0.064(4) 0.015(3) -0.005(3) 0.009(2) C15P 0.062(4) 0.075(4) 0.074(5) 0.031(4) -0.020(3) 0.006(3) C16P 0.070(4) 0.062(4) 0.089(5) 0.042(4) -0.033(4) -0.012(3) C17P 0.075(4) 0.066(4) 0.058(4) 0.028(3) -0.015(3) -0.008(3) C18P 0.048(3) 0.055(3) 0.046(3) 0.014(2) -0.003(2) -0.004(2) C19P 0.038(2) 0.033(2) 0.037(2) 0.0008(18) 0.0027(19) -0.0033(18) C20P 0.051(3) 0.042(3) 0.057(3) -0.014(2) -0.004(3) 0.008(2) C21P 0.076(4) 0.045(3) 0.059(4) -0.012(3) -0.002(3) -0.005(3) C22P 0.082(4) 0.060(4) 0.043(3) -0.011(3) -0.007(3) -0.019(3) C23P 0.050(3) 0.080(4) 0.057(4) 0.000(3) -0.012(3) -0.004(3) C24P 0.042(3) 0.052(3) 0.048(3) -0.002(2) -0.006(2) 0.006(2) C25P 0.072(4) 0.036(2) 0.027(2) -0.0035(19) 0.003(2) -0.005(2) C26P 0.077(4) 0.049(3) 0.037(3) -0.007(2) 0.007(3) -0.001(3) C27P 0.114(6) 0.056(4) 0.044(3) -0.018(3) 0.008(4) -0.013(4) C28P 0.132(7) 0.057(4) 0.036(3) -0.004(3) -0.020(4) -0.016(4) C29P 0.100(5) 0.047(3) 0.060(4) 0.004(3) -0.030(4) 0.003(3) C30P 0.080(4) 0.037(3) 0.040(3) -0.006(2) -0.015(3) 0.003(3) C31P 0.057(3) 0.037(3) 0.073(4) 0.001(3) 0.028(3) -0.001(2) C32P 0.050(4) 0.153(8) 0.100(6) 0.054(6) 0.011(4) 0.013(5) C33P 0.056(4) 0.166(10) 0.146(10) 0.050(8) 0.022(5) 0.007(5) C34P 0.097(6) 0.095(6) 0.163(9) 0.031(6) 0.077(6) 0.003(5) C35P 0.109(6) 0.100(6) 0.149(9) 0.048(6) 0.082(6) 0.019(5) C36P 0.083(5) 0.094(5) 0.070(5) 0.023(4) 0.028(4) 0.003(4) C37P 0.052(3) 0.036(2) 0.033(2) 0.0007(19) 0.003(2) 0.000(2) C38P 0.056(3) 0.044(3) 0.043(3) -0.008(2) -0.002(2) 0.006(2) C39P 0.082(4) 0.061(4) 0.046(3) 0.006(3) -0.018(3) 0.016(3) C40P 0.062(4) 0.046(3) 0.076(5) 0.012(3) -0.006(3) 0.010(3) C41P 0.097(5) 0.038(3) 0.071(4) -0.001(3) -0.002(4) 0.021(3) C42P 0.080(4) 0.048(3) 0.049(3) -0.011(3) -0.014(3) 0.012(3) C43P 0.060(3) 0.044(3) 0.033(3) -0.006(2) -0.008(2) -0.001(2) C44P 0.081(5) 0.088(5) 0.068(5) -0.019(4) 0.020(4) -0.037(4) C45P 0.077(5) 0.097(6) 0.097(6) -0.021(5) 0.015(5) -0.031(4) C46P 0.082(5) 0.079(5) 0.095(6) -0.017(4) -0.023(5) -0.024(4) C47P 0.082(5) 0.073(4) 0.058(4) -0.015(3) -0.020(4) -0.007(4) C48P 0.082(4) 0.052(3) 0.043(3) -0.009(2) -0.003(3) -0.012(3) _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 N1 1.999(4) . ? Pd1 P1 2.3194(13) . ? Pd1 P2 2.3357(13) . ? Pd1 Cl1 2.3363(14) . ? Pd1 Pd2 3.2457(7) . ? Pd2 N1 2.001(4) . ? Pd2 P3 2.3141(13) . ? Pd2 P4 2.3264(12) . ? Pd2 Cl2 2.3497(13) . ? P1 C7P 1.812(6) . ? P1 C1P 1.818(5) . ? P1 C1 1.837(5) . ? P3 C31P 1.813(5) . ? P3 C25P 1.815(5) . ? P3 C2 1.849(5) . ? P4 C43P 1.813(5) . ? P4 C37P 1.829(5) . ? P4 C1 1.840(5) . ? P2 C13P 1.814(5) . ? P2 C19P 1.826(5) . ? P2 C2 1.830(5) . ? N1 C3 1.319(7) . ? C3 O1 1.295(7) . ? C3 C4 1.479(7) . ? C4 C5 1.363(8) . ? C4 C9 1.382(8) . ? C5 C6 1.402(9) . ? C6 C7 1.415(9) . ? C7 C8 1.340(9) . ? C7 O2 1.348(7) . ? C8 C9 1.445(8) . ? O2 C10 1.415(10) . ? C1P C2P 1.380(8) . ? C1P C6P 1.401(8) . ? C2P C3P 1.416(8) . ? C3P C4P 1.332(11) . ? C4P C5P 1.381(12) . ? C5P C6P 1.368(9) . ? C7P C8P 1.383(8) . ? C7P C12P 1.401(8) . ? C8P C9P 1.370(9) . ? C9P C10P 1.323(11) . ? C10P C11P 1.403(13) . ? C11P C12P 1.403(10) . ? C13P C14P 1.388(7) . ? C13P C18P 1.393(7) . ? C14P C15P 1.408(8) . ? C15P C16P 1.355(10) . ? C16P C17P 1.348(10) . ? C17P C18P 1.380(8) . ? C19P C24P 1.374(7) . ? C19P C20P 1.397(7) . ? C20P C21P 1.376(8) . ? C21P C22P 1.371(9) . ? C22P C23P 1.356(9) . ? C23P C24P 1.376(8) . ? C25P C30P 1.387(8) . ? C25P C26P 1.407(7) . ? C26P C27P 1.382(9) . ? C27P C28P 1.352(11) . ? C28P C29P 1.376(10) . ? C29P C30P 1.385(8) . ? C31P C32P 1.379(10) . ? C31P C36P 1.419(10) . ? C32P C33P 1.390(11) . ? C33P C34P 1.345(15) . ? C34P C35P 1.365(16) . ? C35P C36P 1.365(10) . ? C37P C38P 1.366(7) . ? C37P C42P 1.378(7) . ? C38P C39P 1.392(8) . ? C39P C40P 1.372(9) . ? C40P C41P 1.347(10) . ? C41P C42P 1.392(9) . ? C43P C48P 1.380(7) . ? C43P C44P 1.415(9) . ? C44P C45P 1.366(10) . ? C45P C46P 1.369(12) . ? C46P C47P 1.333(11) . ? C47P C48P 1.371(9) . ? 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 N1 Pd1 P1 88.39(11) . . ? N1 Pd1 P2 86.68(11) . . ? P1 Pd1 P2 175.04(5) . . ? N1 Pd1 Cl1 178.30(13) . . ? P1 Pd1 Cl1 90.50(5) . . ? P2 Pd1 Cl1 94.43(5) . . ? N1 Pd1 Pd2 35.77(11) . . ? P1 Pd1 Pd2 85.71(3) . . ? P2 Pd1 Pd2 89.96(3) . . ? Cl1 Pd1 Pd2 145.41(4) . . ? N1 Pd2 P3 87.98(11) . . ? N1 Pd2 P4 85.74(11) . . ? P3 Pd2 P4 173.64(4) . . ? N1 Pd2 Cl2 176.46(12) . . ? P3 Pd2 Cl2 91.19(5) . . ? P4 Pd2 Cl2 95.01(5) . . ? N1 Pd2 Pd1 35.73(11) . . ? P3 Pd2 Pd1 85.83(3) . . ? P4 Pd2 Pd1 89.67(3) . . ? Cl2 Pd2 Pd1 147.63(4) . . ? C7P P1 C1P 103.7(3) . . ? C7P P1 C1 105.1(2) . . ? C1P P1 C1 104.0(2) . . ? C7P P1 Pd1 115.87(18) . . ? C1P P1 Pd1 113.99(17) . . ? C1 P1 Pd1 112.95(17) . . ? C31P P3 C25P 103.8(3) . . ? C31P P3 C2 102.5(2) . . ? C25P P3 C2 105.1(2) . . ? C31P P3 Pd2 116.46(18) . . ? C25P P3 Pd2 113.70(18) . . ? C2 P3 Pd2 113.87(16) . . ? C43P P4 C37P 104.7(2) . . ? C43P P4 C1 102.3(2) . . ? C37P P4 C1 103.9(2) . . ? C43P P4 Pd2 111.35(18) . . ? C37P P4 Pd2 119.34(16) . . ? C1 P4 Pd2 113.47(15) . . ? C13P P2 C19P 104.6(2) . . ? C13P P2 C2 103.6(2) . . ? C19P P2 C2 103.6(2) . . ? C13P P2 Pd1 111.17(17) . . ? C19P P2 Pd1 119.35(16) . . ? C2 P2 Pd1 113.03(15) . . ? P1 C1 P4 114.2(2) . . ? P2 C2 P3 114.4(2) . . ? C3 N1 Pd1 134.8(3) . . ? C3 N1 Pd2 115.6(3) . . ? Pd1 N1 Pd2 108.50(18) . . ? O1 C3 N1 119.4(5) . . ? O1 C3 C4 115.8(5) . . ? N1 C3 C4 124.8(5) . . ? C5 C4 C9 117.5(5) . . ? C5 C4 C3 119.2(5) . . ? C9 C4 C3 123.1(5) . . ? C4 C5 C6 123.8(6) . . ? C5 C6 C7 117.9(6) . . ? C8 C7 O2 116.9(6) . . ? C8 C7 C6 120.0(6) . . ? O2 C7 C6 123.1(6) . . ? C7 C8 C9 120.5(6) . . ? C4 C9 C8 120.3(6) . . ? C7 O2 C10 120.1(6) . . ? C2P C1P C6P 119.8(5) . . ? C2P C1P P1 122.0(4) . . ? C6P C1P P1 118.1(4) . . ? C1P C2P C3P 118.4(6) . . ? C4P C3P C2P 120.9(7) . . ? C3P C4P C5P 120.7(7) . . ? C6P C5P C4P 120.3(7) . . ? C5P C6P C1P 119.7(7) . . ? C8P C7P C12P 119.2(5) . . ? C8P C7P P1 122.1(4) . . ? C12P C7P P1 118.8(4) . . ? C9P C8P C7P 120.5(6) . . ? C10P C9P C8P 122.0(8) . . ? C9P C10P C11P 119.7(7) . . ? C12P C11P C10P 120.1(7) . . ? C7P C12P C11P 118.5(7) . . ? C14P C13P C18P 118.9(5) . . ? C14P C13P P2 123.2(4) . . ? C18P C13P P2 117.9(4) . . ? C13P C14P C15P 119.2(6) . . ? C16P C15P C14P 120.2(6) . . ? C17P C16P C15P 121.0(6) . . ? C16P C17P C18P 120.6(6) . . ? C17P C18P C13P 120.2(6) . . ? C24P C19P C20P 119.6(5) . . ? C24P C19P P2 121.4(4) . . ? C20P C19P P2 118.9(4) . . ? C21P C20P C19P 120.2(5) . . ? C22P C21P C20P 119.5(6) . . ? C23P C22P C21P 120.1(5) . . ? C22P C23P C24P 121.8(6) . . ? C19P C24P C23P 118.9(5) . . ? C30P C25P C26P 118.4(5) . . ? C30P C25P P3 120.4(4) . . ? C26P C25P P3 121.1(5) . . ? C27P C26P C25P 118.9(6) . . ? C28P C27P C26P 121.8(6) . . ? C27P C28P C29P 120.5(6) . . ? C28P C29P C30P 119.0(7) . . ? C29P C30P C25P 121.4(6) . . ? C32P C31P C36P 117.6(6) . . ? C32P C31P P3 123.1(5) . . ? C36P C31P P3 119.2(5) . . ? C31P C32P C33P 120.1(8) . . ? C34P C33P C32P 120.1(10) . . ? C33P C34P C35P 122.0(9) . . ? C34P C35P C36P 118.5(10) . . ? C35P C36P C31P 121.2(8) . . ? C38P C37P C42P 118.8(5) . . ? C38P C37P P4 120.3(4) . . ? C42P C37P P4 120.9(4) . . ? C37P C38P C39P 121.1(5) . . ? C40P C39P C38P 118.4(6) . . ? C41P C40P C39P 121.7(6) . . ? C40P C41P C42P 119.3(6) . . ? C37P C42P C41P 120.5(6) . . ? C48P C43P C44P 117.6(6) . . ? C48P C43P P4 124.3(5) . . ? C44P C43P P4 118.1(4) . . ? C45P C44P C43P 119.8(7) . . ? C44P C45P C46P 120.1(8) . . ? C47P C46P C45P 121.2(7) . . ? C46P C47P C48P 120.3(7) . . ? C47P C48P C43P 121.0(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P1 Pd1 Pd2 N1 -93.20(19) . . . . ? P2 Pd1 Pd2 N1 84.37(19) . . . . ? Cl1 Pd1 Pd2 N1 -177.9(2) . . . . ? N1 Pd1 Pd2 P3 -92.35(19) . . . . ? P1 Pd1 Pd2 P3 174.44(5) . . . . ? P2 Pd1 Pd2 P3 -7.98(4) . . . . ? Cl1 Pd1 Pd2 P3 89.79(7) . . . . ? N1 Pd1 Pd2 P4 83.14(19) . . . . ? P1 Pd1 Pd2 P4 -10.06(4) . . . . ? P2 Pd1 Pd2 P4 167.51(4) . . . . ? Cl1 Pd1 Pd2 P4 -94.72(7) . . . . ? N1 Pd1 Pd2 Cl2 -178.0(2) . . . . ? P1 Pd1 Pd2 Cl2 88.81(8) . . . . ? P2 Pd1 Pd2 Cl2 -93.62(8) . . . . ? Cl1 Pd1 Pd2 Cl2 4.15(10) . . . . ? N1 Pd1 P1 C7P -121.7(2) . . . . ? P2 Pd1 P1 C7P -115.3(5) . . . . ? Cl1 Pd1 P1 C7P 59.59(19) . . . . ? Pd2 Pd1 P1 C7P -85.99(19) . . . . ? N1 Pd1 P1 C1P 118.0(2) . . . . ? P2 Pd1 P1 C1P 124.4(5) . . . . ? Cl1 Pd1 P1 C1P -60.7(2) . . . . ? Pd2 Pd1 P1 C1P 153.7(2) . . . . ? N1 Pd1 P1 C1 -0.4(2) . . . . ? P2 Pd1 P1 C1 6.0(6) . . . . ? Cl1 Pd1 P1 C1 -179.07(17) . . . . ? Pd2 Pd1 P1 C1 35.35(17) . . . . ? N1 Pd2 P3 C31P 116.3(3) . . . . ? P4 Pd2 P3 C31P 106.9(5) . . . . ? Cl2 Pd2 P3 C31P -60.2(3) . . . . ? Pd1 Pd2 P3 C31P 152.0(3) . . . . ? N1 Pd2 P3 C25P -123.0(2) . . . . ? P4 Pd2 P3 C25P -132.4(5) . . . . ? Cl2 Pd2 P3 C25P 60.46(19) . . . . ? Pd1 Pd2 P3 C25P -87.27(19) . . . . ? N1 Pd2 P3 C2 -2.7(2) . . . . ? P4 Pd2 P3 C2 -12.1(5) . . . . ? Cl2 Pd2 P3 C2 -179.24(18) . . . . ? Pd1 Pd2 P3 C2 33.03(17) . . . . ? N1 Pd2 P4 C43P -94.8(2) . . . . ? P3 Pd2 P4 C43P -85.4(5) . . . . ? Cl2 Pd2 P4 C43P 81.69(19) . . . . ? Pd1 Pd2 P4 C43P -130.38(18) . . . . ? N1 Pd2 P4 C37P 143.0(2) . . . . ? P3 Pd2 P4 C37P 152.4(4) . . . . ? Cl2 Pd2 P4 C37P -40.48(19) . . . . ? Pd1 Pd2 P4 C37P 107.45(19) . . . . ? N1 Pd2 P4 C1 20.0(2) . . . . ? P3 Pd2 P4 C1 29.4(5) . . . . ? Cl2 Pd2 P4 C1 -163.48(19) . . . . ? Pd1 Pd2 P4 C1 -15.55(19) . . . . ? N1 Pd1 P2 C13P -97.7(2) . . . . ? P1 Pd1 P2 C13P -104.1(5) . . . . ? Cl1 Pd1 P2 C13P 81.02(17) . . . . ? Pd2 Pd1 P2 C13P -133.33(16) . . . . ? N1 Pd1 P2 C19P 140.5(2) . . . . ? P1 Pd1 P2 C19P 134.1(5) . . . . ? Cl1 Pd1 P2 C19P -40.83(18) . . . . ? Pd2 Pd1 P2 C19P 104.82(17) . . . . ? N1 Pd1 P2 C2 18.3(2) . . . . ? P1 Pd1 P2 C2 11.9(6) . . . . ? Cl1 Pd1 P2 C2 -163.02(18) . . . . ? Pd2 Pd1 P2 C2 -17.37(18) . . . . ? C7P P1 C1 P4 68.6(3) . . . . ? C1P P1 C1 P4 177.2(3) . . . . ? Pd1 P1 C1 P4 -58.7(3) . . . . ? C43P P4 C1 P1 166.3(3) . . . . ? C37P P4 C1 P1 -84.9(3) . . . . ? Pd2 P4 C1 P1 46.2(3) . . . . ? C13P P2 C2 P3 167.1(3) . . . . ? C19P P2 C2 P3 -84.0(3) . . . . ? Pd1 P2 C2 P3 46.7(3) . . . . ? C31P P3 C2 P2 176.1(3) . . . . ? C25P P3 C2 P2 67.9(3) . . . . ? Pd2 P3 C2 P2 -57.2(3) . . . . ? P1 Pd1 N1 C3 -108.0(5) . . . . ? P2 Pd1 N1 C3 72.5(5) . . . . ? Cl1 Pd1 N1 C3 -58(4) . . . . ? Pd2 Pd1 N1 C3 167.1(6) . . . . ? P1 Pd1 N1 Pd2 84.90(15) . . . . ? P2 Pd1 N1 Pd2 -94.55(16) . . . . ? Cl1 Pd1 N1 Pd2 134(4) . . . . ? P3 Pd2 N1 C3 -84.2(4) . . . . ? P4 Pd2 N1 C3 94.7(4) . . . . ? Cl2 Pd2 N1 C3 -8(2) . . . . ? Pd1 Pd2 N1 C3 -169.9(5) . . . . ? P3 Pd2 N1 Pd1 85.65(15) . . . . ? P4 Pd2 N1 Pd1 -95.39(16) . . . . ? Cl2 Pd2 N1 Pd1 162.3(17) . . . . ? Pd1 N1 C3 O1 -165.6(4) . . . . ? Pd2 N1 C3 O1 0.8(7) . . . . ? Pd1 N1 C3 C4 15.1(8) . . . . ? Pd2 N1 C3 C4 -178.5(4) . . . . ? O1 C3 C4 C5 12.9(8) . . . . ? N1 C3 C4 C5 -167.8(5) . . . . ? O1 C3 C4 C9 -162.7(6) . . . . ? N1 C3 C4 C9 16.6(9) . . . . ? C9 C4 C5 C6 0.5(9) . . . . ? C3 C4 C5 C6 -175.3(6) . . . . ? C4 C5 C6 C7 1.0(10) . . . . ? C5 C6 C7 C8 -2.1(10) . . . . ? C5 C6 C7 O2 175.7(6) . . . . ? O2 C7 C8 C9 -176.2(6) . . . . ? C6 C7 C8 C9 1.8(10) . . . . ? C5 C4 C9 C8 -0.9(9) . . . . ? C3 C4 C9 C8 174.8(5) . . . . ? C7 C8 C9 C4 -0.3(10) . . . . ? C8 C7 O2 C10 170.0(8) . . . . ? C6 C7 O2 C10 -7.9(11) . . . . ? C7P P1 C1P C2P 143.0(5) . . . . ? C1 P1 C1P C2P 33.3(5) . . . . ? Pd1 P1 C1P C2P -90.1(5) . . . . ? C7P P1 C1P C6P -40.4(5) . . . . ? C1 P1 C1P C6P -150.1(5) . . . . ? Pd1 P1 C1P C6P 86.5(5) . . . . ? C6P C1P C2P C3P 1.2(9) . . . . ? P1 C1P C2P C3P 177.6(5) . . . . ? C1P C2P C3P C4P -4.8(11) . . . . ? C2P C3P C4P C5P 6.0(13) . . . . ? C3P C4P C5P C6P -3.6(13) . . . . ? C4P C5P C6P C1P 0.0(12) . . . . ? C2P C1P C6P C5P 1.1(10) . . . . ? P1 C1P C6P C5P -175.5(6) . . . . ? C1P P1 C7P C8P 122.0(5) . . . . ? C1 P1 C7P C8P -129.2(5) . . . . ? Pd1 P1 C7P C8P -3.7(5) . . . . ? C1P P1 C7P C12P -56.9(5) . . . . ? C1 P1 C7P C12P 51.9(5) . . . . ? Pd1 P1 C7P C12P 177.4(4) . . . . ? C12P C7P C8P C9P -1.4(9) . . . . ? P1 C7P C8P C9P 179.6(5) . . . . ? C7P C8P C9P C10P 0.0(10) . . . . ? C8P C9P C10P C11P 2.4(12) . . . . ? C9P C10P C11P C12P -3.3(12) . . . . ? C8P C7P C12P C11P 0.5(9) . . . . ? P1 C7P C12P C11P 179.4(5) . . . . ? C10P C11P C12P C7P 1.9(11) . . . . ? C19P P2 C13P C14P -84.0(5) . . . . ? C2 P2 C13P C14P 24.2(5) . . . . ? Pd1 P2 C13P C14P 145.9(4) . . . . ? C19P P2 C13P C18P 94.4(4) . . . . ? C2 P2 C13P C18P -157.3(4) . . . . ? Pd1 P2 C13P C18P -35.7(4) . . . . ? C18P C13P C14P C15P -0.6(9) . . . . ? P2 C13P C14P C15P 177.8(5) . . . . ? C13P C14P C15P C16P 0.1(10) . . . . ? C14P C15P C16P C17P 0.5(11) . . . . ? C15P C16P C17P C18P -0.6(11) . . . . ? C16P C17P C18P C13P 0.1(10) . . . . ? C14P C13P C18P C17P 0.5(8) . . . . ? P2 C13P C18P C17P -178.0(5) . . . . ? C13P P2 C19P C24P -136.7(4) . . . . ? C2 P2 C19P C24P 115.1(4) . . . . ? Pd1 P2 C19P C24P -11.6(5) . . . . ? C13P P2 C19P C20P 46.6(5) . . . . ? C2 P2 C19P C20P -61.6(4) . . . . ? Pd1 P2 C19P C20P 171.7(4) . . . . ? C24P C19P C20P C21P -1.3(8) . . . . ? P2 C19P C20P C21P 175.4(5) . . . . ? C19P C20P C21P C22P 1.3(9) . . . . ? C20P C21P C22P C23P -0.3(10) . . . . ? C21P C22P C23P C24P -0.7(10) . . . . ? C20P C19P C24P C23P 0.4(8) . . . . ? P2 C19P C24P C23P -176.3(4) . . . . ? C22P C23P C24P C19P 0.6(9) . . . . ? C31P P3 C25P C30P 132.3(5) . . . . ? C2 P3 C25P C30P -120.4(5) . . . . ? Pd2 P3 C25P C30P 4.8(5) . . . . ? C31P P3 C25P C26P -51.0(5) . . . . ? C2 P3 C25P C26P 56.3(5) . . . . ? Pd2 P3 C25P C26P -178.5(4) . . . . ? C30P C25P C26P C27P -2.6(8) . . . . ? P3 C25P C26P C27P -179.4(5) . . . . ? C25P C26P C27P C28P 0.4(10) . . . . ? C26P C27P C28P C29P 1.3(11) . . . . ? C27P C28P C29P C30P -0.9(11) . . . . ? C28P C29P C30P C25P -1.4(10) . . . . ? C26P C25P C30P C29P 3.1(9) . . . . ? P3 C25P C30P C29P 179.9(5) . . . . ? C25P P3 C31P C32P 142.2(7) . . . . ? C2 P3 C31P C32P 33.1(8) . . . . ? Pd2 P3 C31P C32P -91.9(7) . . . . ? C25P P3 C31P C36P -42.5(6) . . . . ? C2 P3 C31P C36P -151.6(5) . . . . ? Pd2 P3 C31P C36P 83.4(6) . . . . ? C36P C31P C32P C33P 4.2(14) . . . . ? P3 C31P C32P C33P 179.6(9) . . . . ? C31P C32P C33P C34P -4.6(18) . . . . ? C32P C33P C34P C35P 6.4(19) . . . . ? C33P C34P C35P C36P -7.9(18) . . . . ? C34P C35P C36P C31P 7.5(15) . . . . ? C32P C31P C36P C35P -5.8(12) . . . . ? P3 C31P C36P C35P 178.6(8) . . . . ? C43P P4 C37P C38P -141.2(4) . . . . ? C1 P4 C37P C38P 111.8(4) . . . . ? Pd2 P4 C37P C38P -15.8(5) . . . . ? C43P P4 C37P C42P 39.0(5) . . . . ? C1 P4 C37P C42P -68.0(5) . . . . ? Pd2 P4 C37P C42P 164.5(4) . . . . ? C42P C37P C38P C39P 1.4(8) . . . . ? P4 C37P C38P C39P -178.4(5) . . . . ? C37P C38P C39P C40P -1.3(9) . . . . ? C38P C39P C40P C41P -1.4(10) . . . . ? C39P C40P C41P C42P 3.9(11) . . . . ? C38P C37P C42P C41P 1.2(9) . . . . ? P4 C37P C42P C41P -179.1(5) . . . . ? C40P C41P C42P C37P -3.8(11) . . . . ? C37P P4 C43P C48P -81.1(5) . . . . ? C1 P4 C43P C48P 27.0(6) . . . . ? Pd2 P4 C43P C48P 148.6(5) . . . . ? C37P P4 C43P C44P 100.6(6) . . . . ? C1 P4 C43P C44P -151.2(5) . . . . ? Pd2 P4 C43P C44P -29.7(6) . . . . ? C48P C43P C44P C45P -0.6(11) . . . . ? P4 C43P C44P C45P 177.7(7) . . . . ? C43P C44P C45P C46P 0.5(14) . . . . ? C44P C45P C46P C47P 0.8(15) . . . . ? C45P C46P C47P C48P -1.9(13) . . . . ? C46P C47P C48P C43P 1.7(11) . . . . ? C44P C43P C48P C47P -0.4(9) . . . . ? P4 C43P C48P C47P -178.6(5) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 31.97 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.237 _refine_diff_density_min -1.552 _refine_diff_density_rms 0.112