# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr JoseLuis Serrano' _publ_contact_author_email jose.serrano@upct.es _publ_section_title ; Bis(imidate)palladium(II) complexes with labile ligands. Mimics of classical precursors? ; loop_ _publ_author_name J.Serrano G.Sanchez J.Garcia M.L.Martinez J.Perez A.Kapdi # Attachment '- CrystalData.cif' data_compound_2 _database_code_depnum_ccdc_archive 'CCDC 817736' #TrackingRef '- CrystalData.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H20 N2 O4 Pd S2' _chemical_formula_sum 'C20 H20 N2 O4 Pd S2' _chemical_formula_weight 522.90 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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 11.4738(8) _cell_length_b 8.2218(6) _cell_length_c 21.4360(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2022.2(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.718 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1056 _exptl_absorpt_coefficient_mu 1.154 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8739 _exptl_absorpt_correction_T_max 0.9340 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 21400 _diffrn_reflns_av_R_equivalents 0.0353 _diffrn_reflns_av_sigmaI/netI 0.0214 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 28.18 _reflns_number_total 2410 _reflns_number_gt 2262 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^)+(0.0360P)^2^+8.7557P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2410 _refine_ls_number_parameters 133 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0466 _refine_ls_R_factor_gt 0.0421 _refine_ls_wR_factor_ref 0.0910 _refine_ls_wR_factor_gt 0.0885 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _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 0.5000 0.0000 0.5000 0.01031(11) Uani 1 2 d S . . N1 N 0.4531(2) 0.1125(3) 0.41978(11) 0.0111(5) Uani 1 1 d . . . C1 C 0.3517(3) 0.0824(4) 0.38658(14) 0.0117(6) Uani 1 1 d . . . O1 O 0.2734(2) -0.0083(3) 0.40289(11) 0.0181(5) Uani 1 1 d . . . C2 C 0.3573(3) 0.1788(4) 0.32740(13) 0.0110(6) Uani 1 1 d . . . C3 C 0.2814(3) 0.1860(4) 0.27708(14) 0.0147(6) Uani 1 1 d . . . H3 H 0.2114 0.1291 0.2771 0.018 Uiso 1 1 calc R . . C4 C 0.3145(3) 0.2822(4) 0.22646(15) 0.0157(6) Uani 1 1 d . . . H4 H 0.2667 0.2880 0.1915 0.019 Uiso 1 1 calc R . . C5 C 0.4185(3) 0.3695(4) 0.22786(15) 0.0164(6) Uani 1 1 d . . . H5 H 0.4385 0.4337 0.1938 0.020 Uiso 1 1 calc R . . C6 C 0.4934(3) 0.3634(4) 0.27888(15) 0.0147(6) Uani 1 1 d . . . H6 H 0.5625 0.4226 0.2798 0.018 Uiso 1 1 calc R . . C7 C 0.4605(3) 0.2655(4) 0.32810(14) 0.0108(6) Uani 1 1 d . . . C8 C 0.5211(3) 0.2262(4) 0.38845(14) 0.0122(6) Uani 1 1 d . . . O2 O 0.6126(2) 0.2828(3) 0.40712(11) 0.0195(5) Uani 1 1 d . . . S1 S 0.40993(7) 0.18930(9) 0.56340(3) 0.01233(16) Uani 1 1 d . . . C9 C 0.5311(3) 0.3151(4) 0.58694(18) 0.0220(7) Uani 1 1 d . . . H9A H 0.5831 0.2529 0.6127 0.033 Uiso 1 1 calc R . . H9B H 0.5027 0.4069 0.6101 0.033 Uiso 1 1 calc R . . H9C H 0.5720 0.3525 0.5506 0.033 Uiso 1 1 calc R . . C10 C 0.3307(3) 0.3344(4) 0.51726(16) 0.0179(7) Uani 1 1 d . . . H10A H 0.2616 0.2843 0.5009 0.027 Uiso 1 1 calc R . . H10B H 0.3788 0.3710 0.4834 0.027 Uiso 1 1 calc R . . H10C H 0.3094 0.4256 0.5428 0.027 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 0.01281(17) 0.01039(17) 0.00773(17) 0.00166(12) -0.00083(12) 0.00014(12) N1 0.0127(12) 0.0131(12) 0.0076(11) 0.0024(10) -0.0003(9) -0.0004(10) C1 0.0134(14) 0.0103(13) 0.0114(13) -0.0004(11) 0.0005(11) 0.0021(12) O1 0.0163(12) 0.0208(12) 0.0172(11) 0.0053(10) 0.0006(9) -0.0043(9) C2 0.0143(13) 0.0092(13) 0.0094(13) 0.0001(11) 0.0028(11) 0.0009(11) C3 0.0143(14) 0.0148(14) 0.0150(14) -0.0001(12) -0.0020(12) -0.0007(12) C4 0.0197(16) 0.0158(15) 0.0116(14) -0.0002(12) -0.0023(12) 0.0057(12) C5 0.0236(16) 0.0146(15) 0.0109(14) 0.0032(11) 0.0022(13) 0.0022(13) C6 0.0168(15) 0.0129(14) 0.0144(15) 0.0005(12) 0.0004(12) -0.0010(12) C7 0.0131(13) 0.0091(13) 0.0103(14) -0.0007(11) 0.0002(11) 0.0025(11) C8 0.0137(14) 0.0102(13) 0.0128(14) -0.0002(11) 0.0003(11) 0.0011(11) O2 0.0176(11) 0.0232(12) 0.0177(11) 0.0031(10) -0.0066(9) -0.0051(10) S1 0.0158(3) 0.0122(3) 0.0089(3) 0.0016(3) 0.0002(3) 0.0015(3) C9 0.0230(17) 0.0157(15) 0.0274(18) -0.0062(14) -0.0064(14) 0.0003(14) C10 0.0194(15) 0.0163(15) 0.0179(15) 0.0019(13) 0.0007(13) 0.0087(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N1 2.025(2) 5_656 ? Pd1 N1 2.025(2) . ? Pd1 S1 2.3102(7) 5_656 ? Pd1 S1 2.3102(7) . ? N1 C1 1.386(4) . ? N1 C8 1.390(4) . ? C1 O1 1.219(4) . ? C1 C2 1.497(4) . ? C2 C7 1.383(4) . ? C2 C3 1.387(4) . ? C3 C4 1.395(5) . ? C4 C5 1.394(5) . ? C5 C6 1.392(4) . ? C6 C7 1.380(4) . ? C7 C8 1.504(4) . ? C8 O2 1.216(4) . ? S1 C10 1.797(3) . ? S1 C9 1.805(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pd1 N1 180 5_656 . ? N1 Pd1 S1 94.20(7) 5_656 5_656 ? N1 Pd1 S1 85.80(7) . 5_656 ? N1 Pd1 S1 85.80(7) 5_656 . ? N1 Pd1 S1 94.20(7) . . ? S1 Pd1 S1 180 5_656 . ? C1 N1 C8 110.0(2) . . ? C1 N1 Pd1 125.3(2) . . ? C8 N1 Pd1 124.6(2) . . ? O1 C1 N1 125.5(3) . . ? O1 C1 C2 126.7(3) . . ? N1 C1 C2 107.8(2) . . ? C7 C2 C3 121.6(3) . . ? C7 C2 C1 107.5(3) . . ? C3 C2 C1 130.9(3) . . ? C2 C3 C4 117.3(3) . . ? C3 C4 C5 120.5(3) . . ? C6 C5 C4 121.8(3) . . ? C7 C6 C5 116.9(3) . . ? C6 C7 C2 121.8(3) . . ? C6 C7 C8 131.0(3) . . ? C2 C7 C8 107.1(3) . . ? O2 C8 N1 125.6(3) . . ? O2 C8 C7 126.9(3) . . ? N1 C8 C7 107.5(3) . . ? C10 S1 C9 99.38(17) . . ? C10 S1 Pd1 110.48(11) . . ? C9 S1 Pd1 101.89(12) . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 0.50 _diffrn_measured_fraction_theta_full 0.000 _refine_diff_density_max 0.684 _refine_diff_density_min -0.562 _refine_diff_density_rms 0.098 #===END data_compound_2a _database_code_depnum_ccdc_archive 'CCDC 817737' #TrackingRef '- CrystalData.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H38 N2 O4 P2 Pd, 2(C H Cl3)' _chemical_formula_sum 'C54 H40 Cl6 N2 O4 P2 Pd' _chemical_formula_weight 1161.92 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' Cl Cl 0.1484 0.1585 '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 9.3071(6) _cell_length_b 18.2983(11) _cell_length_c 15.0459(9) _cell_angle_alpha 90.00 _cell_angle_beta 105.5430(10) _cell_angle_gamma 90.00 _cell_volume 2468.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.563 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1176 _exptl_absorpt_coefficient_mu 0.815 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7310 _exptl_absorpt_correction_T_max 0.9085 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 36885 _diffrn_reflns_av_R_equivalents 0.0169 _diffrn_reflns_av_sigmaI/netI 0.0115 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 28.71 _reflns_number_total 6026 _reflns_number_gt 5873 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^)+(0.0305P)^2^+1.7537P] 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 6026 _refine_ls_number_parameters 317 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0241 _refine_ls_R_factor_gt 0.0234 _refine_ls_wR_factor_ref 0.0601 _refine_ls_wR_factor_gt 0.0596 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _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 0.5000 0.5000 0.5000 0.00927(4) Uani 1 2 d S . . N1 N 0.57173(12) 0.60530(6) 0.51177(8) 0.0124(2) Uani 1 1 d . . . C1 C 0.48976(14) 0.66509(7) 0.46867(9) 0.0132(2) Uani 1 1 d . . . O1 O 0.36741(11) 0.66251(5) 0.41339(7) 0.0187(2) Uani 1 1 d . . . C2 C 0.58000(14) 0.73249(7) 0.50195(9) 0.0139(2) Uani 1 1 d . . . C3 C 0.54946(16) 0.80564(8) 0.48190(10) 0.0177(3) Uani 1 1 d . . . H3 H 0.4577 0.8210 0.4413 0.021 Uiso 1 1 calc R . . C4 C 0.65966(17) 0.85587(8) 0.52407(11) 0.0217(3) Uani 1 1 d . . . H4 H 0.6431 0.9065 0.5115 0.026 Uiso 1 1 calc R . . C5 C 0.79327(17) 0.83308(8) 0.58411(11) 0.0246(3) Uani 1 1 d . . . H5 H 0.8661 0.8685 0.6120 0.030 Uiso 1 1 calc R . . C6 C 0.82253(16) 0.75902(8) 0.60419(11) 0.0217(3) Uani 1 1 d . . . H6 H 0.9137 0.7433 0.6451 0.026 Uiso 1 1 calc R . . C7 C 0.71301(15) 0.70992(7) 0.56191(9) 0.0147(2) Uani 1 1 d . . . C8 C 0.70663(15) 0.62834(7) 0.56845(9) 0.0140(2) Uani 1 1 d . . . O2 O 0.80243(11) 0.58862(6) 0.61609(7) 0.0204(2) Uani 1 1 d . . . P1 P 0.57435(4) 0.487566(18) 0.36340(2) 0.01066(7) Uani 1 1 d . . . C9 C 0.74066(14) 0.53931(7) 0.36179(9) 0.0127(2) Uani 1 1 d . . . C10 C 0.72289(15) 0.61401(7) 0.34115(10) 0.0163(3) Uani 1 1 d . . . H10 H 0.6257 0.6347 0.3245 0.020 Uiso 1 1 calc R . . C11 C 0.84581(16) 0.65806(8) 0.34485(10) 0.0201(3) Uani 1 1 d . . . H11 H 0.8324 0.7086 0.3303 0.024 Uiso 1 1 calc R . . C12 C 0.98862(16) 0.62832(8) 0.36981(10) 0.0197(3) Uani 1 1 d . . . H12 H 1.0730 0.6584 0.3730 0.024 Uiso 1 1 calc R . . C13 C 1.00670(15) 0.55432(8) 0.38997(10) 0.0183(3) Uani 1 1 d . . . H13 H 1.1041 0.5339 0.4070 0.022 Uiso 1 1 calc R . . C14 C 0.88397(15) 0.50971(8) 0.38551(9) 0.0153(3) Uani 1 1 d . . . H14 H 0.8978 0.4590 0.3986 0.018 Uiso 1 1 calc R . . C15 C 0.60189(14) 0.39207(7) 0.33818(9) 0.0135(2) Uani 1 1 d . . . C16 C 0.71130(15) 0.35019(8) 0.39904(10) 0.0171(3) Uani 1 1 d . . . H16 H 0.7788 0.3729 0.4503 0.021 Uiso 1 1 calc R . . C17 C 0.72145(17) 0.27545(8) 0.38478(11) 0.0215(3) Uani 1 1 d . . . H17 H 0.7970 0.2475 0.4256 0.026 Uiso 1 1 calc R . . C18 C 0.62128(18) 0.24155(8) 0.31093(11) 0.0228(3) Uani 1 1 d . . . H18 H 0.6285 0.1905 0.3012 0.027 Uiso 1 1 calc R . . C19 C 0.51113(17) 0.28226(8) 0.25162(10) 0.0209(3) Uani 1 1 d . . . H19 H 0.4418 0.2589 0.2017 0.025 Uiso 1 1 calc R . . C20 C 0.50110(15) 0.35733(8) 0.26459(10) 0.0168(3) Uani 1 1 d . . . H20 H 0.4255 0.3850 0.2233 0.020 Uiso 1 1 calc R . . C21 C 0.43616(14) 0.52104(7) 0.26205(9) 0.0131(2) Uani 1 1 d . . . C22 C 0.29572(15) 0.54088(7) 0.26944(9) 0.0157(2) Uani 1 1 d . . . H22 H 0.2736 0.5381 0.3274 0.019 Uiso 1 1 calc R . . C23 C 0.18740(15) 0.56481(8) 0.19180(10) 0.0198(3) Uani 1 1 d . . . H23 H 0.0919 0.5790 0.1971 0.024 Uiso 1 1 calc R . . C24 C 0.21851(16) 0.56803(8) 0.10675(10) 0.0205(3) Uani 1 1 d . . . H24 H 0.1437 0.5834 0.0537 0.025 Uiso 1 1 calc R . . C25 C 0.35934(16) 0.54879(8) 0.09921(10) 0.0191(3) Uani 1 1 d . . . H25 H 0.3809 0.5515 0.0411 0.023 Uiso 1 1 calc R . . C26 C 0.46844(15) 0.52566(8) 0.17639(9) 0.0166(3) Uani 1 1 d . . . H26 H 0.5648 0.5130 0.1712 0.020 Uiso 1 1 calc R . . C27 C -0.03110(16) 0.38709(9) 0.18577(10) 0.0214(3) Uani 1 1 d . . . H27 H 0.023(2) 0.3939(11) 0.2455(14) 0.024(5) Uiso 1 1 d . . . Cl1 Cl 0.09331(4) 0.37257(2) 0.11721(3) 0.02598(8) Uani 1 1 d . . . Cl2 Cl -0.14209(5) 0.30903(2) 0.18409(3) 0.03525(10) Uani 1 1 d . . . Cl3 Cl -0.14709(4) 0.46334(2) 0.14461(3) 0.02575(8) Uani 1 1 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 0.00962(7) 0.00753(7) 0.00989(7) -0.00002(4) 0.00129(5) -0.00040(4) N1 0.0132(5) 0.0099(5) 0.0136(5) 0.0002(4) 0.0026(4) -0.0007(4) C1 0.0162(6) 0.0104(6) 0.0136(6) 0.0001(5) 0.0048(5) -0.0008(5) O1 0.0160(5) 0.0157(5) 0.0205(5) 0.0001(4) -0.0016(4) 0.0001(4) C2 0.0156(6) 0.0119(6) 0.0145(6) -0.0012(5) 0.0047(5) -0.0027(5) C3 0.0206(6) 0.0135(6) 0.0188(6) 0.0007(5) 0.0046(5) 0.0008(5) C4 0.0273(7) 0.0102(6) 0.0275(7) 0.0001(5) 0.0071(6) -0.0024(5) C5 0.0249(7) 0.0150(7) 0.0311(8) -0.0040(6) 0.0027(6) -0.0076(5) C6 0.0188(6) 0.0175(7) 0.0248(7) -0.0012(6) -0.0012(5) -0.0037(5) C7 0.0169(6) 0.0115(6) 0.0155(6) 0.0000(5) 0.0039(5) -0.0009(5) C8 0.0158(6) 0.0124(6) 0.0136(6) -0.0006(5) 0.0034(5) -0.0015(5) O2 0.0186(5) 0.0147(5) 0.0232(5) 0.0016(4) -0.0026(4) 0.0006(4) P1 0.01082(14) 0.00967(14) 0.01099(15) -0.00012(11) 0.00205(11) 0.00020(11) C9 0.0132(6) 0.0135(6) 0.0112(5) -0.0009(4) 0.0031(4) -0.0015(4) C10 0.0139(6) 0.0143(6) 0.0204(7) 0.0013(5) 0.0039(5) 0.0014(5) C11 0.0200(7) 0.0143(6) 0.0256(7) 0.0019(5) 0.0056(5) -0.0023(5) C12 0.0155(6) 0.0227(7) 0.0211(7) 0.0004(5) 0.0053(5) -0.0055(5) C13 0.0126(6) 0.0243(7) 0.0178(6) 0.0019(5) 0.0040(5) 0.0021(5) C14 0.0157(6) 0.0157(6) 0.0145(6) 0.0014(5) 0.0040(5) 0.0023(5) C15 0.0156(6) 0.0108(6) 0.0155(6) -0.0009(5) 0.0064(5) 0.0004(5) C16 0.0190(6) 0.0147(6) 0.0172(6) 0.0005(5) 0.0038(5) 0.0002(5) C17 0.0255(7) 0.0146(6) 0.0246(7) 0.0046(5) 0.0071(6) 0.0048(5) C18 0.0334(8) 0.0110(6) 0.0270(7) -0.0011(5) 0.0134(6) -0.0001(5) C19 0.0280(7) 0.0149(7) 0.0197(7) -0.0040(5) 0.0066(6) -0.0052(5) C20 0.0186(6) 0.0146(6) 0.0166(6) -0.0006(5) 0.0036(5) -0.0014(5) C21 0.0129(6) 0.0118(6) 0.0130(6) 0.0002(5) 0.0008(5) -0.0007(5) C22 0.0149(6) 0.0153(6) 0.0167(6) -0.0004(5) 0.0036(5) -0.0008(5) C23 0.0135(6) 0.0204(7) 0.0234(7) 0.0004(5) 0.0010(5) 0.0018(5) C24 0.0194(7) 0.0190(7) 0.0182(7) 0.0020(5) -0.0033(5) -0.0001(5) C25 0.0228(7) 0.0198(7) 0.0131(6) 0.0007(5) 0.0022(5) -0.0018(5) C26 0.0164(6) 0.0176(6) 0.0157(6) 0.0001(5) 0.0043(5) 0.0006(5) C27 0.0168(6) 0.0278(8) 0.0174(7) -0.0008(6) 0.0009(5) 0.0023(5) Cl1 0.01990(16) 0.02866(19) 0.03081(19) 0.00059(15) 0.00928(14) 0.00451(14) Cl2 0.02393(18) 0.0328(2) 0.0494(3) 0.01166(19) 0.01040(17) -0.00095(15) Cl3 0.02130(17) 0.02649(19) 0.02745(18) -0.00401(14) 0.00302(14) 0.00612(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N1 2.0314(11) 3_666 ? Pd1 N1 2.0314(11) . ? Pd1 P1 2.3489(3) . ? Pd1 P1 2.3489(3) 3_666 ? Pd1 Pd1 9.3071(6) 1_655 ? N1 C8 1.3811(16) . ? N1 C1 1.3908(16) . ? C1 O1 1.2178(16) . ? C1 C2 1.5005(18) . ? C2 C3 1.3847(19) . ? C2 C7 1.3851(18) . ? C3 C4 1.397(2) . ? C4 C5 1.391(2) . ? C5 C6 1.399(2) . ? C6 C7 1.3796(19) . ? C7 C8 1.4982(18) . ? C8 O2 1.2226(17) . ? O2 C13 3.1767(18) 3_766 ? P1 C21 1.8176(13) . ? P1 C9 1.8201(13) . ? P1 C15 1.8207(13) . ? C9 C14 1.3946(18) . ? C9 C10 1.4017(18) . ? C10 C11 1.3884(19) . ? C11 C12 1.392(2) . ? C12 C13 1.388(2) . ? C12 O1 3.4657(17) 1_655 ? C13 C14 1.3909(19) . ? C15 C20 1.3976(19) . ? C15 C16 1.4011(19) . ? C16 C17 1.392(2) . ? C17 C18 1.391(2) . ? C18 C19 1.383(2) . ? C19 C20 1.3940(19) . ? C21 C22 1.3895(18) . ? C21 C26 1.4022(18) . ? C22 C23 1.3934(19) . ? C23 C24 1.387(2) . ? C24 C25 1.391(2) . ? C25 C26 1.3880(19) . ? C27 Cl2 1.7589(16) . ? C27 Cl1 1.7651(15) . ? C27 Cl3 1.7713(16) . ? C27 O2 3.1959(18) 3_666 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pd1 N1 180 3_666 . ? N1 Pd1 P1 89.93(3) 3_666 . ? N1 Pd1 P1 90.07(3) . . ? N1 Pd1 P1 90.07(3) 3_666 3_666 ? N1 Pd1 P1 89.93(3) . 3_666 ? P1 Pd1 P1 180 . 3_666 ? N1 Pd1 Pd1 107.77(3) 3_666 1_655 ? N1 Pd1 Pd1 72.23(3) . 1_655 ? P1 Pd1 Pd1 58.057(8) . 1_655 ? P1 Pd1 Pd1 121.943(8) 3_666 1_655 ? C8 N1 C1 110.00(11) . . ? C8 N1 Pd1 124.51(9) . . ? C1 N1 Pd1 125.39(9) . . ? O1 C1 N1 125.70(12) . . ? O1 C1 C2 126.67(12) . . ? N1 C1 C2 107.63(11) . . ? C3 C2 C7 121.70(12) . . ? C3 C2 C1 131.14(12) . . ? C7 C2 C1 107.16(11) . . ? C2 C3 C4 117.02(13) . . ? C5 C4 C3 121.17(13) . . ? C4 C5 C6 121.27(13) . . ? C7 C6 C5 117.01(13) . . ? C6 C7 C2 121.82(13) . . ? C6 C7 C8 130.99(13) . . ? C2 C7 C8 107.19(11) . . ? O2 C8 N1 125.45(12) . . ? O2 C8 C7 126.54(12) . . ? N1 C8 C7 108.00(11) . . ? C8 O2 C13 142.97(9) . 3_766 ? C21 P1 C9 103.10(6) . . ? C21 P1 C15 104.84(6) . . ? C9 P1 C15 109.19(6) . . ? C21 P1 Pd1 113.16(4) . . ? C9 P1 Pd1 114.34(4) . . ? C15 P1 Pd1 111.48(4) . . ? C14 C9 C10 118.91(12) . . ? C14 C9 P1 123.58(10) . . ? C10 C9 P1 117.38(10) . . ? C11 C10 C9 120.69(12) . . ? C10 C11 C12 120.06(13) . . ? C13 C12 C11 119.45(13) . . ? C13 C12 O1 94.42(9) . 1_655 ? C11 C12 O1 146.11(10) . 1_655 ? C12 C13 C14 120.80(13) . . ? C13 C14 C9 120.08(13) . . ? C20 C15 C16 119.01(12) . . ? C20 C15 P1 119.97(10) . . ? C16 C15 P1 120.46(10) . . ? C17 C16 C15 120.28(13) . . ? C18 C17 C16 120.20(14) . . ? C19 C18 C17 119.85(13) . . ? C18 C19 C20 120.43(14) . . ? C19 C20 C15 120.21(13) . . ? C22 C21 C26 119.72(12) . . ? C22 C21 P1 119.36(10) . . ? C26 C21 P1 120.91(10) . . ? C21 C22 C23 119.99(13) . . ? C24 C23 C22 120.26(13) . . ? C23 C24 C25 119.92(13) . . ? C26 C25 C24 120.20(13) . . ? C25 C26 C21 119.90(13) . . ? Cl2 C27 Cl1 110.13(9) . . ? Cl2 C27 Cl3 109.52(8) . . ? Cl1 C27 Cl3 110.37(8) . . ? Cl2 C27 O2 111.60(7) . 3_666 ? Cl1 C27 O2 100.89(6) . 3_666 ? Cl3 C27 O2 114.06(7) . 3_666 ? _diffrn_measured_fraction_theta_max 0.943 _diffrn_reflns_theta_full 0.50 _diffrn_measured_fraction_theta_full 0.000 _refine_diff_density_max 0.395 _refine_diff_density_min -0.513 _refine_diff_density_rms 0.072 #===END data_compound_3a _database_code_depnum_ccdc_archive 'CCDC 817738' #TrackingRef '- CrystalData.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H39 Cl3 N2 O6 P2 Pd' _chemical_formula_weight 978.47 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' 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 11.9234(9) _cell_length_b 12.1823(9) _cell_length_c 15.5656(12) _cell_angle_alpha 86.2140(10) _cell_angle_beta 89.4510(10) _cell_angle_gamma 68.0110(10) _cell_volume 2091.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.554 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 996 _exptl_absorpt_coefficient_mu 0.764 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8088 _exptl_absorpt_correction_T_max 0.8940 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 25392 _diffrn_reflns_av_R_equivalents 0.0147 _diffrn_reflns_av_sigmaI/netI 0.0184 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.31 _diffrn_reflns_theta_max 28.53 _reflns_number_total 9726 _reflns_number_gt 9609 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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. Restraints to bond distances in water molecules were applied to obtain reasonable values. ; _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^)+(0.0258P)^2^+1.7131P] 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 9726 _refine_ls_number_parameters 564 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0314 _refine_ls_R_factor_gt 0.0309 _refine_ls_wR_factor_ref 0.0831 _refine_ls_wR_factor_gt 0.0824 _refine_ls_goodness_of_fit_ref 1.479 _refine_ls_restrained_S_all 1.479 _refine_ls_shift/su_max 0.042 _refine_ls_shift/su_mean 0.003 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 0.629228(13) 0.741027(12) 0.737249(9) 0.00856(5) Uani 1 1 d . . . N1 N 0.72241(15) 0.57489(15) 0.79072(11) 0.0116(3) Uani 1 1 d . . . C1 C 0.72682(18) 0.54819(18) 0.87877(13) 0.0135(4) Uani 1 1 d . . . O1 O 0.68198(15) 0.61853(14) 0.93309(10) 0.0187(3) Uani 1 1 d . . . C2 C 0.7964(2) 0.4179(2) 0.89610(15) 0.0201(4) Uani 1 1 d . . . H2 H 0.807(3) 0.380(3) 0.953(2) 0.025(7) Uiso 1 1 d . . . C3 C 0.8295(2) 0.3722(2) 0.82097(16) 0.0214(5) Uani 1 1 d . . . H3 H 0.878(3) 0.292(3) 0.8051(19) 0.026(7) Uiso 1 1 d . . . C4 C 0.78163(18) 0.47126(18) 0.75191(14) 0.0144(4) Uani 1 1 d . . . O2 O 0.79430(15) 0.45936(14) 0.67465(10) 0.0209(3) Uani 1 1 d . . . N2 N 0.53277(15) 0.90817(15) 0.68925(11) 0.0111(3) Uani 1 1 d . . . C5 C 0.47032(18) 0.94077(18) 0.61160(13) 0.0127(4) Uani 1 1 d . . . O3 O 0.46829(14) 0.87436(14) 0.55680(10) 0.0176(3) Uani 1 1 d . . . C6 C 0.4065(2) 1.07362(19) 0.60536(14) 0.0160(4) Uani 1 1 d . . . H6 H 0.359(3) 1.113(3) 0.556(2) 0.034(8) Uiso 1 1 d . . . C7 C 0.4336(2) 1.11426(19) 0.67592(14) 0.0162(4) Uani 1 1 d . . . H7 H 0.409(3) 1.193(3) 0.690(2) 0.030(8) Uiso 1 1 d . . . C8 C 0.51435(18) 1.00967(18) 0.73213(13) 0.0130(4) Uani 1 1 d . . . O4 O 0.55480(15) 1.01258(14) 0.80291(10) 0.0183(3) Uani 1 1 d . . . P1 P 0.44968(4) 0.72381(4) 0.78557(3) 0.00972(10) Uani 1 1 d . . . C9 C 0.46557(18) 0.56909(17) 0.79920(13) 0.0119(4) Uani 1 1 d . . . H9 H 0.4516 0.6513 0.7939 0.014 Uiso 1 1 calc R . . C10 C 0.44898(18) 0.51602(18) 0.87795(13) 0.0132(4) Uani 1 1 d . . . H10 H 0.4256 0.5616 0.9269 0.016 Uiso 1 1 calc R . . C11 C 0.4668(2) 0.39608(19) 0.88474(14) 0.0166(4) Uani 1 1 d . . . H11 H 0.4563 0.3598 0.9385 0.020 Uiso 1 1 calc R . . C12 C 0.5000(2) 0.32917(19) 0.81324(15) 0.0175(4) Uani 1 1 d . . . H12 H 0.5104 0.2478 0.8179 0.021 Uiso 1 1 calc R . . C13 C 0.5178(2) 0.38150(19) 0.73490(14) 0.0167(4) Uani 1 1 d . . . H13 H 0.5402 0.3358 0.6859 0.020 Uiso 1 1 calc R . . C14 C 0.50290(19) 0.50028(18) 0.72810(13) 0.0143(4) Uani 1 1 d . . . H14 H 0.5181 0.5350 0.6750 0.017 Uiso 1 1 calc R . . C15 C 0.31953(18) 0.79849(18) 0.71315(13) 0.0120(4) Uani 1 1 d . . . H15 H 0.3828 0.7549 0.7531 0.014 Uiso 1 1 calc R . . C16 C 0.25856(19) 0.92025(19) 0.71838(14) 0.0152(4) Uani 1 1 d . . . H16 H 0.2805 0.9596 0.7621 0.018 Uiso 1 1 calc R . . C17 C 0.1661(2) 0.9844(2) 0.66019(15) 0.0206(5) Uani 1 1 d . . . H17 H 0.1244 1.0673 0.6644 0.025 Uiso 1 1 calc R . . C18 C 0.1347(2) 0.9271(2) 0.59581(16) 0.0237(5) Uani 1 1 d . . . H18 H 0.0721 0.9709 0.5555 0.028 Uiso 1 1 calc R . . C19 C 0.1949(2) 0.8059(2) 0.59038(15) 0.0200(4) Uani 1 1 d . . . H19 H 0.1731 0.7668 0.5464 0.024 Uiso 1 1 calc R . . C20 C 0.28703(19) 0.74109(19) 0.64886(14) 0.0155(4) Uani 1 1 d . . . C21 C 0.39556(18) 0.79085(17) 0.88686(13) 0.0114(4) Uani 1 1 d . . . H21 H 0.4246 0.7546 0.8346 0.014 Uiso 1 1 calc R . . C22 C 0.46221(19) 0.84377(17) 0.93019(13) 0.0128(4) Uani 1 1 d . . . H22 H 0.5356 0.8452 0.9068 0.015 Uiso 1 1 calc R . . C23 C 0.4207(2) 0.89445(18) 1.00777(13) 0.0155(4) Uani 1 1 d . . . H23 H 0.4660 0.9302 1.0374 0.019 Uiso 1 1 calc R . . C24 C 0.3132(2) 0.89280(19) 1.04179(14) 0.0173(4) Uani 1 1 d . . . H24 H 0.2856 0.9265 1.0950 0.021 Uiso 1 1 calc R . . C25 C 0.2460(2) 0.84195(19) 0.99811(15) 0.0183(4) Uani 1 1 d . . . H25 H 0.1721 0.8418 1.0214 0.022 Uiso 1 1 calc R . . C26 C 0.28609(19) 0.79114(18) 0.92031(14) 0.0154(4) Uani 1 1 d . . . P2 P 0.80844(4) 0.75950(4) 0.68805(3) 0.00997(10) Uani 1 1 d . . . C27 C 0.93926(18) 0.66857(17) 0.75506(13) 0.0124(4) Uani 1 1 d . . . H27 H 0.8736 0.7125 0.7170 0.015 Uiso 1 1 calc R . . C28 C 1.05284(19) 0.60462(19) 0.72217(15) 0.0171(4) Uani 1 1 d . . . H28 H 1.0648 0.6051 0.6617 0.020 Uiso 1 1 calc R . . C29 C 1.1487(2) 0.5401(2) 0.77855(16) 0.0213(5) Uani 1 1 d . . . H29 H 1.2261 0.4970 0.7563 0.026 Uiso 1 1 calc R . . C30 C 1.1314(2) 0.5386(2) 0.86683(16) 0.0211(5) Uani 1 1 d . . . H30 H 1.1966 0.4937 0.9049 0.025 Uiso 1 1 calc R . . C31 C 1.0186(2) 0.6028(2) 0.89943(15) 0.0192(4) Uani 1 1 d . . . H31 H 1.0071 0.6023 0.9599 0.023 Uiso 1 1 calc R . . C32 C 0.92240(19) 0.66771(19) 0.84412(14) 0.0153(4) Uani 1 1 d . . . C33 C 0.81091(18) 0.90883(18) 0.68756(13) 0.0123(4) Uani 1 1 d . . . H33 H 0.8131 0.8300 0.6886 0.015 Uiso 1 1 calc R . . C34 C 0.8731(2) 0.94100(19) 0.75054(14) 0.0165(4) Uani 1 1 d . . . H34 H 0.9177 0.8841 0.7946 0.020 Uiso 1 1 calc R . . C35 C 0.8696(2) 1.0563(2) 0.74877(15) 0.0206(4) Uani 1 1 d . . . H35 H 0.9125 1.0779 0.7914 0.025 Uiso 1 1 calc R . . C36 C 0.8038(2) 1.14010(19) 0.68504(15) 0.0198(4) Uani 1 1 d . . . H36 H 0.8011 1.2191 0.6843 0.024 Uiso 1 1 calc R . . C37 C 0.7419(2) 1.10809(19) 0.62217(15) 0.0183(4) Uani 1 1 d . . . H37 H 0.6971 1.1655 0.5784 0.022 Uiso 1 1 calc R . . C38 C 0.74530(19) 0.99315(19) 0.62288(14) 0.0150(4) Uani 1 1 d . . . C39 C 0.84488(18) 0.72020(18) 0.57744(13) 0.0126(4) Uani 1 1 d . . . H39 H 0.8235 0.7435 0.6343 0.015 Uiso 1 1 calc R . . C40 C 0.7877(2) 0.65648(19) 0.53726(14) 0.0156(4) Uani 1 1 d . . . H40 H 0.7251 0.6387 0.5657 0.019 Uiso 1 1 calc R . . C41 C 0.8226(2) 0.6186(2) 0.45506(14) 0.0201(4) Uani 1 1 d . . . H41 H 0.7831 0.5756 0.4272 0.024 Uiso 1 1 calc R . . C42 C 0.9149(2) 0.6437(2) 0.41384(14) 0.0201(4) Uani 1 1 d . . . H42 H 0.9405 0.6152 0.3588 0.024 Uiso 1 1 calc R . . C43 C 0.9700(2) 0.7103(2) 0.45280(15) 0.0194(4) Uani 1 1 d . . . C44 C 0.9344(2) 0.75030(19) 0.53417(14) 0.0166(4) Uani 1 1 d . . . C45 C 0.8070(2) 0.8530(2) 1.09870(16) 0.0212(5) Uani 1 1 d . . . H45 H 0.753(3) 0.931(3) 1.1018(18) 0.020(7) Uiso 1 1 d . . . O5 O 0.67921(17) 0.43064(17) 0.52145(13) 0.0306(4) Uani 1 1 d D . . H51 H 0.631(2) 0.4953(19) 0.514(2) 0.037 Uiso 1 1 d D . . H52 H 0.716(3) 0.423(3) 0.5648(15) 0.037 Uiso 1 1 d D . . O6 O 0.50563(19) 0.65375(17) 0.48789(15) 0.0350(5) Uani 1 1 d D . . H61 H 0.503(3) 0.709(2) 0.512(2) 0.042 Uiso 1 1 d D . . H62 H 0.448(2) 0.641(3) 0.491(2) 0.042 Uiso 1 1 d D . . Cl1 Cl 0.93848(5) 0.86187(6) 1.05061(5) 0.03137(14) Uani 1 1 d . . . Cl2 Cl 0.74530(5) 0.77487(5) 1.03606(4) 0.02516(12) Uani 1 1 d . . . Cl3 Cl 0.84100(6) 0.78396(6) 1.20366(4) 0.03034(14) Uani 1 1 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 0.00890(8) 0.00797(8) 0.00878(8) -0.00067(5) 0.00034(5) -0.00311(5) N1 0.0121(8) 0.0099(8) 0.0121(8) 0.0007(6) -0.0005(6) -0.0035(6) C1 0.0126(9) 0.0138(9) 0.0149(10) 0.0006(7) -0.0012(7) -0.0061(7) O1 0.0216(8) 0.0176(7) 0.0151(7) -0.0026(6) 0.0023(6) -0.0050(6) C2 0.0248(12) 0.0141(10) 0.0197(11) 0.0033(8) -0.0067(9) -0.0060(9) C3 0.0252(12) 0.0118(10) 0.0233(11) -0.0006(8) -0.0085(9) -0.0022(9) C4 0.0118(9) 0.0123(9) 0.0180(10) -0.0022(8) -0.0012(7) -0.0030(7) O2 0.0246(8) 0.0189(8) 0.0162(8) -0.0046(6) 0.0014(6) -0.0043(6) N2 0.0121(8) 0.0088(7) 0.0119(8) -0.0003(6) -0.0002(6) -0.0035(6) C5 0.0121(9) 0.0135(9) 0.0129(9) 0.0000(7) 0.0017(7) -0.0055(7) O3 0.0222(8) 0.0185(8) 0.0139(7) -0.0034(6) 0.0000(6) -0.0094(6) C6 0.0168(10) 0.0124(9) 0.0169(10) 0.0027(8) -0.0010(8) -0.0036(8) C7 0.0188(10) 0.0107(9) 0.0176(10) -0.0002(8) 0.0021(8) -0.0041(8) C8 0.0128(9) 0.0122(9) 0.0145(9) -0.0012(7) 0.0030(7) -0.0051(7) O4 0.0257(8) 0.0181(8) 0.0131(7) -0.0027(6) -0.0017(6) -0.0101(6) P1 0.0102(2) 0.0093(2) 0.0098(2) -0.00118(17) 0.00061(18) -0.00375(18) C9 0.0109(9) 0.0096(9) 0.0159(10) -0.0003(7) -0.0011(7) -0.0049(7) C10 0.0126(9) 0.0141(9) 0.0130(9) -0.0020(7) -0.0001(7) -0.0049(7) C11 0.0192(10) 0.0146(10) 0.0165(10) 0.0028(8) -0.0012(8) -0.0074(8) C12 0.0189(10) 0.0115(9) 0.0221(11) 0.0000(8) -0.0026(8) -0.0060(8) C13 0.0189(10) 0.0143(10) 0.0169(10) -0.0049(8) 0.0014(8) -0.0056(8) C14 0.0148(10) 0.0148(10) 0.0134(9) -0.0011(7) 0.0013(7) -0.0057(8) C15 0.0095(9) 0.0156(9) 0.0112(9) 0.0012(7) -0.0011(7) -0.0051(7) C16 0.0141(10) 0.0167(10) 0.0149(10) -0.0012(8) -0.0012(8) -0.0057(8) C17 0.0172(10) 0.0175(10) 0.0226(11) 0.0000(9) -0.0040(9) -0.0015(8) C18 0.0174(11) 0.0295(12) 0.0202(11) 0.0016(9) -0.0079(9) -0.0047(9) C19 0.0172(10) 0.0285(12) 0.0171(10) -0.0049(9) -0.0023(8) -0.0113(9) C20 0.0146(10) 0.0198(10) 0.0145(10) -0.0029(8) 0.0017(8) -0.0091(8) C21 0.0131(9) 0.0102(9) 0.0099(9) -0.0018(7) 0.0021(7) -0.0030(7) C22 0.0139(9) 0.0111(9) 0.0125(9) 0.0017(7) -0.0008(7) -0.0043(7) C23 0.0210(10) 0.0125(9) 0.0125(9) -0.0005(7) -0.0021(8) -0.0056(8) C24 0.0216(11) 0.0131(9) 0.0131(10) -0.0012(8) 0.0040(8) -0.0019(8) C25 0.0174(10) 0.0167(10) 0.0196(11) -0.0007(8) 0.0067(8) -0.0054(8) C26 0.0152(10) 0.0137(9) 0.0172(10) -0.0004(8) 0.0021(8) -0.0054(8) P2 0.0100(2) 0.0103(2) 0.0100(2) -0.00122(18) 0.00070(18) -0.00414(18) C27 0.0119(9) 0.0107(9) 0.0148(10) 0.0002(7) -0.0025(7) -0.0046(7) C28 0.0152(10) 0.0165(10) 0.0183(10) -0.0021(8) 0.0019(8) -0.0045(8) C29 0.0132(10) 0.0195(11) 0.0269(12) -0.0011(9) 0.0005(9) -0.0012(8) C30 0.0174(11) 0.0191(11) 0.0248(12) 0.0036(9) -0.0071(9) -0.0052(9) C31 0.0216(11) 0.0214(11) 0.0156(10) 0.0017(8) -0.0039(8) -0.0097(9) C32 0.0151(10) 0.0165(10) 0.0155(10) -0.0008(8) -0.0012(8) -0.0074(8) C33 0.0131(9) 0.0100(9) 0.0147(9) -0.0029(7) 0.0035(7) -0.0053(7) C34 0.0179(10) 0.0153(10) 0.0164(10) -0.0014(8) -0.0013(8) -0.0063(8) C35 0.0240(11) 0.0197(11) 0.0216(11) -0.0058(9) -0.0004(9) -0.0114(9) C36 0.0227(11) 0.0131(10) 0.0247(11) -0.0032(8) 0.0045(9) -0.0078(8) C37 0.0192(11) 0.0141(10) 0.0195(11) 0.0021(8) 0.0016(8) -0.0044(8) C38 0.0152(10) 0.0159(10) 0.0145(10) -0.0007(8) 0.0019(8) -0.0064(8) C39 0.0137(9) 0.0127(9) 0.0103(9) -0.0014(7) 0.0009(7) -0.0035(7) C40 0.0176(10) 0.0155(10) 0.0152(10) -0.0013(8) 0.0011(8) -0.0078(8) C41 0.0275(12) 0.0201(11) 0.0153(10) -0.0047(8) 0.0003(9) -0.0115(9) C42 0.0264(12) 0.0192(10) 0.0125(10) -0.0038(8) 0.0049(8) -0.0058(9) C43 0.0185(10) 0.0222(11) 0.0162(10) -0.0005(8) 0.0047(8) -0.0064(9) C44 0.0160(10) 0.0188(10) 0.0159(10) -0.0008(8) 0.0015(8) -0.0076(8) C45 0.0189(11) 0.0197(11) 0.0222(11) -0.0039(9) -0.0023(9) -0.0036(9) O5 0.0254(10) 0.0286(10) 0.0363(11) -0.0132(8) -0.0062(8) -0.0064(8) O6 0.0377(11) 0.0232(10) 0.0498(13) -0.0141(9) 0.0072(10) -0.0159(9) Cl1 0.0185(3) 0.0276(3) 0.0460(4) 0.0067(3) -0.0025(3) -0.0076(2) Cl2 0.0240(3) 0.0290(3) 0.0243(3) -0.0066(2) -0.0023(2) -0.0111(2) Cl3 0.0379(3) 0.0283(3) 0.0205(3) -0.0028(2) -0.0044(2) -0.0071(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 N2 2.0221(17) . ? Pd1 N1 2.0334(17) . ? Pd1 P1 2.3403(5) . ? Pd1 P2 2.3471(5) . ? N1 C4 1.372(3) . ? N1 C1 1.385(3) . ? C1 O1 1.216(3) . ? C1 C2 1.498(3) . ? C2 C3 1.321(3) . ? C3 C4 1.504(3) . ? C4 O2 1.222(3) . ? O2 O5 2.868(2) . ? N2 C5 1.381(3) . ? N2 C8 1.388(3) . ? C5 O3 1.220(3) . ? C5 C6 1.505(3) . ? O3 O6 2.837(2) . ? C6 C7 1.325(3) . ? C7 C8 1.505(3) . ? C8 O4 1.215(3) . ? P1 C9 1.820(2) . ? P1 C21 1.823(2) . ? P1 C15 1.830(2) . ? C9 C10 1.395(3) . ? C9 C14 1.400(3) . ? C10 C11 1.392(3) . ? C11 C12 1.389(3) . ? C12 C13 1.390(3) . ? C13 C14 1.387(3) . ? C15 C20 1.394(3) . ? C15 C16 1.394(3) . ? C16 C17 1.388(3) . ? C17 C18 1.388(3) . ? C18 C19 1.388(3) . ? C19 C20 1.390(3) . ? C21 C22 1.398(3) . ? C21 C26 1.399(3) . ? C22 C23 1.394(3) . ? C23 C24 1.388(3) . ? C24 C25 1.388(3) . ? C25 C26 1.394(3) . ? P2 C39 1.822(2) . ? P2 C27 1.826(2) . ? P2 C33 1.830(2) . ? C27 C28 1.397(3) . ? C27 C32 1.399(3) . ? C28 C29 1.396(3) . ? C29 C30 1.388(3) . ? C30 C31 1.389(3) . ? C31 C32 1.390(3) . ? C33 C34 1.395(3) . ? C33 C38 1.399(3) . ? C34 C35 1.388(3) . ? C35 C36 1.387(3) . ? C36 C37 1.391(3) . ? C37 C38 1.385(3) . ? C39 C40 1.388(3) . ? C39 C44 1.405(3) . ? C40 C41 1.395(3) . ? C41 C42 1.389(3) . ? C42 C43 1.389(3) . ? C43 C44 1.392(3) . ? C45 Cl2 1.749(2) . ? C45 Cl3 1.765(3) . ? C45 Cl1 1.767(3) . ? O5 O6 2.750(3) . ? O5 O6 2.767(3) 2_666 ? 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 N2 Pd1 N1 177.39(7) . . ? N2 Pd1 P1 89.40(5) . . ? N1 Pd1 P1 88.97(5) . . ? N2 Pd1 P2 90.19(5) . . ? N1 Pd1 P2 91.45(5) . . ? P1 Pd1 P2 179.562(19) . . ? C4 N1 C1 107.89(17) . . ? C4 N1 Pd1 129.83(14) . . ? C1 N1 Pd1 122.11(14) . . ? O1 C1 N1 125.87(19) . . ? O1 C1 C2 125.6(2) . . ? N1 C1 C2 108.53(18) . . ? C3 C2 C1 107.4(2) . . ? C2 C3 C4 107.77(19) . . ? O2 C4 N1 126.8(2) . . ? O2 C4 C3 124.9(2) . . ? N1 C4 C3 108.38(18) . . ? C4 O2 O5 143.83(15) . . ? C5 N2 C8 108.66(16) . . ? C5 N2 Pd1 126.64(13) . . ? C8 N2 Pd1 124.64(14) . . ? O3 C5 N2 126.34(19) . . ? O3 C5 C6 125.71(19) . . ? N2 C5 C6 107.94(17) . . ? C5 O3 O6 156.46(15) . . ? C7 C6 C5 107.79(19) . . ? C6 C7 C8 107.95(19) . . ? O4 C8 N2 125.79(19) . . ? O4 C8 C7 126.56(19) . . ? N2 C8 C7 107.65(17) . . ? C9 P1 C21 107.47(9) . . ? C9 P1 C15 106.40(9) . . ? C21 P1 C15 102.28(9) . . ? C9 P1 Pd1 111.27(7) . . ? C21 P1 Pd1 114.56(7) . . ? C15 P1 Pd1 114.11(7) . . ? C10 C9 C14 119.50(19) . . ? C10 C9 P1 122.78(16) . . ? C14 C9 P1 117.60(15) . . ? C11 C10 C9 119.90(19) . . ? C12 C11 C10 120.3(2) . . ? C11 C12 C13 119.9(2) . . ? C14 C13 C12 120.1(2) . . ? C13 C14 C9 120.19(19) . . ? C20 C15 C16 119.51(19) . . ? C20 C15 P1 122.72(16) . . ? C16 C15 P1 117.50(15) . . ? C17 C16 C15 120.5(2) . . ? C18 C17 C16 119.8(2) . . ? C19 C18 C17 120.0(2) . . ? C18 C19 C20 120.5(2) . . ? C19 C20 C15 119.7(2) . . ? C22 C21 C26 120.06(19) . . ? C22 C21 P1 120.03(15) . . ? C26 C21 P1 119.89(16) . . ? C23 C22 C21 119.79(19) . . ? C24 C23 C22 120.1(2) . . ? C25 C24 C23 120.1(2) . . ? C24 C25 C26 120.5(2) . . ? C25 C26 C21 119.4(2) . . ? C39 P2 C27 107.06(9) . . ? C39 P2 C33 103.20(9) . . ? C27 P2 C33 103.87(9) . . ? C39 P2 Pd1 114.19(7) . . ? C27 P2 Pd1 112.09(7) . . ? C33 P2 Pd1 115.42(7) . . ? C28 C27 C32 119.83(19) . . ? C28 C27 P2 123.68(16) . . ? C32 C27 P2 116.46(15) . . ? C27 C28 C29 119.7(2) . . ? C30 C29 C28 120.3(2) . . ? C29 C30 C31 119.9(2) . . ? C32 C31 C30 120.4(2) . . ? C31 C32 C27 119.8(2) . . ? C34 C33 C38 119.73(19) . . ? C34 C33 P2 122.04(16) . . ? C38 C33 P2 118.21(16) . . ? C35 C34 C33 119.9(2) . . ? C36 C35 C34 120.4(2) . . ? C35 C36 C37 119.8(2) . . ? C38 C37 C36 120.5(2) . . ? C37 C38 C33 119.8(2) . . ? C40 C39 C44 120.07(19) . . ? C40 C39 P2 120.01(16) . . ? C44 C39 P2 119.88(16) . . ? C39 C40 C41 119.8(2) . . ? C42 C41 C40 120.1(2) . . ? C41 C42 C43 120.2(2) . . ? C44 C43 C42 120.1(2) . . ? C43 C44 C39 119.6(2) . . ? Cl2 C45 Cl3 110.25(14) . . ? Cl2 C45 Cl1 110.54(13) . . ? Cl3 C45 Cl1 110.27(13) . . ? O6 O5 O6 86.83(8) . 2_666 ? O6 O5 O2 102.06(8) . . ? O6 O5 O2 126.90(10) 2_666 . ? O5 O6 O3 131.90(10) . . ? _diffrn_measured_fraction_theta_max 0.915 _diffrn_reflns_theta_full 0.50 _diffrn_measured_fraction_theta_full 0.000 _refine_diff_density_max 1.043 _refine_diff_density_min -0.993 _refine_diff_density_rms 0.097 #===END data_compound_4a _database_code_depnum_ccdc_archive 'CCDC 817739' #TrackingRef '- CrystalData.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H38 N2 O6 P2 Pd S2' _chemical_formula_weight 995.28 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' S S 0.1246 0.1234 '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 13.6140(14) _cell_length_b 13.2162(13) _cell_length_c 24.102(2) _cell_angle_alpha 90.00 _cell_angle_beta 96.788(2) _cell_angle_gamma 90.00 _cell_volume 4306.1(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.535 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2032 _exptl_absorpt_coefficient_mu 0.657 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8322 _exptl_absorpt_correction_T_max 0.8965 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 52699 _diffrn_reflns_av_R_equivalents 0.0239 _diffrn_reflns_av_sigmaI/netI 0.0194 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 28.73 _reflns_number_total 10498 _reflns_number_gt 9883 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^)+(0.0386P)^2^+3.5995P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10498 _refine_ls_number_parameters 568 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0313 _refine_ls_R_factor_gt 0.0289 _refine_ls_wR_factor_ref 0.0773 _refine_ls_wR_factor_gt 0.0723 _refine_ls_goodness_of_fit_ref 1.101 _refine_ls_restrained_S_all 1.101 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.715660(9) 0.814289(9) 0.872356(5) 0.01036(4) Uani 1 1 d . . . N1 N 0.83723(11) 0.82168(11) 0.83010(6) 0.0143(3) Uani 1 1 d . . . C1 C 0.85461(13) 0.74442(13) 0.79388(7) 0.0145(3) Uani 1 1 d . . . O3 O 0.79500(10) 0.67837(10) 0.77884(6) 0.0193(3) Uani 1 1 d . . . C2 C 0.95696(13) 0.75169(13) 0.77708(7) 0.0150(3) Uani 1 1 d . . . C3 C 1.00310(15) 0.68658(14) 0.74320(8) 0.0188(4) Uani 1 1 d . . . H3 H 0.9698 0.6287 0.7270 0.023 Uiso 1 1 calc R . . C4 C 1.09995(14) 0.70864(15) 0.73361(8) 0.0200(4) Uani 1 1 d . . . H4 H 1.1329 0.6653 0.7103 0.024 Uiso 1 1 calc R . . C5 C 1.14896(14) 0.79310(15) 0.75762(8) 0.0198(4) Uani 1 1 d . . . H5 H 1.2147 0.8068 0.7503 0.024 Uiso 1 1 calc R . . C6 C 1.10329(13) 0.85776(14) 0.79217(8) 0.0183(3) Uani 1 1 d . . . H6 H 1.1364 0.9155 0.8088 0.022 Uiso 1 1 calc R . . C7 C 1.00775(13) 0.83428(13) 0.80115(7) 0.0150(3) Uani 1 1 d . . . S1 S 0.93068(3) 0.89989(3) 0.842072(18) 0.01436(9) Uani 1 1 d . . . O1 O 0.90802(10) 0.99731(10) 0.81736(6) 0.0227(3) Uani 1 1 d . . . O2 O 0.96927(10) 0.89981(11) 0.90030(6) 0.0225(3) Uani 1 1 d . . . N2 N 0.58885(11) 0.79351(11) 0.90770(6) 0.0131(3) Uani 1 1 d . . . C8 C 0.50463(13) 0.76441(13) 0.87420(7) 0.0143(3) Uani 1 1 d . . . O6 O 0.50336(9) 0.73454(10) 0.82617(5) 0.0175(3) Uani 1 1 d . . . C9 C 0.41520(13) 0.77905(13) 0.90370(7) 0.0150(3) Uani 1 1 d . . . C10 C 0.31744(13) 0.76957(14) 0.88107(8) 0.0184(3) Uani 1 1 d . . . H10 H 0.3005 0.7432 0.8445 0.022 Uiso 1 1 calc R . . C11 C 0.24473(14) 0.79981(15) 0.91355(9) 0.0214(4) Uani 1 1 d . . . H11 H 0.1771 0.7955 0.8986 0.026 Uiso 1 1 calc R . . C12 C 0.26919(14) 0.83614(15) 0.96745(8) 0.0222(4) Uani 1 1 d . . . H12 H 0.2180 0.8563 0.9887 0.027 Uiso 1 1 calc R . . C13 C 0.36756(14) 0.84363(14) 0.99109(8) 0.0185(3) Uani 1 1 d . . . H13 H 0.3848 0.8668 1.0283 0.022 Uiso 1 1 calc R . . C14 C 0.43849(13) 0.81561(13) 0.95763(8) 0.0151(3) Uani 1 1 d . . . S2 S 0.56828(3) 0.82438(3) 0.971676(17) 0.01326(9) Uani 1 1 d . . . O4 O 0.60034(9) 0.92657(10) 0.98400(5) 0.0178(3) Uani 1 1 d . . . O5 O 0.60526(10) 0.74859(10) 1.01165(5) 0.0186(3) Uani 1 1 d . . . P1 P 0.63969(3) 0.95014(3) 0.819022(18) 0.01257(9) Uani 1 1 d . . . C15 C 0.65571(13) 0.93049(14) 0.74592(7) 0.0154(3) Uani 1 1 d . . . C16 C 0.63334(15) 0.83412(14) 0.72428(8) 0.0214(4) Uani 1 1 d . . . H16 H 0.6130 0.7824 0.7478 0.026 Uiso 1 1 calc R . . C17 C 0.64081(16) 0.81388(15) 0.66820(8) 0.0240(4) Uani 1 1 d . . . H17 H 0.6250 0.7484 0.6535 0.029 Uiso 1 1 calc R . . C18 C 0.67128(14) 0.88887(16) 0.63385(8) 0.0221(4) Uani 1 1 d . . . H18 H 0.6769 0.8748 0.5957 0.027 Uiso 1 1 calc R . . C19 C 0.69351(14) 0.98422(16) 0.65536(8) 0.0229(4) Uani 1 1 d . . . H19 H 0.7139 1.0357 0.6317 0.027 Uiso 1 1 calc R . . C20 C 0.68634(13) 1.00574(15) 0.71133(8) 0.0197(4) Uani 1 1 d . . . H20 H 0.7023 1.0713 0.7258 0.024 Uiso 1 1 calc R . . C21 C 0.68555(13) 1.07544(13) 0.84042(7) 0.0157(3) Uani 1 1 d . . . C22 C 0.63824(15) 1.16188(15) 0.81643(9) 0.0224(4) Uani 1 1 d . . . H22 H 0.5857 1.1550 0.7871 0.027 Uiso 1 1 calc R . . C23 C 0.66805(16) 1.25751(15) 0.83551(10) 0.0286(5) Uani 1 1 d . . . H23 H 0.6349 1.3158 0.8196 0.034 Uiso 1 1 calc R . . C24 C 0.74574(17) 1.26841(16) 0.87763(10) 0.0299(5) Uani 1 1 d . . . H24 H 0.7662 1.3340 0.8904 0.036 Uiso 1 1 calc R . . C25 C 0.79350(16) 1.18370(15) 0.90112(9) 0.0249(4) Uani 1 1 d . . . H25 H 0.8476 1.1913 0.9295 0.030 Uiso 1 1 calc R . . C26 C 0.76284(14) 1.08727(14) 0.88339(8) 0.0184(4) Uani 1 1 d . . . H26 H 0.7946 1.0294 0.9006 0.022 Uiso 1 1 calc R . . C27 C 0.50755(13) 0.97467(13) 0.81872(7) 0.0145(3) Uani 1 1 d . . . C28 C 0.47408(13) 1.00804(13) 0.86829(7) 0.0159(3) Uani 1 1 d . . . H28 H 0.5185 1.0095 0.9018 0.019 Uiso 1 1 calc R . . C29 C 0.37700(13) 1.03892(13) 0.86914(8) 0.0178(3) Uani 1 1 d . . . H29 H 0.3546 1.0601 0.9032 0.021 Uiso 1 1 calc R . . C30 C 0.31255(13) 1.03867(14) 0.81983(8) 0.0199(4) Uani 1 1 d . . . H30 H 0.2465 1.0619 0.8199 0.024 Uiso 1 1 calc R . . C31 C 0.34456(14) 1.00460(15) 0.77072(8) 0.0218(4) Uani 1 1 d . . . H31 H 0.3000 1.0036 0.7373 0.026 Uiso 1 1 calc R . . C32 C 0.44150(14) 0.97179(14) 0.76990(8) 0.0187(4) Uani 1 1 d . . . H32 H 0.4626 0.9475 0.7362 0.022 Uiso 1 1 calc R . . P2 P 0.79468(3) 0.68713(3) 0.929747(18) 0.01212(9) Uani 1 1 d . . . C33 C 0.70993(12) 0.58482(13) 0.94109(7) 0.0142(3) Uani 1 1 d . . . C34 C 0.63762(13) 0.56217(13) 0.89691(7) 0.0152(3) Uani 1 1 d . . . H34 H 0.6337 0.6004 0.8633 0.018 Uiso 1 1 calc R . . C35 C 0.57117(13) 0.48346(14) 0.90206(8) 0.0185(4) Uani 1 1 d . . . H35 H 0.5221 0.4680 0.8719 0.022 Uiso 1 1 calc R . . C36 C 0.57628(14) 0.42769(14) 0.95092(8) 0.0215(4) Uani 1 1 d . . . H36 H 0.5302 0.3748 0.9545 0.026 Uiso 1 1 calc R . . C37 C 0.64883(15) 0.44917(15) 0.99469(8) 0.0225(4) Uani 1 1 d . . . H37 H 0.6530 0.4102 1.0280 0.027 Uiso 1 1 calc R . . C38 C 0.71563(14) 0.52761(14) 0.98999(8) 0.0185(3) Uani 1 1 d . . . H38 H 0.7651 0.5422 1.0201 0.022 Uiso 1 1 calc R . . C39 C 0.89794(13) 0.61973(13) 0.90452(7) 0.0152(3) Uani 1 1 d . . . C40 C 0.87818(14) 0.53728(14) 0.86883(8) 0.0186(4) Uani 1 1 d . . . H40 H 0.8118 0.5154 0.8593 0.022 Uiso 1 1 calc R . . C41 C 0.95428(15) 0.48692(15) 0.84707(8) 0.0226(4) Uani 1 1 d . . . H41 H 0.9398 0.4320 0.8220 0.027 Uiso 1 1 calc R . . C42 C 1.05142(15) 0.51665(15) 0.86182(9) 0.0263(4) Uani 1 1 d . . . H42 H 1.1037 0.4816 0.8473 0.032 Uiso 1 1 calc R . . C43 C 1.07193(14) 0.59756(15) 0.89771(10) 0.0263(4) Uani 1 1 d . . . H43 H 1.1386 0.6174 0.9081 0.032 Uiso 1 1 calc R . . C44 C 0.99587(14) 0.65024(15) 0.91872(9) 0.0214(4) Uani 1 1 d . . . H44 H 1.0105 0.7067 0.9426 0.026 Uiso 1 1 calc R . . C45 C 0.84679(13) 0.74376(13) 0.99533(7) 0.0152(3) Uani 1 1 d . . . C46 C 0.83175(14) 0.84688(14) 1.00285(8) 0.0198(4) Uani 1 1 d . . . H46 H 0.7913 0.8840 0.9751 0.024 Uiso 1 1 calc R . . C47 C 0.87523(17) 0.89590(16) 1.05038(9) 0.0278(4) Uani 1 1 d . . . H47 H 0.8650 0.9664 1.0550 0.033 Uiso 1 1 calc R . . C48 C 0.93356(18) 0.84229(17) 1.09112(9) 0.0307(5) Uani 1 1 d . . . H48 H 0.9636 0.8759 1.1236 0.037 Uiso 1 1 calc R . . C49 C 0.94802(17) 0.73948(16) 1.08443(9) 0.0284(5) Uani 1 1 d . . . H49 H 0.9871 0.7026 1.1128 0.034 Uiso 1 1 calc R . . C50 C 0.90592(15) 0.68989(14) 1.03666(8) 0.0219(4) Uani 1 1 d . . . H50 H 0.9172 0.6196 1.0321 0.026 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 0.01128(7) 0.00937(7) 0.01044(7) 0.00079(4) 0.00135(4) -0.00111(4) N1 0.0146(7) 0.0143(7) 0.0146(7) 0.0003(5) 0.0034(5) -0.0027(5) C1 0.0171(8) 0.0140(8) 0.0124(7) 0.0011(6) 0.0017(6) 0.0004(6) O3 0.0200(6) 0.0179(6) 0.0198(6) -0.0028(5) 0.0009(5) -0.0049(5) C2 0.0160(8) 0.0158(8) 0.0129(8) 0.0007(6) 0.0010(6) -0.0004(6) C3 0.0222(9) 0.0169(9) 0.0174(9) -0.0022(7) 0.0029(7) -0.0005(7) C4 0.0227(9) 0.0206(9) 0.0180(9) -0.0005(7) 0.0070(7) 0.0045(7) C5 0.0163(8) 0.0250(9) 0.0187(9) 0.0025(7) 0.0048(7) 0.0006(7) C6 0.0167(8) 0.0192(9) 0.0189(8) 0.0007(7) 0.0017(7) -0.0019(7) C7 0.0170(8) 0.0146(8) 0.0138(8) 0.0002(6) 0.0034(6) 0.0014(6) S1 0.01481(19) 0.01219(19) 0.0167(2) -0.00184(15) 0.00435(15) -0.00273(15) O1 0.0252(7) 0.0124(6) 0.0325(8) 0.0020(5) 0.0110(6) -0.0004(5) O2 0.0240(7) 0.0251(7) 0.0184(6) -0.0062(5) 0.0019(5) -0.0057(6) N2 0.0149(7) 0.0129(7) 0.0118(7) 0.0002(5) 0.0033(5) -0.0009(5) C8 0.0158(8) 0.0100(7) 0.0171(8) 0.0029(6) 0.0012(6) -0.0005(6) O6 0.0203(6) 0.0180(6) 0.0141(6) -0.0015(5) 0.0015(5) -0.0004(5) C9 0.0169(8) 0.0117(8) 0.0166(8) 0.0020(6) 0.0029(6) -0.0021(6) C10 0.0180(8) 0.0171(8) 0.0196(9) 0.0026(7) -0.0001(7) -0.0027(7) C11 0.0148(8) 0.0222(9) 0.0272(10) 0.0071(8) 0.0019(7) -0.0013(7) C12 0.0180(9) 0.0240(9) 0.0261(10) 0.0052(8) 0.0096(7) 0.0015(7) C13 0.0209(9) 0.0178(8) 0.0179(8) 0.0016(7) 0.0062(7) -0.0007(7) C14 0.0150(8) 0.0136(8) 0.0166(8) 0.0029(6) 0.0020(6) -0.0017(6) S2 0.01424(19) 0.01362(19) 0.01205(19) 0.00055(15) 0.00204(15) -0.00127(14) O4 0.0194(6) 0.0154(6) 0.0182(6) -0.0025(5) 0.0006(5) -0.0021(5) O5 0.0207(6) 0.0196(6) 0.0155(6) 0.0050(5) 0.0018(5) 0.0009(5) P1 0.0146(2) 0.01090(19) 0.0123(2) 0.00142(15) 0.00201(15) 0.00052(15) C15 0.0160(8) 0.0179(8) 0.0123(8) 0.0009(6) 0.0021(6) 0.0041(6) C16 0.0326(10) 0.0139(8) 0.0180(9) 0.0030(7) 0.0044(7) 0.0041(7) C17 0.0346(11) 0.0182(9) 0.0189(9) -0.0027(7) 0.0020(8) 0.0075(8) C18 0.0198(9) 0.0327(11) 0.0143(8) -0.0008(7) 0.0033(7) 0.0060(8) C19 0.0199(9) 0.0325(11) 0.0167(9) 0.0054(8) 0.0042(7) -0.0041(8) C20 0.0183(8) 0.0225(9) 0.0180(9) 0.0019(7) 0.0012(7) -0.0049(7) C21 0.0183(8) 0.0117(8) 0.0183(8) -0.0005(6) 0.0076(7) -0.0015(6) C22 0.0218(9) 0.0160(8) 0.0307(10) 0.0046(8) 0.0090(8) 0.0015(7) C23 0.0323(11) 0.0132(9) 0.0435(12) 0.0028(8) 0.0186(9) 0.0019(8) C24 0.0388(12) 0.0164(9) 0.0393(12) -0.0096(8) 0.0244(10) -0.0102(8) C25 0.0290(10) 0.0264(10) 0.0216(9) -0.0082(8) 0.0124(8) -0.0124(8) C26 0.0201(9) 0.0194(9) 0.0172(8) -0.0016(7) 0.0083(7) -0.0034(7) C27 0.0161(8) 0.0106(7) 0.0168(8) 0.0026(6) 0.0017(6) 0.0008(6) C28 0.0180(8) 0.0131(8) 0.0162(8) 0.0021(6) 0.0007(6) -0.0005(6) C29 0.0200(9) 0.0134(8) 0.0210(9) 0.0004(7) 0.0058(7) -0.0008(7) C30 0.0151(8) 0.0155(8) 0.0290(10) 0.0020(7) 0.0015(7) 0.0010(7) C31 0.0198(9) 0.0220(9) 0.0220(9) 0.0008(7) -0.0044(7) 0.0019(7) C32 0.0216(9) 0.0180(9) 0.0161(8) 0.0001(7) 0.0002(7) 0.0018(7) P2 0.0129(2) 0.01024(19) 0.0129(2) 0.00088(15) 0.00012(15) -0.00129(15) C33 0.0147(8) 0.0105(7) 0.0177(8) 0.0002(6) 0.0034(6) -0.0013(6) C34 0.0156(8) 0.0136(8) 0.0163(8) 0.0013(6) 0.0015(6) 0.0001(6) C35 0.0155(8) 0.0158(8) 0.0240(9) -0.0034(7) 0.0017(7) -0.0024(7) C36 0.0207(9) 0.0158(8) 0.0294(10) -0.0004(7) 0.0083(7) -0.0055(7) C37 0.0293(10) 0.0184(9) 0.0207(9) 0.0053(7) 0.0064(8) -0.0039(8) C38 0.0219(9) 0.0174(8) 0.0158(8) 0.0007(7) 0.0011(7) -0.0022(7) C39 0.0158(8) 0.0129(8) 0.0173(8) 0.0031(6) 0.0026(6) 0.0010(6) C40 0.0181(8) 0.0173(8) 0.0201(9) 0.0004(7) 0.0012(7) 0.0003(7) C41 0.0260(10) 0.0175(9) 0.0244(9) -0.0028(7) 0.0038(8) 0.0029(7) C42 0.0234(10) 0.0188(9) 0.0384(12) 0.0014(8) 0.0106(8) 0.0055(7) C43 0.0157(9) 0.0212(9) 0.0421(12) -0.0002(9) 0.0046(8) -0.0001(7) C44 0.0184(9) 0.0157(9) 0.0297(10) -0.0004(7) 0.0013(7) -0.0016(7) C45 0.0150(8) 0.0152(8) 0.0147(8) 0.0002(6) -0.0008(6) -0.0028(6) C46 0.0221(9) 0.0174(9) 0.0188(9) 0.0000(7) -0.0025(7) 0.0000(7) C47 0.0378(12) 0.0178(9) 0.0254(10) -0.0044(8) -0.0065(9) -0.0017(8) C48 0.0409(12) 0.0272(10) 0.0210(10) -0.0039(8) -0.0092(9) -0.0064(9) C49 0.0333(11) 0.0250(10) 0.0231(10) 0.0055(8) -0.0123(8) -0.0046(8) C50 0.0250(10) 0.0168(9) 0.0219(9) 0.0030(7) -0.0054(8) -0.0029(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 N2 2.0321(15) . ? Pd1 N1 2.0456(15) . ? Pd1 P2 2.3544(5) . ? Pd1 P1 2.3731(5) . ? N1 C1 1.382(2) . ? N1 S1 1.6381(15) . ? C1 O3 1.218(2) . ? C1 C2 1.499(2) . ? C2 C7 1.382(2) . ? C2 C3 1.387(3) . ? C3 C4 1.396(3) . ? C4 C5 1.391(3) . ? C5 C6 1.390(3) . ? C6 C7 1.379(2) . ? C7 S1 1.7523(18) . ? S1 O1 1.4368(14) . ? S1 O2 1.4392(14) . ? N2 C8 1.377(2) . ? N2 S2 1.6505(15) . ? C8 O6 1.221(2) . ? C8 C9 1.493(2) . ? C9 C10 1.383(2) . ? C9 C14 1.388(2) . ? C10 C11 1.391(3) . ? C11 C12 1.388(3) . ? C12 C13 1.396(3) . ? C13 C14 1.380(3) . ? C14 S2 1.7631(18) . ? S2 O5 1.4388(13) . ? S2 O4 1.4396(13) . ? P1 C15 1.8194(18) . ? P1 C21 1.8226(18) . ? P1 C27 1.8270(18) . ? C15 C20 1.393(3) . ? C15 C16 1.396(3) . ? C16 C17 1.393(3) . ? C17 C18 1.386(3) . ? C18 C19 1.383(3) . ? C19 C20 1.393(3) . ? C21 C26 1.395(3) . ? C21 C22 1.402(3) . ? C22 C23 1.389(3) . ? C23 C24 1.384(3) . ? C24 C25 1.382(3) . ? C25 C26 1.392(3) . ? C27 C32 1.394(2) . ? C27 C28 1.399(2) . ? C28 C29 1.386(2) . ? C29 C30 1.391(3) . ? C30 C31 1.384(3) . ? C31 C32 1.391(3) . ? P2 C45 1.8157(18) . ? P2 C33 1.8191(17) . ? P2 C39 1.8279(18) . ? C33 C34 1.394(2) . ? C33 C38 1.395(2) . ? C34 C35 1.394(2) . ? C35 C36 1.384(3) . ? C36 C37 1.387(3) . ? C37 C38 1.392(3) . ? C39 C40 1.395(3) . ? C39 C44 1.396(3) . ? C40 C41 1.386(3) . ? C41 C42 1.385(3) . ? C42 C43 1.383(3) . ? C43 C44 1.392(3) . ? C45 C46 1.393(3) . ? C45 C50 1.399(2) . ? C46 C47 1.387(3) . ? C47 C48 1.383(3) . ? C48 C49 1.385(3) . ? C49 C50 1.388(3) . ? 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 N2 Pd1 N1 173.05(6) . . ? N2 Pd1 P2 90.52(4) . . ? N1 Pd1 P2 89.21(4) . . ? N2 Pd1 P1 89.53(4) . . ? N1 Pd1 P1 91.18(4) . . ? P2 Pd1 P1 176.310(16) . . ? C1 N1 S1 112.97(12) . . ? C1 N1 Pd1 119.22(11) . . ? S1 N1 Pd1 126.84(8) . . ? O3 C1 N1 124.06(16) . . ? O3 C1 C2 124.99(16) . . ? N1 C1 C2 110.93(15) . . ? C7 C2 C3 119.87(17) . . ? C7 C2 C1 111.84(15) . . ? C3 C2 C1 128.27(16) . . ? C2 C3 C4 118.05(17) . . ? C5 C4 C3 120.99(17) . . ? C6 C5 C4 121.06(17) . . ? C7 C6 C5 116.91(17) . . ? C6 C7 C2 123.11(17) . . ? C6 C7 S1 128.00(14) . . ? C2 C7 S1 108.89(13) . . ? O1 S1 O2 116.14(9) . . ? O1 S1 N1 111.61(8) . . ? O2 S1 N1 110.97(8) . . ? O1 S1 C7 108.88(8) . . ? O2 S1 C7 112.00(9) . . ? N1 S1 C7 95.33(8) . . ? C8 N2 S2 113.30(12) . . ? C8 N2 Pd1 118.80(11) . . ? S2 N2 Pd1 127.20(8) . . ? O6 C8 N2 124.32(16) . . ? O6 C8 C9 124.90(16) . . ? N2 C8 C9 110.72(15) . . ? C10 C9 C14 120.23(17) . . ? C10 C9 C8 126.96(16) . . ? C14 C9 C8 112.47(15) . . ? C9 C10 C11 117.88(17) . . ? C12 C11 C10 121.20(18) . . ? C11 C12 C13 121.27(18) . . ? C14 C13 C12 116.52(18) . . ? C13 C14 C9 122.86(17) . . ? C13 C14 S2 128.67(15) . . ? C9 C14 S2 108.39(13) . . ? O5 S2 O4 116.19(8) . . ? O5 S2 N2 111.65(8) . . ? O4 S2 N2 110.11(8) . . ? O5 S2 C14 110.25(8) . . ? O4 S2 C14 111.95(8) . . ? N2 S2 C14 94.66(8) . . ? C15 P1 C21 109.12(8) . . ? C15 P1 C27 104.61(8) . . ? C21 P1 C27 98.29(8) . . ? C15 P1 Pd1 108.79(6) . . ? C21 P1 Pd1 114.92(6) . . ? C27 P1 Pd1 120.15(6) . . ? C20 C15 C16 119.69(17) . . ? C20 C15 P1 123.80(14) . . ? C16 C15 P1 116.50(14) . . ? C17 C16 C15 119.99(18) . . ? C18 C17 C16 120.23(18) . . ? C19 C18 C17 119.70(18) . . ? C18 C19 C20 120.79(18) . . ? C15 C20 C19 119.60(18) . . ? C26 C21 C22 118.95(17) . . ? C26 C21 P1 120.99(14) . . ? C22 C21 P1 119.89(14) . . ? C23 C22 C21 120.2(2) . . ? C24 C23 C22 120.4(2) . . ? C25 C24 C23 119.86(19) . . ? C24 C25 C26 120.4(2) . . ? C25 C26 C21 120.19(18) . . ? C32 C27 C28 119.10(16) . . ? C32 C27 P1 122.34(14) . . ? C28 C27 P1 118.19(13) . . ? C29 C28 C27 120.85(17) . . ? C28 C29 C30 119.55(17) . . ? C31 C30 C29 120.04(17) . . ? C30 C31 C32 120.57(17) . . ? C31 C32 C27 119.85(17) . . ? C45 P2 C33 111.42(8) . . ? C45 P2 C39 104.70(8) . . ? C33 P2 C39 102.37(8) . . ? C45 P2 Pd1 108.76(6) . . ? C33 P2 Pd1 111.40(6) . . ? C39 P2 Pd1 117.93(6) . . ? C34 C33 C38 119.52(16) . . ? C34 C33 P2 116.61(13) . . ? C38 C33 P2 123.84(14) . . ? C35 C34 C33 119.95(16) . . ? C36 C35 C34 120.36(17) . . ? C35 C36 C37 119.87(17) . . ? C36 C37 C38 120.26(17) . . ? C37 C38 C33 120.04(17) . . ? C40 C39 C44 119.08(17) . . ? C40 C39 P2 119.08(14) . . ? C44 C39 P2 121.82(14) . . ? C41 C40 C39 120.69(17) . . ? C42 C41 C40 120.04(18) . . ? C43 C42 C41 119.72(18) . . ? C42 C43 C44 120.70(19) . . ? C43 C44 C39 119.74(18) . . ? C46 C45 C50 119.09(16) . . ? C46 C45 P2 117.92(13) . . ? C50 C45 P2 122.87(14) . . ? C47 C46 C45 120.65(18) . . ? C48 C47 C46 120.03(19) . . ? C47 C48 C49 119.85(19) . . ? C48 C49 C50 120.61(19) . . ? C49 C50 C45 119.77(18) . . ? _diffrn_measured_fraction_theta_max 0.942 _diffrn_reflns_theta_full 0.50 _diffrn_measured_fraction_theta_full 0.000 _refine_diff_density_max 0.812 _refine_diff_density_min -0.407 _refine_diff_density_rms 0.101 #===END data_compound_4b _database_code_depnum_ccdc_archive 'CCDC 817740' #TrackingRef '- CrystalData.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C50 H38 N2 O6 P2 Pd S2, C H2 CL2' _chemical_formula_sum 'C51 H40 Cl2 N2 O6 P2 Pd S2' _chemical_formula_weight 1080.21 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' S S 0.1246 0.1234 '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 11.5868(12) _cell_length_b 12.4344(13) _cell_length_c 17.7515(18) _cell_angle_alpha 73.790(2) _cell_angle_beta 85.524(2) _cell_angle_gamma 69.586(2) _cell_volume 2301.1(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.559 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1100 _exptl_absorpt_coefficient_mu 0.734 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8671 _exptl_absorpt_correction_T_max 0.9855 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 28830 _diffrn_reflns_av_R_equivalents 0.0283 _diffrn_reflns_av_sigmaI/netI 0.0375 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.19 _diffrn_reflns_theta_max 28.70 _reflns_number_total 10860 _reflns_number_gt 9981 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^)+(0.0795P)^2^+12.7774P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10860 _refine_ls_number_parameters 595 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0665 _refine_ls_R_factor_gt 0.0612 _refine_ls_wR_factor_ref 0.1699 _refine_ls_wR_factor_gt 0.1661 _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_restrained_S_all 1.105 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.78368(3) 0.95174(3) 0.736410(17) 0.00873(10) Uani 1 1 d . . . N1 N 0.6746(3) 1.1218(3) 0.6865(2) 0.0113(6) Uani 1 1 d . . . C1 C 0.6316(4) 1.1546(4) 0.6110(2) 0.0126(8) Uani 1 1 d . . . O3 O 0.6663(3) 1.0921(3) 0.56542(18) 0.0163(6) Uani 1 1 d . . . C2 C 0.5348(4) 1.2759(4) 0.5922(2) 0.0130(8) Uani 1 1 d . . . C3 C 0.4659(4) 1.3375(4) 0.5228(3) 0.0169(8) Uani 1 1 d . . . H3 H 0.4788 1.3047 0.4793 0.020 Uiso 1 1 calc R . . C4 C 0.3778(4) 1.4486(4) 0.5194(3) 0.0212(9) Uani 1 1 d . . . H4 H 0.3296 1.4922 0.4727 0.025 Uiso 1 1 calc R . . C5 C 0.3589(4) 1.4971(4) 0.5830(3) 0.0216(9) Uani 1 1 d . . . H5 H 0.2983 1.5733 0.5791 0.026 Uiso 1 1 calc R . . C6 C 0.4279(4) 1.4350(4) 0.6526(3) 0.0205(9) Uani 1 1 d . . . H6 H 0.4159 1.4675 0.6963 0.025 Uiso 1 1 calc R . . C7 C 0.5141(4) 1.3248(4) 0.6551(2) 0.0137(8) Uani 1 1 d . . . S1 S 0.61393(9) 1.22484(9) 0.73332(6) 0.0124(2) Uani 1 1 d . . . O1 O 0.7030(3) 1.2737(3) 0.74779(19) 0.0189(6) Uani 1 1 d . . . O2 O 0.5478(3) 1.1828(3) 0.80053(18) 0.0192(6) Uani 1 1 d . . . N2 N 0.8927(3) 0.7780(3) 0.7773(2) 0.0121(7) Uani 1 1 d . . . C8 C 0.9638(4) 0.7156(4) 0.7271(2) 0.0138(8) Uani 1 1 d . . . O6 O 0.9633(3) 0.7555(3) 0.65613(18) 0.0191(6) Uani 1 1 d . . . C9 C 1.0425(4) 0.5937(4) 0.7715(3) 0.0170(8) Uani 1 1 d . . . C10 C 1.0280(4) 0.5746(4) 0.8513(3) 0.0211(9) Uani 1 1 d . . . C11 C 1.0934(6) 0.4686(5) 0.9036(3) 0.0383(14) Uani 1 1 d . . . H11 H 1.0809 0.4551 0.9585 0.046 Uiso 1 1 calc R . . C12 C 1.1781(6) 0.3828(5) 0.8726(4) 0.0450(17) Uani 1 1 d . . . H12 H 1.2260 0.3094 0.9071 0.054 Uiso 1 1 calc R . . C13 C 1.1945(6) 0.4015(5) 0.7928(4) 0.0367(14) Uani 1 1 d . . . H13 H 1.2538 0.3412 0.7733 0.044 Uiso 1 1 calc R . . C14 C 1.1262(5) 0.5063(4) 0.7410(3) 0.0246(10) Uani 1 1 d . . . H14 H 1.1362 0.5185 0.6860 0.030 Uiso 1 1 calc R . . S2 S 0.91378(10) 0.70072(9) 0.86979(6) 0.0147(2) Uani 1 1 d . . . O4 O 0.8078(3) 0.6703(3) 0.90089(19) 0.0225(7) Uani 1 1 d . . . O5 O 0.9600(3) 0.7576(3) 0.9141(2) 0.0250(7) Uani 1 1 d . . . P1 P 0.60827(10) 0.89398(9) 0.74802(6) 0.0116(2) Uani 1 1 d . . . C15 C 0.5437(4) 0.8788(4) 0.8453(2) 0.0133(8) Uani 1 1 d . . . C16 C 0.4343(4) 0.8527(4) 0.8588(3) 0.0191(9) Uani 1 1 d . . . H16 H 0.3930 0.8469 0.8167 0.023 Uiso 1 1 calc R . . C17 C 0.3858(5) 0.8354(4) 0.9340(3) 0.0252(10) Uani 1 1 d . . . H17 H 0.3121 0.8169 0.9435 0.030 Uiso 1 1 calc R . . C18 C 0.4462(5) 0.8454(4) 0.9945(3) 0.0280(11) Uani 1 1 d . . . H18 H 0.4140 0.8327 1.0458 0.034 Uiso 1 1 calc R . . C19 C 0.5526(5) 0.8736(4) 0.9815(3) 0.0236(10) Uani 1 1 d . . . H19 H 0.5922 0.8814 1.0236 0.028 Uiso 1 1 calc R . . C20 C 0.6021(4) 0.8905(4) 0.9065(3) 0.0173(8) Uani 1 1 d . . . H20 H 0.6752 0.9100 0.8975 0.021 Uiso 1 1 calc R . . C21 C 0.6488(4) 0.7510(4) 0.7262(3) 0.0135(8) Uani 1 1 d . . . C22 C 0.7080(4) 0.7404(4) 0.6554(3) 0.0154(8) Uani 1 1 d . . . H22 H 0.7241 0.8069 0.6206 0.019 Uiso 1 1 calc R . . C23 C 0.7431(4) 0.6331(4) 0.6360(3) 0.0186(9) Uani 1 1 d . . . H23 H 0.7824 0.6263 0.5877 0.022 Uiso 1 1 calc R . . C24 C 0.7210(4) 0.5351(4) 0.6872(3) 0.0202(9) Uani 1 1 d . . . H24 H 0.7442 0.4619 0.6736 0.024 Uiso 1 1 calc R . . C25 C 0.6651(4) 0.5445(4) 0.7581(3) 0.0206(9) Uani 1 1 d . . . H25 H 0.6522 0.4770 0.7937 0.025 Uiso 1 1 calc R . . C26 C 0.6277(4) 0.6526(4) 0.7774(3) 0.0175(9) Uani 1 1 d . . . H26 H 0.5877 0.6592 0.8255 0.021 Uiso 1 1 calc R . . C27 C 0.4750(4) 0.9927(4) 0.6839(2) 0.0124(8) Uani 1 1 d . . . C28 C 0.3913(4) 1.0890(4) 0.7073(3) 0.0153(8) Uani 1 1 d . . . H28 H 0.4029 1.1012 0.7562 0.018 Uiso 1 1 calc R . . C29 C 0.2912(4) 1.1668(4) 0.6591(3) 0.0179(9) Uani 1 1 d . . . H29 H 0.2343 1.2320 0.6753 0.022 Uiso 1 1 calc R . . C30 C 0.2737(4) 1.1501(4) 0.5868(3) 0.0180(9) Uani 1 1 d . . . H30 H 0.2054 1.2039 0.5537 0.022 Uiso 1 1 calc R . . C31 C 0.3566(4) 1.0543(4) 0.5638(3) 0.0179(9) Uani 1 1 d . . . H31 H 0.3450 1.0422 0.5148 0.022 Uiso 1 1 calc R . . C32 C 0.4566(4) 0.9761(4) 0.6120(2) 0.0155(8) Uani 1 1 d . . . H32 H 0.5130 0.9106 0.5959 0.019 Uiso 1 1 calc R . . P2 P 0.95784(10) 1.01120(9) 0.72822(6) 0.0114(2) Uani 1 1 d . . . C33 C 1.1033(4) 0.9013(4) 0.7127(3) 0.0138(8) Uani 1 1 d . . . C34 C 1.1630(4) 0.8079(4) 0.7775(3) 0.0194(9) Uani 1 1 d . . . H34 H 1.1284 0.8040 0.8281 0.023 Uiso 1 1 calc R . . C35 C 1.2730(4) 0.7212(4) 0.7673(3) 0.0221(9) Uani 1 1 d . . . H35 H 1.3132 0.6576 0.8111 0.026 Uiso 1 1 calc R . . C36 C 1.3243(4) 0.7266(4) 0.6939(3) 0.0238(10) Uani 1 1 d . . . H36 H 1.4001 0.6676 0.6877 0.029 Uiso 1 1 calc R . . C37 C 1.2656(4) 0.8179(4) 0.6295(3) 0.0227(10) Uani 1 1 d . . . H37 H 1.3004 0.8209 0.5790 0.027 Uiso 1 1 calc R . . C38 C 1.1561(4) 0.9048(4) 0.6387(3) 0.0179(9) Uani 1 1 d . . . H38 H 1.1163 0.9675 0.5944 0.022 Uiso 1 1 calc R . . C39 C 0.9877(4) 1.0490(4) 0.8146(2) 0.0151(8) Uani 1 1 d . . . C40 C 1.1019(4) 1.0594(4) 0.8241(3) 0.0201(9) Uani 1 1 d . . . H40 H 1.1668 1.0361 0.7895 0.024 Uiso 1 1 calc R . . C41 C 1.1203(5) 1.1036(4) 0.8841(3) 0.0267(11) Uani 1 1 d . . . H41 H 1.1978 1.1104 0.8908 0.032 Uiso 1 1 calc R . . C42 C 1.0246(6) 1.1381(5) 0.9345(3) 0.0321(12) Uani 1 1 d . . . H42 H 1.0361 1.1705 0.9747 0.039 Uiso 1 1 calc R . . C43 C 0.9134(5) 1.1253(5) 0.9259(3) 0.0293(11) Uani 1 1 d . . . H43 H 0.8490 1.1474 0.9611 0.035 Uiso 1 1 calc R . . C44 C 0.8945(4) 1.0806(4) 0.8666(3) 0.0209(9) Uani 1 1 d . . . H44 H 0.8176 1.0715 0.8614 0.025 Uiso 1 1 calc R . . C45 C 0.9451(4) 1.1438(4) 0.6475(2) 0.0145(8) Uani 1 1 d . . . C46 C 0.9623(4) 1.2435(4) 0.6591(3) 0.0160(8) Uani 1 1 d . . . H46 H 0.9766 1.2457 0.7105 0.019 Uiso 1 1 calc R . . C47 C 0.9584(4) 1.3404(4) 0.5949(3) 0.0212(9) Uani 1 1 d . . . H47 H 0.9690 1.4089 0.6029 0.025 Uiso 1 1 calc R . . C48 C 0.9393(4) 1.3366(4) 0.5202(3) 0.0249(11) Uani 1 1 d . . . H48 H 0.9406 1.4011 0.4766 0.030 Uiso 1 1 calc R . . C49 C 0.9181(4) 1.2393(5) 0.5081(3) 0.0237(10) Uani 1 1 d . . . H49 H 0.9030 1.2380 0.4566 0.028 Uiso 1 1 calc R . . C50 C 0.9190(4) 1.1434(4) 0.5721(3) 0.0190(9) Uani 1 1 d . . . H50 H 0.9020 1.0778 0.5643 0.023 Uiso 1 1 calc R . . C51 C 0.6241(8) 0.5516(9) 1.0051(5) 0.071(3) Uani 1 1 d . . . H51A H 0.5617 0.5666 0.9649 0.085 Uiso 1 1 calc R . . H51B H 0.6592 0.6165 0.9888 0.085 Uiso 1 1 calc R . . Cl1 Cl 0.7425(2) 0.41553(19) 1.00710(15) 0.0718(6) Uani 1 1 d . . . Cl2 Cl 0.5488(2) 0.5579(2) 1.09670(15) 0.0802(7) Uani 1 1 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 0.00959(15) 0.00776(15) 0.00905(15) -0.00171(10) 0.00034(10) -0.00368(11) N1 0.0124(16) 0.0103(15) 0.0120(16) -0.0045(13) -0.0005(13) -0.0035(13) C1 0.0130(18) 0.0112(18) 0.0156(19) -0.0020(15) 0.0021(15) -0.0082(15) O3 0.0190(15) 0.0165(15) 0.0153(15) -0.0068(12) 0.0022(12) -0.0069(12) C2 0.0113(18) 0.0117(18) 0.0146(19) -0.0011(15) 0.0004(15) -0.0043(15) C3 0.018(2) 0.018(2) 0.015(2) -0.0015(16) -0.0001(16) -0.0080(17) C4 0.017(2) 0.018(2) 0.024(2) 0.0012(18) -0.0048(18) -0.0048(17) C5 0.017(2) 0.015(2) 0.028(2) -0.0035(18) -0.0003(18) -0.0012(17) C6 0.021(2) 0.015(2) 0.026(2) -0.0070(18) 0.0020(18) -0.0056(18) C7 0.0129(18) 0.0120(19) 0.0149(19) -0.0008(15) -0.0010(15) -0.0047(15) S1 0.0139(5) 0.0097(4) 0.0141(5) -0.0044(4) -0.0006(4) -0.0035(4) O1 0.0205(16) 0.0136(14) 0.0247(17) -0.0066(12) -0.0051(13) -0.0061(12) O2 0.0243(17) 0.0211(16) 0.0144(15) -0.0057(12) 0.0017(12) -0.0101(13) N2 0.0153(16) 0.0103(16) 0.0093(15) -0.0016(12) -0.0001(13) -0.0034(13) C8 0.0164(19) 0.0144(19) 0.0145(19) -0.0046(15) 0.0018(15) -0.0097(16) O6 0.0207(16) 0.0263(17) 0.0116(14) -0.0050(12) 0.0029(12) -0.0101(13) C9 0.018(2) 0.0123(19) 0.019(2) -0.0054(16) 0.0042(17) -0.0039(16) C10 0.021(2) 0.015(2) 0.019(2) -0.0014(17) 0.0061(17) 0.0001(17) C11 0.041(3) 0.025(3) 0.026(3) 0.005(2) 0.006(2) 0.005(2) C12 0.051(4) 0.020(3) 0.039(3) 0.004(2) 0.006(3) 0.008(3) C13 0.035(3) 0.019(2) 0.044(3) -0.010(2) 0.013(3) 0.003(2) C14 0.027(2) 0.020(2) 0.026(2) -0.0104(19) 0.008(2) -0.0043(19) S2 0.0169(5) 0.0122(5) 0.0098(4) -0.0007(4) 0.0020(4) -0.0007(4) O4 0.0244(17) 0.0183(16) 0.0176(16) 0.0010(13) 0.0077(13) -0.0045(13) O5 0.0286(18) 0.0306(19) 0.0156(16) -0.0100(14) -0.0011(13) -0.0064(15) P1 0.0117(5) 0.0106(5) 0.0135(5) -0.0037(4) 0.0017(4) -0.0052(4) C15 0.0160(19) 0.0089(18) 0.0137(19) -0.0033(15) 0.0029(15) -0.0031(15) C16 0.020(2) 0.020(2) 0.020(2) -0.0050(17) 0.0043(17) -0.0099(18) C17 0.027(2) 0.024(2) 0.024(2) -0.0065(19) 0.014(2) -0.010(2) C18 0.037(3) 0.021(2) 0.020(2) -0.0062(19) 0.013(2) -0.005(2) C19 0.031(3) 0.020(2) 0.015(2) -0.0079(17) -0.0013(19) -0.0001(19) C20 0.020(2) 0.0116(19) 0.019(2) -0.0064(16) 0.0002(17) -0.0014(16) C21 0.0110(18) 0.0112(18) 0.019(2) -0.0063(16) -0.0015(15) -0.0032(15) C22 0.0146(19) 0.0128(19) 0.019(2) -0.0037(16) 0.0024(16) -0.0052(16) C23 0.020(2) 0.019(2) 0.017(2) -0.0085(17) 0.0020(17) -0.0044(17) C24 0.025(2) 0.012(2) 0.026(2) -0.0094(17) 0.0004(18) -0.0052(17) C25 0.027(2) 0.011(2) 0.025(2) -0.0036(17) 0.0022(19) -0.0100(18) C26 0.020(2) 0.016(2) 0.019(2) -0.0069(17) 0.0057(17) -0.0092(17) C27 0.0121(18) 0.0119(18) 0.0141(19) -0.0017(15) 0.0007(15) -0.0069(15) C28 0.0154(19) 0.018(2) 0.016(2) -0.0063(16) 0.0022(16) -0.0088(16) C29 0.015(2) 0.015(2) 0.024(2) -0.0083(17) 0.0033(17) -0.0044(16) C30 0.0127(19) 0.020(2) 0.020(2) -0.0030(17) -0.0014(16) -0.0053(17) C31 0.018(2) 0.022(2) 0.015(2) -0.0050(17) 0.0009(16) -0.0086(18) C32 0.017(2) 0.016(2) 0.014(2) -0.0040(16) 0.0025(16) -0.0071(16) P2 0.0120(5) 0.0122(5) 0.0110(5) -0.0031(4) 0.0009(4) -0.0056(4) C33 0.0116(18) 0.0147(19) 0.019(2) -0.0062(16) 0.0016(15) -0.0078(16) C34 0.020(2) 0.019(2) 0.024(2) -0.0076(18) 0.0013(18) -0.0098(18) C35 0.019(2) 0.016(2) 0.032(3) -0.0049(18) -0.0051(19) -0.0059(18) C36 0.015(2) 0.018(2) 0.042(3) -0.018(2) 0.003(2) -0.0041(17) C37 0.020(2) 0.024(2) 0.032(3) -0.017(2) 0.0102(19) -0.0112(19) C38 0.017(2) 0.021(2) 0.019(2) -0.0081(17) 0.0032(17) -0.0094(17) C39 0.018(2) 0.016(2) 0.0124(19) -0.0037(15) -0.0022(16) -0.0066(16) C40 0.021(2) 0.021(2) 0.022(2) -0.0072(18) -0.0006(18) -0.0093(18) C41 0.032(3) 0.023(2) 0.030(3) -0.009(2) -0.010(2) -0.011(2) C42 0.048(3) 0.034(3) 0.020(2) -0.015(2) -0.006(2) -0.013(3) C43 0.036(3) 0.034(3) 0.019(2) -0.014(2) 0.005(2) -0.008(2) C44 0.022(2) 0.022(2) 0.016(2) -0.0035(17) -0.0002(17) -0.0063(18) C45 0.0113(18) 0.016(2) 0.0143(19) -0.0011(15) 0.0021(15) -0.0048(15) C46 0.0108(18) 0.0143(19) 0.020(2) -0.0026(16) 0.0012(16) -0.0022(15) C47 0.014(2) 0.013(2) 0.031(3) 0.0000(18) 0.0013(18) -0.0020(16) C48 0.014(2) 0.026(2) 0.023(2) 0.0109(19) 0.0005(17) -0.0065(18) C49 0.018(2) 0.033(3) 0.015(2) -0.0012(19) 0.0014(17) -0.007(2) C50 0.014(2) 0.026(2) 0.016(2) -0.0049(18) 0.0008(16) -0.0070(18) C51 0.055(5) 0.085(6) 0.054(5) 0.006(4) 0.011(4) -0.022(5) Cl1 0.0776(15) 0.0468(11) 0.0881(16) -0.0028(10) -0.0047(12) -0.0285(10) Cl2 0.0664(14) 0.0729(15) 0.0738(15) 0.0091(12) 0.0072(11) -0.0140(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 N1 2.030(3) . ? Pd1 N2 2.038(3) . ? Pd1 P1 2.3578(11) . ? Pd1 P2 2.3612(11) . ? N1 C1 1.367(5) . ? N1 S1 1.643(3) . ? C1 O3 1.226(5) . ? C1 C2 1.496(6) . ? C2 C7 1.382(6) . ? C2 C3 1.393(6) . ? C3 C4 1.390(6) . ? C4 C5 1.392(7) . ? C5 C6 1.397(7) . ? C6 C7 1.377(6) . ? C7 S1 1.760(4) . ? S1 O1 1.437(3) . ? S1 O2 1.440(3) . ? N2 C8 1.379(5) . ? N2 S2 1.642(4) . ? C8 O6 1.218(5) . ? C8 C9 1.494(6) . ? C9 C10 1.376(6) . ? C9 C14 1.387(6) . ? C10 C11 1.380(7) . ? C10 S2 1.758(5) . ? C11 C12 1.385(8) . ? C12 C13 1.380(9) . ? C13 C14 1.376(8) . ? S2 O5 1.430(4) . ? S2 O4 1.434(4) . ? P1 C15 1.814(4) . ? P1 C21 1.819(4) . ? P1 C27 1.833(4) . ? C15 C20 1.390(6) . ? C15 C16 1.403(6) . ? C16 C17 1.397(6) . ? C17 C18 1.383(8) . ? C18 C19 1.381(8) . ? C19 C20 1.397(6) . ? C21 C26 1.391(6) . ? C21 C22 1.401(6) . ? C22 C23 1.386(6) . ? C23 C24 1.393(6) . ? C24 C25 1.385(7) . ? C25 C26 1.392(6) . ? C27 C32 1.391(6) . ? C27 C28 1.397(6) . ? C28 C29 1.386(6) . ? C29 C30 1.396(6) . ? C30 C31 1.386(6) . ? C31 C32 1.388(6) . ? P2 C39 1.814(4) . ? P2 C33 1.821(4) . ? P2 C45 1.827(4) . ? C33 C38 1.400(6) . ? C33 C34 1.403(6) . ? C34 C35 1.392(7) . ? C35 C36 1.383(7) . ? C36 C37 1.384(8) . ? C37 C38 1.383(6) . ? C39 C44 1.387(6) . ? C39 C40 1.400(6) . ? C40 C41 1.387(7) . ? C41 C42 1.393(8) . ? C42 C43 1.377(8) . ? C43 C44 1.384(7) . ? C45 C46 1.393(6) . ? C45 C50 1.397(6) . ? C46 C47 1.398(6) . ? C47 C48 1.379(7) . ? C48 C49 1.390(8) . ? C49 C50 1.396(7) . ? C51 Cl1 1.761(10) . ? C51 Cl2 1.793(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pd1 N2 174.98(13) . . ? N1 Pd1 P1 88.76(10) . . ? N2 Pd1 P1 90.17(10) . . ? N1 Pd1 P2 91.06(10) . . ? N2 Pd1 P2 90.15(10) . . ? P1 Pd1 P2 178.34(4) . . ? C1 N1 S1 113.8(3) . . ? C1 N1 Pd1 120.5(3) . . ? S1 N1 Pd1 125.1(2) . . ? O3 C1 N1 124.4(4) . . ? O3 C1 C2 124.8(4) . . ? N1 C1 C2 110.8(3) . . ? C7 C2 C3 120.1(4) . . ? C7 C2 C1 111.9(4) . . ? C3 C2 C1 127.9(4) . . ? C4 C3 C2 117.9(4) . . ? C3 C4 C5 121.2(4) . . ? C4 C5 C6 120.8(4) . . ? C7 C6 C5 117.1(4) . . ? C6 C7 C2 122.8(4) . . ? C6 C7 S1 128.2(4) . . ? C2 C7 S1 108.9(3) . . ? O1 S1 O2 116.0(2) . . ? O1 S1 N1 111.46(19) . . ? O2 S1 N1 110.70(19) . . ? O1 S1 C7 110.2(2) . . ? O2 S1 C7 112.0(2) . . ? N1 S1 C7 94.40(19) . . ? C8 N2 S2 113.1(3) . . ? C8 N2 Pd1 121.0(3) . . ? S2 N2 Pd1 125.8(2) . . ? O6 C8 N2 124.3(4) . . ? O6 C8 C9 124.8(4) . . ? N2 C8 C9 110.9(4) . . ? C10 C9 C14 120.4(4) . . ? C10 C9 C8 112.1(4) . . ? C14 C9 C8 127.4(4) . . ? C9 C10 C11 121.9(5) . . ? C9 C10 S2 108.9(3) . . ? C11 C10 S2 129.2(4) . . ? C10 C11 C12 117.1(5) . . ? C13 C12 C11 121.4(5) . . ? C14 C13 C12 120.9(5) . . ? C13 C14 C9 118.1(5) . . ? O5 S2 O4 115.7(2) . . ? O5 S2 N2 110.5(2) . . ? O4 S2 N2 112.0(2) . . ? O5 S2 C10 112.6(2) . . ? O4 S2 C10 109.3(2) . . ? N2 S2 C10 94.9(2) . . ? C15 P1 C21 107.69(19) . . ? C15 P1 C27 103.06(19) . . ? C21 P1 C27 105.15(19) . . ? C15 P1 Pd1 113.27(14) . . ? C21 P1 Pd1 109.48(14) . . ? C27 P1 Pd1 117.46(13) . . ? C20 C15 C16 119.8(4) . . ? C20 C15 P1 121.1(3) . . ? C16 C15 P1 119.1(3) . . ? C17 C16 C15 120.1(4) . . ? C18 C17 C16 119.2(5) . . ? C19 C18 C17 121.1(4) . . ? C18 C19 C20 120.0(5) . . ? C15 C20 C19 119.7(4) . . ? C26 C21 C22 119.6(4) . . ? C26 C21 P1 123.1(3) . . ? C22 C21 P1 117.3(3) . . ? C23 C22 C21 120.0(4) . . ? C22 C23 C24 120.2(4) . . ? C25 C24 C23 119.9(4) . . ? C24 C25 C26 120.2(4) . . ? C21 C26 C25 120.0(4) . . ? C32 C27 C28 119.3(4) . . ? C32 C27 P1 121.9(3) . . ? C28 C27 P1 118.8(3) . . ? C29 C28 C27 120.0(4) . . ? C28 C29 C30 120.4(4) . . ? C31 C30 C29 119.5(4) . . ? C30 C31 C32 120.2(4) . . ? C31 C32 C27 120.6(4) . . ? C39 P2 C33 104.0(2) . . ? C39 P2 C45 104.6(2) . . ? C33 P2 C45 104.48(19) . . ? C39 P2 Pd1 114.54(15) . . ? C33 P2 Pd1 115.35(13) . . ? C45 P2 Pd1 112.71(14) . . ? C38 C33 C34 119.0(4) . . ? C38 C33 P2 122.8(3) . . ? C34 C33 P2 118.2(3) . . ? C35 C34 C33 119.6(4) . . ? C36 C35 C34 120.6(5) . . ? C35 C36 C37 120.2(4) . . ? C38 C37 C36 119.9(5) . . ? C37 C38 C33 120.7(4) . . ? C44 C39 C40 119.5(4) . . ? C44 C39 P2 120.6(3) . . ? C40 C39 P2 119.5(3) . . ? C41 C40 C39 120.1(5) . . ? C40 C41 C42 119.7(5) . . ? C43 C42 C41 120.0(5) . . ? C42 C43 C44 120.6(5) . . ? C43 C44 C39 120.0(5) . . ? C46 C45 C50 119.7(4) . . ? C46 C45 P2 121.9(3) . . ? C50 C45 P2 118.4(3) . . ? C45 C46 C47 119.9(4) . . ? C48 C47 C46 120.1(4) . . ? C47 C48 C49 120.5(4) . . ? C48 C49 C50 119.7(5) . . ? C49 C50 C45 120.0(4) . . ? Cl1 C51 Cl2 114.6(5) . . ? _diffrn_measured_fraction_theta_max 0.912 _diffrn_reflns_theta_full 0.50 _diffrn_measured_fraction_theta_full 0.000 _refine_diff_density_max 0.844 _refine_diff_density_min -2.511 _refine_diff_density_rms 0.161 #===END data_compound_5a _database_code_depnum_ccdc_archive 'CCDC 817741' #TrackingRef '- CrystalData.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H42 N2 O4 P2 Pd' _chemical_formula_sum 'C46 H42 N2 O4 P2 Pd' _chemical_formula_weight 855.16 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' 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' N N 0.0061 0.0033 '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/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 9.3935(4) _cell_length_b 19.6173(9) _cell_length_c 10.4028(5) _cell_angle_alpha 90.00 _cell_angle_beta 104.9470(10) _cell_angle_gamma 90.00 _cell_volume 1852.12(15) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.533 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 880 _exptl_absorpt_coefficient_mu 0.638 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8777 _exptl_absorpt_correction_T_max 0.9332 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 21017 _diffrn_reflns_av_R_equivalents 0.0200 _diffrn_reflns_av_sigmaI/netI 0.0157 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 28.19 _reflns_number_total 4286 _reflns_number_gt 4120 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^)+(0.0418P)^2^+3.0045P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4286 _refine_ls_number_parameters 250 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0273 _refine_ls_R_factor_gt 0.0260 _refine_ls_wR_factor_ref 0.0659 _refine_ls_wR_factor_gt 0.0647 _refine_ls_goodness_of_fit_ref 0.837 _refine_ls_restrained_S_all 0.837 _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 0.5000 0.0000 0.5000 0.00941(6) Uani 1 2 d S . . N1 N 0.47299(15) 0.07941(7) 0.61917(13) 0.0122(3) Uani 1 1 d . . . C1 C 0.56608(18) 0.13449(8) 0.63315(16) 0.0136(3) Uani 1 1 d . . . O1 O 0.65699(13) 0.13882(6) 0.56725(12) 0.0172(2) Uani 1 1 d . . . C2 C 0.55720(19) 0.18890(8) 0.73420(17) 0.0177(3) Uani 1 1 d . . . H2A H 0.6211 0.1758 0.8221 0.021 Uiso 1 1 calc R . . H2B H 0.5946 0.2325 0.7078 0.021 Uiso 1 1 calc R . . C3 C 0.40109(19) 0.19903(8) 0.74581(17) 0.0179(3) Uani 1 1 d . . . H3A H 0.3385 0.2173 0.6613 0.021 Uiso 1 1 calc R . . H3B H 0.4002 0.2320 0.8177 0.021 Uiso 1 1 calc R . . C4 C 0.3419(2) 0.13057(9) 0.77681(19) 0.0226(4) Uani 1 1 d . . . H4A H 0.3904 0.1183 0.8702 0.027 Uiso 1 1 calc R . . H4B H 0.2350 0.1351 0.7689 0.027 Uiso 1 1 calc R . . C5 C 0.36542(18) 0.07340(8) 0.68704(16) 0.0148(3) Uani 1 1 d . . . O2 O 0.29013(14) 0.02172(7) 0.67594(13) 0.0199(3) Uani 1 1 d . . . P1 P 0.32462(4) 0.04896(2) 0.32243(4) 0.01083(9) Uani 1 1 d . . . C6 C 0.23845(18) -0.00889(8) 0.18607(16) 0.0130(3) Uani 1 1 d . . . C7 C 0.2692(2) -0.00234(8) 0.06175(18) 0.0181(3) Uani 1 1 d . . . H7 H 0.3356 0.0320 0.0489 0.022 Uiso 1 1 calc R . . C8 C 0.2037(2) -0.04550(9) -0.04306(17) 0.0212(4) Uani 1 1 d . . . H8 H 0.2241 -0.0400 -0.1273 0.025 Uiso 1 1 calc R . . C9 C 0.10880(19) -0.09652(9) -0.02461(17) 0.0192(3) Uani 1 1 d . . . H9 H 0.0636 -0.1259 -0.0961 0.023 Uiso 1 1 calc R . . C10 C 0.08022(19) -0.10444(9) 0.09900(18) 0.0192(3) Uani 1 1 d . . . H10 H 0.0153 -0.1395 0.1117 0.023 Uiso 1 1 calc R . . C11 C 0.14555(18) -0.06163(8) 0.20452(17) 0.0162(3) Uani 1 1 d . . . H11 H 0.1270 -0.0683 0.2892 0.019 Uiso 1 1 calc R . . C12 C 0.17571(17) 0.09399(8) 0.37121(15) 0.0127(3) Uani 1 1 d . . . C13 C 0.19442(18) 0.16311(8) 0.40411(16) 0.0160(3) Uani 1 1 d . . . H13 H 0.2812 0.1859 0.3967 0.019 Uiso 1 1 calc R . . C14 C 0.0877(2) 0.19897(9) 0.44755(17) 0.0188(3) Uani 1 1 d . . . H14 H 0.1005 0.2462 0.4670 0.023 Uiso 1 1 calc R . . C15 C -0.03763(19) 0.16558(9) 0.46251(17) 0.0180(3) Uani 1 1 d . . . H15 H -0.1097 0.1897 0.4939 0.022 Uiso 1 1 calc R . . C16 C -0.05676(18) 0.09681(9) 0.43128(17) 0.0176(3) Uani 1 1 d . . . H16 H -0.1423 0.0739 0.4413 0.021 Uiso 1 1 calc R . . C17 C 0.04832(18) 0.06134(8) 0.38547(16) 0.0157(3) Uani 1 1 d . . . H17 H 0.0335 0.0144 0.3636 0.019 Uiso 1 1 calc R . . C18 C 0.40125(17) 0.11560(8) 0.23786(15) 0.0123(3) Uani 1 1 d . . . C19 C 0.55245(18) 0.12388(9) 0.26192(16) 0.0158(3) Uani 1 1 d . . . H19 H 0.6174 0.0953 0.3241 0.019 Uiso 1 1 calc R . . C20 C 0.60904(19) 0.17461(9) 0.19416(17) 0.0183(3) Uani 1 1 d . . . H20 H 0.7126 0.1801 0.2097 0.022 Uiso 1 1 calc R . . C21 C 0.51461(19) 0.21664(8) 0.10479(16) 0.0166(3) Uani 1 1 d . . . H21 H 0.5535 0.2512 0.0596 0.020 Uiso 1 1 calc R . . C22 C 0.36268(19) 0.20864(8) 0.08044(16) 0.0163(3) Uani 1 1 d . . . H22 H 0.2981 0.2378 0.0191 0.020 Uiso 1 1 calc R . . C23 C 0.30621(18) 0.15817(8) 0.14588(16) 0.0148(3) Uani 1 1 d . . . H23 H 0.2026 0.1523 0.1285 0.018 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 0.00976(9) 0.00850(9) 0.01023(9) -0.00013(5) 0.00301(6) 0.00018(5) N1 0.0133(6) 0.0112(6) 0.0124(6) -0.0011(5) 0.0039(5) 0.0005(5) C1 0.0147(7) 0.0116(7) 0.0135(7) 0.0014(6) 0.0017(6) 0.0019(6) O1 0.0175(6) 0.0163(6) 0.0196(6) 0.0005(4) 0.0081(5) -0.0018(4) C2 0.0201(8) 0.0140(8) 0.0189(8) -0.0042(6) 0.0049(6) -0.0025(6) C3 0.0215(8) 0.0148(8) 0.0181(8) -0.0044(6) 0.0067(6) 0.0010(6) C4 0.0298(10) 0.0182(8) 0.0260(9) -0.0073(7) 0.0184(8) -0.0047(7) C5 0.0169(8) 0.0141(7) 0.0138(7) 0.0002(6) 0.0047(6) 0.0004(6) O2 0.0221(6) 0.0180(6) 0.0224(6) -0.0028(5) 0.0110(5) -0.0054(5) P1 0.01045(18) 0.01031(18) 0.01175(18) 0.00033(14) 0.00288(14) 0.00035(14) C6 0.0123(7) 0.0116(7) 0.0139(7) -0.0007(5) 0.0012(6) 0.0020(6) C7 0.0208(9) 0.0161(8) 0.0179(8) -0.0009(6) 0.0062(7) -0.0021(6) C8 0.0269(9) 0.0221(9) 0.0145(8) -0.0016(6) 0.0051(7) 0.0004(7) C9 0.0174(8) 0.0185(8) 0.0187(8) -0.0047(6) -0.0007(6) 0.0002(6) C10 0.0157(8) 0.0160(8) 0.0256(9) -0.0036(7) 0.0047(7) -0.0018(6) C11 0.0163(8) 0.0152(8) 0.0172(8) -0.0001(6) 0.0046(6) 0.0014(6) C12 0.0117(7) 0.0141(7) 0.0120(7) 0.0011(5) 0.0025(6) 0.0028(6) C13 0.0159(8) 0.0153(8) 0.0180(8) -0.0002(6) 0.0065(6) -0.0015(6) C14 0.0229(9) 0.0139(8) 0.0213(8) -0.0023(6) 0.0090(7) 0.0005(6) C15 0.0157(8) 0.0205(8) 0.0186(8) -0.0013(6) 0.0062(6) 0.0047(6) C16 0.0128(7) 0.0200(8) 0.0199(8) 0.0007(6) 0.0037(6) -0.0005(6) C17 0.0152(8) 0.0132(7) 0.0185(8) -0.0002(6) 0.0039(6) -0.0013(6) C18 0.0154(7) 0.0103(7) 0.0120(7) -0.0003(5) 0.0054(6) -0.0005(6) C19 0.0142(8) 0.0169(8) 0.0156(7) 0.0014(6) 0.0025(6) 0.0008(6) C20 0.0136(8) 0.0216(8) 0.0197(8) 0.0006(6) 0.0045(6) -0.0038(6) C21 0.0203(8) 0.0137(7) 0.0170(8) -0.0002(6) 0.0069(6) -0.0031(6) C22 0.0187(8) 0.0142(7) 0.0162(8) 0.0027(6) 0.0048(6) 0.0035(6) C23 0.0129(7) 0.0163(7) 0.0159(7) 0.0017(6) 0.0049(6) 0.0016(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N1 2.0470(13) 3_656 ? Pd1 N1 2.0470(13) . ? Pd1 P1 2.3408(4) 3_656 ? Pd1 P1 2.3408(4) . ? N1 C1 1.374(2) . ? N1 C5 1.379(2) . ? C1 O1 1.228(2) . ? C1 C2 1.515(2) . ? C2 C3 1.515(2) . ? C3 C4 1.519(2) . ? C4 C5 1.512(2) . ? C5 O2 1.224(2) . ? P1 C18 1.8242(16) . ? P1 C12 1.8332(16) . ? P1 C6 1.8338(16) . ? C6 C11 1.398(2) . ? C6 C7 1.402(2) . ? C7 C8 1.392(2) . ? C8 C9 1.386(3) . ? C9 C10 1.389(3) . ? C10 C11 1.393(2) . ? C12 C13 1.398(2) . ? C12 C17 1.398(2) . ? C13 C14 1.392(2) . ? C14 C15 1.391(2) . ? C15 C16 1.388(2) . ? C16 C17 1.389(2) . ? C18 C19 1.387(2) . ? C18 C23 1.403(2) . ? C19 C20 1.401(2) . ? C20 C21 1.380(2) . ? C21 C22 1.392(2) . ? C22 C23 1.383(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 N1 Pd1 N1 180 3_656 . ? N1 Pd1 P1 89.64(4) 3_656 3_656 ? N1 Pd1 P1 90.36(4) . 3_656 ? N1 Pd1 P1 90.36(4) 3_656 . ? N1 Pd1 P1 89.64(4) . . ? P1 Pd1 P1 180 3_656 . ? C1 N1 C5 122.93(14) . . ? C1 N1 Pd1 119.19(10) . . ? C5 N1 Pd1 117.81(11) . . ? O1 C1 N1 120.70(14) . . ? O1 C1 C2 120.60(15) . . ? N1 C1 C2 118.68(14) . . ? C3 C2 C1 112.04(14) . . ? C2 C3 C4 108.40(14) . . ? C5 C4 C3 113.88(14) . . ? O2 C5 N1 120.28(15) . . ? O2 C5 C4 119.98(15) . . ? N1 C5 C4 119.73(14) . . ? C18 P1 C12 102.26(7) . . ? C18 P1 C6 102.76(7) . . ? C12 P1 C6 107.23(7) . . ? C18 P1 Pd1 112.93(5) . . ? C12 P1 Pd1 114.28(5) . . ? C6 P1 Pd1 115.90(5) . . ? C11 C6 C7 118.62(15) . . ? C11 C6 P1 121.22(13) . . ? C7 C6 P1 120.12(13) . . ? C8 C7 C6 120.79(16) . . ? C9 C8 C7 120.06(16) . . ? C8 C9 C10 119.60(16) . . ? C9 C10 C11 120.75(16) . . ? C10 C11 C6 120.12(16) . . ? C13 C12 C17 118.36(15) . . ? C13 C12 P1 118.57(12) . . ? C17 C12 P1 122.93(12) . . ? C14 C13 C12 120.93(15) . . ? C15 C14 C13 119.97(16) . . ? C16 C15 C14 119.59(15) . . ? C15 C16 C17 120.43(16) . . ? C16 C17 C12 120.69(15) . . ? C19 C18 C23 119.69(14) . . ? C19 C18 P1 120.67(12) . . ? C23 C18 P1 119.63(12) . . ? C18 C19 C20 119.75(15) . . ? C21 C20 C19 120.12(15) . . ? C20 C21 C22 120.37(15) . . ? C23 C22 C21 119.78(15) . . ? C22 C23 C18 120.29(15) . . ? _diffrn_measured_fraction_theta_max 0.942 _diffrn_reflns_theta_full 0.50 _diffrn_measured_fraction_theta_full 0.000 _refine_diff_density_max 0.551 _refine_diff_density_min -0.281 _refine_diff_density_rms 0.066 #===END data_compound_4c _database_code_depnum_ccdc_archive 'CCDC 817742' #TrackingRef '- CrystalData.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H18 N4 O6 Pd S2' _chemical_formula_sum 'C24 H18 N4 O6 Pd S2' _chemical_formula_weight 628.94 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 7.9905(7) _cell_length_b 8.2529(7) _cell_length_c 10.1032(9) _cell_angle_alpha 89.6280(10) _cell_angle_beta 74.4790(10) _cell_angle_gamma 72.6580(10) _cell_volume 610.83(9) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.710 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 316 _exptl_absorpt_coefficient_mu 0.980 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8670 _exptl_absorpt_correction_T_max 0.9526 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 7519 _diffrn_reflns_av_R_equivalents 0.0180 _diffrn_reflns_av_sigmaI/netI 0.0206 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 28.63 _reflns_number_total 2869 _reflns_number_gt 2798 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^)+(0.0465P)^2^+0.5790P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2869 _refine_ls_number_parameters 169 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0232 _refine_ls_R_factor_gt 0.0226 _refine_ls_wR_factor_ref 0.0613 _refine_ls_wR_factor_gt 0.0608 _refine_ls_goodness_of_fit_ref 0.878 _refine_ls_restrained_S_all 0.878 _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 0.5000 0.0000 0.0000 0.01228(7) Uani 1 2 d S . . N1 N 0.70758(19) -0.05789(18) -0.17531(15) 0.0153(3) Uani 1 1 d . . . C1 C 0.8623(2) -0.0088(2) -0.19877(17) 0.0148(3) Uani 1 1 d . . . O3 O 0.88167(17) 0.09490(16) -0.12352(13) 0.0202(3) Uani 1 1 d . . . C2 C 1.0011(2) -0.1005(2) -0.32770(17) 0.0147(3) Uani 1 1 d . . . C3 C 1.1779(2) -0.0943(2) -0.38087(18) 0.0181(3) Uani 1 1 d . . . H3 H 1.2233 -0.0218 -0.3371 0.022 Uiso 1 1 calc R . . C4 C 1.2879(2) -0.1975(2) -0.50066(19) 0.0211(3) Uani 1 1 d . . . H4 H 1.4104 -0.1973 -0.5374 0.025 Uiso 1 1 calc R . . C5 C 1.2197(3) -0.3008(2) -0.56674(18) 0.0204(3) Uani 1 1 d . . . H5 H 1.2961 -0.3689 -0.6485 0.024 Uiso 1 1 calc R . . C6 C 1.0415(2) -0.3055(2) -0.51477(18) 0.0191(3) Uani 1 1 d . . . H6 H 0.9936 -0.3739 -0.5603 0.023 Uiso 1 1 calc R . . C7 C 0.9371(2) -0.2064(2) -0.39386(17) 0.0153(3) Uani 1 1 d . . . S1 S 0.71790(5) -0.19900(5) -0.29309(4) 0.01613(10) Uani 1 1 d . . . O1 O 0.58043(18) -0.13211(19) -0.36307(14) 0.0264(3) Uani 1 1 d . . . O2 O 0.72315(19) -0.36068(16) -0.23569(14) 0.0230(3) Uani 1 1 d . . . N2 N 0.36873(19) 0.20885(18) -0.07906(14) 0.0145(3) Uani 1 1 d . . . C8 C 0.4402(2) 0.3378(2) -0.10690(18) 0.0186(3) Uani 1 1 d . . . H8 H 0.5540 0.3286 -0.0902 0.022 Uiso 1 1 calc R . . C9 C 0.3513(3) 0.4839(2) -0.1594(2) 0.0230(4) Uani 1 1 d . . . H9 H 0.4031 0.5741 -0.1781 0.028 Uiso 1 1 calc R . . C10 C 0.1852(3) 0.4962(2) -0.1841(2) 0.0247(4) Uani 1 1 d . . . H10 H 0.1224 0.5948 -0.2207 0.030 Uiso 1 1 calc R . . C11 C 0.1124(2) 0.3632(3) -0.15486(19) 0.0223(4) Uani 1 1 d . . . H11 H -0.0010 0.3693 -0.1710 0.027 Uiso 1 1 calc R . . C12 C 0.2075(2) 0.2208(2) -0.10164(17) 0.0168(3) Uani 1 1 d . . . H12 H 0.1574 0.1298 -0.0807 0.020 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 0.01023(9) 0.01250(10) 0.01386(10) 0.00162(6) -0.00366(6) -0.00286(6) N1 0.0135(6) 0.0161(6) 0.0166(7) -0.0005(5) -0.0038(5) -0.0055(5) C1 0.0131(7) 0.0146(7) 0.0165(7) 0.0038(6) -0.0051(6) -0.0029(6) O3 0.0188(6) 0.0213(6) 0.0209(6) -0.0029(5) -0.0043(5) -0.0078(5) C2 0.0148(7) 0.0133(7) 0.0158(7) 0.0031(6) -0.0058(6) -0.0028(6) C3 0.0154(8) 0.0178(8) 0.0214(8) 0.0026(6) -0.0049(6) -0.0057(6) C4 0.0155(8) 0.0218(8) 0.0231(9) 0.0040(7) -0.0018(7) -0.0047(7) C5 0.0202(8) 0.0191(8) 0.0168(8) -0.0002(6) -0.0006(7) -0.0027(7) C6 0.0224(9) 0.0182(8) 0.0173(8) 0.0019(6) -0.0055(7) -0.0072(7) C7 0.0137(7) 0.0166(7) 0.0158(7) 0.0034(6) -0.0046(6) -0.0043(6) S1 0.0141(2) 0.0192(2) 0.0164(2) -0.00037(15) -0.00420(15) -0.00711(16) O1 0.0185(6) 0.0385(8) 0.0261(7) 0.0000(6) -0.0113(5) -0.0097(6) O2 0.0261(7) 0.0197(6) 0.0238(7) -0.0005(5) -0.0013(5) -0.0127(5) N2 0.0134(6) 0.0145(6) 0.0143(6) 0.0008(5) -0.0034(5) -0.0026(5) C8 0.0162(8) 0.0189(8) 0.0204(8) 0.0021(6) -0.0045(6) -0.0057(6) C9 0.0224(9) 0.0176(8) 0.0287(9) 0.0063(7) -0.0053(7) -0.0075(7) C10 0.0242(9) 0.0203(8) 0.0282(9) 0.0088(7) -0.0095(8) -0.0027(7) C11 0.0179(8) 0.0251(8) 0.0250(9) 0.0048(7) -0.0105(7) -0.0043(7) C12 0.0156(8) 0.0178(8) 0.0176(8) 0.0013(6) -0.0056(6) -0.0050(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N2 2.0154(14) 2_655 ? Pd1 N2 2.0154(14) . ? Pd1 N1 2.0206(14) . ? Pd1 N1 2.0206(14) 2_655 ? N1 C1 1.374(2) . ? N1 S1 1.6393(14) . ? C1 O3 1.219(2) . ? C1 C2 1.496(2) . ? C2 C7 1.389(2) . ? C2 C3 1.387(2) . ? C3 C4 1.400(3) . ? C4 C5 1.395(3) . ? C5 C6 1.392(3) . ? C6 C7 1.385(2) . ? C7 S1 1.7582(17) . ? S1 O1 1.4354(14) . ? S1 O2 1.4450(13) . ? N2 C12 1.342(2) . ? N2 C8 1.345(2) . ? C8 C9 1.386(2) . ? C9 C10 1.389(3) . ? C10 C11 1.384(3) . ? C11 C12 1.388(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 N2 Pd1 N2 180 2_655 . ? N2 Pd1 N1 89.69(6) 2_655 . ? N2 Pd1 N1 90.31(6) . . ? N2 Pd1 N1 90.31(6) 2_655 2_655 ? N2 Pd1 N1 89.69(6) . 2_655 ? N1 Pd1 N1 180 . 2_655 ? C1 N1 S1 113.74(12) . . ? C1 N1 Pd1 125.33(11) . . ? S1 N1 Pd1 120.14(8) . . ? O3 C1 N1 123.91(16) . . ? O3 C1 C2 125.45(15) . . ? N1 C1 C2 110.64(14) . . ? C7 C2 C3 119.92(16) . . ? C7 C2 C1 112.10(15) . . ? C3 C2 C1 127.94(15) . . ? C2 C3 C4 118.28(16) . . ? C5 C4 C3 120.81(17) . . ? C6 C5 C4 121.05(16) . . ? C7 C6 C5 117.13(16) . . ? C6 C7 C2 122.76(16) . . ? C6 C7 S1 128.57(13) . . ? C2 C7 S1 108.55(12) . . ? O1 S1 O2 116.31(9) . . ? O1 S1 N1 110.86(8) . . ? O2 S1 N1 110.39(8) . . ? O1 S1 C7 112.49(8) . . ? O2 S1 C7 109.88(8) . . ? N1 S1 C7 94.88(8) . . ? C12 N2 C8 119.78(15) . . ? C12 N2 Pd1 119.87(11) . . ? C8 N2 Pd1 120.33(12) . . ? N2 C8 C9 121.46(16) . . ? C10 C9 C8 118.97(17) . . ? C11 C10 C9 119.23(17) . . ? C10 C11 C12 119.05(17) . . ? N2 C12 C11 121.51(16) . . ? _diffrn_measured_fraction_theta_max 0.915 _diffrn_reflns_theta_full 0.50 _diffrn_measured_fraction_theta_full 0.000 _refine_diff_density_max 0.629 _refine_diff_density_min -0.700 _refine_diff_density_rms 0.081 #===END data_compound_2c _database_code_depnum_ccdc_archive 'CCDC 817743' #TrackingRef '- CrystalData.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H32 N2 O4 P2 Pd, 2(C H Cl3), H2 O' _chemical_formula_sum 'C48 H36 Cl6 N2 O5 P2 Pd' _chemical_formula_weight 1101.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 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 11.3871(8) _cell_length_b 18.2940(13) _cell_length_c 23.2075(17) _cell_angle_alpha 90.00 _cell_angle_beta 103.7600(10) _cell_angle_gamma 90.00 _cell_volume 4695.7(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.559 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2224 _exptl_absorpt_coefficient_mu 0.854 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8546 _exptl_absorpt_correction_T_max 0.9195 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 53623 _diffrn_reflns_av_R_equivalents 0.0259 _diffrn_reflns_av_sigmaI/netI 0.0214 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 28.20 _reflns_number_total 10921 _reflns_number_gt 10156 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^)+(0.0385P)^2^+9.7004P] 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 10921 _refine_ls_number_parameters 593 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0449 _refine_ls_R_factor_gt 0.0411 _refine_ls_wR_factor_ref 0.0967 _refine_ls_wR_factor_gt 0.0943 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _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 0.043008(16) 0.250366(9) 0.368055(8) 0.01246(6) Uani 1 1 d . . . N1 N 0.19835(19) 0.22928(12) 0.43414(9) 0.0171(4) Uani 1 1 d . . . C1 C 0.2649(2) 0.28428(14) 0.46699(11) 0.0201(5) Uani 1 1 d . . . O1 O 0.23351(19) 0.34810(11) 0.46751(10) 0.0320(5) Uani 1 1 d . . . C2 C 0.3820(2) 0.25274(14) 0.50211(11) 0.0189(5) Uani 1 1 d . . . C3 C 0.4806(2) 0.28532(15) 0.53938(12) 0.0233(5) Uani 1 1 d . . . H3 H 0.4822 0.3352 0.5474 0.028 Uiso 1 1 calc R . . C4 C 0.5785(2) 0.23962(16) 0.56462(12) 0.0246(6) Uani 1 1 d . . . H4 H 0.6469 0.2595 0.5899 0.029 Uiso 1 1 calc R . . C5 C 0.5748(2) 0.16550(16) 0.55239(12) 0.0246(6) Uani 1 1 d . . . H5 H 0.6402 0.1363 0.5702 0.030 Uiso 1 1 calc R . . C6 C 0.4750(2) 0.13370(15) 0.51391(12) 0.0233(5) Uani 1 1 d . . . H6 H 0.4732 0.0840 0.5052 0.028 Uiso 1 1 calc R . . C7 C 0.3791(2) 0.17870(14) 0.48927(11) 0.0176(5) Uani 1 1 d . . . C8 C 0.2606(2) 0.16364(14) 0.44551(11) 0.0178(5) Uani 1 1 d . . . O2 O 0.22535(18) 0.10453(10) 0.42448(9) 0.0253(4) Uani 1 1 d . . . N2 N 0.14976(19) 0.27601(11) 0.30925(9) 0.0164(4) Uani 1 1 d . . . C9 C 0.1767(2) 0.34499(13) 0.29196(11) 0.0179(5) Uani 1 1 d . . . O3 O 0.14337(18) 0.40293(10) 0.30857(9) 0.0256(4) Uani 1 1 d . . . C10 C 0.2563(2) 0.33643(14) 0.24933(11) 0.0190(5) Uani 1 1 d . . . C11 C 0.3035(3) 0.38773(16) 0.21724(12) 0.0266(6) Uani 1 1 d . . . H11 H 0.2884 0.4374 0.2200 0.032 Uiso 1 1 calc R . . C12 C 0.3746(3) 0.36137(18) 0.18061(13) 0.0321(7) Uani 1 1 d . . . H12 H 0.4072 0.3942 0.1580 0.038 Uiso 1 1 calc R . . C13 C 0.3980(3) 0.28721(19) 0.17698(13) 0.0305(6) Uani 1 1 d . . . H13 H 0.4466 0.2714 0.1524 0.037 Uiso 1 1 calc R . . C14 C 0.3496(2) 0.23583(16) 0.20971(12) 0.0246(6) Uani 1 1 d . . . H14 H 0.3650 0.1861 0.2076 0.029 Uiso 1 1 calc R . . C15 C 0.2780(2) 0.26259(14) 0.24528(11) 0.0184(5) Uani 1 1 d . . . C16 C 0.2071(2) 0.22398(14) 0.28294(11) 0.0161(5) Uani 1 1 d . . . O4 O 0.19840(17) 0.15773(10) 0.28810(8) 0.0212(4) Uani 1 1 d . . . P1 P -0.08043(6) 0.22781(3) 0.42842(3) 0.01414(12) Uani 1 1 d . . . C17 C -0.2245(2) 0.27281(13) 0.39759(11) 0.0154(5) Uani 1 1 d . . . C18 C -0.3126(2) 0.28473(14) 0.42927(11) 0.0198(5) Uani 1 1 d . . . H18 H -0.2995 0.2695 0.4685 0.024 Uiso 1 1 calc R . . C19 C -0.4197(2) 0.31931(14) 0.40216(12) 0.0209(5) Uani 1 1 d . . . H19 H -0.4784 0.3273 0.4233 0.025 Uiso 1 1 calc R . . C20 C -0.4400(2) 0.34221(14) 0.34340(12) 0.0201(5) Uani 1 1 d . . . H20 H -0.5120 0.3656 0.3256 0.024 Uiso 1 1 calc R . . C21 C -0.3536(2) 0.33036(13) 0.31146(11) 0.0184(5) Uani 1 1 d . . . H21 H -0.3675 0.3457 0.2722 0.022 Uiso 1 1 calc R . . C22 C -0.2453(2) 0.29526(13) 0.33828(11) 0.0153(4) Uani 1 1 d . . . C23 C -0.1170(2) 0.13241(13) 0.43723(11) 0.0162(5) Uani 1 1 d . . . C24 C -0.0812(3) 0.07916(14) 0.40207(12) 0.0233(5) Uani 1 1 d . . . H24 H -0.0353 0.0919 0.3754 0.028 Uiso 1 1 calc R . . C25 C -0.1147(3) 0.00631(15) 0.40716(14) 0.0296(6) Uani 1 1 d . . . H25 H -0.0924 -0.0293 0.3832 0.036 Uiso 1 1 calc R . . C26 C -0.1806(3) -0.01283(15) 0.44745(14) 0.0270(6) Uani 1 1 d . . . H26 H -0.2024 -0.0614 0.4507 0.032 Uiso 1 1 calc R . . C27 C -0.2148(2) 0.03980(15) 0.48324(12) 0.0240(5) Uani 1 1 d . . . H27 H -0.2581 0.0264 0.5109 0.029 Uiso 1 1 calc R . . C28 C -0.1844(2) 0.11230(14) 0.47770(12) 0.0214(5) Uani 1 1 d . . . H28 H -0.2089 0.1478 0.5011 0.026 Uiso 1 1 calc R . . C29 C -0.0281(2) 0.26231(14) 0.50316(11) 0.0167(5) Uani 1 1 d . . . C30 C 0.0409(2) 0.21745(14) 0.54707(11) 0.0207(5) Uani 1 1 d . . . H30 H 0.0575 0.1696 0.5381 0.025 Uiso 1 1 calc R . . C31 C 0.0844(3) 0.24425(16) 0.60386(12) 0.0265(6) Uani 1 1 d . . . H31 H 0.1299 0.2142 0.6331 0.032 Uiso 1 1 calc R . . C32 C 0.0605(3) 0.31576(17) 0.61744(12) 0.0281(6) Uani 1 1 d . . . H32 H 0.0894 0.3333 0.6558 0.034 Uiso 1 1 calc R . . C33 C -0.0065(3) 0.36106(16) 0.57388(13) 0.0283(6) Uani 1 1 d . . . H33 H -0.0223 0.4090 0.5830 0.034 Uiso 1 1 calc R . . C34 C -0.0501(2) 0.33456(15) 0.51654(12) 0.0231(5) Uani 1 1 d . . . H34 H -0.0940 0.3651 0.4871 0.028 Uiso 1 1 calc R . . P2 P -0.12848(5) 0.27329(3) 0.29989(3) 0.01326(12) Uani 1 1 d . . . C35 C -0.1820(2) 0.19369(13) 0.25424(10) 0.0164(5) Uani 1 1 d . . . C36 C -0.1007(2) 0.13897(14) 0.24876(12) 0.0220(5) Uani 1 1 d . . . H36 H -0.0197 0.1430 0.2685 0.026 Uiso 1 1 calc R . . C37 C -0.1409(3) 0.07798(15) 0.21353(13) 0.0270(6) Uani 1 1 d . . . H37 H -0.0866 0.0414 0.2097 0.032 Uiso 1 1 calc R . . C38 C -0.2615(3) 0.07180(15) 0.18431(12) 0.0254(6) Uani 1 1 d . . . H38 H -0.2882 0.0311 0.1609 0.030 Uiso 1 1 calc R . . C39 C -0.3422(3) 0.12616(16) 0.19000(13) 0.0285(6) Uani 1 1 d . . . H39 H -0.4232 0.1219 0.1703 0.034 Uiso 1 1 calc R . . C40 C -0.3029(2) 0.18709(15) 0.22496(12) 0.0244(6) Uani 1 1 d . . . H40 H -0.3576 0.2235 0.2288 0.029 Uiso 1 1 calc R . . C41 C -0.1299(2) 0.34758(13) 0.24803(11) 0.0162(5) Uani 1 1 d . . . C42 C -0.1129(2) 0.33350(14) 0.19152(11) 0.0195(5) Uani 1 1 d . . . H42 H -0.1021 0.2858 0.1799 0.023 Uiso 1 1 calc R . . C43 C -0.1121(3) 0.39122(16) 0.15259(12) 0.0251(6) Uani 1 1 d . . . H43 H -0.1002 0.3820 0.1150 0.030 Uiso 1 1 calc R . . C44 C -0.1291(2) 0.46249(16) 0.16948(13) 0.0263(6) Uani 1 1 d . . . H44 H -0.1306 0.5007 0.1429 0.032 Uiso 1 1 calc R . . C45 C -0.1438(2) 0.47641(14) 0.22593(13) 0.0244(6) Uani 1 1 d . . . H45 H -0.1534 0.5243 0.2375 0.029 Uiso 1 1 calc R . . C46 C -0.1444(2) 0.41947(14) 0.26546(12) 0.0192(5) Uani 1 1 d . . . H46 H -0.1544 0.4292 0.3033 0.023 Uiso 1 1 calc R . . C47 C -0.3072(3) 0.51288(18) 0.45913(15) 0.0351(7) Uani 1 1 d . . . C48 C 0.4272(3) 0.06783(16) 0.33191(14) 0.0308(6) Uani 1 1 d . . . Cl1 Cl -0.44960(9) 0.51500(5) 0.40726(5) 0.0597(3) Uani 1 1 d . . . Cl2 Cl -0.19414(8) 0.48647(4) 0.42394(4) 0.03731(18) Uani 1 1 d . . . Cl3 Cl -0.31200(10) 0.45496(5) 0.51838(4) 0.0508(2) Uani 1 1 d . . . Cl4 Cl 0.46137(7) 0.00027(4) 0.38700(4) 0.03559(17) Uani 1 1 d . . . Cl5 Cl 0.44206(8) 0.03262(5) 0.26302(4) 0.04030(19) Uani 1 1 d . . . Cl6 Cl 0.51733(11) 0.14505(5) 0.35334(5) 0.0626(3) Uani 1 1 d . . . O5 O 0.0250(2) 0.42615(15) 0.39982(12) 0.0406(6) Uani 1 1 d . . . H50 H 0.065(4) 0.426(2) 0.372(2) 0.053(13) Uiso 1 1 d . . . H49 H 0.079(4) 0.408(3) 0.428(2) 0.064(14) Uiso 1 1 d . . . H48 H 0.348(3) 0.0820(18) 0.3278(14) 0.025(8) Uiso 1 1 d . . . H47 H -0.293(3) 0.560(2) 0.4725(16) 0.038(10) Uiso 1 1 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 0.01524(9) 0.00991(9) 0.01156(9) 0.00047(6) 0.00184(7) 0.00001(6) N1 0.0176(10) 0.0169(10) 0.0159(10) 0.0000(8) 0.0020(8) 0.0017(8) C1 0.0230(13) 0.0175(12) 0.0187(12) -0.0020(9) 0.0028(10) -0.0008(10) O1 0.0341(11) 0.0175(10) 0.0357(12) -0.0068(8) -0.0087(9) 0.0038(8) C2 0.0199(12) 0.0202(12) 0.0159(11) 0.0014(9) 0.0031(10) 0.0004(9) C3 0.0244(13) 0.0223(13) 0.0228(13) -0.0007(10) 0.0047(11) -0.0025(10) C4 0.0177(12) 0.0364(16) 0.0186(12) 0.0011(11) 0.0023(10) -0.0030(11) C5 0.0197(12) 0.0332(15) 0.0206(13) 0.0037(11) 0.0040(10) 0.0057(11) C6 0.0242(13) 0.0239(13) 0.0210(13) 0.0021(10) 0.0039(10) 0.0051(10) C7 0.0186(12) 0.0210(12) 0.0135(11) 0.0013(9) 0.0045(9) -0.0010(9) C8 0.0205(12) 0.0177(12) 0.0149(11) 0.0029(9) 0.0039(9) 0.0009(9) O2 0.0288(10) 0.0155(9) 0.0269(10) -0.0013(7) -0.0027(8) 0.0003(7) N2 0.0183(10) 0.0135(9) 0.0169(10) 0.0024(8) 0.0030(8) -0.0005(8) C9 0.0179(11) 0.0158(12) 0.0175(12) 0.0025(9) -0.0009(9) -0.0026(9) O3 0.0293(10) 0.0146(9) 0.0322(11) -0.0009(8) 0.0060(8) -0.0014(7) C10 0.0156(11) 0.0234(13) 0.0156(11) 0.0029(10) -0.0011(9) -0.0043(9) C11 0.0268(14) 0.0265(14) 0.0240(13) 0.0077(11) 0.0010(11) -0.0090(11) C12 0.0281(15) 0.0443(18) 0.0237(14) 0.0113(13) 0.0060(12) -0.0115(13) C13 0.0228(14) 0.0485(19) 0.0215(14) 0.0030(13) 0.0080(11) -0.0036(13) C14 0.0210(13) 0.0303(14) 0.0224(13) 0.0017(11) 0.0051(11) 0.0013(11) C15 0.0153(11) 0.0238(13) 0.0147(11) 0.0025(9) 0.0009(9) -0.0025(9) C16 0.0138(11) 0.0183(12) 0.0148(11) 0.0011(9) 0.0004(9) -0.0006(9) O4 0.0235(9) 0.0146(9) 0.0263(10) 0.0002(7) 0.0078(8) 0.0011(7) P1 0.0177(3) 0.0124(3) 0.0119(3) 0.0008(2) 0.0026(2) 0.0004(2) C17 0.0163(11) 0.0123(10) 0.0165(11) 0.0001(9) 0.0019(9) -0.0001(9) C18 0.0257(13) 0.0181(12) 0.0160(12) -0.0002(9) 0.0055(10) -0.0013(10) C19 0.0206(12) 0.0197(12) 0.0243(13) -0.0032(10) 0.0091(10) -0.0013(10) C20 0.0165(11) 0.0171(12) 0.0248(13) -0.0021(10) 0.0011(10) 0.0007(9) C21 0.0199(12) 0.0164(11) 0.0169(11) 0.0000(9) 0.0002(9) 0.0007(9) C22 0.0170(11) 0.0133(11) 0.0156(11) -0.0018(9) 0.0039(9) -0.0007(9) C23 0.0189(11) 0.0130(11) 0.0157(11) 0.0022(9) 0.0020(9) -0.0002(9) C24 0.0287(14) 0.0174(12) 0.0271(14) 0.0012(10) 0.0131(11) 0.0010(10) C25 0.0367(16) 0.0157(13) 0.0397(17) -0.0026(11) 0.0155(13) 0.0013(11) C26 0.0281(14) 0.0142(12) 0.0396(16) 0.0044(11) 0.0096(12) -0.0011(10) C27 0.0261(13) 0.0219(13) 0.0261(14) 0.0054(11) 0.0106(11) -0.0022(10) C28 0.0252(13) 0.0199(12) 0.0199(12) 0.0002(10) 0.0070(10) 0.0001(10) C29 0.0178(11) 0.0190(12) 0.0130(11) -0.0008(9) 0.0032(9) -0.0006(9) C30 0.0238(13) 0.0184(12) 0.0189(12) 0.0006(10) 0.0031(10) 0.0001(10) C31 0.0295(15) 0.0284(15) 0.0179(13) 0.0040(11) -0.0019(11) 0.0018(11) C32 0.0316(15) 0.0342(16) 0.0157(12) -0.0069(11) -0.0001(11) -0.0023(12) C33 0.0339(15) 0.0239(14) 0.0251(14) -0.0065(11) 0.0033(12) 0.0030(11) C34 0.0283(14) 0.0201(13) 0.0188(12) -0.0002(10) 0.0012(11) 0.0037(10) P2 0.0163(3) 0.0113(3) 0.0115(3) 0.0006(2) 0.0018(2) 0.0002(2) C35 0.0215(12) 0.0129(11) 0.0135(11) 0.0010(9) 0.0017(9) -0.0022(9) C36 0.0193(12) 0.0189(12) 0.0258(13) -0.0048(10) 0.0013(10) 0.0003(10) C37 0.0276(14) 0.0185(13) 0.0331(15) -0.0077(11) 0.0039(12) 0.0023(11) C38 0.0327(15) 0.0174(12) 0.0233(13) -0.0063(10) 0.0012(11) -0.0049(11) C39 0.0242(14) 0.0273(14) 0.0283(15) -0.0073(12) -0.0053(11) -0.0037(11) C40 0.0237(13) 0.0212(13) 0.0249(14) -0.0057(10) -0.0010(11) 0.0038(10) C41 0.0155(11) 0.0148(11) 0.0165(11) 0.0047(9) 0.0006(9) 0.0003(9) C42 0.0220(12) 0.0182(12) 0.0178(12) 0.0018(9) 0.0035(10) -0.0008(10) C43 0.0270(14) 0.0300(14) 0.0178(12) 0.0073(11) 0.0045(11) -0.0017(11) C44 0.0227(13) 0.0244(14) 0.0299(14) 0.0138(11) 0.0021(11) -0.0012(10) C45 0.0195(12) 0.0146(12) 0.0367(15) 0.0060(11) 0.0018(11) 0.0007(9) C46 0.0192(12) 0.0163(12) 0.0211(12) 0.0020(9) 0.0025(10) 0.0006(9) C47 0.0283(15) 0.0321(17) 0.0406(18) -0.0158(14) -0.0003(13) 0.0037(12) C48 0.0309(16) 0.0179(13) 0.0377(17) 0.0020(12) -0.0030(13) 0.0024(11) Cl1 0.0411(5) 0.0404(5) 0.0809(7) -0.0215(5) -0.0188(5) 0.0173(4) Cl2 0.0433(4) 0.0282(4) 0.0425(4) 0.0043(3) 0.0143(3) 0.0038(3) Cl3 0.0668(6) 0.0496(5) 0.0415(5) -0.0074(4) 0.0237(4) -0.0008(4) Cl4 0.0426(4) 0.0268(4) 0.0399(4) 0.0057(3) 0.0148(3) 0.0104(3) Cl5 0.0476(5) 0.0340(4) 0.0413(4) 0.0055(3) 0.0145(4) 0.0020(3) Cl6 0.0770(7) 0.0400(5) 0.0556(6) 0.0073(4) -0.0143(5) -0.0310(5) O5 0.0332(13) 0.0568(16) 0.0315(12) 0.0045(11) 0.0069(11) 0.0145(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N1 2.083(2) . ? Pd1 N2 2.085(2) . ? Pd1 P2 2.2410(6) . ? Pd1 P1 2.2461(6) . ? N1 C1 1.376(3) . ? N1 C8 1.388(3) . ? C1 O1 1.222(3) . ? C1 C2 1.503(4) . ? C2 C3 1.379(4) . ? C2 C7 1.386(4) . ? C3 C4 1.405(4) . ? C4 C5 1.384(4) . ? C5 C6 1.395(4) . ? C6 C7 1.378(4) . ? C7 C8 1.509(3) . ? C8 O2 1.215(3) . ? N2 C16 1.377(3) . ? N2 C9 1.381(3) . ? C9 O3 1.219(3) . ? C9 C10 1.500(4) . ? C10 C15 1.381(4) . ? C10 C11 1.384(4) . ? C11 C12 1.392(4) . ? C12 C13 1.389(5) . ? C13 C14 1.401(4) . ? C14 C15 1.381(4) . ? C15 C16 1.500(3) . ? C16 O4 1.224(3) . ? P1 C29 1.809(3) . ? P1 C23 1.817(2) . ? P1 C17 1.823(2) . ? C17 C18 1.395(3) . ? C17 C22 1.402(3) . ? C18 C19 1.385(4) . ? C19 C20 1.392(4) . ? C20 C21 1.382(4) . ? C21 C22 1.399(3) . ? C22 P2 1.813(2) . ? C23 C24 1.393(4) . ? C23 C28 1.396(4) . ? C24 C25 1.399(4) . ? C25 C26 1.376(4) . ? C26 C27 1.386(4) . ? C27 C28 1.384(4) . ? C29 C34 1.394(4) . ? C29 C30 1.395(3) . ? C30 C31 1.383(4) . ? C31 C32 1.388(4) . ? C32 C33 1.387(4) . ? C33 C34 1.392(4) . ? P2 C41 1.813(2) . ? P2 C35 1.818(2) . ? C35 C40 1.388(4) . ? C35 C36 1.390(4) . ? C36 C37 1.395(4) . ? C37 C38 1.384(4) . ? C38 C39 1.381(4) . ? C39 C40 1.389(4) . ? C41 C42 1.395(3) . ? C41 C46 1.397(3) . ? C42 C43 1.391(4) . ? C43 C44 1.388(4) . ? C44 C45 1.383(4) . ? C45 C46 1.389(4) . ? C47 Cl3 1.747(4) . ? C47 Cl2 1.749(3) . ? C47 Cl1 1.775(3) . ? C48 Cl6 1.747(3) . ? C48 Cl4 1.754(3) . ? C48 Cl5 1.769(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pd1 N2 89.90(8) . . ? N1 Pd1 P2 177.61(6) . . ? N2 Pd1 P2 92.39(6) . . ? N1 Pd1 P1 93.13(6) . . ? N2 Pd1 P1 176.44(6) . . ? P2 Pd1 P1 84.56(2) . . ? C1 N1 C8 109.8(2) . . ? C1 N1 Pd1 122.12(17) . . ? C8 N1 Pd1 127.32(17) . . ? O1 C1 N1 125.5(2) . . ? O1 C1 C2 125.8(2) . . ? N1 C1 C2 108.7(2) . . ? C3 C2 C7 122.1(2) . . ? C3 C2 C1 131.2(2) . . ? C7 C2 C1 106.6(2) . . ? C2 C3 C4 116.8(3) . . ? C5 C4 C3 121.0(3) . . ? C4 C5 C6 121.4(3) . . ? C7 C6 C5 117.5(3) . . ? C6 C7 C2 121.3(2) . . ? C6 C7 C8 131.6(2) . . ? C2 C7 C8 107.2(2) . . ? O2 C8 N1 126.1(2) . . ? O2 C8 C7 126.2(2) . . ? N1 C8 C7 107.7(2) . . ? C16 N2 C9 110.0(2) . . ? C16 N2 Pd1 123.14(16) . . ? C9 N2 Pd1 126.87(17) . . ? O3 C9 N2 126.6(2) . . ? O3 C9 C10 125.6(2) . . ? N2 C9 C10 107.9(2) . . ? C15 C10 C11 121.9(3) . . ? C15 C10 C9 107.0(2) . . ? C11 C10 C9 131.1(3) . . ? C10 C11 C12 116.8(3) . . ? C13 C12 C11 121.5(3) . . ? C12 C13 C14 121.1(3) . . ? C15 C14 C13 116.8(3) . . ? C10 C15 C14 121.9(2) . . ? C10 C15 C16 106.9(2) . . ? C14 C15 C16 131.1(2) . . ? O4 C16 N2 125.7(2) . . ? O4 C16 C15 126.2(2) . . ? N2 C16 C15 108.1(2) . . ? C29 P1 C23 105.03(11) . . ? C29 P1 C17 106.23(11) . . ? C23 P1 C17 105.61(11) . . ? C29 P1 Pd1 114.93(8) . . ? C23 P1 Pd1 116.16(8) . . ? C17 P1 Pd1 108.09(8) . . ? C18 C17 C22 119.8(2) . . ? C18 C17 P1 123.84(19) . . ? C22 C17 P1 116.36(18) . . ? C19 C18 C17 119.9(2) . . ? C18 C19 C20 120.4(2) . . ? C21 C20 C19 120.3(2) . . ? C20 C21 C22 119.9(2) . . ? C21 C22 C17 119.8(2) . . ? C21 C22 P2 123.74(19) . . ? C17 C22 P2 116.43(18) . . ? C24 C23 C28 119.6(2) . . ? C24 C23 P1 119.93(19) . . ? C28 C23 P1 120.41(19) . . ? C23 C24 C25 119.5(3) . . ? C26 C25 C24 120.2(3) . . ? C25 C26 C27 120.4(3) . . ? C28 C27 C26 119.8(2) . . ? C27 C28 C23 120.3(2) . . ? C34 C29 C30 119.7(2) . . ? C34 C29 P1 120.58(19) . . ? C30 C29 P1 119.67(19) . . ? C31 C30 C29 120.0(2) . . ? C30 C31 C32 120.4(3) . . ? C33 C32 C31 120.1(3) . . ? C32 C33 C34 119.9(3) . . ? C33 C34 C29 120.1(2) . . ? C41 P2 C22 105.55(11) . . ? C41 P2 C35 105.35(11) . . ? C22 P2 C35 106.29(11) . . ? C41 P2 Pd1 118.54(8) . . ? C22 P2 Pd1 108.21(8) . . ? C35 P2 Pd1 112.10(8) . . ? C40 C35 C36 119.8(2) . . ? C40 C35 P2 120.71(19) . . ? C36 C35 P2 119.47(19) . . ? C35 C36 C37 119.8(2) . . ? C38 C37 C36 120.1(3) . . ? C39 C38 C37 120.0(2) . . ? C38 C39 C40 120.3(3) . . ? C35 C40 C39 120.0(3) . . ? C42 C41 C46 119.9(2) . . ? C42 C41 P2 120.30(19) . . ? C46 C41 P2 119.77(19) . . ? C43 C42 C41 119.6(2) . . ? C44 C43 C42 120.4(3) . . ? C45 C44 C43 119.8(2) . . ? C44 C45 C46 120.5(3) . . ? C45 C46 C41 119.7(2) . . ? Cl3 C47 Cl2 111.37(18) . . ? Cl3 C47 Cl1 110.6(2) . . ? Cl2 C47 Cl1 110.16(18) . . ? Cl6 C48 Cl4 110.42(17) . . ? Cl6 C48 Cl5 112.08(19) . . ? Cl4 C48 Cl5 110.49(16) . . ? _diffrn_measured_fraction_theta_max 0.944 _diffrn_reflns_theta_full 0.50 _diffrn_measured_fraction_theta_full 0.000 _refine_diff_density_max 1.914 _refine_diff_density_min -1.305 _refine_diff_density_rms 0.088