# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2001 # CCDC Number: 440/240 data_cad4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H29 Cl4 N O3 P Pd' _chemical_formula_weight 730.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.795(3) _cell_length_b 12.090(3) _cell_length_c 17.268(2) _cell_angle_alpha 90.00 _cell_angle_beta 116.549(12) _cell_angle_gamma 90.00 _cell_volume 3136.6(10) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.547 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1476 _exptl_absorpt_coefficient_mu 1.015 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.6307 _exptl_absorpt_correction_T_max 0.7641 _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7456 _diffrn_reflns_av_R_equivalents 0.0184 _diffrn_reflns_av_sigmaI/netI 0.0365 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 27.46 _reflns_number_total 7172 _reflns_number_gt 5938 _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 w=1/[\s^2^(Fo^2^)+(0.0364P)^2^+0.9581P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7172 _refine_ls_number_parameters 418 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0448 _refine_ls_R_factor_gt 0.0340 _refine_ls_wR_factor_ref 0.0864 _refine_ls_wR_factor_gt 0.0826 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.633233(12) 0.854341(15) 0.616501(11) 0.03189(7) Uani 1 d . . . Cl1 Cl 0.52959(5) 0.73411(6) 0.63410(5) 0.04722(16) Uani 1 d . . . C1 C 0.69597(16) 0.9682(2) 0.57733(15) 0.0341(5) Uani 1 d . . . C2 C 0.76211(17) 0.9592(2) 0.55016(16) 0.0373(5) Uani 1 d . . . H2A H 0.7910 0.8918 0.5563 0.045 Uiso 1 calc R . . C3 C 0.78633(17) 1.0482(2) 0.51397(16) 0.0377(6) Uani 1 d . . . O1 O 0.84872(14) 1.04394(17) 0.48353(14) 0.0527(5) Uani 1 d . . . C8 C 0.7397(3) 1.3420(3) 0.4710(3) 0.0780(12) Uani 1 d . . . H8A H 0.7692 1.3952 0.4514 0.117 Uiso 1 calc R . . H8B H 0.7494 1.3605 0.5286 0.117 Uiso 1 calc R . . H8C H 0.6771 1.3427 0.4329 0.117 Uiso 1 calc R . . C4 C 0.74575(18) 1.1513(2) 0.50639(18) 0.0407(6) Uani 1 d . . . O2 O 0.77479(15) 1.23435(17) 0.47094(15) 0.0560(5) Uani 1 d . . . C9 C 0.8824(2) 0.9385(3) 0.4778(3) 0.0666(10) Uani 1 d . . . H9A H 0.9212 0.9456 0.4508 0.100 Uiso 1 calc R . . H9B H 0.8338 0.8903 0.4438 0.100 Uiso 1 calc R . . H9C H 0.9149 0.9082 0.5348 0.100 Uiso 1 calc R . . C5 C 0.68035(19) 1.1625(2) 0.53277(18) 0.0422(6) Uani 1 d . . . H5A H 0.6528 1.2306 0.5279 0.051 Uiso 1 calc R . . C6 C 0.65502(17) 1.0722(2) 0.56687(16) 0.0376(5) Uani 1 d . . . C7 C 0.58253(18) 1.0804(2) 0.59007(17) 0.0417(6) Uani 1 d . . . H7A H 0.5534 1.1474 0.5852 0.050 Uiso 1 calc R . . N1 N 0.55925(14) 0.99426(18) 0.61737(14) 0.0378(5) Uani 1 d . . . C10 C 0.49018(19) 1.0034(2) 0.6470(2) 0.0485(7) Uani 1 d . . . H10A H 0.4623 0.9318 0.6423 0.058 Uiso 1 calc R . . H10B H 0.4448 1.0548 0.6101 0.058 Uiso 1 calc R . . C11 C 0.5279(2) 1.0424(3) 0.7388(2) 0.0589(8) Uani 1 d . . . H11A H 0.4832 1.0361 0.7596 0.071 Uiso 1 calc R . . H11B H 0.5782 0.9964 0.7750 0.071 Uiso 1 calc R . . O3 O 0.5557(2) 1.1534(2) 0.74462(19) 0.0744(8) Uani 1 d . . . H3A H 0.5394 1.1879 0.7759 0.112 Uiso 1 calc R . . P1 P 0.72504(4) 0.71348(5) 0.62385(4) 0.03361(14) Uani 1 d . . . C12 C 0.83903(17) 0.7272(2) 0.70868(16) 0.0407(6) Uani 1 d . . . C13 C 0.8950(2) 0.6350(3) 0.7369(2) 0.0549(8) Uani 1 d . . . H13A H 0.8753 0.5666 0.7107 0.066 Uiso 1 calc R . . C14 C 0.9800(2) 0.6459(4) 0.8042(2) 0.0718(11) Uani 1 d . . . H14A H 1.0174 0.5848 0.8227 0.086 Uiso 1 calc R . . C15 C 1.0091(2) 0.7459(4) 0.8432(2) 0.0759(11) Uani 1 d . . . H15A H 1.0660 0.7521 0.8886 0.091 Uiso 1 calc R . . C16 C 0.9551(2) 0.8375(4) 0.8160(2) 0.0686(10) Uani 1 d . . . H16A H 0.9755 0.9055 0.8427 0.082 Uiso 1 calc R . . C17 C 0.8698(2) 0.8280(3) 0.74841(18) 0.0499(7) Uani 1 d . . . H17A H 0.8332 0.8899 0.7298 0.060 Uiso 1 calc R . . C18 C 0.68961(17) 0.5801(2) 0.64695(17) 0.0395(6) Uani 1 d . . . C19 C 0.6331(2) 0.5116(2) 0.5804(2) 0.0499(7) Uani 1 d . . . H19A H 0.6178 0.5302 0.5232 0.060 Uiso 1 calc R . . C20 C 0.5994(2) 0.4159(3) 0.5986(3) 0.0619(9) Uani 1 d . . . H20A H 0.5604 0.3716 0.5537 0.074 Uiso 1 calc R . . C21 C 0.6236(3) 0.3866(3) 0.6827(3) 0.0666(10) Uani 1 d . . . H21A H 0.6019 0.3213 0.6946 0.080 Uiso 1 calc R . . C22 C 0.6788(2) 0.4519(3) 0.7491(2) 0.0658(9) Uani 1 d . . . H22A H 0.6949 0.4311 0.8061 0.079 Uiso 1 calc R . . C23 C 0.7116(2) 0.5503(3) 0.7318(2) 0.0532(7) Uani 1 d . . . H23A H 0.7481 0.5959 0.7771 0.064 Uiso 1 calc R . . C24 C 0.73153(17) 0.6902(2) 0.52257(16) 0.0367(5) Uani 1 d . . . C25 C 0.6577(2) 0.7174(3) 0.44652(18) 0.0485(7) Uani 1 d . . . H25A H 0.6075 0.7467 0.4487 0.058 Uiso 1 calc R . . C26 C 0.6579(2) 0.7015(3) 0.36707(19) 0.0612(9) Uani 1 d . . . H26A H 0.6080 0.7203 0.3163 0.073 Uiso 1 calc R . . C27 C 0.7306(3) 0.6587(3) 0.3631(2) 0.0620(9) Uani 1 d . . . H27A H 0.7302 0.6476 0.3096 0.074 Uiso 1 calc R . . C28 C 0.8048(2) 0.6317(3) 0.4378(2) 0.0606(9) Uani 1 d . . . H28A H 0.8547 0.6030 0.4347 0.073 Uiso 1 calc R . . C29 C 0.8055(2) 0.6472(3) 0.5176(2) 0.0506(7) Uani 1 d . . . H29A H 0.8558 0.6285 0.5680 0.061 Uiso 1 calc R . . C30 C 0.8698(2) 1.2653(3) 0.3520(2) 0.0710(10) Uani 1 d D . . Cl2 Cl 0.9579(11) 1.3478(18) 0.4267(11) 0.157(7) Uani 0.34 d PD . . Cl3 Cl 0.8060(15) 1.3614(14) 0.2726(15) 0.131(7) Uani 0.34 d PD . . Cl4 Cl 0.9125(15) 1.1784(14) 0.2982(13) 0.169(8) Uani 0.34 d PD . . Cl2' Cl 0.9611(7) 1.3198(10) 0.4372(8) 0.085(2) Uani 0.33 d PD . . Cl3' Cl 0.7903(12) 1.3495(15) 0.2832(12) 0.117(5) Uani 0.33 d PD . . Cl4' Cl 0.9025(8) 1.1554(10) 0.3070(11) 0.087(3) Uani 0.33 d PD . . Cl2" Cl 0.9454(7) 1.3576(10) 0.4309(7) 0.093(3) Uani 0.33 d PD . . Cl3" Cl 0.8042(9) 1.3427(15) 0.2610(9) 0.102(4) Uani 0.33 d PD . . Cl4" Cl 0.9299(10) 1.1704(16) 0.3243(12) 0.118(6) Uani 0.33 d PD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.03557(11) 0.03352(11) 0.03151(10) -0.00005(7) 0.01939(8) -0.00002(8) Cl1 0.0471(4) 0.0472(4) 0.0569(4) 0.0058(3) 0.0318(3) -0.0023(3) C1 0.0383(13) 0.0343(13) 0.0323(12) -0.0014(10) 0.0181(10) -0.0040(10) C2 0.0400(13) 0.0337(13) 0.0417(14) -0.0009(11) 0.0213(11) 0.0000(11) C3 0.0370(13) 0.0425(14) 0.0380(13) -0.0023(11) 0.0207(11) -0.0038(11) O1 0.0595(12) 0.0478(12) 0.0714(14) 0.0009(10) 0.0476(12) -0.0030(10) C8 0.098(3) 0.0416(19) 0.119(3) 0.021(2) 0.070(3) 0.0053(18) C4 0.0450(14) 0.0378(14) 0.0419(14) 0.0032(11) 0.0218(12) -0.0045(12) O2 0.0693(14) 0.0409(11) 0.0731(14) 0.0118(10) 0.0456(12) -0.0012(10) C9 0.076(2) 0.059(2) 0.094(3) -0.0002(19) 0.063(2) 0.0066(18) C5 0.0479(15) 0.0337(14) 0.0470(15) 0.0037(11) 0.0230(13) 0.0019(11) C6 0.0397(13) 0.0366(13) 0.0393(13) -0.0020(11) 0.0200(11) -0.0013(11) C7 0.0443(15) 0.0365(14) 0.0470(15) -0.0026(11) 0.0229(13) 0.0037(11) N1 0.0394(11) 0.0378(12) 0.0424(12) -0.0047(9) 0.0238(10) -0.0001(9) C10 0.0464(15) 0.0430(15) 0.073(2) -0.0075(14) 0.0414(15) -0.0013(13) C11 0.080(2) 0.0536(19) 0.069(2) 0.0046(16) 0.0559(19) 0.0051(17) O3 0.104(2) 0.0635(16) 0.0868(18) -0.0276(13) 0.0700(17) -0.0267(14) P1 0.0366(3) 0.0345(3) 0.0319(3) 0.0022(3) 0.0173(3) 0.0022(3) C12 0.0366(13) 0.0535(16) 0.0337(12) 0.0065(12) 0.0172(11) 0.0007(12) C13 0.0498(17) 0.061(2) 0.0513(17) 0.0127(15) 0.0206(14) 0.0076(15) C14 0.0506(19) 0.096(3) 0.059(2) 0.024(2) 0.0155(17) 0.017(2) C15 0.0445(18) 0.120(4) 0.0477(19) 0.004(2) 0.0070(15) -0.003(2) C16 0.055(2) 0.094(3) 0.0507(19) -0.0155(18) 0.0181(16) -0.016(2) C17 0.0453(15) 0.0644(19) 0.0415(15) -0.0020(14) 0.0207(13) -0.0027(14) C18 0.0410(13) 0.0357(14) 0.0470(15) 0.0065(11) 0.0242(12) 0.0061(11) C19 0.0552(17) 0.0400(15) 0.0611(18) -0.0043(14) 0.0320(15) 0.0009(13) C20 0.062(2) 0.0397(17) 0.093(3) -0.0098(17) 0.0427(19) -0.0069(15) C21 0.076(2) 0.0390(17) 0.104(3) 0.0086(19) 0.057(2) -0.0006(17) C22 0.074(2) 0.063(2) 0.074(2) 0.0287(19) 0.046(2) 0.0122(19) C23 0.0584(18) 0.0506(17) 0.0529(17) 0.0106(14) 0.0270(15) 0.0031(15) C24 0.0424(13) 0.0351(13) 0.0365(13) -0.0025(10) 0.0210(11) -0.0001(11) C25 0.0500(16) 0.0540(18) 0.0384(14) -0.0001(13) 0.0170(13) 0.0085(14) C26 0.072(2) 0.071(2) 0.0348(15) 0.0002(15) 0.0186(15) 0.0062(18) C27 0.080(2) 0.073(2) 0.0440(17) -0.0114(15) 0.0376(17) -0.0104(19) C28 0.0593(19) 0.077(2) 0.059(2) -0.0089(17) 0.0385(17) 0.0038(17) C29 0.0503(16) 0.062(2) 0.0452(16) 0.0007(13) 0.0261(14) 0.0075(14) C30 0.063(2) 0.085(3) 0.068(2) 0.011(2) 0.0310(18) 0.000(2) Cl2 0.119(8) 0.194(14) 0.133(10) -0.022(8) 0.034(6) -0.084(8) Cl3 0.143(12) 0.095(5) 0.115(11) 0.040(6) 0.022(7) 0.035(6) Cl4 0.263(17) 0.123(10) 0.237(15) -0.011(9) 0.214(14) -0.001(9) Cl2' 0.047(4) 0.114(6) 0.072(4) -0.002(4) 0.006(3) 0.013(4) Cl3' 0.089(6) 0.142(10) 0.081(6) 0.005(6) 0.003(5) 0.017(5) Cl4' 0.090(7) 0.081(4) 0.098(7) -0.010(5) 0.051(6) 0.001(4) Cl2" 0.056(4) 0.136(10) 0.068(3) 0.019(5) 0.010(3) 0.018(4) Cl3" 0.074(4) 0.134(9) 0.074(5) 0.038(6) 0.012(4) -0.005(4) Cl4" 0.091(8) 0.153(12) 0.112(8) 0.018(6) 0.047(6) 0.030(7) _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 C1 2.025(2) . ? Pd1 N1 2.103(2) . ? Pd1 P1 2.2625(8) . ? Pd1 Cl1 2.3892(8) . ? C1 C2 1.390(3) . ? C1 C6 1.406(4) . ? C2 C3 1.393(4) . ? C2 H2A 0.9300 . ? C3 O1 1.367(3) . ? C3 C4 1.399(4) . ? O1 C9 1.416(4) . ? C8 O2 1.429(4) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C4 C5 1.371(4) . ? C4 O2 1.373(3) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C5 C6 1.394(4) . ? C5 H5A 0.9300 . ? C6 C7 1.445(3) . ? C7 N1 1.275(3) . ? C7 H7A 0.9300 . ? N1 C10 1.467(3) . ? C10 C11 1.496(4) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 O3 1.409(4) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? O3 H3A 0.8200 . ? P1 C24 1.822(3) . ? P1 C18 1.823(3) . ? P1 C12 1.825(3) . ? C12 C17 1.380(4) . ? C12 C13 1.398(4) . ? C13 C14 1.386(5) . ? C13 H13A 0.9300 . ? C14 C15 1.363(6) . ? C14 H14A 0.9300 . ? C15 C16 1.375(5) . ? C15 H15A 0.9300 . ? C16 C17 1.391(4) . ? C16 H16A 0.9300 . ? C17 H17A 0.9300 . ? C18 C23 1.389(4) . ? C18 C19 1.390(4) . ? C19 C20 1.384(4) . ? C19 H19A 0.9300 . ? C20 C21 1.368(5) . ? C20 H20A 0.9300 . ? C21 C22 1.360(5) . ? C21 H21A 0.9300 . ? C22 C23 1.398(4) . ? C22 H22A 0.9300 . ? C23 H23A 0.9300 . ? C24 C29 1.384(4) . ? C24 C25 1.384(4) . ? C25 C26 1.387(4) . ? C25 H25A 0.9300 . ? C26 C27 1.355(5) . ? C26 H26A 0.9300 . ? C27 C28 1.373(5) . ? C27 H27A 0.9300 . ? C28 C29 1.386(4) . ? C28 H28A 0.9300 . ? C29 H29A 0.9300 . ? C30 Cl3' 1.677(10) . ? C30 Cl2' 1.712(9) . ? C30 Cl4" 1.732(11) . ? C30 Cl3" 1.736(10) . ? C30 Cl4' 1.747(9) . ? C30 Cl3 1.751(11) . ? C30 Cl4 1.755(11) . ? C30 Cl2 1.773(11) . ? C30 Cl2" 1.780(10) . ? Cl2' Cl2" 0.515(11) . ? Cl3' Cl3" 0.54(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pd1 N1 81.53(9) . . ? C1 Pd1 P1 95.01(7) . . ? N1 Pd1 P1 174.34(6) . . ? C1 Pd1 Cl1 166.81(7) . . ? N1 Pd1 Cl1 91.27(6) . . ? P1 Pd1 Cl1 92.98(3) . . ? C2 C1 C6 116.5(2) . . ? C2 C1 Pd1 132.32(19) . . ? C6 C1 Pd1 110.70(17) . . ? C1 C2 C3 121.9(2) . . ? C1 C2 H2A 119.0 . . ? C3 C2 H2A 119.0 . . ? O1 C3 C2 124.8(2) . . ? O1 C3 C4 115.0(2) . . ? C2 C3 C4 120.2(2) . . ? C3 O1 C9 117.4(2) . . ? O2 C8 H8A 109.5 . . ? O2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? O2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C5 C4 O2 125.0(3) . . ? C5 C4 C3 119.1(2) . . ? O2 C4 C3 116.0(2) . . ? C4 O2 C8 115.9(2) . . ? O1 C9 H9A 109.5 . . ? O1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? O1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C4 C5 C6 120.3(3) . . ? C4 C5 H5A 119.8 . . ? C6 C5 H5A 119.8 . . ? C5 C6 C1 122.0(2) . . ? C5 C6 C7 121.2(2) . . ? C1 C6 C7 116.8(2) . . ? N1 C7 C6 118.8(2) . . ? N1 C7 H7A 120.6 . . ? C6 C7 H7A 120.6 . . ? C7 N1 C10 119.3(2) . . ? C7 N1 Pd1 112.02(17) . . ? C10 N1 Pd1 128.69(18) . . ? N1 C10 C11 111.5(2) . . ? N1 C10 H10A 109.3 . . ? C11 C10 H10A 109.3 . . ? N1 C10 H10B 109.3 . . ? C11 C10 H10B 109.3 . . ? H10A C10 H10B 108.0 . . ? O3 C11 C10 110.2(3) . . ? O3 C11 H11A 109.6 . . ? C10 C11 H11A 109.6 . . ? O3 C11 H11B 109.6 . . ? C10 C11 H11B 109.6 . . ? H11A C11 H11B 108.1 . . ? C11 O3 H3A 109.5 . . ? C24 P1 C18 103.81(12) . . ? C24 P1 C12 107.04(12) . . ? C18 P1 C12 103.45(12) . . ? C24 P1 Pd1 113.21(9) . . ? C18 P1 Pd1 113.39(9) . . ? C12 P1 Pd1 114.88(10) . . ? C17 C12 C13 119.1(3) . . ? C17 C12 P1 120.3(2) . . ? C13 C12 P1 120.6(2) . . ? C14 C13 C12 119.8(3) . . ? C14 C13 H13A 120.1 . . ? C12 C13 H13A 120.1 . . ? C15 C14 C13 120.4(3) . . ? C15 C14 H14A 119.8 . . ? C13 C14 H14A 119.8 . . ? C14 C15 C16 120.7(3) . . ? C14 C15 H15A 119.7 . . ? C16 C15 H15A 119.7 . . ? C15 C16 C17 119.6(4) . . ? C15 C16 H16A 120.2 . . ? C17 C16 H16A 120.2 . . ? C12 C17 C16 120.4(3) . . ? C12 C17 H17A 119.8 . . ? C16 C17 H17A 119.8 . . ? C23 C18 C19 118.6(3) . . ? C23 C18 P1 120.1(2) . . ? C19 C18 P1 121.0(2) . . ? C20 C19 C18 120.5(3) . . ? C20 C19 H19A 119.8 . . ? C18 C19 H19A 119.8 . . ? C21 C20 C19 120.0(3) . . ? C21 C20 H20A 120.0 . . ? C19 C20 H20A 120.0 . . ? C22 C21 C20 120.8(3) . . ? C22 C21 H21A 119.6 . . ? C20 C21 H21A 119.6 . . ? C21 C22 C23 119.9(3) . . ? C21 C22 H22A 120.0 . . ? C23 C22 H22A 120.0 . . ? C18 C23 C22 120.2(3) . . ? C18 C23 H23A 119.9 . . ? C22 C23 H23A 119.9 . . ? C29 C24 C25 118.6(2) . . ? C29 C24 P1 123.9(2) . . ? C25 C24 P1 117.5(2) . . ? C24 C25 C26 120.5(3) . . ? C24 C25 H25A 119.7 . . ? C26 C25 H25A 119.7 . . ? C27 C26 C25 120.3(3) . . ? C27 C26 H26A 119.9 . . ? C25 C26 H26A 119.9 . . ? C26 C27 C28 120.2(3) . . ? C26 C27 H27A 119.9 . . ? C28 C27 H27A 119.9 . . ? C27 C28 C29 120.2(3) . . ? C27 C28 H28A 119.9 . . ? C29 C28 H28A 119.9 . . ? C24 C29 C28 120.2(3) . . ? C24 C29 H29A 119.9 . . ? C28 C29 H29A 119.9 . . ? Cl3' C30 Cl2' 119.9(8) . . ? Cl3' C30 Cl4" 125.7(11) . . ? Cl2' C30 Cl4" 94.8(6) . . ? Cl3' C30 Cl3" 18.0(8) . . ? Cl2' C30 Cl3" 122.2(8) . . ? Cl4" C30 Cl3" 108.6(9) . . ? Cl3' C30 Cl4' 117.0(9) . . ? Cl2' C30 Cl4' 109.6(6) . . ? Cl4" C30 Cl4' 15.2(6) . . ? Cl3" C30 Cl4' 101.8(10) . . ? Cl3' C30 Cl3 13.5(19) . . ? Cl2' C30 Cl3 114.7(9) . . ? Cl4" C30 Cl3 116.8(14) . . ? Cl3" C30 Cl3 9.7(14) . . ? Cl4' C30 Cl3 111.1(12) . . ? Cl3' C30 Cl4 111.8(12) . . ? Cl2' C30 Cl4 105.3(9) . . ? Cl4" C30 Cl4 14.0(12) . . ? Cl3" C30 Cl4 95.0(11) . . ? Cl4' C30 Cl4 12.8(9) . . ? Cl3 C30 Cl4 103.5(11) . . ? Cl3' C30 Cl2 108.4(11) . . ? Cl2' C30 Cl2 12.2(11) . . ? Cl4" C30 Cl2 100.0(10) . . ? Cl3" C30 Cl2 110.0(10) . . ? Cl4' C30 Cl2 115.1(9) . . ? Cl3 C30 Cl2 102.5(9) . . ? Cl4 C30 Cl2 108.4(9) . . ? Cl3' C30 Cl2" 103.4(8) . . ? Cl2' C30 Cl2" 16.8(3) . . ? Cl4" C30 Cl2" 108.8(6) . . ? Cl3" C30 Cl2" 107.6(8) . . ? Cl4' C30 Cl2" 123.9(6) . . ? Cl3 C30 Cl2" 99.2(8) . . ? Cl4 C30 Cl2" 117.3(10) . . ? Cl2 C30 Cl2" 8.9(11) . . ? Cl2" Cl2' C30 89.1(16) . . ? Cl3" Cl3' C30 87.2(19) . . ? Cl2' Cl2" C30 74.1(17) . . ? Cl3' Cl3" C30 74.9(16) . . ? _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.954 _refine_diff_density_max 0.500 _refine_diff_density_min -0.513 _refine_diff_density_rms 0.068 ###################END OF CIF CORRESPONDING TO COMPOUND 4#################### ############################################################################# ##################BEGIN OF CIF CORRESPONDING TO COMPOUND 7################### data_cad6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H29 Cl N O7 P Pd' _chemical_formula_weight 676.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 23.732(2) _cell_length_b 8.039(2) _cell_length_c 14.922(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2846.8(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.578 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1376 _exptl_absorpt_coefficient_mu 0.850 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.822 _exptl_absorpt_correction_T_max 0.905 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2606 _diffrn_reflns_av_R_equivalents 0.0436 _diffrn_reflns_av_sigmaI/netI 0.1133 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 24.96 _reflns_number_total 2600 _reflns_number_gt 1683 _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 w=1/[\s^2^(Fo^2^)+(0.0394P)^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 -0.02(7) _refine_ls_number_reflns 2600 _refine_ls_number_parameters 363 _refine_ls_number_restraints 22 _refine_ls_R_factor_all 0.0927 _refine_ls_R_factor_gt 0.0506 _refine_ls_wR_factor_ref 0.1170 _refine_ls_wR_factor_gt 0.1054 _refine_ls_goodness_of_fit_ref 0.963 _refine_ls_restrained_S_all 0.962 _refine_ls_shift/su_max 0.028 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.07044(3) 0.40306(9) 0.71534(8) 0.0401(2) Uani 1 d . . . C1 C 0.0678(5) 0.3246(18) 0.8426(8) 0.049(3) Uani 1 d . . . C2 C 0.0142(5) 0.2464(15) 0.8584(9) 0.047(3) Uani 1 d . . . C3 C 0.0011(5) 0.1817(17) 0.9443(10) 0.059(4) Uani 1 d . . . H3 H -0.0334 0.1304 0.9553 0.071 Uiso 1 calc R . . C4 C 0.0413(6) 0.1975(18) 1.0115(9) 0.059(4) Uani 1 d . . . C5 C 0.0938(7) 0.268(2) 0.9949(9) 0.058(4) Uani 1 d . . . C6 C 0.1052(5) 0.3320(16) 0.9097(7) 0.045(3) Uani 1 d . . . H6 H 0.1400 0.3811 0.8992 0.054 Uiso 1 calc R . . O2 O 0.0336(4) 0.1291(17) 1.0954(8) 0.095(4) Uani 1 d . . . C7 C -0.0124(7) 0.139(3) 1.1393(11) 0.123(8) Uani 1 d . . . H7A H -0.0195 0.2529 1.1547 0.148 Uiso 1 calc R . . H7B H -0.0095 0.0737 1.1930 0.148 Uiso 1 calc R . . H7C H -0.0428 0.0975 1.1031 0.148 Uiso 1 calc R . . O3 O 0.1307(5) 0.2752(15) 1.0657(7) 0.070(3) Uani 1 d . . . C8 C 0.1810(6) 0.3569(18) 1.0548(9) 0.066(4) Uani 1 d . . . H8A H 0.2038 0.2979 1.0122 0.079 Uiso 1 calc R . . H8B H 0.2003 0.3623 1.1112 0.079 Uiso 1 calc R . . H8C H 0.1740 0.4675 1.0333 0.079 Uiso 1 calc R . . C9 C -0.0262(5) 0.2475(18) 0.7865(10) 0.053(4) Uani 1 d . . . H9 H -0.0630 0.2098 0.7935 0.064 Uiso 1 calc R . . N1 N -0.0076(3) 0.3042(12) 0.7120(10) 0.055(3) Uani 1 d . . . C10 C -0.0408(6) 0.333(2) 0.6295(11) 0.077(5) Uani 1 d . . . H10A H -0.0670 0.2420 0.6206 0.093 Uiso 1 calc R . . H10B H -0.0624 0.4349 0.6356 0.093 Uiso 1 calc R . . C11 C -0.0033(7) 0.346(3) 0.5519(11) 0.108(7) Uani 1 d . . . H11A H 0.0091 0.2359 0.5340 0.130 Uiso 1 calc R . . H11B H -0.0234 0.3955 0.5020 0.130 Uiso 1 calc R . . O1 O 0.0450(3) 0.4471(11) 0.5744(6) 0.057(2) Uani 1 d . . . H1 H 0.0659 0.4541 0.5308 0.068 Uiso 1 calc R . . P1 P 0.15451(10) 0.5347(3) 0.7262(3) 0.0359(7) Uani 1 d . . . C12 C 0.1624(8) 0.670(2) 0.8227(11) 0.055(5) Uani 1 d . . . C13 C 0.1127(6) 0.7488(14) 0.8514(9) 0.055(3) Uani 1 d . . . H13 H 0.0787 0.7269 0.8229 0.066 Uiso 1 calc R . . C14 C 0.1148(8) 0.8612(17) 0.9233(10) 0.075(5) Uani 1 d . . . H14 H 0.0822 0.9152 0.9420 0.090 Uiso 1 calc R . . C15 C 0.1648(11) 0.891(3) 0.9657(12) 0.094(8) Uani 1 d . . . H15 H 0.1663 0.9635 1.0143 0.113 Uiso 1 calc R . . C16 C 0.2126(9) 0.814(2) 0.9364(11) 0.085(5) Uani 1 d . . . H16 H 0.2470 0.8368 0.9638 0.103 Uiso 1 calc R . . C17 C 0.2102(6) 0.6998(16) 0.8652(10) 0.060(4) Uani 1 d . . . H17 H 0.2428 0.6444 0.8476 0.072 Uiso 1 calc R . . C18 C 0.2161(4) 0.4030(12) 0.7276(10) 0.035(3) Uani 1 d . . . C19 C 0.2123(5) 0.2374(14) 0.7474(7) 0.047(3) Uani 1 d . . . H19 H 0.1772 0.1912 0.7603 0.056 Uiso 1 calc R . . C20 C 0.2596(5) 0.1381(17) 0.7486(9) 0.063(4) Uani 1 d . . . H20 H 0.2562 0.0262 0.7633 0.076 Uiso 1 calc R . . C21 C 0.3110(5) 0.2013(16) 0.7288(13) 0.057(4) Uani 1 d . . . H21 H 0.3421 0.1313 0.7261 0.068 Uiso 1 calc R . . C22 C 0.3173(4) 0.3687(16) 0.7126(15) 0.064(4) Uani 1 d . . . H22 H 0.3530 0.4160 0.7092 0.077 Uiso 1 calc R . . C23 C 0.2693(4) 0.4661(14) 0.7015(10) 0.044(3) Uani 1 d . . . H23 H 0.2722 0.5722 0.6770 0.053 Uiso 1 calc R . . C24 C 0.1626(6) 0.670(2) 0.6297(9) 0.038(4) Uani 1 d . . . C25 C 0.1624(5) 0.8420(18) 0.6373(10) 0.059(4) Uani 1 d . . . H25 H 0.1611 0.8918 0.6935 0.071 Uiso 1 calc R . . C26 C 0.1644(7) 0.940(2) 0.5599(12) 0.078(5) Uani 1 d . . . H26 H 0.1630 1.0555 0.5654 0.093 Uiso 1 calc R . . C27 C 0.1682(9) 0.875(3) 0.4806(15) 0.083(7) Uani 1 d . . . H27 H 0.1692 0.9436 0.4304 0.100 Uiso 1 calc R . . C28 C 0.1707(6) 0.698(2) 0.4702(9) 0.071(5) Uani 1 d . . . H28 H 0.1742 0.6502 0.4137 0.086 Uiso 1 calc R . . C29 C 0.1678(5) 0.5991(18) 0.5472(9) 0.057(4) Uani 1 d . . . H29 H 0.1695 0.4839 0.5420 0.068 Uiso 1 calc R . . Cl1 Cl 0.1004(2) 0.2772(6) 0.3545(3) 0.0772(12) Uani 1 d D . . O4 O 0.0653(8) 0.398(2) 0.3357(16) 0.252(12) Uani 1 d D . . O5 O 0.0789(8) 0.1302(15) 0.3345(13) 0.181(9) Uani 1 d D . . O6 O 0.1140(8) 0.280(2) 0.4413(9) 0.170(8) Uani 1 d D . . O7 O 0.1456(8) 0.298(3) 0.3025(13) 0.257(13) Uani 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0311(3) 0.0463(4) 0.0428(4) -0.0010(9) -0.0016(7) -0.0017(4) C1 0.045(7) 0.066(8) 0.036(7) -0.010(6) 0.000(7) -0.003(7) C2 0.040(7) 0.038(7) 0.064(8) -0.002(7) 0.014(7) 0.006(6) C3 0.049(7) 0.056(9) 0.073(9) 0.025(8) 0.023(7) 0.016(7) C4 0.053(8) 0.074(10) 0.050(9) 0.013(8) 0.012(8) 0.011(8) C5 0.067(9) 0.059(10) 0.050(9) 0.006(8) -0.002(7) 0.029(8) C6 0.039(6) 0.061(8) 0.036(7) -0.002(6) 0.001(6) -0.009(6) O2 0.056(6) 0.147(11) 0.083(8) 0.055(8) 0.025(6) 0.009(7) C7 0.114(15) 0.18(2) 0.080(12) 0.059(14) 0.031(12) 0.082(15) O3 0.082(8) 0.083(8) 0.044(6) -0.004(6) -0.012(6) 0.008(7) C8 0.069(9) 0.074(11) 0.055(9) 0.019(8) -0.026(7) 0.001(8) C9 0.028(6) 0.063(10) 0.068(10) -0.008(9) -0.017(7) 0.005(7) N1 0.036(5) 0.073(7) 0.058(6) -0.006(10) -0.030(8) -0.002(5) C10 0.053(9) 0.110(15) 0.068(10) -0.010(10) -0.010(9) -0.019(10) C11 0.078(12) 0.165(19) 0.081(13) 0.045(13) -0.031(10) -0.075(13) O1 0.046(5) 0.081(7) 0.043(5) 0.002(5) -0.013(4) -0.014(5) P1 0.0326(12) 0.0403(14) 0.0350(18) 0.001(2) -0.0001(18) -0.0011(10) C12 0.068(12) 0.043(11) 0.054(10) -0.011(9) -0.004(9) -0.009(10) C13 0.071(9) 0.047(8) 0.047(7) 0.000(7) 0.007(7) 0.012(7) C14 0.114(14) 0.048(9) 0.065(10) -0.024(8) 0.012(10) -0.004(9) C15 0.16(2) 0.075(16) 0.042(10) -0.008(10) -0.019(13) 0.003(16) C16 0.128(16) 0.068(12) 0.061(10) 0.001(9) -0.019(11) -0.016(12) C17 0.079(10) 0.043(8) 0.059(9) 0.009(8) -0.014(8) 0.015(8) C18 0.037(5) 0.038(5) 0.031(8) 0.003(8) -0.007(6) -0.001(5) C19 0.044(6) 0.043(7) 0.054(8) -0.010(6) -0.005(5) 0.000(6) C20 0.053(8) 0.061(9) 0.074(11) -0.010(7) 0.003(7) -0.007(7) C21 0.046(6) 0.067(8) 0.058(11) -0.012(10) -0.007(8) 0.026(6) C22 0.029(5) 0.084(10) 0.079(9) -0.025(15) -0.024(11) 0.010(6) C23 0.037(5) 0.044(6) 0.052(10) 0.008(7) 0.006(6) -0.006(5) C24 0.030(8) 0.045(10) 0.040(8) 0.002(7) -0.001(6) -0.003(8) C25 0.048(8) 0.069(10) 0.060(9) 0.014(8) -0.016(7) -0.001(7) C26 0.092(12) 0.070(12) 0.071(11) 0.018(10) -0.010(10) -0.012(9) C27 0.096(15) 0.073(16) 0.081(15) 0.039(13) -0.026(12) -0.029(13) C28 0.057(8) 0.127(15) 0.031(7) 0.019(9) 0.003(6) -0.015(10) C29 0.049(7) 0.060(9) 0.062(9) -0.019(9) -0.013(7) 0.006(7) Cl1 0.099(3) 0.061(3) 0.071(3) -0.009(2) 0.002(3) 0.012(3) O4 0.30(3) 0.21(2) 0.25(3) 0.00(2) -0.04(2) 0.18(2) O5 0.28(2) 0.082(10) 0.178(18) 0.018(11) -0.056(16) -0.077(13) O6 0.28(2) 0.117(15) 0.117(14) -0.006(13) -0.036(16) -0.002(16) O7 0.23(2) 0.36(3) 0.18(2) -0.02(2) 0.086(19) -0.13(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 C1 2.002(12) . ? Pd1 N1 2.015(8) . ? Pd1 O1 2.216(8) . ? Pd1 P1 2.264(3) . ? C1 C6 1.339(16) . ? C1 C2 1.438(16) . ? C2 C3 1.418(18) . ? C2 C9 1.439(17) . ? C3 C4 1.391(19) . ? C3 H3 0.9300 . ? C4 O2 1.380(17) . ? C4 C5 1.39(2) . ? C5 O3 1.374(17) . ? C5 C6 1.397(18) . ? C6 H6 0.9300 . ? O2 C7 1.275(17) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? O3 C8 1.370(16) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 N1 1.279(17) . ? C9 H9 0.9300 . ? N1 C10 1.480(19) . ? C10 C11 1.46(2) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 O1 1.445(15) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? O1 H1 0.8200 . ? P1 C18 1.806(10) . ? P1 C12 1.812(16) . ? P1 C24 1.815(16) . ? C12 C17 1.32(2) . ? C12 C13 1.41(2) . ? C13 C14 1.404(17) . ? C13 H13 0.9300 . ? C14 C15 1.37(2) . ? C14 H14 0.9300 . ? C15 C16 1.36(3) . ? C15 H15 0.9300 . ? C16 C17 1.41(2) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C19 1.367(14) . ? C18 C23 1.415(14) . ? C19 C20 1.378(16) . ? C19 H19 0.9300 . ? C20 C21 1.353(16) . ? C20 H20 0.9300 . ? C21 C22 1.375(17) . ? C21 H21 0.9300 . ? C22 C23 1.391(14) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 C29 1.364(19) . ? C24 C25 1.39(2) . ? C25 C26 1.40(2) . ? C25 H25 0.9300 . ? C26 C27 1.30(2) . ? C26 H26 0.9300 . ? C27 C28 1.43(3) . ? C27 H27 0.9300 . ? C28 C29 1.399(19) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? Cl1 O4 1.310(12) . ? Cl1 O5 1.322(11) . ? Cl1 O6 1.334(12) . ? Cl1 O7 1.336(13) . ? 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 C1 Pd1 N1 82.6(5) . . ? C1 Pd1 O1 160.4(4) . . ? N1 Pd1 O1 77.9(5) . . ? C1 Pd1 P1 96.1(4) . . ? N1 Pd1 P1 174.6(3) . . ? O1 Pd1 P1 103.5(2) . . ? C6 C1 C2 118.9(12) . . ? C6 C1 Pd1 132.4(10) . . ? C2 C1 Pd1 108.7(9) . . ? C3 C2 C1 120.2(12) . . ? C3 C2 C9 122.0(12) . . ? C1 C2 C9 117.7(12) . . ? C4 C3 C2 117.9(12) . . ? C4 C3 H3 121.1 . . ? C2 C3 H3 121.1 . . ? O2 C4 C3 121.8(13) . . ? O2 C4 C5 116.3(13) . . ? C3 C4 C5 121.6(12) . . ? O3 C5 C4 116.8(13) . . ? O3 C5 C6 124.2(15) . . ? C4 C5 C6 119.0(13) . . ? C1 C6 C5 122.4(12) . . ? C1 C6 H6 118.8 . . ? C5 C6 H6 118.8 . . ? C7 O2 C4 123.7(13) . . ? O2 C7 H7A 109.5 . . ? O2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? O2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C8 O3 C5 118.8(12) . . ? O3 C8 H8A 109.5 . . ? O3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? O3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N1 C9 C2 114.9(12) . . ? N1 C9 H9 122.6 . . ? C2 C9 H9 122.6 . . ? C9 N1 C10 126.5(9) . . ? C9 N1 Pd1 115.8(9) . . ? C10 N1 Pd1 116.6(10) . . ? C11 C10 N1 110.2(12) . . ? C11 C10 H10A 109.6 . . ? N1 C10 H10A 109.6 . . ? C11 C10 H10B 109.6 . . ? N1 C10 H10B 109.6 . . ? H10A C10 H10B 108.1 . . ? O1 C11 C10 109.8(14) . . ? O1 C11 H11A 109.7 . . ? C10 C11 H11A 109.7 . . ? O1 C11 H11B 109.7 . . ? C10 C11 H11B 109.7 . . ? H11A C11 H11B 108.2 . . ? C11 O1 Pd1 110.3(8) . . ? C11 O1 H1 109.5 . . ? Pd1 O1 H1 126.9 . . ? C18 P1 C12 105.0(8) . . ? C18 P1 C24 106.0(6) . . ? C12 P1 C24 105.0(6) . . ? C18 P1 Pd1 116.1(3) . . ? C12 P1 Pd1 115.3(6) . . ? C24 P1 Pd1 108.5(5) . . ? C17 C12 C13 119.3(15) . . ? C17 C12 P1 125.4(14) . . ? C13 C12 P1 115.3(13) . . ? C14 C13 C12 119.7(15) . . ? C14 C13 H13 120.2 . . ? C12 C13 H13 120.2 . . ? C15 C14 C13 119.8(17) . . ? C15 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? C16 C15 C14 119.6(18) . . ? C16 C15 H15 120.2 . . ? C14 C15 H15 120.2 . . ? C15 C16 C17 120.3(18) . . ? C15 C16 H16 119.8 . . ? C17 C16 H16 119.8 . . ? C12 C17 C16 121.2(16) . . ? C12 C17 H17 119.4 . . ? C16 C17 H17 119.4 . . ? C19 C18 C23 118.0(10) . . ? C19 C18 P1 121.2(8) . . ? C23 C18 P1 120.6(8) . . ? C18 C19 C20 120.8(11) . . ? C18 C19 H19 119.6 . . ? C20 C19 H19 119.6 . . ? C21 C20 C19 120.9(12) . . ? C21 C20 H20 119.5 . . ? C19 C20 H20 119.5 . . ? C20 C21 C22 120.2(11) . . ? C20 C21 H21 119.9 . . ? C22 C21 H21 119.9 . . ? C21 C22 C23 118.9(10) . . ? C21 C22 H22 120.6 . . ? C23 C22 H22 120.6 . . ? C22 C23 C18 119.7(11) . . ? C22 C23 H23 120.2 . . ? C18 C23 H23 120.2 . . ? C29 C24 C25 119.5(15) . . ? C29 C24 P1 118.3(13) . . ? C25 C24 P1 122.2(12) . . ? C24 C25 C26 119.7(15) . . ? C24 C25 H25 120.2 . . ? C26 C25 H25 120.2 . . ? C27 C26 C25 121.8(17) . . ? C27 C26 H26 119.1 . . ? C25 C26 H26 119.1 . . ? C26 C27 C28 120.2(18) . . ? C26 C27 H27 119.9 . . ? C28 C27 H27 119.9 . . ? C29 C28 C27 118.3(15) . . ? C29 C28 H28 120.9 . . ? C27 C28 H28 120.9 . . ? C24 C29 C28 120.5(14) . . ? C24 C29 H29 119.8 . . ? C28 C29 H29 119.8 . . ? O4 Cl1 O5 111.7(12) . . ? O4 Cl1 O6 110.3(12) . . ? O5 Cl1 O6 109.3(11) . . ? O4 Cl1 O7 107.0(13) . . ? O5 Cl1 O7 107.0(12) . . ? O6 Cl1 O7 111.5(13) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Pd1 C1 C6 179.4(14) . . . . ? O1 Pd1 C1 C6 176.0(10) . . . . ? P1 Pd1 C1 C6 -5.9(14) . . . . ? N1 Pd1 C1 C2 -0.1(9) . . . . ? O1 Pd1 C1 C2 -3(2) . . . . ? P1 Pd1 C1 C2 174.6(8) . . . . ? C6 C1 C2 C3 1.4(19) . . . . ? Pd1 C1 C2 C3 -179.0(9) . . . . ? C6 C1 C2 C9 177.0(12) . . . . ? Pd1 C1 C2 C9 -3.4(15) . . . . ? C1 C2 C3 C4 0.3(19) . . . . ? C9 C2 C3 C4 -175.2(13) . . . . ? C2 C3 C4 O2 -175.9(13) . . . . ? C2 C3 C4 C5 -2(2) . . . . ? O2 C4 C5 O3 -5(2) . . . . ? C3 C4 C5 O3 -178.9(14) . . . . ? O2 C4 C5 C6 176.7(14) . . . . ? C3 C4 C5 C6 3(2) . . . . ? C2 C1 C6 C5 -1(2) . . . . ? Pd1 C1 C6 C5 179.6(11) . . . . ? O3 C5 C6 C1 -179.2(14) . . . . ? C4 C5 C6 C1 -1(2) . . . . ? C3 C4 O2 C7 -44(3) . . . . ? C5 C4 O2 C7 141.8(19) . . . . ? C4 C5 O3 C8 -174.4(13) . . . . ? C6 C5 O3 C8 4(2) . . . . ? C3 C2 C9 N1 -177.6(12) . . . . ? C1 C2 C9 N1 6.9(18) . . . . ? C2 C9 N1 C10 -174.4(12) . . . . ? C2 C9 N1 Pd1 -6.8(16) . . . . ? C1 Pd1 N1 C9 4.0(10) . . . . ? O1 Pd1 N1 C9 -177.2(10) . . . . ? P1 Pd1 N1 C9 -72(5) . . . . ? C1 Pd1 N1 C10 172.9(11) . . . . ? O1 Pd1 N1 C10 -8.3(10) . . . . ? P1 Pd1 N1 C10 97(5) . . . . ? C9 N1 C10 C11 -161.7(15) . . . . ? Pd1 N1 C10 C11 30.7(19) . . . . ? N1 C10 C11 O1 -43(2) . . . . ? C10 C11 O1 Pd1 36.1(19) . . . . ? C1 Pd1 O1 C11 -12(2) . . . . ? N1 Pd1 O1 C11 -15.5(11) . . . . ? P1 Pd1 O1 C11 169.8(11) . . . . ? C1 Pd1 P1 C18 75.9(7) . . . . ? N1 Pd1 P1 C18 152(4) . . . . ? O1 Pd1 P1 C18 -104.7(6) . . . . ? C1 Pd1 P1 C12 -47.5(8) . . . . ? N1 Pd1 P1 C12 28(5) . . . . ? O1 Pd1 P1 C12 131.8(7) . . . . ? C1 Pd1 P1 C24 -164.9(7) . . . . ? N1 Pd1 P1 C24 -89(5) . . . . ? O1 Pd1 P1 C24 14.4(6) . . . . ? C18 P1 C12 C17 19.4(18) . . . . ? C24 P1 C12 C17 -92.2(16) . . . . ? Pd1 P1 C12 C17 148.5(14) . . . . ? C18 P1 C12 C13 -161.9(12) . . . . ? C24 P1 C12 C13 86.5(13) . . . . ? Pd1 P1 C12 C13 -32.8(15) . . . . ? C17 C12 C13 C14 1(2) . . . . ? P1 C12 C13 C14 -177.4(11) . . . . ? C12 C13 C14 C15 -1(2) . . . . ? C13 C14 C15 C16 1(3) . . . . ? C14 C15 C16 C17 -2(3) . . . . ? C13 C12 C17 C16 -2(2) . . . . ? P1 C12 C17 C16 176.4(12) . . . . ? C15 C16 C17 C12 3(3) . . . . ? C12 P1 C18 C19 110.1(13) . . . . ? C24 P1 C18 C19 -139.0(12) . . . . ? Pd1 P1 C18 C19 -18.5(14) . . . . ? C12 P1 C18 C23 -74.7(14) . . . . ? C24 P1 C18 C23 36.2(14) . . . . ? Pd1 P1 C18 C23 156.7(10) . . . . ? C23 C18 C19 C20 5(2) . . . . ? P1 C18 C19 C20 -179.7(10) . . . . ? C18 C19 C20 C21 -1(2) . . . . ? C19 C20 C21 C22 4(3) . . . . ? C20 C21 C22 C23 -11(3) . . . . ? C21 C22 C23 C18 15(3) . . . . ? C19 C18 C23 C22 -12(2) . . . . ? P1 C18 C23 C22 172.7(13) . . . . ? C18 P1 C24 C29 58.6(13) . . . . ? C12 P1 C24 C29 169.5(15) . . . . ? Pd1 P1 C24 C29 -66.8(12) . . . . ? C18 P1 C24 C25 -122.6(13) . . . . ? C12 P1 C24 C25 -11.7(12) . . . . ? Pd1 P1 C24 C25 112.0(12) . . . . ? C29 C24 C25 C26 4(2) . . . . ? P1 C24 C25 C26 -175.0(11) . . . . ? C24 C25 C26 C27 -2(3) . . . . ? C25 C26 C27 C28 0(3) . . . . ? C26 C27 C28 C29 1(3) . . . . ? C25 C24 C29 C28 -3(2) . . . . ? P1 C24 C29 C28 176.1(10) . . . . ? C27 C28 C29 C24 0(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 O6 0.82 2.24 2.90(2) 137.5 . _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.96 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.434 _refine_diff_density_min -0.453 _refine_diff_density_rms 0.096 ######################END OF CIF CORRESPONDING TO COMPOUND 7#################