# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2003 data_global _journal_coden_Cambridge 440 loop_ _publ_author_name 'Jose Perez' _publ_contact_author_name 'Dr Jose Perez' _publ_contact_author_address ; Ingenieria Minera, Geologica y Cartografica Universidad Politecnica de Cartagena ETSII Campus Muralla del Mar Cartagena Murcia 30202 SPAIN ; _publ_contact_author_email JOSE.PPEREZ@UPCT.ES _publ_requested_journal 'New Journal of Chemistry' _publ_section_title ; Solid state conformational and theoretical study of complexes containing the (CxN)Pd moiety (CxN= phenylazophenyl and its derivatives). ; data_compound_1 _database_code_CSD 210648 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H25 F3 N3 O2 P Pd' _chemical_formula_weight 701.94 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' F F 0.0171 0.0103 '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 monoclinic _symmetry_space_group_name_H-M C2/c 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' '-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 32.628(7) _cell_length_b 11.079(3) _cell_length_c 17.333(4) _cell_angle_alpha 90.00 _cell_angle_beta 101.969(10) _cell_angle_gamma 90.00 _cell_volume 6129(3) _cell_formula_units_Z 8 _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 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.521 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2832 _exptl_absorpt_coefficient_mu 0.712 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 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 17757 _diffrn_reflns_av_R_equivalents 0.0500 _diffrn_reflns_av_sigmaI/netI 0.0779 _diffrn_reflns_limit_h_min -40 _diffrn_reflns_limit_h_max 44 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 29.16 _reflns_number_total 8114 _reflns_number_gt 4933 _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^)+(0.0634P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8114 _refine_ls_number_parameters 397 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0925 _refine_ls_R_factor_gt 0.0410 _refine_ls_wR_factor_ref 0.1213 _refine_ls_wR_factor_gt 0.0946 _refine_ls_goodness_of_fit_ref 0.921 _refine_ls_restrained_S_all 0.921 _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 0.149842(7) 0.63125(2) 0.008019(13) 0.04030(9) Uani 1 1 d . . . P1 P 0.10410(3) 0.57890(8) -0.10309(5) 0.0426(2) Uani 1 1 d . . . N2 N 0.20026(8) 0.6807(2) 0.09952(14) 0.0413(6) Uani 1 1 d . . . C1 C 0.19751(10) 0.5427(3) -0.02397(17) 0.0428(7) Uani 1 1 d . . . C29 C 0.12418(10) 0.6298(3) -0.18814(18) 0.0443(7) Uani 1 1 d . . . C17 C 0.05219(11) 0.6472(3) -0.11562(19) 0.0477(8) Uani 1 1 d . . . N1 N 0.23666(9) 0.6541(3) 0.08904(16) 0.0473(7) Uani 1 1 d . . . C7 C 0.19976(10) 0.7498(3) 0.16894(17) 0.0457(7) Uani 1 1 d . . . C30 C 0.14530(12) 0.7395(4) -0.1820(2) 0.0629(10) Uani 1 1 d . . . H30 H 0.1486 0.7838 -0.1355 0.076 Uiso 1 1 calc R . . C34 C 0.12087(12) 0.5646(3) -0.25718(19) 0.0547(9) Uani 1 1 d . . . H34 H 0.1071 0.4906 -0.2623 0.066 Uiso 1 1 calc R . . C6 C 0.23599(10) 0.5810(3) 0.02326(18) 0.0458(7) Uani 1 1 d . . . C5 C 0.27471(11) 0.5451(3) 0.0098(2) 0.0549(9) Uani 1 1 d . . . H5 H 0.2992 0.5753 0.0409 0.066 Uiso 1 1 calc R . . C22 C 0.04506(12) 0.7640(3) -0.1431(2) 0.0605(9) Uani 1 1 d . . . H22 H 0.0666 0.8064 -0.1586 0.073 Uiso 1 1 calc R . . C9 C 0.23005(16) 0.8921(4) 0.2667(3) 0.0821(13) Uani 1 1 d . . . H9 H 0.2514 0.9458 0.2874 0.099 Uiso 1 1 calc R . . C3 C 0.23957(12) 0.4207(4) -0.0945(2) 0.0617(10) Uani 1 1 d . . . H3 H 0.2405 0.3630 -0.1330 0.074 Uiso 1 1 calc R . . F3 F 0.17343(9) 0.7586(3) -0.37189(14) 0.1051(10) Uani 1 1 d . . . C12 C 0.16683(12) 0.7337(3) 0.2061(2) 0.0559(9) Uani 1 1 d . . . H12 H 0.1452 0.6807 0.1854 0.067 Uiso 1 1 calc R . . C2 C 0.20087(11) 0.4612(3) -0.0829(2) 0.0533(8) Uani 1 1 d . . . H2 H 0.1766 0.4327 -0.1158 0.064 Uiso 1 1 calc R . . F1 F -0.06274(8) 0.8068(3) -0.1324(2) 0.1081(10) Uani 1 1 d . . . C33 C 0.13760(14) 0.6076(4) -0.3185(2) 0.0671(11) Uani 1 1 d . . . H33 H 0.1355 0.5626 -0.3645 0.081 Uiso 1 1 calc R . . C20 C -0.02485(12) 0.7541(4) -0.1263(3) 0.0696(11) Uani 1 1 d . . . C8 C 0.23172(12) 0.8295(3) 0.1987(2) 0.0598(9) Uani 1 1 d . . . H8 H 0.2539 0.8406 0.1733 0.072 Uiso 1 1 calc R . . C18 C 0.01936(11) 0.5858(4) -0.0930(2) 0.0621(10) Uani 1 1 d . . . H18 H 0.0236 0.5077 -0.0733 0.075 Uiso 1 1 calc R . . C19 C -0.01945(13) 0.6391(4) -0.0993(3) 0.0742(12) Uani 1 1 d . . . H19 H -0.0415 0.5970 -0.0852 0.089 Uiso 1 1 calc R . . C32 C 0.15695(13) 0.7150(4) -0.3112(2) 0.0683(11) Uani 1 1 d . . . C21 C 0.00657(13) 0.8191(4) -0.1479(3) 0.0704(11) Uani 1 1 d . . . H21 H 0.0022 0.8983 -0.1654 0.084 Uiso 1 1 calc R . . C11 C 0.16605(15) 0.7971(4) 0.2747(2) 0.0733(12) Uani 1 1 d . . . H11 H 0.1441 0.7855 0.3006 0.088 Uiso 1 1 calc R . . C4 C 0.27655(12) 0.4646(4) -0.0497(2) 0.0625(10) Uani 1 1 d . . . H4 H 0.3022 0.4402 -0.0597 0.075 Uiso 1 1 calc R . . C31 C 0.16148(13) 0.7836(4) -0.2442(2) 0.0738(12) Uani 1 1 d . . . H31 H 0.1751 0.8578 -0.2406 0.089 Uiso 1 1 calc R . . C10 C 0.19739(18) 0.8764(4) 0.3045(3) 0.0866(15) Uani 1 1 d . . . H10 H 0.1966 0.9195 0.3502 0.104 Uiso 1 1 calc R . . N3 N 0.10568(8) 0.7454(2) 0.04176(15) 0.0452(6) Uani 1 1 d . . . O1 O 0.06818(9) 0.6188(3) 0.10495(18) 0.0789(9) Uani 1 1 d . . . F2 F 0.06156(10) 0.0603(2) -0.1401(2) 0.1208(11) Uani 1 1 d . . . O2 O 0.12823(9) 0.9141(3) -0.0136(2) 0.0793(8) Uani 1 1 d . . . C24 C 0.06283(11) 0.3764(3) -0.1809(2) 0.0580(9) Uani 1 1 d . . . H24 H 0.0499 0.4303 -0.2195 0.070 Uiso 1 1 calc R . . C23 C 0.09173(10) 0.4189(3) -0.11519(18) 0.0452(7) Uani 1 1 d . . . C16 C 0.10452(13) 0.8657(3) 0.0236(2) 0.0579(9) Uani 1 1 d . . . C13 C 0.07412(11) 0.7173(4) 0.0802(2) 0.0564(9) Uani 1 1 d . . . C28 C 0.10969(12) 0.3361(3) -0.0580(2) 0.0529(9) Uani 1 1 d . . . H28 H 0.1288 0.3628 -0.0139 0.063 Uiso 1 1 calc R . . C26 C 0.07149(15) 0.1788(4) -0.1307(3) 0.0735(12) Uani 1 1 d . . . C27 C 0.09970(13) 0.2150(4) -0.0654(3) 0.0699(11) Uani 1 1 d . . . H27 H 0.1118 0.1598 -0.0269 0.084 Uiso 1 1 calc R . . C25 C 0.05354(13) 0.2552(4) -0.1886(3) 0.0713(12) Uani 1 1 d . . . H25 H 0.0351 0.2263 -0.2331 0.086 Uiso 1 1 calc R . . C15 C 0.06987(15) 0.9288(4) 0.0525(3) 0.0823(13) Uani 1 1 d . . . H15A H 0.0507 0.9674 0.0093 0.099 Uiso 1 1 calc R . . H15B H 0.0810 0.9892 0.0918 0.099 Uiso 1 1 calc R . . C14 C 0.04840(16) 0.8293(5) 0.0879(3) 0.0851(14) Uani 1 1 d . . . H14A H 0.0197 0.8195 0.0593 0.102 Uiso 1 1 calc R . . H14B H 0.0483 0.8460 0.1428 0.102 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 0.03823(14) 0.04168(15) 0.03937(14) -0.00249(10) 0.00435(9) -0.00140(11) P1 0.0392(4) 0.0458(5) 0.0408(4) -0.0009(4) 0.0035(3) -0.0041(4) N2 0.0424(15) 0.0394(14) 0.0396(13) -0.0008(12) 0.0027(11) -0.0022(12) C1 0.0401(17) 0.0445(18) 0.0427(16) 0.0005(14) 0.0061(14) 0.0009(14) C29 0.0414(17) 0.0471(19) 0.0427(16) -0.0006(15) 0.0045(13) -0.0038(15) C17 0.0431(18) 0.050(2) 0.0473(18) -0.0014(15) 0.0034(14) -0.0026(15) N1 0.0426(16) 0.0507(17) 0.0462(15) 0.0018(13) 0.0034(12) -0.0034(13) C7 0.0512(19) 0.0419(18) 0.0400(16) -0.0023(14) 0.0006(14) 0.0027(15) C30 0.064(2) 0.068(3) 0.054(2) -0.0054(19) 0.0048(18) -0.028(2) C34 0.070(2) 0.047(2) 0.0474(19) 0.0028(16) 0.0133(17) -0.0068(18) C6 0.0485(19) 0.0462(18) 0.0409(16) 0.0027(15) 0.0052(14) -0.0006(15) C5 0.0416(19) 0.063(2) 0.058(2) 0.0034(19) 0.0065(16) -0.0004(17) C22 0.051(2) 0.050(2) 0.076(2) -0.0014(19) 0.0054(19) -0.0048(18) C9 0.085(3) 0.070(3) 0.082(3) -0.031(2) -0.002(3) -0.010(2) C3 0.057(2) 0.063(2) 0.067(2) -0.013(2) 0.0170(19) 0.002(2) F3 0.130(2) 0.123(2) 0.0720(15) 0.0197(16) 0.0414(16) -0.0420(19) C12 0.060(2) 0.059(2) 0.0470(18) -0.0017(17) 0.0075(17) -0.0013(18) C2 0.0432(19) 0.055(2) 0.060(2) -0.0110(18) 0.0077(16) -0.0036(16) F1 0.0518(15) 0.0794(18) 0.187(3) -0.0265(19) 0.0113(17) 0.0168(13) C33 0.091(3) 0.066(3) 0.047(2) 0.0010(18) 0.020(2) -0.011(2) C20 0.045(2) 0.060(3) 0.099(3) -0.019(2) 0.002(2) 0.0039(19) C8 0.061(2) 0.053(2) 0.062(2) -0.0098(18) 0.0038(18) -0.0069(19) C18 0.052(2) 0.060(2) 0.077(3) 0.008(2) 0.0203(19) 0.0028(19) C19 0.052(2) 0.069(3) 0.107(3) 0.001(2) 0.030(2) -0.004(2) C32 0.069(3) 0.079(3) 0.057(2) 0.015(2) 0.016(2) -0.014(2) C21 0.059(3) 0.045(2) 0.100(3) -0.006(2) 0.000(2) 0.005(2) C11 0.086(3) 0.087(3) 0.049(2) -0.003(2) 0.019(2) 0.014(3) C4 0.050(2) 0.072(3) 0.068(2) -0.006(2) 0.0184(19) 0.0064(19) C31 0.075(3) 0.071(3) 0.074(3) 0.006(2) 0.013(2) -0.034(2) C10 0.108(4) 0.086(3) 0.059(3) -0.030(2) 0.000(3) 0.021(3) N3 0.0441(15) 0.0439(16) 0.0469(14) -0.0018(12) 0.0082(12) 0.0006(12) O1 0.073(2) 0.077(2) 0.090(2) 0.0320(16) 0.0235(16) -0.0018(15) F2 0.135(3) 0.0609(17) 0.165(3) -0.0184(18) 0.028(2) -0.0473(17) O2 0.0695(19) 0.0580(17) 0.116(2) 0.0092(17) 0.0327(18) -0.0072(15) C24 0.048(2) 0.065(3) 0.058(2) -0.0057(18) 0.0041(17) -0.0109(18) C23 0.0457(18) 0.0459(18) 0.0449(17) -0.0027(15) 0.0112(15) -0.0086(15) C16 0.058(2) 0.051(2) 0.065(2) -0.0079(18) 0.0131(19) -0.0010(18) C13 0.051(2) 0.069(3) 0.0502(19) 0.0048(19) 0.0120(16) 0.0019(19) C28 0.056(2) 0.054(2) 0.0492(19) 0.0012(17) 0.0115(17) -0.0104(17) C26 0.075(3) 0.048(2) 0.102(3) -0.010(2) 0.030(3) -0.026(2) C27 0.077(3) 0.053(2) 0.082(3) 0.013(2) 0.020(2) -0.015(2) C25 0.058(2) 0.073(3) 0.081(3) -0.025(2) 0.011(2) -0.029(2) C15 0.098(4) 0.056(3) 0.102(3) -0.010(2) 0.040(3) 0.016(2) C14 0.089(3) 0.096(3) 0.084(3) 0.009(3) 0.047(3) 0.026(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 C1 2.012(3) . ? Pd1 N3 2.090(3) . ? Pd1 N2 2.107(3) . ? Pd1 P1 2.2540(9) . ? P1 C23 1.821(4) . ? P1 C29 1.822(3) . ? P1 C17 1.827(4) . ? N2 N1 1.273(4) . ? N2 C7 1.429(4) . ? C1 C2 1.385(4) . ? C1 C6 1.414(4) . ? C29 C34 1.382(4) . ? C29 C30 1.391(5) . ? C17 C22 1.382(5) . ? C17 C18 1.392(5) . ? N1 C6 1.395(4) . ? C7 C12 1.374(5) . ? C7 C8 1.382(5) . ? C30 C31 1.383(5) . ? C34 C33 1.377(5) . ? C6 C5 1.390(5) . ? C5 C4 1.374(5) . ? C22 C21 1.383(5) . ? C9 C10 1.372(7) . ? C9 C8 1.379(6) . ? C3 C4 1.380(5) . ? C3 C2 1.393(5) . ? F3 C32 1.366(4) . ? C12 C11 1.385(5) . ? F1 C20 1.352(4) . ? C33 C32 1.341(5) . ? C20 C19 1.356(6) . ? C20 C21 1.367(6) . ? C18 C19 1.381(5) . ? C32 C31 1.370(6) . ? C11 C10 1.366(6) . ? N3 C16 1.368(4) . ? N3 C13 1.373(4) . ? O1 C13 1.204(4) . ? F2 C26 1.354(5) . ? O2 C16 1.228(4) . ? C24 C25 1.377(5) . ? C24 C23 1.401(5) . ? C23 C28 1.387(5) . ? C16 C15 1.501(5) . ? C13 C14 1.519(6) . ? C28 C27 1.381(5) . ? C26 C25 1.350(6) . ? C26 C27 1.363(6) . ? C15 C14 1.503(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pd1 N3 171.75(11) . . ? C1 Pd1 N2 78.86(11) . . ? N3 Pd1 N2 96.19(10) . . ? C1 Pd1 P1 92.97(9) . . ? N3 Pd1 P1 91.26(8) . . ? N2 Pd1 P1 170.16(7) . . ? C23 P1 C29 108.44(14) . . ? C23 P1 C17 102.23(15) . . ? C29 P1 C17 104.82(15) . . ? C23 P1 Pd1 116.14(11) . . ? C29 P1 Pd1 109.04(11) . . ? C17 P1 Pd1 115.36(11) . . ? N1 N2 C7 114.7(3) . . ? N1 N2 Pd1 115.99(19) . . ? C7 N2 Pd1 129.0(2) . . ? C2 C1 C6 115.2(3) . . ? C2 C1 Pd1 134.8(2) . . ? C6 C1 Pd1 109.8(2) . . ? C34 C29 C30 118.1(3) . . ? C34 C29 P1 124.2(3) . . ? C30 C29 P1 117.6(3) . . ? C22 C17 C18 118.1(3) . . ? C22 C17 P1 121.0(3) . . ? C18 C17 P1 120.8(3) . . ? N2 N1 C6 113.2(3) . . ? C12 C7 C8 120.7(3) . . ? C12 C7 N2 118.1(3) . . ? C8 C7 N2 121.1(3) . . ? C31 C30 C29 120.8(4) . . ? C33 C34 C29 121.1(3) . . ? C5 C6 N1 116.3(3) . . ? C5 C6 C1 123.1(3) . . ? N1 C6 C1 120.6(3) . . ? C4 C5 C6 119.6(3) . . ? C17 C22 C21 121.3(4) . . ? C10 C9 C8 121.1(4) . . ? C4 C3 C2 121.3(3) . . ? C7 C12 C11 119.5(4) . . ? C1 C2 C3 121.9(3) . . ? C32 C33 C34 119.2(4) . . ? F1 C20 C19 118.9(4) . . ? F1 C20 C21 118.5(4) . . ? C19 C20 C21 122.6(4) . . ? C9 C8 C7 118.7(4) . . ? C19 C18 C17 121.0(4) . . ? C20 C19 C18 118.7(4) . . ? C33 C32 F3 119.6(4) . . ? C33 C32 C31 122.6(4) . . ? F3 C32 C31 117.8(4) . . ? C20 C21 C22 118.3(4) . . ? C10 C11 C12 120.3(4) . . ? C5 C4 C3 118.8(3) . . ? C32 C31 C30 118.2(4) . . ? C11 C10 C9 119.7(4) . . ? C16 N3 C13 110.2(3) . . ? C16 N3 Pd1 120.9(2) . . ? C13 N3 Pd1 128.9(2) . . ? C25 C24 C23 120.3(4) . . ? C28 C23 C24 118.2(3) . . ? C28 C23 P1 120.7(3) . . ? C24 C23 P1 121.1(3) . . ? O2 C16 N3 123.8(3) . . ? O2 C16 C15 124.9(4) . . ? N3 C16 C15 111.3(3) . . ? O1 C13 N3 124.8(4) . . ? O1 C13 C14 125.2(3) . . ? N3 C13 C14 109.9(3) . . ? C27 C28 C23 121.3(4) . . ? C25 C26 F2 117.5(4) . . ? C25 C26 C27 123.2(4) . . ? F2 C26 C27 119.2(5) . . ? C26 C27 C28 117.9(4) . . ? C26 C25 C24 119.1(4) . . ? C16 C15 C14 104.0(3) . . ? C15 C14 C13 104.5(3) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 0.50 _diffrn_measured_fraction_theta_full 0.000 _refine_diff_density_max 0.742 _refine_diff_density_min -0.930 _refine_diff_density_rms 0.186 #===END data_compound_2 _database_code_CSD 210649 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37.13 H34.25 Cl0.25 N3 O5 P Pd' _chemical_formula_weight 748.66 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.0010(2) _cell_length_b 15.7410(2) _cell_length_c 18.1390(3) _cell_angle_alpha 92.7670(6) _cell_angle_beta 105.6230(7) _cell_angle_gamma 114.9541(5) _cell_volume 3675.00(9) _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 ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.353 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1533 _exptl_absorpt_coefficient_mu 0.611 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 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 45274 _diffrn_reflns_av_R_equivalents 0.0476 _diffrn_reflns_av_sigmaI/netI 0.0718 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.19 _diffrn_reflns_theta_max 29.12 _reflns_number_total 19544 _reflns_number_gt 11435 _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^)+(0.1036P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 19544 _refine_ls_number_parameters 869 _refine_ls_number_restraints 31 _refine_ls_R_factor_all 0.1071 _refine_ls_R_factor_gt 0.0531 _refine_ls_wR_factor_ref 0.1849 _refine_ls_wR_factor_gt 0.1503 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.089 _refine_ls_shift/su_mean 0.004 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 0.28628(2) 0.297338(17) 0.004270(15) 0.04369(10) Uani 1 1 d . . . Pd2 Pd 0.10124(2) -0.27373(2) 0.565973(16) 0.05606(11) Uani 1 1 d . . . P1 P 0.29119(7) 0.15679(6) -0.01468(5) 0.0432(2) Uani 1 1 d . . . P2 P 0.26814(9) -0.19627(7) 0.64371(6) 0.0564(3) Uani 1 1 d . . . C1 C 0.4243(3) 0.3637(2) 0.0896(2) 0.0512(9) Uani 1 1 d . . . N3 N 0.1446(2) 0.2459(2) -0.08364(17) 0.0473(7) Uani 1 1 d . . . N2 N 0.3063(3) 0.4361(2) 0.02027(19) 0.0546(8) Uani 1 1 d . . . C23 C 0.1780(3) 0.0624(2) -0.0883(2) 0.0456(8) Uani 1 1 d . . . O5 O 0.2839(2) -0.0039(2) 0.27591(15) 0.0641(7) Uani 1 1 d . . . C17 C 0.3974(3) 0.1665(2) -0.0493(2) 0.0448(8) Uani 1 1 d . . . C29 C 0.2982(3) 0.1065(2) 0.0736(2) 0.0437(8) Uani 1 1 d . . . C33 C 0.2487(3) 0.0915(3) 0.1906(2) 0.0540(9) Uani 1 1 d . . . H33 H 0.2179 0.1076 0.2234 0.065 Uiso 1 1 calc R . . O4 O -0.0845(2) -0.1503(2) -0.25281(16) 0.0682(8) Uani 1 1 d . . . C31 C 0.3390(3) 0.0070(3) 0.1602(2) 0.0545(9) Uani 1 1 d . . . H31 H 0.3688 -0.0337 0.1726 0.065 Uiso 1 1 calc R . . C18 C 0.4661(3) 0.2557(2) -0.0571(2) 0.0515(9) Uani 1 1 d . . . H18 H 0.4603 0.3094 -0.0404 0.062 Uiso 1 1 calc R . . O8 O 0.2687(3) -0.1788(2) 0.97366(17) 0.0718(8) Uani 1 1 d . . . C27 C 0.0112(3) -0.0744(3) -0.1247(2) 0.0555(10) Uani 1 1 d . . . H27 H -0.0422 -0.1197 -0.1104 0.067 Uiso 1 1 calc R . . C32 C 0.2916(3) 0.0296(2) 0.2087(2) 0.0494(9) Uani 1 1 d . . . C57 C 0.2662(3) -0.1813(3) 0.8976(2) 0.0573(10) Uani 1 1 d . . . C25 C 0.0828(3) -0.0099(3) -0.2238(2) 0.0571(10) Uani 1 1 d . . . H25 H 0.0777 -0.0111 -0.2762 0.068 Uiso 1 1 calc R . . C26 C 0.0037(3) -0.0779(3) -0.2017(2) 0.0504(9) Uani 1 1 d . . . C28 C 0.0963(3) -0.0050(2) -0.0681(2) 0.0492(9) Uani 1 1 d . . . H28 H 0.0995 -0.0030 -0.0161 0.059 Uiso 1 1 calc R . . C24 C 0.1688(3) 0.0590(3) -0.1670(2) 0.0541(9) Uani 1 1 d . . . H24 H 0.2219 0.1044 -0.1816 0.065 Uiso 1 1 calc R . . C54 C 0.2729(3) -0.1893(3) 0.7452(2) 0.0560(10) Uani 1 1 d . . . C20 C 0.5542(3) 0.1877(3) -0.1135(2) 0.0516(9) Uani 1 1 d . . . N6 N 0.1199(3) -0.1564(2) 0.51065(18) 0.0602(9) Uani 1 1 d . . . C21 C 0.4852(3) 0.0976(2) -0.1057(2) 0.0521(9) Uani 1 1 d . . . H21 H 0.4918 0.0440 -0.1215 0.062 Uiso 1 1 calc R . . N1 N 0.3951(3) 0.5001(2) 0.0607(2) 0.0717(11) Uani 1 1 d . . . C30 C 0.3418(3) 0.0452(3) 0.0937(2) 0.0509(9) Uani 1 1 d . . . H30 H 0.3735 0.0295 0.0614 0.061 Uiso 1 1 calc R . . C58 C 0.3521(3) -0.1788(3) 0.8823(2) 0.0609(10) Uani 1 1 d . . . H58 H 0.4082 -0.1742 0.9229 0.073 Uiso 1 1 calc R . . C34 C 0.2517(3) 0.1296(3) 0.1232(2) 0.0526(9) Uani 1 1 d . . . H34 H 0.2225 0.1708 0.1110 0.063 Uiso 1 1 calc R . . C22 C 0.4082(3) 0.0879(2) -0.0752(2) 0.0510(9) Uani 1 1 d . . . H22 H 0.3620 0.0274 -0.0717 0.061 Uiso 1 1 calc R . . C7 C 0.2349(4) 0.4702(3) -0.0208(2) 0.0602(11) Uani 1 1 d . . . N5 N -0.0606(3) -0.3538(3) 0.51137(18) 0.0634(9) Uani 1 1 d . . . C66 C 0.3395(3) -0.0726(3) 0.6360(2) 0.0614(11) Uani 1 1 d . . . C59 C 0.3557(3) -0.1832(3) 0.8068(2) 0.0582(10) Uani 1 1 d . . . H59 H 0.4139 -0.1819 0.7971 0.070 Uiso 1 1 calc R . . C2 C 0.4885(3) 0.3330(3) 0.1377(2) 0.0636(11) Uani 1 1 d . . . H2 H 0.4697 0.2681 0.1321 0.076 Uiso 1 1 calc R . . C55 C 0.1887(4) -0.1888(3) 0.7624(2) 0.0667(11) Uani 1 1 d . . . H55 H 0.1336 -0.1910 0.7222 0.080 Uiso 1 1 calc R . . N4 N -0.1047(3) -0.4347(3) 0.5296(2) 0.0745(11) Uani 1 1 d . . . C38 C 0.0713(3) -0.3916(3) 0.6129(2) 0.0638(11) Uani 1 1 d . . . C56 C 0.1840(3) -0.1852(3) 0.8378(2) 0.0648(11) Uani 1 1 d . . . H56 H 0.1263 -0.1854 0.8479 0.078 Uiso 1 1 calc R . . C60 C 0.3506(3) -0.2489(3) 0.6293(2) 0.0581(10) Uani 1 1 d . . . C44 C -0.1318(3) -0.3235(3) 0.4665(2) 0.0638(11) Uani 1 1 d . . . C3 C 0.5812(3) 0.3970(3) 0.1949(3) 0.0775(14) Uani 1 1 d . . . H3 H 0.6215 0.3738 0.2276 0.093 Uiso 1 1 calc R . . C65 C 0.4575(4) -0.2012(3) 0.6614(3) 0.0707(12) Uani 1 1 d . . . H65 H 0.4883 -0.1404 0.6914 0.085 Uiso 1 1 calc R . . C12 C 0.2659(5) 0.5433(3) -0.0621(3) 0.0840(16) Uani 1 1 d . . . H12 H 0.3341 0.5720 -0.0624 0.101 Uiso 1 1 calc R . . C39 C 0.1305(4) -0.4208(3) 0.6683(3) 0.0707(12) Uani 1 1 d . . . H39 H 0.2000 -0.3787 0.6933 0.085 Uiso 1 1 calc R . . C43 C -0.0348(4) -0.4586(3) 0.5809(2) 0.0693(13) Uani 1 1 d . . . C6 C 0.4589(3) 0.4623(3) 0.1005(3) 0.0677(12) Uani 1 1 d . . . C72 C 0.1767(4) -0.1942(4) 0.9912(3) 0.0799(14) Uani 1 1 d . . . H72A H 0.1897 -0.1902 1.0464 0.120 Uiso 1 1 calc R . . H72B H 0.1223 -0.2562 0.9647 0.120 Uiso 1 1 calc R . . H72C H 0.1559 -0.1465 0.9745 0.120 Uiso 1 1 calc R . . C62 C 0.3671(4) -0.3796(3) 0.5715(3) 0.0820(15) Uani 1 1 d . . . H62 H 0.3363 -0.4399 0.5407 0.098 Uiso 1 1 calc R . . C71 C 0.3516(4) 0.0031(3) 0.6889(3) 0.0740(13) Uani 1 1 d . . . H71 H 0.3223 -0.0100 0.7287 0.089 Uiso 1 1 calc R . . C61 C 0.3075(4) -0.3384(3) 0.5841(2) 0.0670(12) Uani 1 1 d . . . H61 H 0.2358 -0.3715 0.5617 0.080 Uiso 1 1 calc R . . O6 O 0.0814(3) -0.0753(3) 0.5946(2) 0.1019(12) Uani 1 1 d . . . C53 C 0.1516(4) -0.1419(3) 0.4468(3) 0.0693(12) Uani 1 1 d . . . C67 C 0.3796(4) -0.0488(3) 0.5754(3) 0.0759(13) Uani 1 1 d . . . H67 H 0.3704 -0.0977 0.5387 0.091 Uiso 1 1 calc R . . C64 C 0.5187(4) -0.2415(3) 0.6502(3) 0.0810(14) Uani 1 1 d . . . H64 H 0.5904 -0.2088 0.6729 0.097 Uiso 1 1 calc R . . C4 C 0.6134(4) 0.4939(4) 0.2032(3) 0.0952(18) Uani 1 1 d . . . H4 H 0.6757 0.5358 0.2407 0.114 Uiso 1 1 calc R . . C42 C -0.0763(4) -0.5487(3) 0.6008(3) 0.0865(17) Uani 1 1 d . . . H42 H -0.1463 -0.5906 0.5781 0.104 Uiso 1 1 calc R . . C50 C 0.1061(4) -0.0818(4) 0.5367(3) 0.0746(13) Uani 1 1 d . . . C11 C 0.1970(7) 0.5732(4) -0.1021(4) 0.115(3) Uani 1 1 d . . . H11 H 0.2172 0.6215 -0.1306 0.138 Uiso 1 1 calc R . . C40 C 0.0898(4) -0.5115(3) 0.6882(3) 0.0774(14) Uani 1 1 d . . . H40 H 0.1332 -0.5284 0.7248 0.093 Uiso 1 1 calc R . . O9 O 0.5343(3) -0.3705(3) 0.5919(3) 0.1329(19) Uani 1 1 d D . . C49 C -0.1148(5) -0.2814(4) 0.4040(3) 0.0831(15) Uani 1 1 d . . . H49 H -0.0568 -0.2724 0.3899 0.100 Uiso 1 1 calc R . . C37 C 0.3184(4) -0.0741(4) 0.2938(3) 0.0852(15) Uani 1 1 d . . . H37A H 0.3088 -0.0919 0.3420 0.128 Uiso 1 1 calc R . . H37B H 0.3906 -0.0486 0.2986 0.128 Uiso 1 1 calc R . . H37C H 0.2791 -0.1291 0.2528 0.128 Uiso 1 1 calc R . . C47 C -0.2687(6) -0.2608(5) 0.3833(4) 0.108(2) Uani 1 1 d . . . H47 H -0.3146 -0.2398 0.3551 0.130 Uiso 1 1 calc R . . C52 C 0.1557(5) -0.0495(4) 0.4247(3) 0.0884(17) Uani 1 1 d . . . H52A H 0.2250 -0.0065 0.4251 0.106 Uiso 1 1 calc R . . H52B H 0.1073 -0.0611 0.3731 0.106 Uiso 1 1 calc R . . C63 C 0.4729(4) -0.3316(4) 0.6044(3) 0.0869(16) Uani 1 1 d . A . C45 C -0.2176(4) -0.3348(4) 0.4889(3) 0.0871(15) Uani 1 1 d . . . H45 H -0.2298 -0.3642 0.5308 0.105 Uiso 1 1 calc R . . C5 C 0.5538(4) 0.5282(3) 0.1562(4) 0.0973(19) Uani 1 1 d . . . H5 H 0.5751 0.5934 0.1607 0.117 Uiso 1 1 calc R . . C41 C -0.0123(5) -0.5753(3) 0.6546(3) 0.0886(17) Uani 1 1 d . . . H41 H -0.0384 -0.6355 0.6676 0.106 Uiso 1 1 calc R . . C10 C 0.0986(7) 0.5312(5) -0.0996(4) 0.133(3) Uani 1 1 d . . . H10 H 0.0514 0.5512 -0.1274 0.159 Uiso 1 1 calc R . . C51 C 0.1267(5) -0.0090(4) 0.4840(3) 0.0952(17) Uani 1 1 d . . . H51A H 0.0651 -0.0012 0.4602 0.114 Uiso 1 1 calc R . . H51B H 0.1827 0.0524 0.5127 0.114 Uiso 1 1 calc R . . C46 C -0.2843(5) -0.3014(5) 0.4476(5) 0.114(2) Uani 1 1 d . . . H46 H -0.3401 -0.3062 0.4633 0.137 Uiso 1 1 calc R . . C8 C 0.1352(4) 0.4269(4) -0.0177(3) 0.0777(13) Uani 1 1 d . . . H8 H 0.1151 0.3775 0.0098 0.093 Uiso 1 1 calc R . . C9 C 0.0652(5) 0.4589(5) -0.0569(4) 0.109(2) Uani 1 1 d . . . H9 H -0.0022 0.4328 -0.0547 0.131 Uiso 1 1 calc R . . C48 C -0.1859(6) -0.2523(5) 0.3621(3) 0.1021(19) Uani 1 1 d . . . H48 H -0.1762 -0.2262 0.3183 0.122 Uiso 1 1 calc R . . O3 O 0.6260(2) 0.19100(19) -0.14602(18) 0.0671(8) Uani 1 1 d . . . O7 O 0.1753(4) -0.1941(2) 0.4138(2) 0.0996(13) Uani 1 1 d . . . O2 O 0.0372(3) 0.1830(3) -0.0119(2) 0.0976(12) Uani 1 1 d . . . O1 O 0.2093(3) 0.2968(3) -0.1812(2) 0.1234(18) Uani 1 1 d . . . O10 O 0.4982(4) 0.2126(3) 0.6218(3) 0.1304(17) Uani 1 1 d . . . C13 C 0.1361(4) 0.2595(3) -0.1571(3) 0.0756(14) Uani 1 1 d . . . C16 C 0.0498(3) 0.1995(3) -0.0736(3) 0.0647(11) Uani 1 1 d . . . C70 C 0.4069(4) 0.0971(3) 0.6820(3) 0.0837(15) Uani 1 1 d . . . H70 H 0.4167 0.1465 0.7185 0.100 Uiso 1 1 calc R . . C36 C -0.0996(4) -0.1555(4) -0.3327(3) 0.104(2) Uani 1 1 d . . . H36A H -0.1640 -0.2099 -0.3610 0.156 Uiso 1 1 calc R . . H36B H -0.0435 -0.1616 -0.3442 0.156 Uiso 1 1 calc R . . H36C H -0.1017 -0.0986 -0.3478 0.156 Uiso 1 1 calc R . . C14 C 0.0214(5) 0.2169(5) -0.2055(3) 0.116(2) Uani 1 1 d . . . H14A H 0.0039 0.2661 -0.2250 0.139 Uiso 1 1 calc R . . H14B H 0.0049 0.1690 -0.2493 0.139 Uiso 1 1 calc R . . C69 C 0.4465(4) 0.1171(4) 0.6230(4) 0.0887(16) Uani 1 1 d . . . C68 C 0.4329(4) 0.0445(4) 0.5672(3) 0.0864(15) Uani 1 1 d . . . H68 H 0.4589 0.0584 0.5258 0.104 Uiso 1 1 calc R . . C15 C -0.0347(4) 0.1741(4) -0.1512(3) 0.0991(19) Uani 1 1 d . . . H15A H -0.0741 0.1054 -0.1679 0.119 Uiso 1 1 calc R . . H15B H -0.0817 0.2003 -0.1477 0.119 Uiso 1 1 calc R . . C74 C 0.5423(9) 0.2376(6) 0.5637(6) 0.199(5) Uani 1 1 d . . . H74A H 0.5765 0.3058 0.5697 0.299 Uiso 1 1 calc R . . H74B H 0.4892 0.2110 0.5139 0.299 Uiso 1 1 calc R . . H74C H 0.5920 0.2133 0.5672 0.299 Uiso 1 1 calc R . . C19 C 0.5430(3) 0.2660(3) -0.0893(2) 0.0583(10) Uani 1 1 d . . . H19 H 0.5875 0.3263 -0.0948 0.070 Uiso 1 1 calc R . . C35 C 0.7003(4) 0.2848(3) -0.1517(3) 0.103(2) Uani 1 1 d . . . H35A H 0.7477 0.2781 -0.1752 0.155 Uiso 1 1 calc R . . H35B H 0.7382 0.3232 -0.1005 0.155 Uiso 1 1 calc R . . H35C H 0.6640 0.3149 -0.1831 0.155 Uiso 1 1 calc R . . C73 C 0.5038(4) -0.4594(3) 0.5489(3) 0.176(7) Uani 0.592(13) 1 d PRDU A 1 H73A H 0.5641 -0.4675 0.5501 0.264 Uiso 0.592(13) 1 calc PR A 1 H73B H 0.4654 -0.4637 0.4960 0.264 Uiso 0.592(13) 1 calc PR A 1 H73C H 0.4609 -0.5085 0.5710 0.264 Uiso 0.592(13) 1 calc PR A 1 C73' C 0.6288(4) -0.3389(3) 0.6338(3) 0.171(10) Uani 0.408(13) 1 d PRDU A 2 H73D H 0.6587 -0.3753 0.6153 0.256 Uiso 0.408(13) 1 calc PR A 2 H73E H 0.6324 -0.3443 0.6869 0.256 Uiso 0.408(13) 1 calc PR A 2 H73F H 0.6666 -0.2731 0.6309 0.256 Uiso 0.408(13) 1 calc PR A 2 Cl1 Cl 0.0990(4) 0.3891(3) 0.2474(3) 0.277(8) Uani 0.25 1 d PRU . . Cl2 Cl 0.2560(4) 0.4759(3) 0.3493(3) 0.244(6) Uani 0.25 1 d PRU . . C75 C 0.2022(4) 0.4361(3) 0.2673(3) 0.200(18) Uani 0.25 1 d PRU . . H75A H 0.2201 0.4875 0.2381 0.240 Uiso 0.25 1 calc PR . . H75B H 0.2274 0.3929 0.2516 0.240 Uiso 0.25 1 calc PR . . 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 0.04072(16) 0.03562(14) 0.05402(17) 0.00678(11) 0.01080(12) 0.01939(11) Pd2 0.05218(19) 0.05862(19) 0.04813(17) 0.01261(13) 0.00627(13) 0.02225(15) P1 0.0411(5) 0.0362(4) 0.0530(5) 0.0071(4) 0.0136(4) 0.0190(4) P2 0.0526(6) 0.0546(6) 0.0531(5) 0.0078(4) 0.0072(5) 0.0223(5) C1 0.046(2) 0.0431(18) 0.058(2) 0.0022(16) 0.0059(17) 0.0221(16) N3 0.0435(17) 0.0411(15) 0.0547(17) 0.0101(13) 0.0078(13) 0.0215(13) N2 0.058(2) 0.0400(16) 0.0672(19) 0.0063(14) 0.0129(16) 0.0278(15) C23 0.0449(19) 0.0385(17) 0.055(2) 0.0095(14) 0.0146(16) 0.0214(15) O5 0.0733(19) 0.0782(19) 0.0585(15) 0.0269(14) 0.0275(14) 0.0449(16) C17 0.0416(19) 0.0376(17) 0.0553(19) 0.0070(14) 0.0145(16) 0.0189(14) C29 0.0412(19) 0.0379(17) 0.0496(18) 0.0045(14) 0.0118(15) 0.0178(14) C33 0.051(2) 0.063(2) 0.058(2) 0.0074(18) 0.0202(18) 0.0322(19) O4 0.0539(16) 0.0658(17) 0.0585(16) -0.0028(13) 0.0067(13) 0.0115(14) C31 0.059(2) 0.052(2) 0.065(2) 0.0185(18) 0.022(2) 0.0349(18) C18 0.051(2) 0.0367(17) 0.068(2) 0.0079(16) 0.0215(19) 0.0200(16) O8 0.077(2) 0.093(2) 0.0580(17) 0.0194(15) 0.0208(15) 0.0502(18) C27 0.043(2) 0.055(2) 0.063(2) 0.0122(18) 0.0144(18) 0.0184(17) C32 0.0399(19) 0.0465(19) 0.054(2) 0.0067(16) 0.0102(16) 0.0151(16) C57 0.063(3) 0.045(2) 0.063(2) 0.0066(17) 0.011(2) 0.0285(18) C25 0.061(3) 0.058(2) 0.047(2) 0.0088(17) 0.0166(18) 0.0231(19) C26 0.047(2) 0.050(2) 0.054(2) 0.0039(16) 0.0117(17) 0.0247(17) C28 0.044(2) 0.0504(19) 0.0488(19) 0.0067(15) 0.0117(16) 0.0194(16) C24 0.055(2) 0.047(2) 0.057(2) 0.0105(17) 0.0218(18) 0.0182(17) C54 0.054(2) 0.052(2) 0.054(2) 0.0085(17) 0.0035(18) 0.0252(18) C20 0.049(2) 0.053(2) 0.061(2) 0.0110(17) 0.0213(18) 0.0285(17) N6 0.065(2) 0.063(2) 0.0520(18) 0.0176(15) 0.0159(16) 0.0296(17) C21 0.061(2) 0.0397(18) 0.064(2) 0.0106(16) 0.0247(19) 0.0277(17) N1 0.067(2) 0.0402(17) 0.090(2) 0.0041(17) 0.000(2) 0.0244(17) C30 0.055(2) 0.050(2) 0.058(2) 0.0112(17) 0.0237(18) 0.0296(17) C58 0.054(2) 0.071(3) 0.056(2) 0.0134(19) 0.0063(19) 0.035(2) C34 0.053(2) 0.048(2) 0.064(2) 0.0096(17) 0.0176(19) 0.0305(17) C22 0.053(2) 0.0369(17) 0.064(2) 0.0071(16) 0.0195(18) 0.0200(16) C7 0.071(3) 0.042(2) 0.065(2) 0.0043(17) 0.007(2) 0.0337(19) N5 0.058(2) 0.068(2) 0.0490(17) 0.0060(16) 0.0014(15) 0.0240(17) C66 0.055(2) 0.055(2) 0.066(2) 0.0069(19) 0.009(2) 0.0231(19) C59 0.050(2) 0.060(2) 0.065(2) 0.0112(18) 0.0130(19) 0.0281(19) C2 0.057(2) 0.047(2) 0.076(3) 0.0061(19) 0.006(2) 0.0234(19) C55 0.063(3) 0.084(3) 0.058(2) 0.006(2) 0.004(2) 0.047(2) N4 0.062(2) 0.067(2) 0.066(2) 0.0121(18) -0.0012(18) 0.0162(19) C38 0.065(3) 0.062(2) 0.050(2) 0.0136(18) 0.0052(19) 0.022(2) C56 0.058(3) 0.077(3) 0.066(3) 0.013(2) 0.014(2) 0.041(2) C60 0.050(2) 0.053(2) 0.057(2) 0.0047(17) 0.0071(18) 0.0181(18) C44 0.054(3) 0.066(3) 0.052(2) 0.0019(19) -0.0025(19) 0.022(2) C3 0.051(3) 0.061(3) 0.097(3) 0.008(2) -0.009(2) 0.024(2) C65 0.063(3) 0.060(2) 0.071(3) -0.009(2) 0.006(2) 0.023(2) C12 0.102(4) 0.053(3) 0.081(3) 0.009(2) 0.003(3) 0.036(3) C39 0.069(3) 0.066(3) 0.066(3) 0.018(2) 0.008(2) 0.028(2) C43 0.068(3) 0.059(2) 0.058(2) 0.0142(19) 0.002(2) 0.019(2) C6 0.054(2) 0.043(2) 0.089(3) 0.002(2) 0.000(2) 0.0202(18) C72 0.083(3) 0.086(3) 0.077(3) 0.017(2) 0.028(3) 0.042(3) C62 0.067(3) 0.059(3) 0.096(3) -0.015(2) 0.008(3) 0.022(2) C71 0.090(3) 0.069(3) 0.063(2) 0.013(2) 0.015(2) 0.043(3) C61 0.058(3) 0.058(2) 0.070(3) -0.002(2) 0.008(2) 0.020(2) O6 0.140(4) 0.125(3) 0.080(2) 0.028(2) 0.055(2) 0.082(3) C53 0.085(3) 0.062(3) 0.056(2) 0.012(2) 0.024(2) 0.027(2) C67 0.080(3) 0.071(3) 0.080(3) 0.019(2) 0.026(3) 0.036(3) C64 0.051(3) 0.077(3) 0.098(3) -0.010(3) 0.005(2) 0.028(2) C4 0.061(3) 0.061(3) 0.117(4) -0.007(3) -0.018(3) 0.015(2) C42 0.082(3) 0.065(3) 0.072(3) 0.013(2) 0.000(3) 0.010(3) C50 0.088(3) 0.090(3) 0.061(3) 0.023(2) 0.023(3) 0.054(3) C11 0.137(6) 0.066(3) 0.112(5) 0.013(3) -0.018(4) 0.053(4) C40 0.086(3) 0.068(3) 0.070(3) 0.020(2) 0.009(3) 0.036(3) O9 0.087(3) 0.104(3) 0.190(5) -0.044(3) 0.015(3) 0.053(3) C49 0.090(4) 0.098(4) 0.062(3) 0.012(3) 0.009(3) 0.052(3) C37 0.099(4) 0.105(4) 0.085(3) 0.050(3) 0.043(3) 0.065(3) C47 0.111(5) 0.122(5) 0.107(5) 0.024(4) 0.013(4) 0.079(4) C52 0.125(5) 0.080(3) 0.066(3) 0.029(2) 0.036(3) 0.047(3) C63 0.070(3) 0.082(3) 0.104(4) -0.007(3) 0.020(3) 0.037(3) C45 0.069(3) 0.092(4) 0.088(3) 0.016(3) 0.010(3) 0.035(3) C5 0.070(3) 0.048(2) 0.134(5) -0.003(3) -0.012(3) 0.019(2) C41 0.106(4) 0.061(3) 0.076(3) 0.020(2) 0.014(3) 0.026(3) C10 0.157(7) 0.101(5) 0.124(5) -0.015(4) -0.039(5) 0.099(5) C51 0.125(5) 0.092(4) 0.099(4) 0.045(3) 0.047(4) 0.067(4) C46 0.084(4) 0.120(5) 0.143(6) 0.012(4) 0.021(4) 0.060(4) C8 0.078(3) 0.083(3) 0.088(3) 0.010(3) 0.021(3) 0.054(3) C9 0.097(4) 0.111(5) 0.132(5) 0.000(4) 0.011(4) 0.077(4) C48 0.125(5) 0.124(5) 0.068(3) 0.022(3) 0.012(3) 0.076(4) O3 0.0691(19) 0.0623(17) 0.090(2) 0.0186(15) 0.0439(17) 0.0365(15) O7 0.148(4) 0.074(2) 0.092(2) 0.0169(18) 0.067(3) 0.047(2) O2 0.078(2) 0.120(3) 0.102(3) 0.049(2) 0.049(2) 0.036(2) O1 0.105(3) 0.138(4) 0.073(2) 0.019(2) 0.040(2) -0.002(3) O10 0.155(4) 0.073(2) 0.165(4) 0.054(3) 0.062(4) 0.043(3) C13 0.073(3) 0.069(3) 0.061(3) 0.011(2) 0.014(2) 0.015(2) C16 0.047(2) 0.059(2) 0.087(3) 0.026(2) 0.016(2) 0.0242(19) C70 0.106(4) 0.061(3) 0.077(3) 0.014(2) 0.016(3) 0.040(3) C36 0.090(4) 0.102(4) 0.057(3) -0.005(3) 0.002(3) 0.002(3) C14 0.086(4) 0.127(5) 0.081(4) 0.026(3) -0.013(3) 0.024(4) C69 0.084(4) 0.066(3) 0.112(4) 0.034(3) 0.023(3) 0.033(3) C68 0.086(4) 0.085(3) 0.100(4) 0.033(3) 0.041(3) 0.040(3) C15 0.051(3) 0.105(4) 0.114(4) 0.020(3) -0.004(3) 0.028(3) C74 0.316(15) 0.117(6) 0.211(9) 0.091(7) 0.165(11) 0.084(8) C19 0.059(2) 0.0383(18) 0.087(3) 0.0149(18) 0.037(2) 0.0217(17) C35 0.103(4) 0.084(3) 0.169(6) 0.049(4) 0.097(4) 0.049(3) C73 0.182(11) 0.146(10) 0.216(11) 0.002(7) 0.060(8) 0.094(8) C73' 0.162(13) 0.182(13) 0.187(13) -0.006(8) 0.061(9) 0.094(9) Cl1 0.277(11) 0.260(10) 0.301(11) 0.043(8) 0.045(8) 0.158(8) Cl2 0.248(10) 0.234(9) 0.256(10) 0.041(7) 0.065(8) 0.125(8) C75 0.19(2) 0.20(2) 0.21(2) 0.039(10) 0.048(11) 0.099(12) _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 2.016(4) . ? Pd1 N2 2.069(3) . ? Pd1 N3 2.077(3) . ? Pd1 P1 2.2575(9) . ? Pd2 C38 2.006(4) . ? Pd2 N6 2.095(3) . ? Pd2 N5 2.113(3) . ? Pd2 P2 2.2583(11) . ? P1 C17 1.816(4) . ? P1 C29 1.818(4) . ? P1 C23 1.825(3) . ? P2 C66 1.817(4) . ? P2 C60 1.817(5) . ? P2 C54 1.820(4) . ? C1 C2 1.380(6) . ? C1 C6 1.398(5) . ? N3 C13 1.341(5) . ? N3 C16 1.365(5) . ? N2 N1 1.264(4) . ? N2 C7 1.445(5) . ? C23 C24 1.393(5) . ? C23 C28 1.395(5) . ? O5 C32 1.366(4) . ? O5 C37 1.421(6) . ? C17 C22 1.390(5) . ? C17 C18 1.390(5) . ? C29 C30 1.388(5) . ? C29 C34 1.396(5) . ? C33 C32 1.386(6) . ? C33 C34 1.391(6) . ? O4 C26 1.369(4) . ? O4 C36 1.398(5) . ? C31 C30 1.376(5) . ? C31 C32 1.386(5) . ? C18 C19 1.383(5) . ? O8 C57 1.368(5) . ? O8 C72 1.425(6) . ? C27 C26 1.367(5) . ? C27 C28 1.373(5) . ? C57 C58 1.375(6) . ? C57 C56 1.383(6) . ? C25 C24 1.378(5) . ? C25 C26 1.393(5) . ? C54 C55 1.384(6) . ? C54 C59 1.392(5) . ? C20 O3 1.346(5) . ? C20 C19 1.380(5) . ? C20 C21 1.400(5) . ? N6 C50 1.360(6) . ? N6 C53 1.361(5) . ? C21 C22 1.366(5) . ? N1 C6 1.392(6) . ? C58 C59 1.384(6) . ? C7 C8 1.375(7) . ? C7 C12 1.385(6) . ? N5 N4 1.271(5) . ? N5 C44 1.425(6) . ? C66 C67 1.385(6) . ? C66 C71 1.409(6) . ? C2 C3 1.402(6) . ? C55 C56 1.387(6) . ? N4 C43 1.396(6) . ? C38 C39 1.385(6) . ? C38 C43 1.418(6) . ? C60 C65 1.383(6) . ? C60 C61 1.382(5) . ? C44 C49 1.369(7) . ? C44 C45 1.397(7) . ? C3 C4 1.378(7) . ? C65 C64 1.366(7) . ? C12 C11 1.362(8) . ? C39 C40 1.405(6) . ? C43 C42 1.397(6) . ? C6 C5 1.415(6) . ? C62 C61 1.364(7) . ? C62 C63 1.370(7) . ? C71 C70 1.390(7) . ? O6 C50 1.218(5) . ? C53 O7 1.213(6) . ? C53 C52 1.508(7) . ? C67 C68 1.383(7) . ? C64 C63 1.389(7) . ? C4 C5 1.363(7) . ? C42 C41 1.388(7) . ? C50 C51 1.512(7) . ? C11 C10 1.354(11) . ? C40 C41 1.366(7) . ? O9 C73' 1.274(6) . ? O9 C63 1.361(7) . ? O9 C73 1.392(6) . ? C49 C48 1.390(8) . ? C47 C48 1.353(9) . ? C47 C46 1.384(9) . ? C52 C51 1.474(7) . ? C45 C46 1.383(9) . ? C10 C9 1.402(11) . ? C8 C9 1.393(8) . ? O3 C35 1.456(5) . ? O2 C16 1.207(5) . ? O1 C13 1.215(6) . ? O10 C69 1.374(6) . ? O10 C74 1.378(9) . ? C13 C14 1.529(7) . ? C16 C15 1.518(6) . ? C70 C69 1.347(8) . ? C14 C15 1.471(8) . ? C69 C68 1.399(8) . ? Cl1 C75 1.3346 . ? Cl2 C75 1.4467 . ? 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 N2 78.28(14) . . ? C1 Pd1 N3 172.74(13) . . ? N2 Pd1 N3 94.47(12) . . ? C1 Pd1 P1 95.64(11) . . ? N2 Pd1 P1 170.51(10) . . ? N3 Pd1 P1 91.51(8) . . ? C38 Pd2 N6 175.25(15) . . ? C38 Pd2 N5 78.47(16) . . ? N6 Pd2 N5 96.83(14) . . ? C38 Pd2 P2 94.09(12) . . ? N6 Pd2 P2 90.66(10) . . ? N5 Pd2 P2 169.84(10) . . ? C17 P1 C29 110.14(17) . . ? C17 P1 C23 102.82(16) . . ? C29 P1 C23 104.11(15) . . ? C17 P1 Pd1 112.57(11) . . ? C29 P1 Pd1 110.98(12) . . ? C23 P1 Pd1 115.64(13) . . ? C66 P2 C60 103.2(2) . . ? C66 P2 C54 103.56(19) . . ? C60 P2 C54 108.48(19) . . ? C66 P2 Pd2 116.24(15) . . ? C60 P2 Pd2 115.02(13) . . ? C54 P2 Pd2 109.51(14) . . ? C2 C1 C6 115.8(3) . . ? C2 C1 Pd1 134.2(3) . . ? C6 C1 Pd1 110.0(3) . . ? C13 N3 C16 111.8(4) . . ? C13 N3 Pd1 123.0(3) . . ? C16 N3 Pd1 125.0(3) . . ? N1 N2 C7 115.4(3) . . ? N1 N2 Pd1 117.4(3) . . ? C7 N2 Pd1 126.3(2) . . ? C24 C23 C28 118.2(3) . . ? C24 C23 P1 120.4(3) . . ? C28 C23 P1 121.3(3) . . ? C32 O5 C37 117.3(3) . . ? C22 C17 C18 117.8(3) . . ? C22 C17 P1 123.2(3) . . ? C18 C17 P1 118.7(3) . . ? C30 C29 C34 118.3(3) . . ? C30 C29 P1 125.7(3) . . ? C34 C29 P1 116.0(3) . . ? C32 C33 C34 119.8(4) . . ? C26 O4 C36 119.0(3) . . ? C30 C31 C32 119.9(4) . . ? C19 C18 C17 121.1(3) . . ? C57 O8 C72 118.5(4) . . ? C26 C27 C28 121.0(4) . . ? O5 C32 C33 114.9(4) . . ? O5 C32 C31 125.1(4) . . ? C33 C32 C31 119.9(4) . . ? O8 C57 C58 116.3(4) . . ? O8 C57 C56 123.7(4) . . ? C58 C57 C56 120.0(4) . . ? C24 C25 C26 119.0(3) . . ? C27 C26 O4 115.9(3) . . ? C27 C26 C25 120.0(3) . . ? O4 C26 C25 124.1(3) . . ? C27 C28 C23 120.3(3) . . ? C25 C24 C23 121.5(3) . . ? C55 C54 C59 117.8(4) . . ? C55 C54 P2 117.4(3) . . ? C59 C54 P2 124.8(3) . . ? O3 C20 C19 124.5(3) . . ? O3 C20 C21 116.9(3) . . ? C19 C20 C21 118.6(4) . . ? C50 N6 C53 110.8(4) . . ? C50 N6 Pd2 123.8(3) . . ? C53 N6 Pd2 125.3(3) . . ? C22 C21 C20 120.4(3) . . ? N2 N1 C6 112.4(3) . . ? C31 C30 C29 121.5(4) . . ? C57 C58 C59 120.4(4) . . ? C33 C34 C29 120.7(4) . . ? C21 C22 C17 121.5(3) . . ? C8 C7 C12 121.6(5) . . ? C8 C7 N2 117.4(4) . . ? C12 C7 N2 120.9(4) . . ? N4 N5 C44 113.4(4) . . ? N4 N5 Pd2 117.1(3) . . ? C44 N5 Pd2 128.5(3) . . ? C67 C66 C71 117.0(4) . . ? C67 C66 P2 121.3(3) . . ? C71 C66 P2 121.6(4) . . ? C58 C59 C54 120.7(4) . . ? C1 C2 C3 121.7(4) . . ? C54 C55 C56 121.9(4) . . ? N5 N4 C43 112.8(4) . . ? C39 C38 C43 114.6(4) . . ? C39 C38 Pd2 134.4(3) . . ? C43 C38 Pd2 111.0(3) . . ? C57 C56 C55 119.1(4) . . ? C65 C60 C61 117.8(4) . . ? C65 C60 P2 121.9(3) . . ? C61 C60 P2 120.3(3) . . ? C49 C44 C45 120.5(5) . . ? C49 C44 N5 120.8(5) . . ? C45 C44 N5 118.7(4) . . ? C4 C3 C2 120.9(5) . . ? C64 C65 C60 121.4(4) . . ? C11 C12 C7 120.4(6) . . ? C38 C39 C40 122.7(4) . . ? N4 C43 C42 116.5(4) . . ? N4 C43 C38 120.2(4) . . ? C42 C43 C38 123.2(4) . . ? N1 C6 C1 120.3(3) . . ? N1 C6 C5 116.2(4) . . ? C1 C6 C5 123.3(4) . . ? C61 C62 C63 119.5(4) . . ? C70 C71 C66 120.5(5) . . ? C62 C61 C60 121.8(4) . . ? O7 C53 N6 125.3(4) . . ? O7 C53 C52 125.2(4) . . ? N6 C53 C52 109.4(4) . . ? C68 C67 C66 122.8(5) . . ? C65 C64 C63 119.4(4) . . ? C5 C4 C3 119.8(4) . . ? C41 C42 C43 119.6(5) . . ? O6 C50 N6 124.0(5) . . ? O6 C50 C51 125.6(5) . . ? N6 C50 C51 110.3(4) . . ? C10 C11 C12 118.7(7) . . ? C41 C40 C39 121.1(5) . . ? C73' O9 C63 122.3(4) . . ? C73' O9 C73 107.9(5) . . ? C63 O9 C73 128.0(4) . . ? C44 C49 C48 118.9(6) . . ? C48 C47 C46 119.1(7) . . ? C51 C52 C53 105.5(4) . . ? O9 C63 C62 120.7(5) . . ? O9 C63 C64 119.2(5) . . ? C62 C63 C64 120.1(5) . . ? C46 C45 C44 118.9(6) . . ? C4 C5 C6 118.6(4) . . ? C40 C41 C42 118.8(5) . . ? C11 C10 C9 122.5(6) . . ? C52 C51 C50 103.9(4) . . ? C47 C46 C45 120.7(7) . . ? C7 C8 C9 118.3(6) . . ? C8 C9 C10 118.4(7) . . ? C47 C48 C49 121.8(6) . . ? C20 O3 C35 117.1(3) . . ? C69 O10 C74 117.7(6) . . ? O1 C13 N3 124.4(5) . . ? O1 C13 C14 126.1(5) . . ? N3 C13 C14 109.4(4) . . ? O2 C16 N3 124.3(4) . . ? O2 C16 C15 126.4(5) . . ? N3 C16 C15 109.3(4) . . ? C69 C70 C71 120.5(5) . . ? C15 C14 C13 104.6(4) . . ? C70 C69 O10 115.0(6) . . ? C70 C69 C68 121.2(5) . . ? O10 C69 C68 123.8(6) . . ? C67 C68 C69 117.9(5) . . ? C14 C15 C16 104.6(4) . . ? C20 C19 C18 120.5(3) . . ? Cl1 C75 Cl2 115.3 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 0.50 _diffrn_measured_fraction_theta_full 0.000 _refine_diff_density_max 1.370 _refine_diff_density_min -1.167 _refine_diff_density_rms 0.237 #===END data_compound_3 _database_code_CSD 210650 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C29 H26 N3 O2 P Pd' _chemical_formula_sum 'C29 H26 N3 O2 P Pd' _chemical_formula_weight 585.90 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' 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 P21/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 14.2880(11) _cell_length_b 16.7260(15) _cell_length_c 12.104(2) _cell_angle_alpha 90.00 _cell_angle_beta 112.836(4) _cell_angle_gamma 90.00 _cell_volume 2665.9(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.460 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1192 _exptl_absorpt_coefficient_mu 0.787 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 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 10109 _diffrn_reflns_av_R_equivalents 0.1806 _diffrn_reflns_av_sigmaI/netI 0.1497 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 21.81 _reflns_number_total 3169 _reflns_number_gt 1721 _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^)+(0.0515P)^2^+1.7625P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _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 3169 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1397 _refine_ls_R_factor_gt 0.0610 _refine_ls_wR_factor_ref 0.1492 _refine_ls_wR_factor_gt 0.1215 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.000 _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 0.31771(7) 0.43056(5) 0.51544(7) 0.0456(3) Uani 1 1 d . . . N3 N 0.2228(8) 0.5247(6) 0.4937(7) 0.049(3) Uani 1 1 d . . . P1 P 0.3103(2) 0.44559(18) 0.3274(2) 0.0470(9) Uani 1 1 d . . . N2 N 0.3485(7) 0.4167(5) 0.6957(7) 0.043(2) Uani 1 1 d . . . N1 N 0.4190(8) 0.3687(6) 0.7543(7) 0.054(3) Uani 1 1 d . . . C6 C 0.4530(9) 0.3217(7) 0.6813(9) 0.044(3) Uani 1 1 d . . . C5 C 0.5223(10) 0.2607(7) 0.7333(9) 0.059(4) Uani 1 1 d . . . H5 H 0.5499 0.2543 0.8161 0.071 Uiso 1 1 calc R . . C1 C 0.4140(8) 0.3387(6) 0.5557(9) 0.042(3) Uani 1 1 d . . . C17 C 0.2313(10) 0.5291(7) 0.2453(9) 0.050(3) Uani 1 1 d . . . C12 C 0.2064(10) 0.4741(9) 0.7336(11) 0.069(4) Uani 1 1 d . . . H12 H 0.1629 0.4531 0.6605 0.082 Uiso 1 1 calc R . . C7 C 0.3087(10) 0.4609(7) 0.7700(10) 0.056(3) Uani 1 1 d . . . C3 C 0.5101(10) 0.2229(7) 0.5396(10) 0.063(4) Uani 1 1 d . . . H3 H 0.5274 0.1879 0.4909 0.075 Uiso 1 1 calc R . . C26 C 0.1535(13) 0.2411(9) 0.0740(13) 0.084(5) Uani 1 1 d . . . H26 H 0.1191 0.1998 0.0229 0.100 Uiso 1 1 calc R . . C23 C 0.2543(9) 0.3623(7) 0.2267(9) 0.050(3) Uani 1 1 d . . . C28 C 0.2704(10) 0.3509(7) 0.1226(10) 0.064(4) Uani 1 1 d . . . H28 H 0.3143 0.3842 0.1039 0.076 Uiso 1 1 calc R . . C4 C 0.5494(10) 0.2104(7) 0.6620(9) 0.061(4) Uani 1 1 d . . . H4 H 0.5938 0.1682 0.6954 0.074 Uiso 1 1 calc R . . C8 C 0.3712(10) 0.4906(8) 0.8804(10) 0.064(4) Uani 1 1 d . . . H8 H 0.4406 0.4806 0.9088 0.077 Uiso 1 1 calc R . . C18 C 0.1288(10) 0.5205(8) 0.1755(10) 0.062(4) Uani 1 1 d . . . H18 H 0.0999 0.4699 0.1676 0.074 Uiso 1 1 calc R . . C10 C 0.2297(12) 0.5454(8) 0.9081(12) 0.077(4) Uani 1 1 d . . . H10 H 0.2021 0.5732 0.9549 0.092 Uiso 1 1 calc R . . C19 C 0.0695(10) 0.5823(9) 0.1187(10) 0.070(4) Uani 1 1 d . . . H19 H 0.0018 0.5736 0.0693 0.084 Uiso 1 1 calc R . . C22 C 0.2710(11) 0.6057(8) 0.2612(11) 0.074(4) Uani 1 1 d . . . H22 H 0.3388 0.6142 0.3103 0.089 Uiso 1 1 calc R . . C9 C 0.3324(11) 0.5351(8) 0.9497(11) 0.071(4) Uani 1 1 d . . . H9 H 0.3751 0.5572 1.0222 0.086 Uiso 1 1 calc R . . C24 C 0.1874(12) 0.3132(8) 0.2503(10) 0.075(5) Uani 1 1 d . . . H24 H 0.1756 0.3208 0.3199 0.090 Uiso 1 1 calc R . . C2 C 0.4454(10) 0.2863(7) 0.4874(9) 0.059(4) Uani 1 1 d . . . H2 H 0.4225 0.2940 0.4050 0.070 Uiso 1 1 calc R . . C27 C 0.2195(13) 0.2884(9) 0.0453(10) 0.079(5) Uani 1 1 d . . . H27 H 0.2304 0.2790 -0.0245 0.095 Uiso 1 1 calc R . . C11 C 0.1663(11) 0.5159(9) 0.7991(11) 0.077(4) Uani 1 1 d . . . H11 H 0.0967 0.5247 0.7711 0.092 Uiso 1 1 calc R . . C25 C 0.1385(13) 0.2541(8) 0.1740(12) 0.084(5) Uani 1 1 d . . . H25 H 0.0933 0.2218 0.1918 0.101 Uiso 1 1 calc R . . C20 C 0.1083(12) 0.6573(10) 0.1335(12) 0.080(4) Uani 1 1 d . . . H20 H 0.0669 0.7004 0.0964 0.096 Uiso 1 1 calc R . . C21 C 0.2100(14) 0.6694(9) 0.2042(14) 0.103(6) Uani 1 1 d . . . H21 H 0.2372 0.7206 0.2134 0.123 Uiso 1 1 calc R . . C29 C 0.4329(9) 0.4649(7) 0.3229(10) 0.063(4) Uani 1 1 d . . . H29A H 0.4647 0.5088 0.3750 0.094 Uiso 1 1 calc R . . H29B H 0.4247 0.4780 0.2424 0.094 Uiso 1 1 calc R . . H29C H 0.4748 0.4181 0.3488 0.094 Uiso 1 1 calc R . . O1 O 0.0741(7) 0.4537(6) 0.4022(7) 0.075(3) Uani 1 1 d . . . C13 C 0.1193(13) 0.5181(10) 0.4421(11) 0.067(4) Uani 1 1 d . . . C14 C 0.0672(12) 0.5959(9) 0.4361(13) 0.095(5) Uani 1 1 d . . . H14A H 0.0224 0.5934 0.4790 0.114 Uiso 1 1 calc R . . H14B H 0.0279 0.6110 0.3536 0.114 Uiso 1 1 calc R . . O2 O 0.3332(8) 0.6254(6) 0.5775(9) 0.099(4) Uani 1 1 d . . . C16 C 0.2489(13) 0.6045(10) 0.5262(11) 0.075(5) Uani 1 1 d . . . C15 C 0.1532(12) 0.6545(9) 0.4952(14) 0.104(6) Uani 1 1 d . . . H15A H 0.1491 0.6773 0.5669 0.125 Uiso 1 1 calc R . . H15B H 0.1517 0.6975 0.4407 0.125 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 0.0480(6) 0.0502(5) 0.0368(4) -0.0010(5) 0.0147(4) 0.0013(6) N3 0.043(7) 0.051(7) 0.049(6) -0.005(5) 0.012(5) 0.011(5) P1 0.046(2) 0.050(2) 0.0418(15) -0.0001(14) 0.0130(14) -0.0020(17) N2 0.042(6) 0.043(6) 0.045(5) 0.007(5) 0.018(4) 0.009(5) N1 0.064(7) 0.053(7) 0.041(5) 0.004(5) 0.017(5) -0.012(6) C6 0.043(8) 0.050(8) 0.041(6) -0.002(6) 0.018(6) 0.004(6) C5 0.088(11) 0.052(8) 0.035(6) 0.010(6) 0.020(7) 0.007(8) C1 0.026(7) 0.042(7) 0.051(7) 0.008(5) 0.008(5) 0.000(6) C17 0.060(9) 0.043(8) 0.041(6) 0.008(5) 0.013(6) 0.002(7) C12 0.045(10) 0.105(12) 0.056(7) -0.006(7) 0.020(7) -0.011(8) C7 0.060(9) 0.057(8) 0.048(7) -0.008(6) 0.017(7) -0.010(7) C3 0.088(11) 0.053(8) 0.052(7) -0.012(6) 0.031(7) 0.008(8) C26 0.093(13) 0.053(10) 0.085(11) -0.011(8) 0.013(10) -0.002(9) C23 0.056(9) 0.038(8) 0.045(7) 0.002(5) 0.009(6) 0.004(7) C28 0.076(10) 0.063(9) 0.052(7) -0.012(6) 0.024(7) 0.009(8) C4 0.071(10) 0.060(9) 0.049(7) 0.003(6) 0.019(7) 0.013(8) C8 0.054(9) 0.081(10) 0.052(7) -0.006(7) 0.016(7) 0.014(8) C18 0.061(10) 0.062(9) 0.056(8) 0.012(6) 0.017(7) 0.006(8) C10 0.085(12) 0.081(11) 0.076(9) -0.015(7) 0.044(8) 0.011(9) C19 0.062(9) 0.074(10) 0.062(8) 0.023(7) 0.011(6) -0.005(9) C22 0.063(10) 0.058(9) 0.084(9) 0.022(7) 0.008(7) 0.009(8) C9 0.058(10) 0.097(11) 0.058(8) -0.020(7) 0.021(7) -0.001(8) C24 0.111(13) 0.058(9) 0.056(8) -0.007(7) 0.031(8) -0.030(10) C2 0.082(10) 0.057(9) 0.038(6) 0.002(6) 0.025(6) 0.020(8) C27 0.106(13) 0.082(12) 0.046(7) -0.019(8) 0.026(8) 0.025(10) C11 0.068(10) 0.108(12) 0.064(8) -0.024(8) 0.037(8) -0.008(9) C25 0.125(15) 0.058(10) 0.077(9) -0.016(8) 0.046(10) -0.028(10) C20 0.064(11) 0.079(12) 0.093(10) 0.032(8) 0.026(9) 0.015(9) C21 0.099(15) 0.046(10) 0.141(14) 0.013(9) 0.023(11) 0.010(10) C29 0.066(9) 0.064(9) 0.057(7) 0.007(6) 0.022(6) 0.003(8) O1 0.057(6) 0.081(8) 0.082(6) -0.012(5) 0.021(5) 0.002(6) C13 0.082(13) 0.077(12) 0.045(7) 0.006(7) 0.028(8) 0.021(10) C14 0.078(12) 0.096(13) 0.099(11) 0.001(9) 0.023(9) 0.024(11) O2 0.069(8) 0.085(8) 0.115(8) -0.034(6) 0.005(6) -0.006(7) C16 0.078(13) 0.077(12) 0.059(8) -0.011(7) 0.016(8) 0.025(10) C15 0.085(14) 0.080(11) 0.127(13) -0.036(10) 0.018(10) 0.017(10) _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 1.992(11) . ? Pd1 N3 2.027(10) . ? Pd1 N2 2.065(8) . ? Pd1 P1 2.251(3) . ? N3 C13 1.369(16) . ? N3 C16 1.400(17) . ? P1 C29 1.804(13) . ? P1 C23 1.819(11) . ? P1 C17 1.828(11) . ? N2 N1 1.268(11) . ? N2 C7 1.441(14) . ? N1 C6 1.402(14) . ? C6 C5 1.390(15) . ? C6 C1 1.431(13) . ? C5 C4 1.366(16) . ? C1 C2 1.393(14) . ? C17 C22 1.383(15) . ? C17 C18 1.385(16) . ? C12 C11 1.341(17) . ? C12 C7 1.371(17) . ? C7 C8 1.380(15) . ? C3 C4 1.381(14) . ? C3 C2 1.387(15) . ? C26 C25 1.327(19) . ? C26 C27 1.37(2) . ? C23 C24 1.372(17) . ? C23 C28 1.378(16) . ? C28 C27 1.404(17) . ? C8 C9 1.387(17) . ? C18 C19 1.345(16) . ? C10 C9 1.366(18) . ? C10 C11 1.370(16) . ? C19 C20 1.355(17) . ? C22 C21 1.381(17) . ? C24 C25 1.348(16) . ? C20 C21 1.385(18) . ? O1 C13 1.252(15) . ? C13 C14 1.487(18) . ? C14 C15 1.517(19) . ? O2 C16 1.173(17) . ? C16 C15 1.521(19) . ? 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 N3 173.8(4) . . ? C1 Pd1 N2 79.1(4) . . ? N3 Pd1 N2 94.7(4) . . ? C1 Pd1 P1 95.2(3) . . ? N3 Pd1 P1 90.9(3) . . ? N2 Pd1 P1 171.2(3) . . ? C13 N3 C16 109.1(12) . . ? C13 N3 Pd1 123.1(10) . . ? C16 N3 Pd1 127.8(10) . . ? C29 P1 C23 107.2(6) . . ? C29 P1 C17 104.4(6) . . ? C23 P1 C17 101.7(5) . . ? C29 P1 Pd1 112.7(4) . . ? C23 P1 Pd1 115.3(4) . . ? C17 P1 Pd1 114.3(4) . . ? N1 N2 C7 113.4(9) . . ? N1 N2 Pd1 117.3(7) . . ? C7 N2 Pd1 128.9(8) . . ? N2 N1 C6 113.4(9) . . ? C5 C6 N1 119.1(10) . . ? C5 C6 C1 122.8(10) . . ? N1 C6 C1 118.1(10) . . ? C4 C5 C6 119.6(10) . . ? C2 C1 C6 115.0(10) . . ? C2 C1 Pd1 133.7(8) . . ? C6 C1 Pd1 111.1(8) . . ? C22 C17 C18 117.5(11) . . ? C22 C17 P1 119.9(9) . . ? C18 C17 P1 122.3(10) . . ? C11 C12 C7 122.7(12) . . ? C12 C7 C8 117.5(12) . . ? C12 C7 N2 120.8(11) . . ? C8 C7 N2 121.7(12) . . ? C4 C3 C2 121.8(11) . . ? C25 C26 C27 120.4(13) . . ? C24 C23 C28 119.0(11) . . ? C24 C23 P1 118.6(10) . . ? C28 C23 P1 122.1(10) . . ? C23 C28 C27 119.0(14) . . ? C5 C4 C3 119.1(12) . . ? C7 C8 C9 121.2(12) . . ? C19 C18 C17 122.6(13) . . ? C9 C10 C11 121.6(13) . . ? C18 C19 C20 120.0(13) . . ? C17 C22 C21 120.0(13) . . ? C10 C9 C8 118.0(11) . . ? C25 C24 C23 120.9(13) . . ? C3 C2 C1 121.4(10) . . ? C26 C27 C28 119.2(13) . . ? C12 C11 C10 118.9(14) . . ? C26 C25 C24 121.4(15) . . ? C19 C20 C21 119.6(14) . . ? C22 C21 C20 120.2(15) . . ? O1 C13 N3 123.3(13) . . ? O1 C13 C14 124.1(14) . . ? N3 C13 C14 112.6(14) . . ? C13 C14 C15 104.1(13) . . ? O2 C16 N3 122.6(14) . . ? O2 C16 C15 127.3(15) . . ? N3 C16 C15 109.9(14) . . ? C14 C15 C16 104.3(12) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 0.50 _diffrn_measured_fraction_theta_full 0.000 _refine_diff_density_max 0.490 _refine_diff_density_min -0.545 _refine_diff_density_rms 0.098