# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) 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 'Serrano, JoseLuis' _publ_contact_author_email jose.serrano@upct.es _publ_section_title ; Synthesis and Luminescence Properties of Cyclopalladated Complexes with S^N and O^N donor ligands. ; loop_ _publ_author_name J.Serrano M.D.Santana G.Sanchez J.Garcia G.Garcia J.Perez ; L.Garcia ; R.Garcia-Bueno # Attachment '- I8.cif' data_complexI8 _database_code_depnum_ccdc_archive 'CCDC 795484' #TrackingRef '- I8.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H17 Cl N2 O Pd' _chemical_formula_sum 'C24 H17 Cl N2 O Pd' _chemical_formula_weight 491.25 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' 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 12.2047(5) _cell_length_b 11.7402(5) _cell_length_c 14.5635(6) _cell_angle_alpha 90.00 _cell_angle_beta 114.4780(10) _cell_angle_gamma 90.00 _cell_volume 1899.18(14) _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 0.15 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.718 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 984 _exptl_absorpt_coefficient_mu 1.137 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8480 _exptl_absorpt_correction_T_max 0.9247 _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 21500 _diffrn_reflns_av_R_equivalents 0.0211 _diffrn_reflns_av_sigmaI/netI 0.0171 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 28.18 _reflns_number_total 4421 _reflns_number_gt 4237 _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^)+(0.0258P)^2^+2.1018P] 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 4421 _refine_ls_number_parameters 262 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0242 _refine_ls_R_factor_gt 0.0227 _refine_ls_wR_factor_ref 0.0553 _refine_ls_wR_factor_gt 0.0543 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _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 C9 C 0.72886(17) 0.87369(16) 0.05306(14) 0.0167(4) Uani 1 1 d . . . H9 H 0.7976 0.9186 0.0630 0.020 Uiso 1 1 calc R . . C10 C 0.71660(17) 0.76618(17) 0.00972(14) 0.0176(4) Uani 1 1 d . . . H10 H 0.7785 0.7359 -0.0067 0.021 Uiso 1 1 calc R . . C8 C 0.64115(16) 0.91628(16) 0.08202(13) 0.0148(3) Uani 1 1 d . . . H8 H 0.6516 0.9898 0.1117 0.018 Uiso 1 1 calc R . . Pd1 Pd 0.397790(11) 0.892822(11) 0.100431(9) 0.01110(5) Uani 1 1 d . . . Cl1 Cl 0.98822(4) 1.13082(4) 0.39694(4) 0.02121(10) Uani 1 1 d . . . C11 C 0.61321(17) 0.70393(16) -0.00923(13) 0.0167(4) Uani 1 1 d . . . H11 H 0.6029 0.6313 -0.0404 0.020 Uiso 1 1 calc R . . O1 O 0.23403(12) 0.91292(11) 0.10775(10) 0.0163(3) Uani 1 1 d . . . N1 N 0.32788(13) 0.75508(13) 0.01153(11) 0.0133(3) Uani 1 1 d . . . N2 N 0.46601(13) 1.02549(13) 0.19956(11) 0.0132(3) Uani 1 1 d . . . C7 C 0.53789(16) 0.85330(15) 0.06850(13) 0.0128(3) Uani 1 1 d . . . C17 C 0.27185(16) 1.09157(15) 0.19554(13) 0.0134(3) Uani 1 1 d . . . C22 C 0.83558(16) 1.09837(16) 0.33605(14) 0.0157(4) Uani 1 1 d . . . C18 C 0.39882(17) 1.09542(15) 0.22325(13) 0.0138(3) Uani 1 1 d . . . H18 H 0.4400 1.1578 0.2648 0.017 Uiso 1 1 calc R . . C2 C 0.16976(17) 0.62461(16) -0.07748(14) 0.0175(4) Uani 1 1 d . . . H2 H 0.0877 0.6032 -0.0998 0.021 Uiso 1 1 calc R . . C23 C 0.79541(16) 0.99118(16) 0.34870(13) 0.0161(4) Uani 1 1 d . . . H23 H 0.8509 0.9350 0.3882 0.019 Uiso 1 1 calc R . . C13 C 0.07456(16) 1.00160(16) 0.12945(14) 0.0165(4) Uani 1 1 d . . . H13 H 0.0230 0.9398 0.0964 0.020 Uiso 1 1 calc R . . C4 C 0.36619(17) 0.59428(15) -0.07107(14) 0.0164(4) Uani 1 1 d . . . H4 H 0.4206 0.5507 -0.0883 0.020 Uiso 1 1 calc R . . C5 C 0.40552(16) 0.69370(15) -0.01407(13) 0.0139(3) Uani 1 1 d . . . C16 C 0.22224(17) 1.18243(15) 0.23035(13) 0.0152(3) Uani 1 1 d . . . H16 H 0.2728 1.2437 0.2660 0.018 Uiso 1 1 calc R . . C1 C 0.21302(16) 0.72180(16) -0.01941(14) 0.0158(3) Uani 1 1 d . . . H1 H 0.1599 0.7659 -0.0011 0.019 Uiso 1 1 calc R . . C6 C 0.52351(16) 0.74792(15) 0.01759(13) 0.0140(3) Uani 1 1 d . . . C20 C 0.63454(16) 1.15818(15) 0.23454(13) 0.0148(3) Uani 1 1 d . . . H20 H 0.5793 1.2151 0.1960 0.018 Uiso 1 1 calc R . . C21 C 0.75691(17) 1.18169(16) 0.27899(13) 0.0159(3) Uani 1 1 d . . . H21 H 0.7862 1.2540 0.2703 0.019 Uiso 1 1 calc R . . C19 C 0.59240(16) 1.05121(15) 0.24635(13) 0.0135(3) Uani 1 1 d . . . C12 C 0.19682(16) 0.99891(15) 0.14251(13) 0.0136(3) Uani 1 1 d . . . C24 C 0.67317(16) 0.96749(15) 0.30283(13) 0.0144(3) Uani 1 1 d . . . H24 H 0.6445 0.8942 0.3099 0.017 Uiso 1 1 calc R . . C3 C 0.24789(18) 0.55932(16) -0.10246(14) 0.0176(4) Uani 1 1 d . . . H3 H 0.2206 0.4914 -0.1407 0.021 Uiso 1 1 calc R . . C14 C 0.02932(17) 1.09143(16) 0.16344(14) 0.0179(4) Uani 1 1 d . . . H14 H -0.0529 1.0910 0.1528 0.022 Uiso 1 1 calc R . . C15 C 0.10291(17) 1.18385(16) 0.21368(14) 0.0179(4) Uani 1 1 d . . . H15 H 0.0706 1.2464 0.2358 0.021 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 C9 0.0137(8) 0.0220(9) 0.0148(8) 0.0040(7) 0.0063(7) 0.0005(7) C10 0.0158(9) 0.0239(10) 0.0143(8) 0.0037(7) 0.0075(7) 0.0059(7) C8 0.0173(9) 0.0151(8) 0.0121(8) 0.0021(6) 0.0063(7) 0.0008(7) Pd1 0.01145(7) 0.01055(7) 0.01203(7) -0.00089(4) 0.00559(5) 0.00007(4) Cl1 0.0117(2) 0.0272(2) 0.0220(2) -0.00051(18) 0.00425(18) -0.00149(17) C11 0.0200(9) 0.0167(9) 0.0135(8) 0.0010(7) 0.0071(7) 0.0048(7) O1 0.0153(6) 0.0141(6) 0.0220(7) -0.0048(5) 0.0101(5) -0.0016(5) N1 0.0152(7) 0.0130(7) 0.0121(7) -0.0001(5) 0.0061(6) 0.0000(6) N2 0.0130(7) 0.0130(7) 0.0130(7) 0.0005(5) 0.0049(6) -0.0004(6) C7 0.0140(8) 0.0142(8) 0.0103(8) 0.0029(6) 0.0050(7) 0.0036(6) C17 0.0144(8) 0.0139(8) 0.0124(8) 0.0014(6) 0.0063(7) 0.0009(6) C22 0.0119(8) 0.0218(9) 0.0137(8) -0.0036(7) 0.0056(7) -0.0019(7) C18 0.0165(9) 0.0120(8) 0.0133(8) 0.0014(6) 0.0066(7) -0.0013(6) C2 0.0165(9) 0.0174(9) 0.0175(9) -0.0008(7) 0.0061(7) -0.0039(7) C23 0.0163(9) 0.0186(9) 0.0130(8) 0.0017(7) 0.0057(7) 0.0034(7) C13 0.0137(8) 0.0199(9) 0.0157(8) -0.0013(7) 0.0059(7) -0.0007(7) C4 0.0196(9) 0.0154(9) 0.0155(8) -0.0003(7) 0.0086(7) 0.0037(7) C5 0.0161(8) 0.0144(8) 0.0112(8) 0.0022(6) 0.0057(7) 0.0020(7) C16 0.0184(9) 0.0131(8) 0.0148(8) 0.0005(6) 0.0078(7) 0.0002(7) C1 0.0161(8) 0.0156(8) 0.0164(8) 0.0004(7) 0.0074(7) 0.0006(7) C6 0.0155(8) 0.0156(8) 0.0110(8) 0.0023(6) 0.0053(7) 0.0024(7) C20 0.0159(8) 0.0146(9) 0.0136(8) 0.0007(6) 0.0058(7) 0.0008(7) C21 0.0182(9) 0.0138(8) 0.0169(8) -0.0017(7) 0.0084(7) -0.0016(7) C19 0.0141(8) 0.0153(8) 0.0115(8) -0.0024(6) 0.0057(7) -0.0004(7) C12 0.0152(8) 0.0137(8) 0.0116(8) 0.0010(6) 0.0052(7) 0.0002(7) C24 0.0174(9) 0.0140(8) 0.0135(8) 0.0002(6) 0.0081(7) -0.0006(7) C3 0.0235(9) 0.0136(8) 0.0144(8) -0.0023(7) 0.0066(7) -0.0028(7) C14 0.0135(8) 0.0225(9) 0.0177(9) 0.0006(7) 0.0064(7) 0.0031(7) C15 0.0210(9) 0.0162(9) 0.0192(9) 0.0006(7) 0.0111(8) 0.0059(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 C9 C10 1.391(3) . ? C9 C8 1.396(3) . ? C10 C11 1.383(3) . ? C8 C7 1.403(3) . ? Pd1 C7 2.0035(17) . ? Pd1 N1 2.0258(15) . ? Pd1 N2 2.0511(15) . ? Pd1 O1 2.0587(13) . ? Cl1 C22 1.7415(19) . ? C11 C6 1.404(2) . ? O1 C12 1.293(2) . ? N1 C1 1.341(2) . ? N1 C5 1.360(2) . ? N2 C18 1.304(2) . ? N2 C19 1.437(2) . ? C7 C6 1.415(2) . ? C17 C16 1.420(2) . ? C17 C12 1.426(2) . ? C17 C18 1.431(3) . ? C22 C21 1.381(3) . ? C22 C23 1.390(3) . ? C2 C3 1.384(3) . ? C2 C1 1.388(3) . ? C23 C24 1.387(3) . ? C13 C14 1.374(3) . ? C13 C12 1.424(2) . ? C4 C3 1.384(3) . ? C4 C5 1.397(2) . ? C5 C6 1.463(2) . ? C16 C15 1.374(3) . ? C20 C21 1.387(3) . ? C20 C19 1.395(3) . ? C19 C24 1.394(2) . ? C14 C15 1.405(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 C10 C9 C8 120.68(17) . . ? C11 C10 C9 119.18(17) . . ? C9 C8 C7 121.71(17) . . ? C7 Pd1 N1 80.84(7) . . ? C7 Pd1 N2 101.69(7) . . ? N1 Pd1 N2 175.29(6) . . ? C7 Pd1 O1 168.18(6) . . ? N1 Pd1 O1 87.92(6) . . ? N2 Pd1 O1 89.78(5) . . ? C10 C11 C6 120.13(17) . . ? C12 O1 Pd1 128.00(12) . . ? C1 N1 C5 120.25(15) . . ? C1 N1 Pd1 123.52(12) . . ? C5 N1 Pd1 116.20(12) . . ? C18 N2 C19 114.30(15) . . ? C18 N2 Pd1 123.23(12) . . ? C19 N2 Pd1 122.44(11) . . ? C8 C7 C6 116.32(16) . . ? C8 C7 Pd1 130.45(14) . . ? C6 C7 Pd1 113.05(13) . . ? C16 C17 C12 119.57(16) . . ? C16 C17 C18 116.60(16) . . ? C12 C17 C18 123.67(16) . . ? C21 C22 C23 121.69(17) . . ? C21 C22 Cl1 118.79(14) . . ? C23 C22 Cl1 119.48(14) . . ? N2 C18 C17 129.18(17) . . ? C3 C2 C1 119.07(17) . . ? C24 C23 C22 119.06(17) . . ? C14 C13 C12 121.60(17) . . ? C3 C4 C5 119.91(17) . . ? N1 C5 C4 119.93(16) . . ? N1 C5 C6 112.93(15) . . ? C4 C5 C6 126.98(17) . . ? C15 C16 C17 121.59(17) . . ? N1 C1 C2 121.68(17) . . ? C11 C6 C7 121.70(17) . . ? C11 C6 C5 122.09(16) . . ? C7 C6 C5 115.94(16) . . ? C21 C20 C19 120.16(17) . . ? C22 C21 C20 119.04(17) . . ? C24 C19 C20 120.07(17) . . ? C24 C19 N2 119.31(16) . . ? C20 C19 N2 120.61(16) . . ? O1 C12 C13 118.91(16) . . ? O1 C12 C17 123.84(16) . . ? C13 C12 C17 117.24(16) . . ? C23 C24 C19 119.97(17) . . ? C4 C3 C2 119.14(17) . . ? C13 C14 C15 120.96(17) . . ? C16 C15 C14 118.99(17) . . ? _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 0.50 _diffrn_measured_fraction_theta_full 0.000 _refine_diff_density_max 0.419 _refine_diff_density_min -0.335 _refine_diff_density_rms 0.074 #===END data_complexII3 _database_code_depnum_ccdc_archive 'CCDC 795485' #TrackingRef '- I8.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H27 Cl3 N6 Pd2 S2' _chemical_formula_weight 914.90 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' 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 monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.8956(4) _cell_length_b 28.7252(12) _cell_length_c 12.3772(5) _cell_angle_alpha 90.00 _cell_angle_beta 106.0290(10) _cell_angle_gamma 90.00 _cell_volume 3381.5(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 ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.797 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1816 _exptl_absorpt_coefficient_mu 1.461 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.7998 _exptl_absorpt_correction_T_max 0.9046 _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 38970 _diffrn_reflns_av_R_equivalents 0.0282 _diffrn_reflns_av_sigmaI/netI 0.0231 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 28.23 _reflns_number_total 7845 _reflns_number_gt 7459 _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^)+(0.0347P)^2^+10.6297P] 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 7845 _refine_ls_number_parameters 437 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0461 _refine_ls_R_factor_gt 0.0432 _refine_ls_wR_factor_ref 0.0988 _refine_ls_wR_factor_gt 0.0965 _refine_ls_goodness_of_fit_ref 1.179 _refine_ls_restrained_S_all 1.179 _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 0.99066(3) 0.158388(9) 0.71895(2) 0.01761(8) Uani 1 1 d . . . Pd2 Pd 1.14242(3) 0.087499(10) 0.87630(2) 0.02054(8) Uani 1 1 d . . . S2 S 1.33274(10) 0.09680(4) 0.80486(8) 0.0284(2) Uani 1 1 d . . . Cl1 Cl 1.46312(12) -0.01502(4) 0.80334(10) 0.0411(3) Uani 1 1 d . . . Cl2 Cl 1.70335(12) -0.04728(4) 0.73582(11) 0.0414(3) Uani 1 1 d . . . Cl3 Cl 1.44614(13) -0.10193(4) 0.68282(11) 0.0456(3) Uani 1 1 d . . . S1 S 0.82998(10) 0.10351(3) 0.62879(8) 0.0254(2) Uani 1 1 d . . . N1 N 1.1199(3) 0.21118(10) 0.8022(3) 0.0195(6) Uani 1 1 d . . . N2 N 1.1316(3) 0.13649(10) 0.6250(3) 0.0226(6) Uani 1 1 d . . . N4 N 0.9837(3) 0.08285(11) 0.9555(3) 0.0232(6) Uani 1 1 d . . . N6 N 0.8866(3) 0.01359(11) 0.5929(3) 0.0239(6) Uani 1 1 d . . . N5 N 1.0363(3) 0.04255(11) 0.7437(3) 0.0245(7) Uani 1 1 d . . . C16 C 1.1168(4) 0.14415(14) 0.5155(3) 0.0267(8) Uani 1 1 d . . . H16 H 1.0383 0.1589 0.4655 0.032 Uiso 1 1 calc R . . C12 C 0.9322(4) 0.21788(12) 0.8850(3) 0.0189(7) Uani 1 1 d . . . C13 C 1.0678(4) 0.23293(12) 0.8802(3) 0.0187(7) Uani 1 1 d . . . C27 C 1.3502(4) 0.15596(14) 1.0330(4) 0.0293(8) Uani 1 1 d . . . H27 H 1.4163 0.1518 0.9909 0.035 Uiso 1 1 calc R . . C8 C 0.7345(4) 0.22507(14) 0.9623(3) 0.0260(8) Uani 1 1 d . . . H8 H 0.6885 0.2392 1.0119 0.031 Uiso 1 1 calc R . . C21 C 0.9038(4) 0.11941(15) 1.1034(3) 0.0288(8) Uani 1 1 d . . . C11 C 0.8667(4) 0.18181(12) 0.8109(3) 0.0183(7) Uani 1 1 d . . . C28 C 1.2257(4) 0.13098(13) 1.0031(3) 0.0227(7) Uani 1 1 d . . . C31 C 0.9254(4) 0.05199(13) 0.6574(3) 0.0213(7) Uani 1 1 d . . . C1 C 1.2471(4) 0.22356(13) 0.7956(3) 0.0241(8) Uani 1 1 d . . . H1 H 1.2846 0.2086 0.7418 0.029 Uiso 1 1 calc R . . C7 C 0.8702(4) 0.23935(13) 0.9623(3) 0.0222(7) Uani 1 1 d . . . C30 C 1.0041(4) 0.11310(13) 1.0440(3) 0.0227(7) Uani 1 1 d . . . N3 N 1.3186(3) 0.10853(11) 0.5840(3) 0.0242(7) Uani 1 1 d . . . C14 C 1.2556(4) 0.11441(13) 0.6681(3) 0.0210(7) Uani 1 1 d . . . C29 C 1.1328(4) 0.13841(13) 1.0706(3) 0.0221(7) Uani 1 1 d . . . C6 C 0.9486(4) 0.27467(14) 1.0357(3) 0.0283(8) Uani 1 1 d . . . H6 H 0.9082 0.2890 1.0886 0.034 Uiso 1 1 calc R . . C4 C 1.1415(4) 0.26782(13) 0.9519(3) 0.0252(8) Uani 1 1 d . . . C10 C 0.7344(4) 0.16871(14) 0.8164(3) 0.0245(8) Uani 1 1 d . . . H10 H 0.6866 0.1444 0.7691 0.029 Uiso 1 1 calc R . . C32 C 0.9766(4) -0.02233(14) 0.6414(4) 0.0309(9) Uani 1 1 d . . . H32 H 0.9746 -0.0536 0.6157 0.037 Uiso 1 1 calc R . . C24 C 1.1609(4) 0.16994(14) 1.1611(3) 0.0272(8) Uani 1 1 d . . . C20 C 0.7781(5) 0.09396(16) 1.0685(4) 0.0347(10) Uani 1 1 d . . . H20 H 0.7066 0.0978 1.1056 0.042 Uiso 1 1 calc R . . C5 C 1.0775(4) 0.28807(14) 1.0317(3) 0.0288(8) Uani 1 1 d . . . H5 H 1.1267 0.3112 1.0822 0.035 Uiso 1 1 calc R . . C22 C 0.9353(5) 0.15226(16) 1.1949(4) 0.0340(9) Uani 1 1 d . . . H22 H 0.8694 0.1573 1.2368 0.041 Uiso 1 1 calc R . . C26 C 1.3815(5) 0.18720(15) 1.1237(4) 0.0336(9) Uani 1 1 d . . . H26 H 1.4680 0.2037 1.1416 0.040 Uiso 1 1 calc R . . C9 C 0.6690(4) 0.19063(15) 0.8903(3) 0.0279(8) Uani 1 1 d . . . H9 H 0.5769 0.1813 0.8902 0.034 Uiso 1 1 calc R . . C3 C 1.2758(4) 0.27979(14) 0.9427(4) 0.0310(9) Uani 1 1 d . . . H3 H 1.3299 0.3030 0.9901 0.037 Uiso 1 1 calc R . . C17 C 1.4550(4) 0.08821(15) 0.5940(4) 0.0321(9) Uani 1 1 d . . . H17A H 1.4740 0.0883 0.5204 0.048 Uiso 1 1 calc R . . H17B H 1.4562 0.0561 0.6210 0.048 Uiso 1 1 calc R . . H17C H 1.5273 0.1064 0.6474 0.048 Uiso 1 1 calc R . . C25 C 1.2892(5) 0.19431(15) 1.1869(4) 0.0343(9) Uani 1 1 d . . . H25 H 1.3118 0.2156 1.2480 0.041 Uiso 1 1 calc R . . C2 C 1.3274(4) 0.25766(14) 0.8649(4) 0.0299(9) Uani 1 1 d . . . H2 H 1.4179 0.2655 0.8579 0.036 Uiso 1 1 calc R . . C15 C 1.2304(4) 0.12766(14) 0.4869(3) 0.0283(8) Uani 1 1 d . . . H15 H 1.2466 0.1289 0.4148 0.034 Uiso 1 1 calc R . . C18 C 0.8646(4) 0.05866(15) 0.9261(3) 0.0312(9) Uani 1 1 d . . . H18 H 0.8504 0.0372 0.8656 0.037 Uiso 1 1 calc R . . C33 C 1.0683(4) -0.00352(14) 0.7334(4) 0.0294(8) Uani 1 1 d . . . H33 H 1.1436 -0.0198 0.7834 0.035 Uiso 1 1 calc R . . C23 C 1.0584(5) 0.17605(16) 1.2214(3) 0.0337(9) Uani 1 1 d . . . H23 H 1.0770 0.1975 1.2822 0.040 Uiso 1 1 calc R . . C34 C 0.7680(4) 0.01010(15) 0.4930(4) 0.0314(9) Uani 1 1 d . . . H34A H 0.7635 -0.0215 0.4623 0.047 Uiso 1 1 calc R . . H34B H 0.7798 0.0325 0.4366 0.047 Uiso 1 1 calc R . . H34C H 0.6808 0.0169 0.5129 0.047 Uiso 1 1 calc R . . C19 C 0.7598(5) 0.06362(16) 0.9808(4) 0.0357(10) Uani 1 1 d . . . H19 H 0.6757 0.0459 0.9570 0.043 Uiso 1 1 calc R . . C35 C 1.5576(5) -0.06492(16) 0.7817(4) 0.0329(9) Uani 1 1 d . . . H35 H 1.591(5) -0.0804(18) 0.853(4) 0.038(13) 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 0.01736(13) 0.01845(14) 0.01725(13) -0.00060(10) 0.00518(10) 0.00083(9) Pd2 0.02227(14) 0.01943(14) 0.01882(14) 0.00088(10) 0.00383(10) 0.00019(10) S2 0.0241(5) 0.0337(5) 0.0266(5) 0.0004(4) 0.0057(4) 0.0052(4) Cl1 0.0313(5) 0.0450(6) 0.0468(6) -0.0060(5) 0.0105(5) 0.0041(5) Cl2 0.0378(6) 0.0408(6) 0.0512(7) -0.0044(5) 0.0216(5) -0.0038(5) Cl3 0.0441(6) 0.0331(6) 0.0556(7) -0.0012(5) 0.0072(5) -0.0058(5) S1 0.0207(4) 0.0241(5) 0.0278(5) -0.0041(4) 0.0004(4) 0.0024(3) N1 0.0187(14) 0.0181(14) 0.0226(15) 0.0036(12) 0.0073(12) 0.0018(11) N2 0.0192(15) 0.0172(14) 0.0342(18) 0.0018(13) 0.0120(13) 0.0032(12) N4 0.0256(16) 0.0236(16) 0.0193(15) 0.0034(12) 0.0043(12) -0.0040(12) N6 0.0231(15) 0.0228(16) 0.0261(16) -0.0033(13) 0.0072(13) -0.0018(12) N5 0.0273(16) 0.0233(16) 0.0218(15) 0.0015(13) 0.0050(13) 0.0023(13) C16 0.0259(19) 0.0248(19) 0.029(2) -0.0025(16) 0.0066(16) 0.0009(15) C12 0.0163(16) 0.0211(17) 0.0185(16) 0.0032(13) 0.0036(13) 0.0039(13) C13 0.0201(17) 0.0156(16) 0.0215(17) 0.0045(13) 0.0076(13) 0.0031(13) C27 0.028(2) 0.030(2) 0.029(2) 0.0045(16) 0.0049(16) -0.0003(16) C8 0.0226(18) 0.034(2) 0.0248(19) 0.0025(16) 0.0124(15) 0.0065(15) C21 0.029(2) 0.034(2) 0.0223(19) 0.0064(16) 0.0066(15) -0.0019(17) C11 0.0165(16) 0.0215(17) 0.0164(16) 0.0020(13) 0.0039(13) 0.0026(13) C28 0.0265(19) 0.0197(17) 0.0189(17) 0.0033(14) 0.0010(14) 0.0005(14) C31 0.0230(18) 0.0215(17) 0.0202(17) -0.0007(14) 0.0071(14) 0.0004(14) C1 0.0215(18) 0.0225(18) 0.032(2) 0.0023(15) 0.0132(15) 0.0032(14) C7 0.0211(17) 0.0255(18) 0.0205(17) 0.0035(14) 0.0066(14) 0.0056(14) C30 0.0275(19) 0.0231(18) 0.0153(16) 0.0049(14) 0.0021(14) -0.0017(15) N3 0.0245(16) 0.0221(15) 0.0279(16) -0.0057(13) 0.0102(13) -0.0015(13) C14 0.0203(17) 0.0202(17) 0.0242(18) -0.0065(14) 0.0092(14) -0.0016(13) C29 0.0237(18) 0.0204(17) 0.0186(17) 0.0031(14) -0.0001(14) 0.0005(14) C6 0.036(2) 0.027(2) 0.0238(19) -0.0018(15) 0.0125(16) 0.0046(16) C4 0.0265(19) 0.0211(18) 0.029(2) -0.0020(15) 0.0093(16) -0.0017(15) C10 0.0213(18) 0.0264(19) 0.0241(18) -0.0004(15) 0.0034(14) -0.0034(14) C32 0.030(2) 0.0194(18) 0.043(2) -0.0014(17) 0.0098(18) 0.0001(15) C24 0.035(2) 0.0244(19) 0.0194(18) -0.0002(15) 0.0021(15) -0.0007(16) C20 0.034(2) 0.044(3) 0.030(2) 0.0080(19) 0.0144(18) -0.0064(19) C5 0.034(2) 0.0244(19) 0.029(2) -0.0075(16) 0.0099(17) -0.0026(16) C22 0.040(2) 0.039(2) 0.026(2) 0.0008(18) 0.0147(18) 0.0004(19) C26 0.030(2) 0.031(2) 0.035(2) -0.0018(18) 0.0001(17) -0.0115(17) C9 0.0168(17) 0.038(2) 0.031(2) 0.0032(17) 0.0114(15) -0.0001(15) C3 0.031(2) 0.0227(19) 0.041(2) -0.0057(17) 0.0120(18) -0.0084(16) C17 0.0203(19) 0.037(2) 0.040(2) -0.0129(19) 0.0113(17) -0.0015(16) C25 0.039(2) 0.032(2) 0.026(2) -0.0075(17) -0.0006(17) -0.0055(18) C2 0.0234(19) 0.026(2) 0.044(2) -0.0016(17) 0.0156(17) -0.0073(15) C15 0.031(2) 0.030(2) 0.0258(19) -0.0043(16) 0.0115(16) -0.0037(16) C18 0.035(2) 0.034(2) 0.0229(19) 0.0004(16) 0.0042(16) -0.0106(17) C33 0.028(2) 0.0227(19) 0.036(2) 0.0021(16) 0.0062(17) 0.0002(15) C23 0.042(2) 0.037(2) 0.022(2) -0.0057(17) 0.0092(17) 0.0006(19) C34 0.028(2) 0.031(2) 0.032(2) -0.0083(17) 0.0027(17) -0.0043(16) C19 0.035(2) 0.040(2) 0.034(2) 0.0033(19) 0.0124(18) -0.0134(19) C35 0.029(2) 0.032(2) 0.037(2) 0.0075(18) 0.0074(18) 0.0003(17) _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 C11 2.006(3) . ? Pd1 N1 2.066(3) . ? Pd1 N2 2.141(3) . ? Pd1 S1 2.2976(10) . ? Pd1 Pd2 2.9291(4) . ? Pd2 C28 1.997(4) . ? Pd2 N4 2.073(3) . ? Pd2 N5 2.124(3) . ? Pd2 S2 2.3064(11) . ? S2 C14 1.729(4) . ? Cl1 C35 1.772(5) . ? Cl2 C35 1.764(5) . ? Cl3 C35 1.761(5) . ? S1 C31 1.738(4) . ? N1 C1 1.332(5) . ? N1 C13 1.366(5) . ? N2 C16 1.341(5) . ? N2 C14 1.353(5) . ? N4 C18 1.330(5) . ? N4 C30 1.369(5) . ? N6 C31 1.353(5) . ? N6 C32 1.387(5) . ? N6 C34 1.454(5) . ? N5 C31 1.332(5) . ? N5 C33 1.375(5) . ? C16 C15 1.354(6) . ? C12 C7 1.413(5) . ? C12 C11 1.416(5) . ? C12 C13 1.427(5) . ? C13 C4 1.402(5) . ? C27 C28 1.385(5) . ? C27 C26 1.403(6) . ? C8 C9 1.369(6) . ? C8 C7 1.405(5) . ? C21 C30 1.400(6) . ? C21 C20 1.404(6) . ? C21 C22 1.440(6) . ? C11 C10 1.381(5) . ? C28 C29 1.418(5) . ? C1 C2 1.396(6) . ? C7 C6 1.438(6) . ? C30 C29 1.424(5) . ? N3 C14 1.363(5) . ? N3 C15 1.388(5) . ? N3 C17 1.444(5) . ? C29 C24 1.407(5) . ? C6 C5 1.347(6) . ? C4 C3 1.407(6) . ? C4 C5 1.435(5) . ? C10 C9 1.407(5) . ? C32 C33 1.356(6) . ? C24 C25 1.407(6) . ? C24 C23 1.427(6) . ? C20 C19 1.365(7) . ? C22 C23 1.355(6) . ? C26 C25 1.373(7) . ? C3 C2 1.365(6) . ? C18 C19 1.393(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 Pd1 N1 82.08(13) . . ? C11 Pd1 N2 176.66(13) . . ? N1 Pd1 N2 94.58(12) . . ? C11 Pd1 S1 93.22(10) . . ? N1 Pd1 S1 174.78(9) . . ? N2 Pd1 S1 90.11(9) . . ? C11 Pd1 Pd2 97.90(10) . . ? N1 Pd1 Pd2 92.62(8) . . ? N2 Pd1 Pd2 82.27(8) . . ? S1 Pd1 Pd2 90.28(3) . . ? C28 Pd2 N4 82.55(14) . . ? C28 Pd2 N5 174.94(14) . . ? N4 Pd2 N5 92.80(13) . . ? C28 Pd2 S2 91.47(12) . . ? N4 Pd2 S2 173.92(9) . . ? N5 Pd2 S2 93.21(9) . . ? C28 Pd2 Pd1 96.45(10) . . ? N4 Pd2 Pd1 92.47(9) . . ? N5 Pd2 Pd1 81.69(9) . . ? S2 Pd2 Pd1 89.29(3) . . ? C14 S2 Pd2 102.86(13) . . ? C31 S1 Pd1 102.78(13) . . ? C1 N1 C13 117.9(3) . . ? C1 N1 Pd1 129.1(3) . . ? C13 N1 Pd1 112.7(2) . . ? C16 N2 C14 108.0(3) . . ? C16 N2 Pd1 126.5(3) . . ? C14 N2 Pd1 125.4(3) . . ? C18 N4 C30 118.3(3) . . ? C18 N4 Pd2 129.4(3) . . ? C30 N4 Pd2 112.0(2) . . ? C31 N6 C32 107.9(3) . . ? C31 N6 C34 126.0(3) . . ? C32 N6 C34 126.0(3) . . ? C31 N5 C33 106.3(3) . . ? C31 N5 Pd2 128.2(3) . . ? C33 N5 Pd2 125.4(3) . . ? N2 C16 C15 109.9(4) . . ? C7 C12 C11 123.5(3) . . ? C7 C12 C13 119.0(3) . . ? C11 C12 C13 117.6(3) . . ? N1 C13 C4 122.9(3) . . ? N1 C13 C12 115.7(3) . . ? C4 C13 C12 121.5(3) . . ? C28 C27 C26 121.9(4) . . ? C9 C8 C7 119.4(3) . . ? C30 C21 C20 117.9(4) . . ? C30 C21 C22 117.8(4) . . ? C20 C21 C22 124.3(4) . . ? C10 C11 C12 116.0(3) . . ? C10 C11 Pd1 132.2(3) . . ? C12 C11 Pd1 111.7(2) . . ? C27 C28 C29 116.0(4) . . ? C27 C28 Pd2 132.6(3) . . ? C29 C28 Pd2 111.3(3) . . ? N5 C31 N6 110.1(3) . . ? N5 C31 S1 128.1(3) . . ? N6 C31 S1 121.6(3) . . ? N1 C1 C2 122.5(4) . . ? C8 C7 C12 117.8(3) . . ? C8 C7 C6 123.7(3) . . ? C12 C7 C6 118.5(3) . . ? N4 C30 C21 122.2(4) . . ? N4 C30 C29 115.7(3) . . ? C21 C30 C29 122.1(4) . . ? C14 N3 C15 107.5(3) . . ? C14 N3 C17 126.7(3) . . ? C15 N3 C17 125.7(3) . . ? N2 C14 N3 108.3(3) . . ? N2 C14 S2 129.0(3) . . ? N3 C14 S2 122.7(3) . . ? C24 C29 C28 123.2(4) . . ? C24 C29 C30 118.7(4) . . ? C28 C29 C30 118.1(3) . . ? C5 C6 C7 122.0(4) . . ? C13 C4 C3 117.5(4) . . ? C13 C4 C5 118.3(3) . . ? C3 C4 C5 124.2(4) . . ? C11 C10 C9 121.5(4) . . ? C33 C32 N6 105.5(3) . . ? C25 C24 C29 118.0(4) . . ? C25 C24 C23 123.1(4) . . ? C29 C24 C23 118.9(4) . . ? C19 C20 C21 119.2(4) . . ? C6 C5 C4 120.8(4) . . ? C23 C22 C21 120.4(4) . . ? C25 C26 C27 121.1(4) . . ? C8 C9 C10 121.8(3) . . ? C2 C3 C4 119.2(4) . . ? C26 C25 C24 119.8(4) . . ? C3 C2 C1 120.0(4) . . ? C16 C15 N3 106.3(3) . . ? N4 C18 C19 122.4(4) . . ? C32 C33 N5 110.1(4) . . ? C22 C23 C24 122.2(4) . . ? C20 C19 C18 119.9(4) . . ? Cl3 C35 Cl2 111.1(3) . . ? Cl3 C35 Cl1 109.7(2) . . ? Cl2 C35 Cl1 109.2(2) . . ? _diffrn_measured_fraction_theta_max 0.941 _diffrn_reflns_theta_full 0.50 _diffrn_measured_fraction_theta_full 0.000 _refine_diff_density_max 1.763 _refine_diff_density_min -0.694 _refine_diff_density_rms 0.115 #===END data_complexII9 _database_code_depnum_ccdc_archive 'CCDC 795486' #TrackingRef '- I8.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H12 N2 O PD' _chemical_formula_sum 'C18 H12 N2 O Pd' _chemical_formula_weight 378.70 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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pcab loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z+1/2' 'x+1/2, -y, -z+1/2' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, y-1/2, -z-1/2' '-x-1/2, y, z-1/2' 'x-1/2, -y-1/2, z' _cell_length_a 7.7320(3) _cell_length_b 16.2417(7) _cell_length_c 22.1839(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2785.9(2) _cell_formula_units_Z 8 _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 0.17 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.806 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1504 _exptl_absorpt_coefficient_mu 1.334 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8050 _exptl_absorpt_correction_T_max 0.8563 _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 29838 _diffrn_reflns_av_R_equivalents 0.0226 _diffrn_reflns_av_sigmaI/netI 0.0131 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 28.21 _reflns_number_total 3287 _reflns_number_gt 3142 _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^)+(0.0431P)^2^+7.0956P] 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 3287 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0377 _refine_ls_R_factor_gt 0.0361 _refine_ls_wR_factor_ref 0.0916 _refine_ls_wR_factor_gt 0.0905 _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_restrained_S_all 1.106 _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 C3 C 0.3279(4) -0.0147(2) 0.59634(16) 0.0276(7) Uani 1 1 d . . . H3 H 0.3566 -0.0250 0.6373 0.033 Uiso 1 1 calc R . . C2 C 0.3798(4) 0.05681(19) 0.56859(15) 0.0250(6) Uani 1 1 d . . . H2 H 0.4412 0.0973 0.5908 0.030 Uiso 1 1 calc R . . C1 C 0.3424(4) 0.06998(17) 0.50796(14) 0.0215(6) Uani 1 1 d . . . H1 H 0.3795 0.1197 0.4895 0.026 Uiso 1 1 calc R . . Pd1 Pd 0.18055(3) 0.025975(13) 0.388045(10) 0.02065(9) Uani 1 1 d . . . O1 O 0.3252(3) 0.13749(14) 0.37129(11) 0.0270(5) Uani 1 1 d . . . N1 N 0.2560(3) 0.01496(14) 0.47490(12) 0.0210(5) Uani 1 1 d . . . C13 C 0.1977(4) -0.05494(17) 0.50236(15) 0.0229(6) Uani 1 1 d . . . N2 N 0.0878(3) 0.05370(16) 0.30518(12) 0.0252(5) Uani 1 1 d . . . C6 C 0.0645(4) -0.19897(18) 0.55169(16) 0.0311(7) Uani 1 1 d . . . H6 H 0.0183 -0.2478 0.5689 0.037 Uiso 1 1 calc R . . C8 C -0.0645(4) -0.23282(18) 0.45034(18) 0.0322(8) Uani 1 1 d . . . H8 H -0.1141 -0.2824 0.4652 0.039 Uiso 1 1 calc R . . C11 C 0.0724(4) -0.08319(18) 0.40417(16) 0.0257(6) Uani 1 1 d . . . C12 C 0.0981(4) -0.10768(17) 0.46447(15) 0.0241(6) Uani 1 1 d . . . C7 C 0.0309(4) -0.18132(18) 0.48929(16) 0.0277(7) Uani 1 1 d . . . C4 C 0.2311(4) -0.07269(18) 0.56290(15) 0.0253(6) Uani 1 1 d . . . C9 C -0.0856(4) -0.2112(2) 0.39099(17) 0.0333(8) Uani 1 1 d . . . H9 H -0.1480 -0.2469 0.3650 0.040 Uiso 1 1 calc R . . C5 C 0.1605(4) -0.1478(2) 0.58674(17) 0.0309(7) Uani 1 1 d . . . H5 H 0.1812 -0.1619 0.6277 0.037 Uiso 1 1 calc R . . C18 C -0.0387(5) 0.0338(2) 0.26664(15) 0.0305(7) Uani 1 1 d . . . H18 H -0.1087 -0.0141 0.2697 0.037 Uiso 1 1 calc R . . C14 C 0.2810(4) 0.16628(18) 0.32086(14) 0.0252(6) Uani 1 1 d . . . H14 H 0.3339 0.2155 0.3069 0.030 Uiso 1 1 calc R . . C15 C 0.1560(4) 0.12789(19) 0.28475(15) 0.0265(6) Uani 1 1 d . . . C10 C -0.0163(4) -0.13683(19) 0.36749(17) 0.0309(7) Uani 1 1 d . . . H10 H -0.0314 -0.1240 0.3260 0.037 Uiso 1 1 calc R . . C16 C 0.0698(5) 0.1528(2) 0.23202(15) 0.0317(7) Uani 1 1 d . . . H16 H 0.0923 0.2007 0.2087 0.038 Uiso 1 1 calc R . . C17 C -0.0540(5) 0.0936(2) 0.22094(16) 0.0351(7) Uani 1 1 d . . . H17 H -0.1344 0.0932 0.1886 0.042 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 C3 0.0275(16) 0.0241(15) 0.0310(16) 0.0021(13) 0.0089(12) 0.0063(12) C2 0.0223(14) 0.0205(14) 0.0323(15) -0.0024(12) 0.0037(12) 0.0024(11) C1 0.0183(13) 0.0135(12) 0.0328(15) 0.0014(11) 0.0050(11) 0.0019(10) Pd1 0.02014(14) 0.01416(13) 0.02764(15) -0.00157(8) 0.00179(8) -0.00024(7) O1 0.0296(12) 0.0199(10) 0.0314(11) 0.0004(9) -0.0003(9) -0.0027(8) N1 0.0190(12) 0.0146(10) 0.0295(12) 0.0015(9) 0.0051(10) 0.0032(9) C13 0.0179(13) 0.0133(12) 0.0376(16) 0.0021(11) 0.0092(12) 0.0051(10) N2 0.0268(13) 0.0208(12) 0.0279(13) -0.0046(10) 0.0027(10) 0.0001(10) C6 0.0297(16) 0.0135(13) 0.050(2) 0.0073(13) 0.0166(14) 0.0035(12) C8 0.0219(15) 0.0132(13) 0.061(2) -0.0031(13) 0.0109(14) 0.0023(11) C11 0.0212(14) 0.0163(13) 0.0397(16) -0.0025(12) 0.0040(12) 0.0033(11) C12 0.0181(13) 0.0144(12) 0.0398(17) 0.0001(11) 0.0088(12) 0.0049(10) C7 0.0206(14) 0.0153(13) 0.0471(19) -0.0006(12) 0.0122(13) 0.0038(11) C4 0.0230(14) 0.0159(13) 0.0370(16) 0.0030(12) 0.0101(13) 0.0062(11) C9 0.0206(15) 0.0211(15) 0.058(2) -0.0136(14) 0.0033(14) 0.0004(12) C5 0.0326(17) 0.0208(15) 0.0392(18) 0.0081(13) 0.0125(14) 0.0068(13) C18 0.0333(17) 0.0256(15) 0.0325(16) -0.0067(13) 0.0002(14) -0.0018(13) C14 0.0294(15) 0.0173(13) 0.0290(15) -0.0007(11) 0.0032(12) -0.0002(11) C15 0.0298(16) 0.0201(14) 0.0297(15) -0.0025(12) 0.0033(12) 0.0003(12) C10 0.0273(16) 0.0188(14) 0.0466(19) -0.0050(13) 0.0034(14) 0.0036(12) C16 0.0399(19) 0.0282(16) 0.0270(15) -0.0009(12) 0.0013(13) 0.0014(14) C17 0.0384(19) 0.0385(18) 0.0283(16) -0.0043(14) -0.0054(14) -0.0014(15) _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 C3 C2 1.375(5) . ? C3 C4 1.413(5) . ? C2 C1 1.392(5) . ? C1 N1 1.335(4) . ? Pd1 C11 1.993(3) . ? Pd1 N1 2.021(3) . ? Pd1 N2 2.024(3) . ? Pd1 O1 2.161(2) . ? O1 C14 1.260(4) . ? N1 C13 1.365(4) . ? C13 C4 1.398(5) . ? C13 C12 1.426(4) . ? N2 C18 1.339(4) . ? N2 C15 1.391(4) . ? C6 C5 1.358(5) . ? C6 C7 1.437(5) . ? C8 C9 1.372(5) . ? C8 C7 1.411(5) . ? C11 C10 1.375(5) . ? C11 C12 1.410(5) . ? C12 C7 1.416(4) . ? C4 C5 1.438(4) . ? C9 C10 1.421(5) . ? C18 C17 1.409(5) . ? C14 C15 1.402(4) . ? C15 C16 1.406(5) . ? C16 C17 1.379(5) . ? 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 C2 C3 C4 118.8(3) . . ? C3 C2 C1 120.1(3) . . ? N1 C1 C2 122.1(3) . . ? C11 Pd1 N1 82.60(12) . . ? C11 Pd1 N2 102.26(12) . . ? N1 Pd1 N2 171.06(10) . . ? C11 Pd1 O1 173.63(11) . . ? N1 Pd1 O1 95.09(9) . . ? N2 Pd1 O1 80.83(10) . . ? C14 O1 Pd1 108.9(2) . . ? C1 N1 C13 118.5(3) . . ? C1 N1 Pd1 127.5(2) . . ? C13 N1 Pd1 113.8(2) . . ? N1 C13 C4 122.6(3) . . ? N1 C13 C12 114.5(3) . . ? C4 C13 C12 122.8(3) . . ? C18 N2 C15 106.1(3) . . ? C18 N2 Pd1 141.7(2) . . ? C15 N2 Pd1 110.8(2) . . ? C5 C6 C7 121.9(3) . . ? C9 C8 C7 119.9(3) . . ? C10 C11 C12 116.9(3) . . ? C10 C11 Pd1 131.8(3) . . ? C12 C11 Pd1 111.2(2) . . ? C11 C12 C7 123.8(3) . . ? C11 C12 C13 117.8(3) . . ? C7 C12 C13 118.5(3) . . ? C8 C7 C12 117.1(3) . . ? C8 C7 C6 124.5(3) . . ? C12 C7 C6 118.5(3) . . ? C13 C4 C3 117.7(3) . . ? C13 C4 C5 117.3(3) . . ? C3 C4 C5 125.0(3) . . ? C8 C9 C10 121.7(3) . . ? C6 C5 C4 121.1(3) . . ? N2 C18 C17 110.8(3) . . ? O1 C14 C15 122.0(3) . . ? N2 C15 C14 117.4(3) . . ? N2 C15 C16 109.9(3) . . ? C14 C15 C16 132.4(3) . . ? C11 C10 C9 120.6(3) . . ? C17 C16 C15 106.1(3) . . ? C16 C17 C18 107.1(3) . . ? _diffrn_measured_fraction_theta_max 0.959 _diffrn_reflns_theta_full 0.50 _diffrn_measured_fraction_theta_full 0.000 _refine_diff_density_max 2.067 _refine_diff_density_min -0.401 _refine_diff_density_rms 0.113