# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Yong-Joo Kim' _publ_contact_author_email YJKIM@KANGNUNG.AC.KR _publ_section_title ; Cyclopalladated azido complexes containing C,N-donor (HC~N= 2-(2'-thienyl)pyridine, azobenzene, 3,3'-dimethyl azobenzene, N,N'-dimethylbenzylamine, 2-phenylpyridine) ligands: reactivity toward organic unsaturated compounds and catalytic properties ; loop_ _publ_author_name 'Yong-Joo Kim' 'Jungyeob Ham' 'Sam-Yong Han' 'Hyeong-Tak Jeon' 'Soon W. Lee' 'Kyung-Eun Lee' #=========================================================END data_lke244 _database_code_depnum_ccdc_archive 'CCDC 713100' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H27 N4 P Pd' _chemical_formula_weight 400.78 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' 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 'P2(1)/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 11.2199(18) _cell_length_b 10.2744(17) _cell_length_c 16.122(2) _cell_angle_alpha 90.00 _cell_angle_beta 98.048(13) _cell_angle_gamma 90.00 _cell_volume 1840.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 7.68 _cell_measurement_theta_max 12.48 _exptl_crystal_description 'BLOCK ' _exptl_crystal_colour 'YELLOW ' _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.447 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 824 _exptl_absorpt_coefficient_mu 1.095 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3571 _exptl_absorpt_correction_T_max 0.7730 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 3386 _diffrn_reflns_av_R_equivalents 0.0367 _diffrn_reflns_av_sigmaI/netI 0.0366 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3211 _reflns_number_gt 2785 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _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^)+(0.0433P)^2^+1.7395P] 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 SHELXL _refine_ls_extinction_coef 0.0056(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3211 _refine_ls_number_parameters 191 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0414 _refine_ls_R_factor_gt 0.0331 _refine_ls_wR_factor_ref 0.0921 _refine_ls_wR_factor_gt 0.0837 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.094 _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 0.30151(2) 0.08677(2) 0.078068(14) 0.03214(13) Uani 1 1 d . . . P1 P 0.23095(8) 0.28895(9) 0.04590(6) 0.0366(2) Uani 1 1 d . . . N1 N 0.3646(3) -0.1094(3) 0.10177(18) 0.0385(7) Uani 1 1 d . . . N2 N 0.3159(4) 0.1269(4) 0.2083(2) 0.0541(8) Uani 1 1 d . . . N3 N 0.4022(3) 0.1460(4) 0.2586(2) 0.0555(9) Uani 1 1 d . . . N4 N 0.4818(5) 0.1637(6) 0.3104(3) 0.0991(18) Uani 1 1 d . . . C1 C 0.2741(3) 0.0209(3) -0.0416(2) 0.0367(8) Uani 1 1 d . . . C2 C 0.3365(3) -0.0969(3) -0.0510(2) 0.0401(8) Uani 1 1 d . . . C3 C 0.3283(4) -0.1581(4) -0.1291(3) 0.0524(10) Uani 1 1 d . . . H3 H 0.3709 -0.2347 -0.1342 0.063 Uiso 1 1 calc R . . C4 C 0.2583(5) -0.1072(5) -0.1986(3) 0.0617(12) Uani 1 1 d . . . H4 H 0.2547 -0.1478 -0.2505 0.074 Uiso 1 1 calc R . . C5 C 0.1939(4) 0.0046(5) -0.1898(2) 0.0607(12) Uani 1 1 d . . . H5 H 0.1450 0.0387 -0.2361 0.073 Uiso 1 1 calc R . . C6 C 0.2005(4) 0.0677(4) -0.1127(2) 0.0477(9) Uani 1 1 d . . . H6 H 0.1550 0.1425 -0.1084 0.057 Uiso 1 1 calc R . . C7 C 0.4129(3) -0.1520(4) 0.0244(2) 0.0426(8) Uani 1 1 d . . . H7A H 0.4127 -0.2463 0.0212 0.051 Uiso 1 1 calc R . . H7B H 0.4952 -0.1222 0.0261 0.051 Uiso 1 1 calc R . . C8 C 0.4597(4) -0.1271(4) 0.1748(3) 0.0528(10) Uani 1 1 d . . . H8A H 0.5293 -0.0768 0.1667 0.079 Uiso 1 1 calc R . . H8B H 0.4813 -0.2174 0.1802 0.079 Uiso 1 1 calc R . . H8C H 0.4301 -0.0985 0.2248 0.079 Uiso 1 1 calc R . . C9 C 0.2575(4) -0.1875(4) 0.1147(3) 0.0504(10) Uani 1 1 d . . . H9A H 0.1958 -0.1763 0.0676 0.076 Uiso 1 1 calc R . . H9B H 0.2282 -0.1590 0.1648 0.076 Uiso 1 1 calc R . . H9C H 0.2794 -0.2777 0.1200 0.076 Uiso 1 1 calc R . . C10 C 0.0657(4) 0.2930(4) 0.0260(3) 0.0511(10) Uani 1 1 d . . . H10A H 0.0385 0.3822 0.0293 0.061 Uiso 1 1 calc R . . H10B H 0.0389 0.2614 -0.0302 0.061 Uiso 1 1 calc R . . C11 C 0.0100(4) 0.2106(6) 0.0883(3) 0.0745(15) Uani 1 1 d . . . H11A H -0.0761 0.2151 0.0759 0.112 Uiso 1 1 calc R . . H11B H 0.0352 0.2426 0.1439 0.112 Uiso 1 1 calc R . . H11C H 0.0355 0.1219 0.0844 0.112 Uiso 1 1 calc R . . C12 C 0.2636(4) 0.4054(4) 0.1321(3) 0.0510(10) Uani 1 1 d . . . H12A H 0.2196 0.4850 0.1167 0.061 Uiso 1 1 calc R . . H12B H 0.2334 0.3701 0.1809 0.061 Uiso 1 1 calc R . . C13 C 0.3958(5) 0.4395(5) 0.1565(4) 0.0771(15) Uani 1 1 d . . . H13A H 0.4039 0.5006 0.2020 0.116 Uiso 1 1 calc R . . H13B H 0.4265 0.4774 0.1094 0.116 Uiso 1 1 calc R . . H13C H 0.4404 0.3620 0.1736 0.116 Uiso 1 1 calc R . . C14 C 0.2864(4) 0.3712(4) -0.0426(3) 0.0541(10) Uani 1 1 d . . . H14A H 0.3726 0.3834 -0.0285 0.065 Uiso 1 1 calc R . . H14B H 0.2734 0.3138 -0.0908 0.065 Uiso 1 1 calc R . . C15 C 0.2299(5) 0.5027(5) -0.0680(3) 0.0691(13) Uani 1 1 d . . . H15A H 0.2651 0.5369 -0.1144 0.104 Uiso 1 1 calc R . . H15B H 0.2442 0.5618 -0.0216 0.104 Uiso 1 1 calc R . . H15C H 0.1448 0.4921 -0.0841 0.104 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 0.03935(18) 0.02922(18) 0.02719(17) 0.00081(9) 0.00240(11) 0.00046(10) P1 0.0433(5) 0.0326(5) 0.0343(5) 0.0011(4) 0.0068(4) 0.0037(4) N1 0.0461(17) 0.0340(15) 0.0347(15) 0.0044(12) 0.0028(13) -0.0019(13) N2 0.069(2) 0.057(2) 0.0358(17) 0.0003(16) 0.0039(17) 0.0047(18) N3 0.069(2) 0.060(2) 0.0370(18) -0.0098(16) 0.0041(18) 0.0110(19) N4 0.086(3) 0.143(5) 0.060(3) -0.038(3) -0.021(2) 0.019(3) C1 0.0408(18) 0.0342(18) 0.0346(18) 0.0004(14) 0.0039(14) -0.0041(15) C2 0.046(2) 0.038(2) 0.0373(19) -0.0005(15) 0.0106(16) -0.0087(16) C3 0.064(3) 0.047(2) 0.049(2) -0.0101(19) 0.020(2) -0.002(2) C4 0.083(3) 0.066(3) 0.037(2) -0.017(2) 0.012(2) -0.012(2) C5 0.065(3) 0.081(3) 0.034(2) -0.001(2) -0.0028(19) -0.008(2) C6 0.054(2) 0.052(2) 0.036(2) -0.0014(17) 0.0021(17) 0.0024(18) C7 0.048(2) 0.0311(18) 0.050(2) 0.0012(16) 0.0131(17) 0.0061(16) C8 0.059(2) 0.047(2) 0.048(2) 0.0075(19) -0.0073(19) 0.008(2) C9 0.059(2) 0.042(2) 0.053(2) 0.0082(18) 0.0164(19) -0.0072(19) C10 0.048(2) 0.054(2) 0.051(2) 0.0008(19) 0.0064(18) 0.0101(19) C11 0.046(2) 0.100(4) 0.078(3) 0.014(3) 0.007(2) -0.012(3) C12 0.064(3) 0.041(2) 0.047(2) -0.0029(17) 0.0023(19) 0.0138(18) C13 0.073(3) 0.060(3) 0.094(4) -0.013(3) -0.005(3) -0.009(3) C14 0.074(3) 0.042(2) 0.049(2) 0.0081(19) 0.021(2) 0.002(2) C15 0.100(4) 0.043(2) 0.066(3) 0.015(2) 0.015(3) 0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C1 2.028(3) . ? Pd1 N2 2.124(3) . ? Pd1 N1 2.153(3) . ? Pd1 P1 2.2575(10) . ? P1 C12 1.831(4) . ? P1 C10 1.837(4) . ? P1 C14 1.840(4) . ? N1 C9 1.483(5) . ? N1 C8 1.486(5) . ? N1 C7 1.493(5) . ? N2 N3 1.189(5) . ? N3 N4 1.148(5) . ? C1 C6 1.401(5) . ? C1 C2 1.416(5) . ? C2 C3 1.399(5) . ? C2 C7 1.497(5) . ? C3 C4 1.379(6) . ? C3 H3 0.9300 . ? C4 C5 1.375(7) . ? C4 H4 0.9300 . ? C5 C6 1.396(6) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C11 1.513(6) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C13 1.521(7) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 C15 1.524(6) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pd1 N2 170.51(14) . . ? C1 Pd1 N1 81.86(13) . . ? N2 Pd1 N1 91.65(13) . . ? C1 Pd1 P1 95.00(10) . . ? N2 Pd1 P1 91.38(10) . . ? N1 Pd1 P1 176.79(8) . . ? C12 P1 C10 102.0(2) . . ? C12 P1 C14 103.6(2) . . ? C10 P1 C14 107.3(2) . . ? C12 P1 Pd1 113.59(13) . . ? C10 P1 Pd1 111.94(14) . . ? C14 P1 Pd1 117.07(14) . . ? C9 N1 C8 109.2(3) . . ? C9 N1 C7 110.7(3) . . ? C8 N1 C7 108.8(3) . . ? C9 N1 Pd1 106.2(2) . . ? C8 N1 Pd1 115.9(2) . . ? C7 N1 Pd1 106.0(2) . . ? N3 N2 Pd1 130.4(3) . . ? N4 N3 N2 176.4(5) . . ? C6 C1 C2 116.8(3) . . ? C6 C1 Pd1 131.1(3) . . ? C2 C1 Pd1 112.1(3) . . ? C3 C2 C1 120.6(4) . . ? C3 C2 C7 121.3(3) . . ? C1 C2 C7 118.2(3) . . ? C4 C3 C2 121.3(4) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C5 C4 C3 118.7(4) . . ? C5 C4 H4 120.6 . . ? C3 C4 H4 120.6 . . ? C4 C5 C6 121.2(4) . . ? C4 C5 H5 119.4 . . ? C6 C5 H5 119.4 . . ? C5 C6 C1 121.4(4) . . ? C5 C6 H6 119.3 . . ? C1 C6 H6 119.3 . . ? N1 C7 C2 109.5(3) . . ? N1 C7 H7A 109.8 . . ? C2 C7 H7A 109.8 . . ? N1 C7 H7B 109.8 . . ? C2 C7 H7B 109.8 . . ? H7A C7 H7B 108.2 . . ? N1 C8 H8A 109.5 . . ? N1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N1 C9 H9A 109.5 . . ? N1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 P1 111.9(3) . . ? C11 C10 H10A 109.2 . . ? P1 C10 H10A 109.2 . . ? C11 C10 H10B 109.2 . . ? P1 C10 H10B 109.2 . . ? H10A C10 H10B 107.9 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 P1 115.6(3) . . ? C13 C12 H12A 108.4 . . ? P1 C12 H12A 108.4 . . ? C13 C12 H12B 108.4 . . ? P1 C12 H12B 108.4 . . ? H12A C12 H12B 107.5 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 P1 116.3(3) . . ? C15 C14 H14A 108.2 . . ? P1 C14 H14A 108.2 . . ? C15 C14 H14B 108.2 . . ? P1 C14 H14B 108.2 . . ? H14A C14 H14B 107.4 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.678 _refine_diff_density_min -0.464 _refine_diff_density_rms 0.090 # Attachment 'cif-yjk.CIF' data_cxh257 _database_code_depnum_ccdc_archive 'CCDC 713101' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H15 N4 P Pd S' _chemical_formula_weight 384.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.4930(3) _cell_length_b 11.9648(3) _cell_length_c 12.7272(3) _cell_angle_alpha 90.00 _cell_angle_beta 112.4870(10) _cell_angle_gamma 90.00 _cell_volume 1476.37(7) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9752 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 28.33 _exptl_crystal_description BLOCK _exptl_crystal_colour colourless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.731 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 768 _exptl_absorpt_coefficient_mu 1.498 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4669 _exptl_absorpt_correction_T_max 0.7538 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23540 _diffrn_reflns_av_R_equivalents 0.0231 _diffrn_reflns_av_sigmaI/netI 0.0120 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 28.33 _reflns_number_total 3606 _reflns_number_gt 3360 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0223P)^2^+0.6778P] 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 SHELXL _refine_ls_extinction_coef 0.0132(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3606 _refine_ls_number_parameters 173 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0206 _refine_ls_R_factor_gt 0.0186 _refine_ls_wR_factor_ref 0.0477 _refine_ls_wR_factor_gt 0.0462 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _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 0.716380(12) 0.340596(10) 0.095183(10) 0.03381(6) Uani 1 1 d . . . S1 S 0.26570(5) 0.27851(5) -0.05585(5) 0.05448(13) Uani 1 1 d . . . P1 P 0.83396(5) 0.21334(4) 0.04004(4) 0.03898(10) Uani 1 1 d . . . N1 N 0.59295(15) 0.44422(11) 0.15279(12) 0.0384(3) Uani 1 1 d . . . N2 N 0.89117(18) 0.43000(16) 0.19789(15) 0.0569(4) Uani 1 1 d . . . N3 N 0.97398(16) 0.47337(14) 0.17031(14) 0.0499(4) Uani 1 1 d . . . N4 N 1.0586(2) 0.5175(2) 0.1502(2) 0.0881(7) Uani 1 1 d . . . C1 C 0.6368(2) 0.52501(15) 0.23117(16) 0.0480(4) Uani 1 1 d . . . H1 H 0.7298 0.5440 0.2607 0.058 Uiso 1 1 calc R . . C2 C 0.5478(3) 0.58103(17) 0.26957(18) 0.0574(5) Uani 1 1 d . . . H2 H 0.5805 0.6360 0.3252 0.069 Uiso 1 1 calc R . . C3 C 0.4099(3) 0.55412(18) 0.2242(2) 0.0589(5) Uani 1 1 d . . . H3 H 0.3486 0.5904 0.2495 0.071 Uiso 1 1 calc R . . C4 C 0.3628(2) 0.47343(17) 0.14112(18) 0.0524(5) Uani 1 1 d . . . H4 H 0.2693 0.4565 0.1078 0.063 Uiso 1 1 calc R . . C5 C 0.45772(18) 0.41752(14) 0.10778(15) 0.0396(3) Uani 1 1 d . . . C6 C 0.42874(17) 0.32785(14) 0.02612(15) 0.0394(4) Uani 1 1 d . . . C7 C 0.53163(17) 0.27478(13) 0.00363(14) 0.0372(3) Uani 1 1 d . . . C8 C 0.4735(2) 0.19314(16) -0.08337(17) 0.0474(4) Uani 1 1 d . . . H8 H 0.5265 0.1488 -0.1111 0.057 Uiso 1 1 calc R . . C9 C 0.3344(2) 0.18600(18) -0.12198(19) 0.0553(5) Uani 1 1 d . . . H9 H 0.2822 0.1363 -0.1782 0.066 Uiso 1 1 calc R . . C10 C 1.0183(2) 0.2177(2) 0.1204(3) 0.0765(7) Uani 1 1 d . . . H10A H 1.0366 0.2130 0.2002 0.115 Uiso 1 1 calc R . . H10B H 1.0549 0.2866 0.1050 0.115 Uiso 1 1 calc R . . H10C H 1.0613 0.1559 0.0987 0.115 Uiso 1 1 calc R . . C11 C 0.8202(3) 0.2228(2) -0.10499(18) 0.0609(5) Uani 1 1 d . . . H11A H 0.8403 0.2978 -0.1206 0.091 Uiso 1 1 calc R . . H11B H 0.7282 0.2034 -0.1552 0.091 Uiso 1 1 calc R . . H11C H 0.8846 0.1723 -0.1166 0.091 Uiso 1 1 calc R . . C12 C 0.7938(3) 0.06901(18) 0.0577(2) 0.0627(5) Uani 1 1 d . . . H12A H 0.7995 0.0576 0.1340 0.094 Uiso 1 1 calc R . . H12B H 0.8584 0.0208 0.0432 0.094 Uiso 1 1 calc R . . H12C H 0.7021 0.0521 0.0051 0.094 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 0.03250(8) 0.03717(8) 0.03287(8) -0.00389(4) 0.01375(5) -0.00533(4) S1 0.0342(2) 0.0622(3) 0.0611(3) 0.0082(2) 0.0116(2) -0.0067(2) P1 0.0383(2) 0.0406(2) 0.0377(2) -0.00061(17) 0.01423(18) 0.00192(17) N1 0.0445(8) 0.0364(7) 0.0376(7) 0.0012(5) 0.0195(6) -0.0001(6) N2 0.0486(9) 0.0740(11) 0.0514(9) -0.0205(8) 0.0226(8) -0.0242(8) N3 0.0390(8) 0.0571(9) 0.0538(9) -0.0147(7) 0.0180(7) -0.0117(7) N4 0.0710(14) 0.1010(18) 0.1083(18) -0.0226(14) 0.0521(14) -0.0389(13) C1 0.0616(12) 0.0398(9) 0.0459(10) -0.0038(7) 0.0243(9) -0.0026(8) C2 0.0875(16) 0.0412(10) 0.0517(11) -0.0011(8) 0.0359(11) 0.0091(10) C3 0.0760(15) 0.0538(11) 0.0630(12) 0.0132(10) 0.0444(12) 0.0224(10) C4 0.0516(11) 0.0549(11) 0.0601(12) 0.0143(9) 0.0319(9) 0.0121(9) C5 0.0440(9) 0.0389(8) 0.0408(8) 0.0114(7) 0.0217(7) 0.0043(7) C6 0.0340(8) 0.0431(9) 0.0393(9) 0.0089(7) 0.0122(7) -0.0037(6) C7 0.0367(8) 0.0359(8) 0.0369(8) 0.0032(6) 0.0117(7) -0.0045(6) C8 0.0463(10) 0.0428(9) 0.0475(10) -0.0033(8) 0.0117(8) -0.0078(8) C9 0.0502(11) 0.0498(10) 0.0538(11) -0.0015(9) 0.0064(9) -0.0145(9) C10 0.0391(11) 0.0838(17) 0.0926(19) -0.0187(15) 0.0096(11) 0.0110(11) C11 0.0858(16) 0.0571(12) 0.0521(11) 0.0014(9) 0.0400(11) 0.0091(11) C12 0.0737(15) 0.0455(11) 0.0688(14) 0.0107(10) 0.0271(12) 0.0072(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C7 2.0020(16) . ? Pd1 N2 2.0935(16) . ? Pd1 N1 2.1163(14) . ? Pd1 P1 2.2350(4) . ? S1 C9 1.708(3) . ? S1 C6 1.7316(17) . ? P1 C11 1.799(2) . ? P1 C10 1.811(2) . ? P1 C12 1.812(2) . ? N1 C1 1.338(2) . ? N1 C5 1.350(2) . ? N2 N3 1.175(2) . ? N3 N4 1.143(2) . ? C1 C2 1.382(3) . ? C1 H1 0.9300 . ? C2 C3 1.375(3) . ? C2 H2 0.9300 . ? C3 C4 1.376(3) . ? C3 H3 0.9300 . ? C4 C5 1.394(2) . ? C4 H4 0.9300 . ? C5 C6 1.443(3) . ? C6 C7 1.374(2) . ? C7 C8 1.427(2) . ? C8 C9 1.353(3) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? 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 C7 Pd1 N2 170.55(7) . . ? C7 Pd1 N1 81.22(6) . . ? N2 Pd1 N1 89.45(6) . . ? C7 Pd1 P1 94.43(5) . . ? N2 Pd1 P1 95.00(5) . . ? N1 Pd1 P1 172.92(4) . . ? C9 S1 C6 90.67(9) . . ? C11 P1 C10 103.13(13) . . ? C11 P1 C12 104.83(11) . . ? C10 P1 C12 101.93(13) . . ? C11 P1 Pd1 116.22(8) . . ? C10 P1 Pd1 113.69(9) . . ? C12 P1 Pd1 115.32(8) . . ? C1 N1 C5 119.54(16) . . ? C1 N1 Pd1 126.89(13) . . ? C5 N1 Pd1 113.43(11) . . ? N3 N2 Pd1 127.62(14) . . ? N4 N3 N2 175.8(2) . . ? N1 C1 C2 121.9(2) . . ? N1 C1 H1 119.1 . . ? C2 C1 H1 119.1 . . ? C3 C2 C1 118.8(2) . . ? C3 C2 H2 120.6 . . ? C1 C2 H2 120.6 . . ? C2 C3 C4 119.88(19) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C3 C4 C5 118.8(2) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? N1 C5 C4 120.98(18) . . ? N1 C5 C6 112.30(14) . . ? C4 C5 C6 126.72(18) . . ? C7 C6 C5 121.86(15) . . ? C7 C6 S1 113.02(13) . . ? C5 C6 S1 125.09(14) . . ? C6 C7 C8 109.96(15) . . ? C6 C7 Pd1 111.11(12) . . ? C8 C7 Pd1 138.80(14) . . ? C9 C8 C7 114.01(19) . . ? C9 C8 H8 123.0 . . ? C7 C8 H8 123.0 . . ? C8 C9 S1 112.34(16) . . ? C8 C9 H9 123.8 . . ? S1 C9 H9 123.8 . . ? P1 C10 H10A 109.5 . . ? P1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? P1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? P1 C11 H11A 109.5 . . ? P1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? P1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? P1 C12 H12A 109.5 . . ? P1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? P1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.484 _refine_diff_density_min -0.516 _refine_diff_density_rms 0.049 #=========================================================END data_lke215 _database_code_depnum_ccdc_archive 'CCDC 713102' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H27 N5 P2 Pd' _chemical_formula_weight 481.79 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' 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 'P2(1)/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.473(4) _cell_length_b 9.376(3) _cell_length_c 17.467(5) _cell_angle_alpha 90.00 _cell_angle_beta 91.602(18) _cell_angle_gamma 90.00 _cell_volume 2205.6(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 32 _cell_measurement_theta_min 2.86 _cell_measurement_theta_max 12.52 _exptl_crystal_description 'BLOCK ' _exptl_crystal_colour 'BROWN ' _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.451 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 984 _exptl_absorpt_coefficient_mu 0.998 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3985 _exptl_absorpt_correction_T_max 0.4706 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 4061 _diffrn_reflns_av_R_equivalents 0.0576 _diffrn_reflns_av_sigmaI/netI 0.0425 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 25.02 _reflns_number_total 3884 _reflns_number_gt 3309 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _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^)+(0.0440P)^2^+0.7672P] 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 3884 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0437 _refine_ls_R_factor_gt 0.0339 _refine_ls_wR_factor_ref 0.0880 _refine_ls_wR_factor_gt 0.0821 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _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 0.338485(18) 0.21154(3) 0.653374(13) 0.03317(10) Uani 1 1 d . . . P1 P 0.39700(7) 0.02389(9) 0.72862(5) 0.0396(2) Uani 1 1 d . . . P2 P 0.27314(7) 0.40371(9) 0.58418(5) 0.0389(2) Uani 1 1 d . . . N1 N 0.1212(2) 0.0318(4) 0.63139(18) 0.0524(8) Uani 1 1 d . . . N2 N 0.1903(2) 0.0346(3) 0.58769(18) 0.0521(8) Uani 1 1 d . . . N3 N 0.4737(2) 0.2173(3) 0.5918(2) 0.0515(8) Uani 1 1 d . . . N4 N 0.4742(2) 0.1990(3) 0.5263(2) 0.0491(8) Uani 1 1 d . . . N5 N 0.4791(3) 0.1846(5) 0.4597(2) 0.0813(12) Uani 1 1 d . . . C1 C 0.2151(2) 0.2107(3) 0.71532(18) 0.0353(7) Uani 1 1 d . . . C2 C 0.2069(3) 0.2977(4) 0.78024(19) 0.0414(8) Uani 1 1 d . . . H2 H 0.2613 0.3523 0.7963 0.050 Uiso 1 1 calc R . . C3 C 0.1201(3) 0.3051(4) 0.8214(2) 0.0490(9) Uani 1 1 d . . . H3 H 0.1168 0.3661 0.8632 0.059 Uiso 1 1 calc R . . C4 C 0.0387(3) 0.2225(5) 0.8007(2) 0.0599(11) Uani 1 1 d . . . H4 H -0.0192 0.2272 0.8284 0.072 Uiso 1 1 calc R . . C5 C 0.0445(3) 0.1335(5) 0.7386(2) 0.0587(10) Uani 1 1 d . . . H5 H -0.0094 0.0760 0.7250 0.070 Uiso 1 1 calc R . . C6 C 0.1307(3) 0.1280(4) 0.69530(19) 0.0420(8) Uani 1 1 d . . . C7 C 0.1799(3) -0.0636(4) 0.5231(2) 0.0464(9) Uani 1 1 d . . . C8 C 0.2623(3) -0.0746(5) 0.4784(2) 0.0577(10) Uani 1 1 d . . . H8 H 0.3190 -0.0221 0.4909 0.069 Uiso 1 1 calc R . . C9 C 0.2611(3) -0.1630(5) 0.4156(2) 0.0630(11) Uani 1 1 d . . . H9 H 0.3175 -0.1717 0.3865 0.076 Uiso 1 1 calc R . . C10 C 0.1771(4) -0.2383(5) 0.3954(3) 0.0680(12) Uani 1 1 d . . . H10 H 0.1761 -0.2959 0.3521 0.082 Uiso 1 1 calc R . . C11 C 0.0931(4) -0.2282(5) 0.4401(3) 0.0689(13) Uani 1 1 d . . . H11 H 0.0361 -0.2800 0.4273 0.083 Uiso 1 1 calc R . . C12 C 0.0958(3) -0.1396(4) 0.5042(2) 0.0546(10) Uani 1 1 d . . . H12 H 0.0402 -0.1319 0.5343 0.065 Uiso 1 1 calc R . . C13 C 0.5279(3) -0.0164(5) 0.7200(3) 0.0625(11) Uani 1 1 d . . . H13A H 0.5665 0.0673 0.7317 0.094 Uiso 1 1 calc R . . H13B H 0.5403 -0.0466 0.6686 0.094 Uiso 1 1 calc R . . H13C H 0.5463 -0.0913 0.7551 0.094 Uiso 1 1 calc R . . C14 C 0.3812(3) 0.0384(5) 0.8313(2) 0.0639(11) Uani 1 1 d . . . H14A H 0.3130 0.0595 0.8413 0.096 Uiso 1 1 calc R . . H14B H 0.4227 0.1134 0.8515 0.096 Uiso 1 1 calc R . . H14C H 0.3994 -0.0502 0.8555 0.096 Uiso 1 1 calc R . . C15 C 0.3388(4) -0.1457(4) 0.7051(3) 0.0704(13) Uani 1 1 d . . . H15A H 0.2680 -0.1364 0.7076 0.106 Uiso 1 1 calc R . . H15B H 0.3616 -0.2169 0.7410 0.106 Uiso 1 1 calc R . . H15C H 0.3560 -0.1735 0.6543 0.106 Uiso 1 1 calc R . . C16 C 0.3641(3) 0.5282(4) 0.5476(3) 0.0628(11) Uani 1 1 d . . . H16A H 0.4042 0.5649 0.5894 0.094 Uiso 1 1 calc R . . H16B H 0.3304 0.6055 0.5219 0.094 Uiso 1 1 calc R . . H16C H 0.4057 0.4797 0.5122 0.094 Uiso 1 1 calc R . . C17 C 0.2057(4) 0.3475(5) 0.4978(2) 0.0714(13) Uani 1 1 d . . . H17A H 0.1549 0.2808 0.5109 0.107 Uiso 1 1 calc R . . H17B H 0.2507 0.3030 0.4635 0.107 Uiso 1 1 calc R . . H17C H 0.1757 0.4292 0.4732 0.107 Uiso 1 1 calc R . . C18 C 0.1849(4) 0.5212(5) 0.6299(3) 0.0755(14) Uani 1 1 d . . . H18A H 0.1331 0.4653 0.6517 0.113 Uiso 1 1 calc R . . H18B H 0.1566 0.5856 0.5925 0.113 Uiso 1 1 calc R . . H18C H 0.2185 0.5748 0.6696 0.113 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 0.03491(16) 0.03371(15) 0.03111(14) 0.00094(10) 0.00462(10) 0.00134(11) P1 0.0468(5) 0.0357(4) 0.0363(4) 0.0030(4) 0.0006(4) 0.0030(4) P2 0.0398(5) 0.0390(5) 0.0380(4) 0.0047(4) 0.0011(3) 0.0016(4) N1 0.0486(19) 0.058(2) 0.0511(18) -0.0046(16) 0.0059(15) -0.0047(16) N2 0.0471(19) 0.0532(19) 0.0560(19) -0.0007(16) -0.0006(15) -0.0072(15) N3 0.0394(17) 0.060(2) 0.056(2) 0.0035(16) 0.0125(15) 0.0043(15) N4 0.0467(18) 0.0434(18) 0.058(2) 0.0033(15) 0.0152(15) -0.0013(14) N5 0.096(3) 0.089(3) 0.061(2) -0.007(2) 0.025(2) -0.010(2) C1 0.0366(17) 0.0358(17) 0.0338(16) 0.0018(14) 0.0047(13) 0.0020(14) C2 0.0436(19) 0.045(2) 0.0353(17) -0.0051(15) 0.0029(14) -0.0035(16) C3 0.053(2) 0.055(2) 0.0397(18) -0.0038(17) 0.0095(16) 0.0019(18) C4 0.047(2) 0.073(3) 0.061(2) -0.007(2) 0.0238(19) -0.003(2) C5 0.043(2) 0.069(3) 0.064(2) -0.005(2) 0.0097(18) -0.013(2) C6 0.0434(19) 0.0425(19) 0.0400(17) -0.0023(15) 0.0027(14) -0.0036(16) C7 0.060(2) 0.0394(19) 0.0397(18) 0.0015(15) -0.0056(16) 0.0042(17) C8 0.062(3) 0.056(2) 0.055(2) -0.0022(19) 0.0033(19) -0.002(2) C9 0.063(3) 0.068(3) 0.058(2) -0.010(2) 0.009(2) 0.004(2) C10 0.082(3) 0.072(3) 0.050(2) -0.017(2) -0.003(2) 0.015(3) C11 0.060(3) 0.072(3) 0.075(3) -0.018(2) -0.013(2) -0.005(2) C12 0.051(2) 0.061(2) 0.052(2) 0.0010(19) 0.0070(17) 0.009(2) C13 0.054(2) 0.068(3) 0.065(3) 0.013(2) 0.0030(19) 0.017(2) C14 0.078(3) 0.071(3) 0.042(2) 0.010(2) -0.0004(19) 0.016(2) C15 0.091(3) 0.041(2) 0.079(3) 0.010(2) -0.019(3) -0.006(2) C16 0.060(3) 0.053(2) 0.075(3) 0.021(2) 0.004(2) -0.007(2) C17 0.081(3) 0.076(3) 0.056(2) 0.016(2) -0.026(2) -0.011(3) C18 0.084(3) 0.066(3) 0.077(3) 0.021(2) 0.028(3) 0.034(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C1 2.009(3) . ? Pd1 N3 2.142(3) . ? Pd1 P1 2.3209(10) . ? Pd1 P2 2.3287(10) . ? P1 C15 1.815(4) . ? P1 C13 1.815(4) . ? P1 C14 1.818(4) . ? P2 C17 1.818(4) . ? P2 C16 1.821(4) . ? P2 C18 1.822(4) . ? N1 N2 1.220(4) . ? N1 C6 1.438(5) . ? N2 C7 1.460(5) . ? N3 N4 1.158(5) . ? N4 N5 1.175(5) . ? C1 C2 1.404(5) . ? C1 C6 1.413(5) . ? C2 C3 1.392(5) . ? C2 H2 0.9300 . ? C3 C4 1.383(6) . ? C3 H3 0.9300 . ? C4 C5 1.372(6) . ? C4 H4 0.9300 . ? C5 C6 1.405(5) . ? C5 H5 0.9300 . ? C7 C12 1.371(5) . ? C7 C8 1.378(5) . ? C8 C9 1.375(6) . ? C8 H8 0.9300 . ? C9 C10 1.371(7) . ? C9 H9 0.9300 . ? C10 C11 1.396(7) . ? C10 H10 0.9300 . ? C11 C12 1.393(6) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pd1 N3 177.26(13) . . ? C1 Pd1 P1 88.00(9) . . ? N3 Pd1 P1 91.32(9) . . ? C1 Pd1 P2 88.63(9) . . ? N3 Pd1 P2 91.99(9) . . ? P1 Pd1 P2 176.35(3) . . ? C15 P1 C13 102.3(2) . . ? C15 P1 C14 103.1(2) . . ? C13 P1 C14 103.8(2) . . ? C15 P1 Pd1 113.48(15) . . ? C13 P1 Pd1 115.24(14) . . ? C14 P1 Pd1 117.07(14) . . ? C17 P2 C16 102.7(2) . . ? C17 P2 C18 102.8(3) . . ? C16 P2 C18 102.7(2) . . ? C17 P2 Pd1 112.32(17) . . ? C16 P2 Pd1 115.42(14) . . ? C18 P2 Pd1 118.84(15) . . ? N2 N1 C6 114.8(3) . . ? N1 N2 C7 114.3(3) . . ? N4 N3 Pd1 121.4(3) . . ? N3 N4 N5 176.5(4) . . ? C2 C1 C6 116.0(3) . . ? C2 C1 Pd1 121.2(2) . . ? C6 C1 Pd1 122.8(2) . . ? C3 C2 C1 122.2(3) . . ? C3 C2 H2 118.9 . . ? C1 C2 H2 118.9 . . ? C4 C3 C2 120.6(3) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C5 C4 C3 119.0(4) . . ? C5 C4 H4 120.5 . . ? C3 C4 H4 120.5 . . ? C4 C5 C6 121.0(4) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? C5 C6 C1 121.2(3) . . ? C5 C6 N1 112.6(3) . . ? C1 C6 N1 126.2(3) . . ? C12 C7 C8 119.8(4) . . ? C12 C7 N2 125.1(4) . . ? C8 C7 N2 115.1(3) . . ? C9 C8 C7 120.3(4) . . ? C9 C8 H8 119.8 . . ? C7 C8 H8 119.8 . . ? C10 C9 C8 120.5(4) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C9 C10 C11 119.9(4) . . ? C9 C10 H10 120.1 . . ? C11 C10 H10 120.1 . . ? C12 C11 C10 119.0(4) . . ? C12 C11 H11 120.5 . . ? C10 C11 H11 120.5 . . ? C7 C12 C11 120.5(4) . . ? C7 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? P1 C13 H13A 109.5 . . ? P1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? P1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? P1 C14 H14A 109.5 . . ? P1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? P1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? P1 C15 H15A 109.5 . . ? P1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? P1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? P2 C16 H16A 109.5 . . ? P2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? P2 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? P2 C17 H17A 109.5 . . ? P2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? P2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? P2 C18 H18A 109.5 . . ? P2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? P2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.581 _refine_diff_density_min -0.704 _refine_diff_density_rms 0.074 #=========================================================END data_jht60 _database_code_depnum_ccdc_archive 'CCDC 713103' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H38 N8 P2 Pd2 S2' _chemical_formula_weight 1029.69 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' P P 0.1023 0.0942 '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' Pd Pd -0.9988 1.0072 '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 9.74700(10) _cell_length_b 15.0138(2) _cell_length_c 15.8289(2) _cell_angle_alpha 110.1410(10) _cell_angle_beta 100.5590(10) _cell_angle_gamma 96.7260(10) _cell_volume 2096.76(4) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9988 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 27.42 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_min 0.08 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_max 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.631 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1036 _exptl_absorpt_coefficient_mu 1.078 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8133 _exptl_absorpt_correction_T_max 0.9187 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30837 _diffrn_reflns_av_R_equivalents 0.0440 _diffrn_reflns_av_sigmaI/netI 0.0452 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 27.91 _reflns_number_total 9872 _reflns_number_gt 6814 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0392P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9872 _refine_ls_number_parameters 532 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0557 _refine_ls_R_factor_gt 0.0348 _refine_ls_wR_factor_ref 0.0810 _refine_ls_wR_factor_gt 0.0732 _refine_ls_goodness_of_fit_ref 0.921 _refine_ls_restrained_S_all 0.921 _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 0.95812(2) 0.290915(15) 0.775514(14) 0.04680(7) Uani 1 1 d . . . Pd2 Pd 0.90348(2) 0.192810(15) 0.196204(13) 0.04563(7) Uani 1 1 d . . . S1 S 1.17373(10) 0.42961(7) 1.07393(5) 0.0697(2) Uani 1 1 d . . . S2 S 1.19728(11) 0.15112(7) 0.00942(6) 0.0768(3) Uani 1 1 d . . . P1 P 1.11700(8) 0.26884(6) 0.68821(5) 0.04796(18) Uani 1 1 d . . . P2 P 1.02998(7) 0.25208(5) 0.34399(4) 0.04247(16) Uani 1 1 d . . . N1 N 0.8264(3) 0.30651(17) 0.86979(18) 0.0542(6) Uani 1 1 d . . . N2 N 0.7768(4) 0.2333(4) 0.6668(3) 0.1199(16) Uani 1 1 d . . . N3 N 0.7242(4) 0.2076(3) 0.6092(3) 0.1073(15) Uani 1 1 d . . . N4 N 0.6930(6) 0.1511(4) 0.5185(4) 0.1668(19) Uani 1 1 d . . . N5 N 0.8095(3) 0.12502(17) 0.05246(16) 0.0567(6) Uani 1 1 d . . . N6 N 0.6973(3) 0.1768(2) 0.2194(2) 0.0776(8) Uani 1 1 d . . . N7 N 0.6394(3) 0.2211(2) 0.2729(2) 0.0596(7) Uani 1 1 d . . . N8 N 0.5771(3) 0.2606(3) 0.3232(3) 0.0953(11) Uani 1 1 d . . . C1 C 1.1081(3) 0.3549(2) 0.89479(19) 0.0488(7) Uani 1 1 d . . . C2 C 1.2575(3) 0.3857(2) 0.9236(2) 0.0572(7) Uani 1 1 d . . . H2 H 1.3162 0.3787 0.8825 0.069 Uiso 1 1 calc R . . C3 C 1.3071(4) 0.4265(2) 1.0172(2) 0.0671(9) Uani 1 1 d . . . H3 H 1.4028 0.4502 1.0470 0.081 Uiso 1 1 calc R . . C4 C 1.0487(3) 0.3747(2) 0.96993(19) 0.0521(7) Uani 1 1 d . . . C5 C 0.8984(3) 0.3493(2) 0.9595(2) 0.0558(7) Uani 1 1 d . . . C6 C 0.8270(4) 0.3634(3) 1.0300(3) 0.0790(10) Uani 1 1 d . . . H6 H 0.8763 0.3937 1.0918 0.095 Uiso 1 1 calc R . . C7 C 0.6814(5) 0.3316(3) 1.0066(3) 0.0915(12) Uani 1 1 d . . . H7 H 0.6320 0.3398 1.0529 0.110 Uiso 1 1 calc R . . C8 C 0.6103(4) 0.2884(3) 0.9164(3) 0.0835(11) Uani 1 1 d . . . H8 H 0.5122 0.2667 0.9002 0.100 Uiso 1 1 calc R . . C9 C 0.6855(3) 0.2772(2) 0.8497(3) 0.0682(9) Uani 1 1 d . . . H9 H 0.6365 0.2479 0.7878 0.082 Uiso 1 1 calc R . . C10 C 1.0486(3) 0.2290(2) 0.56248(18) 0.0518(7) Uani 1 1 d . . . H10A H 1.1268 0.2152 0.5331 0.062 Uiso 1 1 calc R . . H10B H 0.9799 0.1690 0.5414 0.062 Uiso 1 1 calc R . . C11 C 0.9786(3) 0.3002(2) 0.52980(18) 0.0499(7) Uani 1 1 d . . . H11A H 1.0488 0.3589 0.5476 0.060 Uiso 1 1 calc R . . H11B H 0.9037 0.3169 0.5617 0.060 Uiso 1 1 calc R . . C12 C 0.9150(3) 0.2635(2) 0.42547(18) 0.0483(7) Uani 1 1 d . . . H12A H 0.8516 0.3059 0.4150 0.058 Uiso 1 1 calc R . . H12B H 0.8561 0.2002 0.4079 0.058 Uiso 1 1 calc R . . C13 C 1.2119(3) 0.1738(2) 0.69813(19) 0.0556(7) Uani 1 1 d . . . C14 C 1.2121(3) 0.1433(2) 0.77020(19) 0.0535(7) Uani 1 1 d . . . H14 H 1.1663 0.1730 0.8159 0.064 Uiso 1 1 calc R . . C15 C 1.2796(3) 0.0687(2) 0.7761(2) 0.0625(8) Uani 1 1 d . . . H15 H 1.2794 0.0493 0.8259 0.075 Uiso 1 1 calc R . . C16 C 1.3458(4) 0.0239(3) 0.7101(3) 0.0738(10) Uani 1 1 d . . . H16 H 1.3878 -0.0279 0.7129 0.089 Uiso 1 1 calc R . . C17 C 1.3502(5) 0.0555(3) 0.6390(3) 0.0999(15) Uani 1 1 d . . . H17 H 1.3991 0.0268 0.5948 0.120 Uiso 1 1 calc R . . C18 C 1.2836(5) 0.1289(3) 0.6323(3) 0.0963(14) Uani 1 1 d . . . H18 H 1.2865 0.1489 0.5830 0.116 Uiso 1 1 calc R . . C19 C 1.2512(3) 0.3761(3) 0.71374(19) 0.0600(8) Uani 1 1 d . . . C20 C 1.2079(4) 0.4642(3) 0.7308(2) 0.0734(9) Uani 1 1 d . . . H20 H 1.1133 0.4668 0.7320 0.088 Uiso 1 1 calc R . . C21 C 1.2990(6) 0.5467(3) 0.7459(3) 0.1006(14) Uani 1 1 d . . . H21 H 1.2676 0.6047 0.7554 0.121 Uiso 1 1 calc R . . C22 C 1.4383(8) 0.5419(5) 0.7466(3) 0.137(3) Uani 1 1 d . . . H22 H 1.5026 0.5981 0.7584 0.164 Uiso 1 1 calc R . . C23 C 1.4860(5) 0.4569(5) 0.7305(3) 0.1158(19) Uani 1 1 d . . . H23 H 1.5814 0.4558 0.7313 0.139 Uiso 1 1 calc R . . C24 C 1.3910(4) 0.3718(3) 0.7127(2) 0.0849(11) Uani 1 1 d . . . H24 H 1.4218 0.3133 0.7005 0.102 Uiso 1 1 calc R . . C25 C 1.1427(3) 0.1688(2) 0.36296(18) 0.0455(6) Uani 1 1 d . . . C26 C 1.2889(3) 0.1897(2) 0.3899(2) 0.0531(7) Uani 1 1 d . . . H26 H 1.3378 0.2511 0.4010 0.064 Uiso 1 1 calc R . . C27 C 1.3638(3) 0.1197(3) 0.4006(2) 0.0637(8) Uani 1 1 d . . . H27 H 1.4627 0.1344 0.4185 0.076 Uiso 1 1 calc R . . C28 C 1.2935(4) 0.0304(3) 0.3853(2) 0.0664(9) Uani 1 1 d . . . H28 H 1.3446 -0.0158 0.3934 0.080 Uiso 1 1 calc R . . C29 C 1.1491(4) 0.0073(2) 0.3580(2) 0.0699(9) Uani 1 1 d . . . H29 H 1.1021 -0.0546 0.3470 0.084 Uiso 1 1 calc R . . C30 C 1.0715(3) 0.0761(2) 0.3466(2) 0.0589(8) Uani 1 1 d . . . H30 H 0.9726 0.0603 0.3281 0.071 Uiso 1 1 calc R . . C31 C 1.1416(3) 0.3709(2) 0.38237(18) 0.0476(6) Uani 1 1 d . . . C32 C 1.2392(3) 0.4141(2) 0.4676(2) 0.0578(8) Uani 1 1 d . . . H32 H 1.2538 0.3802 0.5068 0.069 Uiso 1 1 calc R . . C33 C 1.3150(3) 0.5072(2) 0.4946(2) 0.0659(8) Uani 1 1 d . . . H33 H 1.3800 0.5357 0.5519 0.079 Uiso 1 1 calc R . . C34 C 1.2946(4) 0.5574(2) 0.4376(3) 0.0691(9) Uani 1 1 d . . . H34 H 1.3458 0.6199 0.4560 0.083 Uiso 1 1 calc R . . C35 C 1.1987(3) 0.5155(2) 0.3530(2) 0.0620(8) Uani 1 1 d . . . H35 H 1.1855 0.5501 0.3144 0.074 Uiso 1 1 calc R . . C36 C 1.1216(3) 0.4231(2) 0.3245(2) 0.0526(7) Uani 1 1 d . . . H36 H 1.0568 0.3955 0.2672 0.063 Uiso 1 1 calc R . . C37 C 1.0811(3) 0.19527(19) 0.14889(19) 0.0479(6) Uani 1 1 d . . . C38 C 1.2292(3) 0.2268(2) 0.1845(2) 0.0560(7) Uani 1 1 d . . . H38 H 1.2716 0.2572 0.2475 0.067 Uiso 1 1 calc R . . C39 C 1.3044(4) 0.2085(2) 0.1178(2) 0.0694(9) Uani 1 1 d . . . H39 H 1.4029 0.2254 0.1302 0.083 Uiso 1 1 calc R . . C40 C 1.0485(3) 0.1518(2) 0.0536(2) 0.0567(7) Uani 1 1 d . . . C41 C 0.9045(4) 0.1118(2) 0.0004(2) 0.0607(8) Uani 1 1 d . . . C42 C 0.8628(5) 0.0620(3) -0.0955(2) 0.0851(11) Uani 1 1 d . . . H42 H 0.9291 0.0538 -0.1316 0.102 Uiso 1 1 calc R . . C43 C 0.7179(5) 0.0248(3) -0.1352(3) 0.0976(14) Uani 1 1 d . . . H43 H 0.6867 -0.0103 -0.1987 0.117 Uiso 1 1 calc R . . C44 C 0.6234(5) 0.0396(3) -0.0822(3) 0.0871(12) Uani 1 1 d . . . H44 H 0.5267 0.0161 -0.1088 0.105 Uiso 1 1 calc R . . C45 C 0.6713(4) 0.0901(2) 0.0125(2) 0.0690(9) Uani 1 1 d . . . H45 H 0.6057 0.0999 0.0491 0.083 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 0.04342(12) 0.05648(14) 0.03862(13) 0.01758(10) 0.00645(9) 0.00877(10) Pd2 0.04854(13) 0.05239(14) 0.02942(12) 0.01169(9) 0.00222(9) 0.00760(10) S1 0.0816(6) 0.0812(6) 0.0369(4) 0.0136(4) 0.0086(4) 0.0158(5) S2 0.0952(7) 0.0934(7) 0.0456(5) 0.0212(5) 0.0321(5) 0.0236(5) P1 0.0467(4) 0.0646(5) 0.0343(4) 0.0214(3) 0.0064(3) 0.0135(4) P2 0.0427(4) 0.0515(4) 0.0290(3) 0.0121(3) 0.0045(3) 0.0094(3) N1 0.0529(15) 0.0563(15) 0.0566(16) 0.0219(13) 0.0183(12) 0.0119(12) N2 0.074(2) 0.185(4) 0.077(3) 0.059(3) -0.022(2) -0.032(3) N3 0.095(3) 0.106(3) 0.098(3) 0.066(3) -0.045(2) -0.044(2) N4 0.129(4) 0.201(5) 0.136(5) 0.046(4) -0.002(3) 0.009(4) N5 0.0705(17) 0.0555(15) 0.0342(13) 0.0132(11) -0.0016(12) 0.0088(13) N6 0.0486(16) 0.106(2) 0.0532(17) 0.0111(16) 0.0013(13) -0.0016(15) N7 0.0414(14) 0.082(2) 0.0548(17) 0.0336(15) 0.0022(13) 0.0015(14) N8 0.0570(18) 0.127(3) 0.095(3) 0.029(2) 0.0268(18) 0.0149(19) C1 0.0559(17) 0.0506(16) 0.0370(15) 0.0142(13) 0.0082(13) 0.0106(13) C2 0.0523(17) 0.073(2) 0.0417(17) 0.0204(15) 0.0054(13) 0.0095(15) C3 0.066(2) 0.076(2) 0.0472(19) 0.0191(16) -0.0036(15) 0.0063(17) C4 0.0601(18) 0.0553(17) 0.0410(16) 0.0164(14) 0.0118(13) 0.0173(14) C5 0.0653(19) 0.0565(18) 0.0529(19) 0.0208(15) 0.0240(16) 0.0226(15) C6 0.087(3) 0.097(3) 0.060(2) 0.028(2) 0.035(2) 0.027(2) C7 0.083(3) 0.118(3) 0.092(3) 0.044(3) 0.051(3) 0.027(3) C8 0.065(2) 0.096(3) 0.100(3) 0.042(3) 0.034(2) 0.017(2) C9 0.056(2) 0.080(2) 0.074(2) 0.0314(19) 0.0220(17) 0.0143(17) C10 0.0553(17) 0.0656(19) 0.0352(15) 0.0200(14) 0.0081(12) 0.0155(15) C11 0.0550(17) 0.0601(18) 0.0341(15) 0.0160(13) 0.0087(12) 0.0166(14) C12 0.0472(15) 0.0614(18) 0.0344(14) 0.0164(13) 0.0054(12) 0.0146(13) C13 0.0539(17) 0.078(2) 0.0394(16) 0.0259(15) 0.0080(13) 0.0226(16) C14 0.0603(18) 0.0603(18) 0.0386(16) 0.0185(14) 0.0074(13) 0.0133(15) C15 0.073(2) 0.067(2) 0.0482(18) 0.0240(16) 0.0071(16) 0.0216(17) C16 0.068(2) 0.085(2) 0.068(2) 0.028(2) 0.0055(18) 0.0338(19) C17 0.121(3) 0.144(4) 0.068(3) 0.049(3) 0.039(2) 0.092(3) C18 0.115(3) 0.153(4) 0.070(3) 0.067(3) 0.051(2) 0.087(3) C19 0.0568(19) 0.088(2) 0.0330(15) 0.0284(16) 0.0032(13) -0.0011(17) C20 0.084(2) 0.072(2) 0.052(2) 0.0194(17) 0.0050(17) -0.006(2) C21 0.119(4) 0.092(3) 0.066(3) 0.027(2) 0.002(2) -0.036(3) C22 0.161(6) 0.145(5) 0.057(3) 0.035(3) -0.009(3) -0.084(5) C23 0.061(3) 0.195(6) 0.073(3) 0.051(4) 0.008(2) -0.032(4) C24 0.059(2) 0.136(3) 0.060(2) 0.044(2) 0.0128(17) -0.001(2) C25 0.0470(15) 0.0556(17) 0.0323(14) 0.0138(12) 0.0088(11) 0.0132(13) C26 0.0481(16) 0.0670(19) 0.0487(17) 0.0260(15) 0.0126(13) 0.0130(15) C27 0.0508(17) 0.091(3) 0.0536(19) 0.0283(18) 0.0131(14) 0.0246(18) C28 0.069(2) 0.072(2) 0.071(2) 0.0344(19) 0.0220(18) 0.0328(19) C29 0.074(2) 0.0563(19) 0.081(2) 0.0261(18) 0.0186(19) 0.0192(17) C30 0.0513(17) 0.0565(18) 0.061(2) 0.0156(15) 0.0096(15) 0.0085(15) C31 0.0507(16) 0.0504(16) 0.0360(15) 0.0095(13) 0.0101(12) 0.0097(13) C32 0.0572(18) 0.0636(19) 0.0421(17) 0.0132(15) 0.0053(14) 0.0031(15) C33 0.0587(19) 0.068(2) 0.053(2) 0.0058(17) 0.0100(15) 0.0019(17) C34 0.064(2) 0.0546(19) 0.078(3) 0.0096(19) 0.0272(19) 0.0052(16) C35 0.068(2) 0.0544(19) 0.069(2) 0.0253(17) 0.0219(18) 0.0187(17) C36 0.0556(17) 0.0547(18) 0.0456(17) 0.0147(14) 0.0121(13) 0.0158(14) C37 0.0584(17) 0.0475(16) 0.0386(15) 0.0159(13) 0.0133(13) 0.0118(13) C38 0.0608(19) 0.0636(19) 0.0420(17) 0.0160(14) 0.0166(14) 0.0111(15) C39 0.072(2) 0.080(2) 0.059(2) 0.0234(18) 0.0258(17) 0.0170(18) C40 0.075(2) 0.0574(18) 0.0370(16) 0.0159(14) 0.0132(15) 0.0152(16) C41 0.083(2) 0.0578(19) 0.0336(16) 0.0142(14) 0.0032(15) 0.0125(17) C42 0.113(3) 0.095(3) 0.0327(18) 0.0125(18) 0.0086(19) 0.015(2) C43 0.132(4) 0.098(3) 0.034(2) 0.013(2) -0.016(2) 0.004(3) C44 0.092(3) 0.093(3) 0.050(2) 0.020(2) -0.020(2) 0.001(2) C45 0.068(2) 0.073(2) 0.0501(19) 0.0202(17) -0.0120(16) 0.0071(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C1 2.009(3) . ? Pd1 N2 2.082(4) . ? Pd1 N1 2.113(2) . ? Pd1 P1 2.2375(7) . ? Pd2 C37 2.010(3) . ? Pd2 N6 2.109(3) . ? Pd2 N5 2.115(2) . ? Pd2 P2 2.2442(7) . ? S1 C3 1.706(4) . ? S1 C4 1.723(3) . ? S2 C39 1.700(4) . ? S2 C40 1.721(3) . ? P1 C13 1.824(3) . ? P1 C19 1.825(3) . ? P1 C10 1.834(3) . ? P2 C31 1.814(3) . ? P2 C25 1.822(3) . ? P2 C12 1.836(3) . ? N1 C9 1.335(4) . ? N1 C5 1.350(4) . ? N2 N3 0.885(4) . ? N3 N4 1.348(6) . ? N5 C45 1.336(4) . ? N5 C41 1.337(4) . ? N6 N7 1.163(4) . ? N7 N8 1.137(4) . ? C1 C4 1.374(4) . ? C1 C2 1.413(4) . ? C2 C3 1.360(4) . ? C2 H2 0.9300 . ? C3 H3 0.9300 . ? C4 C5 1.434(4) . ? C5 C6 1.390(4) . ? C6 C7 1.380(5) . ? C6 H6 0.9300 . ? C7 C8 1.353(6) . ? C7 H7 0.9300 . ? C8 C9 1.369(5) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 C11 1.516(4) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.528(4) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.368(4) . ? C13 C18 1.387(4) . ? C14 C15 1.385(4) . ? C14 H14 0.9300 . ? C15 C16 1.351(4) . ? C15 H15 0.9300 . ? C16 C17 1.369(5) . ? C16 H16 0.9300 . ? C17 C18 1.367(5) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C24 1.374(5) . ? C19 C20 1.389(5) . ? C20 C21 1.356(5) . ? C20 H20 0.9300 . ? C21 C22 1.366(8) . ? C21 H21 0.9300 . ? C22 C23 1.366(8) . ? C22 H22 0.9300 . ? C23 C24 1.396(6) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 C26 1.375(4) . ? C25 C30 1.395(4) . ? C26 C27 1.386(4) . ? C26 H26 0.9300 . ? C27 C28 1.351(5) . ? C27 H27 0.9300 . ? C28 C29 1.359(5) . ? C28 H28 0.9300 . ? C29 C30 1.390(4) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 C32 1.389(4) . ? C31 C36 1.399(4) . ? C32 C33 1.383(4) . ? C32 H32 0.9300 . ? C33 C34 1.363(5) . ? C33 H33 0.9300 . ? C34 C35 1.374(5) . ? C34 H34 0.9300 . ? C35 C36 1.376(4) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C37 C40 1.379(4) . ? C37 C38 1.408(4) . ? C38 C39 1.362(4) . ? C38 H38 0.9300 . ? C39 H39 0.9300 . ? C40 C41 1.435(4) . ? C41 C42 1.396(4) . ? C42 C43 1.397(6) . ? C42 H42 0.9300 . ? C43 C44 1.344(6) . ? C43 H43 0.9300 . ? C44 C45 1.384(5) . ? C44 H44 0.9300 . ? C45 H45 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pd1 N2 169.50(15) . . ? C1 Pd1 N1 80.94(11) . . ? N2 Pd1 N1 88.95(14) . . ? C1 Pd1 P1 93.50(8) . . ? N2 Pd1 P1 96.81(13) . . ? N1 Pd1 P1 172.60(7) . . ? C37 Pd2 N6 169.26(11) . . ? C37 Pd2 N5 81.15(11) . . ? N6 Pd2 N5 88.11(11) . . ? C37 Pd2 P2 91.82(8) . . ? N6 Pd2 P2 98.84(8) . . ? N5 Pd2 P2 171.18(7) . . ? C3 S1 C4 90.75(15) . . ? C39 S2 C40 91.01(15) . . ? C13 P1 C19 107.03(15) . . ? C13 P1 C10 102.27(13) . . ? C19 P1 C10 102.22(13) . . ? C13 P1 Pd1 111.73(10) . . ? C19 P1 Pd1 114.93(11) . . ? C10 P1 Pd1 117.31(10) . . ? C31 P2 C25 108.11(13) . . ? C31 P2 C12 105.29(12) . . ? C25 P2 C12 105.69(12) . . ? C31 P2 Pd2 115.50(9) . . ? C25 P2 Pd2 109.83(9) . . ? C12 P2 Pd2 111.88(9) . . ? C9 N1 C5 119.0(3) . . ? C9 N1 Pd1 127.3(2) . . ? C5 N1 Pd1 113.64(19) . . ? N3 N2 Pd1 158.9(5) . . ? N2 N3 N4 155.5(7) . . ? C45 N5 C41 119.7(3) . . ? C45 N5 Pd2 126.7(2) . . ? C41 N5 Pd2 113.4(2) . . ? N7 N6 Pd2 135.9(2) . . ? N8 N7 N6 176.5(3) . . ? C4 C1 C2 110.8(3) . . ? C4 C1 Pd1 111.1(2) . . ? C2 C1 Pd1 138.1(2) . . ? C3 C2 C1 113.4(3) . . ? C3 C2 H2 123.3 . . ? C1 C2 H2 123.3 . . ? C2 C3 S1 112.4(3) . . ? C2 C3 H3 123.8 . . ? S1 C3 H3 123.8 . . ? C1 C4 C5 121.8(3) . . ? C1 C4 S1 112.7(2) . . ? C5 C4 S1 125.5(2) . . ? N1 C5 C6 120.6(3) . . ? N1 C5 C4 112.5(2) . . ? C6 C5 C4 126.9(3) . . ? C7 C6 C5 118.7(4) . . ? C7 C6 H6 120.6 . . ? C5 C6 H6 120.6 . . ? C8 C7 C6 120.3(4) . . ? C8 C7 H7 119.9 . . ? C6 C7 H7 119.9 . . ? C7 C8 C9 118.7(4) . . ? C7 C8 H8 120.7 . . ? C9 C8 H8 120.7 . . ? N1 C9 C8 122.7(4) . . ? N1 C9 H9 118.6 . . ? C8 C9 H9 118.6 . . ? C11 C10 P1 115.43(19) . . ? C11 C10 H10A 108.4 . . ? P1 C10 H10A 108.4 . . ? C11 C10 H10B 108.4 . . ? P1 C10 H10B 108.4 . . ? H10A C10 H10B 107.5 . . ? C10 C11 C12 114.6(2) . . ? C10 C11 H11A 108.6 . . ? C12 C11 H11A 108.6 . . ? C10 C11 H11B 108.6 . . ? C12 C11 H11B 108.6 . . ? H11A C11 H11B 107.6 . . ? C11 C12 P2 120.9(2) . . ? C11 C12 H12A 107.1 . . ? P2 C12 H12A 107.1 . . ? C11 C12 H12B 107.1 . . ? P2 C12 H12B 107.1 . . ? H12A C12 H12B 106.8 . . ? C14 C13 C18 117.9(3) . . ? C14 C13 P1 120.8(2) . . ? C18 C13 P1 121.3(2) . . ? C13 C14 C15 120.9(3) . . ? C13 C14 H14 119.5 . . ? C15 C14 H14 119.5 . . ? C16 C15 C14 120.6(3) . . ? C16 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? C15 C16 C17 119.2(3) . . ? C15 C16 H16 120.4 . . ? C17 C16 H16 120.4 . . ? C18 C17 C16 120.8(3) . . ? C18 C17 H17 119.6 . . ? C16 C17 H17 119.6 . . ? C17 C18 C13 120.6(3) . . ? C17 C18 H18 119.7 . . ? C13 C18 H18 119.7 . . ? C24 C19 C20 119.3(3) . . ? C24 C19 P1 122.5(3) . . ? C20 C19 P1 118.2(3) . . ? C21 C20 C19 122.1(4) . . ? C21 C20 H20 118.9 . . ? C19 C20 H20 118.9 . . ? C20 C21 C22 118.0(5) . . ? C20 C21 H21 121.0 . . ? C22 C21 H21 121.0 . . ? C21 C22 C23 121.9(5) . . ? C21 C22 H22 119.0 . . ? C23 C22 H22 119.0 . . ? C22 C23 C24 119.8(5) . . ? C22 C23 H23 120.1 . . ? C24 C23 H23 120.1 . . ? C19 C24 C23 118.8(4) . . ? C19 C24 H24 120.6 . . ? C23 C24 H24 120.6 . . ? C26 C25 C30 118.8(3) . . ? C26 C25 P2 125.6(2) . . ? C30 C25 P2 115.6(2) . . ? C25 C26 C27 120.5(3) . . ? C25 C26 H26 119.8 . . ? C27 C26 H26 119.8 . . ? C28 C27 C26 120.2(3) . . ? C28 C27 H27 119.9 . . ? C26 C27 H27 119.9 . . ? C27 C28 C29 120.7(3) . . ? C27 C28 H28 119.6 . . ? C29 C28 H28 119.6 . . ? C28 C29 C30 120.2(3) . . ? C28 C29 H29 119.9 . . ? C30 C29 H29 119.9 . . ? C29 C30 C25 119.6(3) . . ? C29 C30 H30 120.2 . . ? C25 C30 H30 120.2 . . ? C32 C31 C36 118.8(3) . . ? C32 C31 P2 123.5(2) . . ? C36 C31 P2 117.6(2) . . ? C33 C32 C31 120.4(3) . . ? C33 C32 H32 119.8 . . ? C31 C32 H32 119.8 . . ? C34 C33 C32 120.2(3) . . ? C34 C33 H33 119.9 . . ? C32 C33 H33 119.9 . . ? C33 C34 C35 120.1(3) . . ? C33 C34 H34 120.0 . . ? C35 C34 H34 120.0 . . ? C34 C35 C36 120.9(3) . . ? C34 C35 H35 119.5 . . ? C36 C35 H35 119.5 . . ? C35 C36 C31 119.6(3) . . ? C35 C36 H36 120.2 . . ? C31 C36 H36 120.2 . . ? C40 C37 C38 110.7(3) . . ? C40 C37 Pd2 110.6(2) . . ? C38 C37 Pd2 138.7(2) . . ? C39 C38 C37 113.6(3) . . ? C39 C38 H38 123.2 . . ? C37 C38 H38 123.2 . . ? C38 C39 S2 112.2(3) . . ? C38 C39 H39 123.9 . . ? S2 C39 H39 123.9 . . ? C37 C40 C41 121.8(3) . . ? C37 C40 S2 112.5(2) . . ? C41 C40 S2 125.7(2) . . ? N5 C41 C42 121.5(3) . . ? N5 C41 C40 113.0(3) . . ? C42 C41 C40 125.5(3) . . ? C41 C42 C43 117.6(4) . . ? C41 C42 H42 121.2 . . ? C43 C42 H42 121.2 . . ? C44 C43 C42 120.3(4) . . ? C44 C43 H43 119.9 . . ? C42 C43 H43 119.9 . . ? C43 C44 C45 119.4(4) . . ? C43 C44 H44 120.3 . . ? C45 C44 H44 120.3 . . ? N5 C45 C44 121.5(4) . . ? N5 C45 H45 119.2 . . ? C44 C45 H45 119.2 . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 27.91 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.228 _refine_diff_density_min -0.444 _refine_diff_density_rms 0.069 #=========================================================END data_jht047 _database_code_depnum_ccdc_archive 'CCDC 713104' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H12 N2 Pd S2' _chemical_formula_weight 426.82 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.3366(3) _cell_length_b 9.9803(3) _cell_length_c 17.2315(6) _cell_angle_alpha 90.00 _cell_angle_beta 104.864(2) _cell_angle_gamma 90.00 _cell_volume 1551.94(9) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9894 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 28.28 _exptl_crystal_description BLOCK _exptl_crystal_colour orange _exptl_crystal_size_min 0.08 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_max 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.827 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 848 _exptl_absorpt_coefficient_mu 1.463 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6679 _exptl_absorpt_correction_T_max 0.8919 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24325 _diffrn_reflns_av_R_equivalents 0.0259 _diffrn_reflns_av_sigmaI/netI 0.0182 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.87 _diffrn_reflns_theta_max 28.36 _reflns_number_total 3863 _reflns_number_gt 3345 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0271P)^2^+0.3317P] 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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3863 _refine_ls_number_parameters 256 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0268 _refine_ls_R_factor_gt 0.0205 _refine_ls_wR_factor_ref 0.0534 _refine_ls_wR_factor_gt 0.0499 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _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 0.078114(14) 0.385213(13) 0.086560(8) 0.03834(6) Uani 1 1 d . . . S1 S 0.31280(7) 0.10425(6) -0.03778(4) 0.06003(15) Uani 1 1 d . . . S2 S 0.25705(7) 0.65312(6) 0.29500(3) 0.05927(14) Uani 1 1 d . . . N1 N -0.05962(17) 0.26911(15) -0.01190(9) 0.0438(3) Uani 1 1 d . . . N2 N -0.08350(17) 0.49703(15) 0.13219(9) 0.0432(3) Uani 1 1 d . . . C1 C -0.2051(2) 0.2715(2) -0.04536(14) 0.0567(5) Uani 1 1 d . . . C2 C -0.2769(3) 0.1835(3) -0.10382(15) 0.0652(6) Uani 1 1 d . . . C3 C -0.1948(3) 0.0899(3) -0.13096(16) 0.0693(7) Uani 1 1 d . . . C4 C -0.0441(3) 0.0871(3) -0.09995(15) 0.0626(6) Uani 1 1 d . . . C5 C 0.0225(2) 0.17845(18) -0.04048(12) 0.0458(4) Uani 1 1 d . . . C6 C 0.1787(2) 0.19236(18) -0.00592(12) 0.0453(4) Uani 1 1 d . . . C7 C 0.2361(2) 0.28788(18) 0.05102(11) 0.0427(4) Uani 1 1 d . . . C8 C 0.3929(2) 0.2886(2) 0.06630(13) 0.0528(5) Uani 1 1 d . . . C9 C 0.4484(3) 0.1960(2) 0.02383(14) 0.0597(6) Uani 1 1 d . . . C10 C -0.2308(2) 0.4999(2) 0.10851(14) 0.0540(5) Uani 1 1 d . . . C11 C -0.3181(3) 0.5830(2) 0.14118(15) 0.0580(5) Uani 1 1 d . . . C12 C -0.2499(3) 0.6688(2) 0.20125(15) 0.0609(6) Uani 1 1 d . . . C13 C -0.0985(3) 0.6678(2) 0.22746(14) 0.0565(5) Uani 1 1 d . . . C14 C -0.0165(2) 0.58110(18) 0.19285(11) 0.0436(4) Uani 1 1 d . . . C15 C 0.1416(2) 0.56703(19) 0.21615(11) 0.0444(4) Uani 1 1 d . . . C16 C 0.2150(2) 0.47822(18) 0.17889(11) 0.0422(4) Uani 1 1 d . . . C17 C 0.3684(2) 0.4799(2) 0.21908(13) 0.0527(5) Uani 1 1 d . . . C18 C 0.4064(3) 0.5680(3) 0.28074(13) 0.0602(5) Uani 1 1 d . . . H1 H -0.260(3) 0.339(3) -0.0257(15) 0.071(7) Uiso 1 1 d . . . H2 H -0.373(3) 0.188(2) -0.1242(15) 0.072(7) Uiso 1 1 d . . . H3 H -0.238(3) 0.030(3) -0.1718(16) 0.084(8) Uiso 1 1 d . . . H4 H 0.016(3) 0.026(3) -0.1158(16) 0.079(8) Uiso 1 1 d . . . H8 H 0.456(3) 0.342(2) 0.0974(15) 0.065(7) Uiso 1 1 d . . . H9 H 0.542(3) 0.179(2) 0.0252(13) 0.058(6) Uiso 1 1 d . . . H10 H -0.274(3) 0.446(3) 0.0688(15) 0.067(7) Uiso 1 1 d . . . H11 H -0.414(3) 0.580(2) 0.1207(15) 0.063(7) Uiso 1 1 d . . . H12 H -0.299(2) 0.726(2) 0.2277(13) 0.058(6) Uiso 1 1 d . . . H13 H -0.048(3) 0.719(2) 0.2668(16) 0.070(8) Uiso 1 1 d . . . H17 H 0.443(3) 0.425(2) 0.2076(14) 0.060(6) Uiso 1 1 d . . . H18 H 0.501(3) 0.590(2) 0.3188(14) 0.063(7) 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 0.04020(8) 0.03697(9) 0.03901(9) -0.00043(5) 0.01227(6) 0.00245(5) S1 0.0707(3) 0.0545(3) 0.0593(3) -0.0026(2) 0.0245(3) 0.0210(3) S2 0.0671(3) 0.0624(3) 0.0443(3) -0.0111(2) 0.0069(2) 0.0010(3) N1 0.0482(8) 0.0430(8) 0.0421(8) 0.0004(6) 0.0151(7) -0.0008(7) N2 0.0473(8) 0.0396(8) 0.0453(9) 0.0019(6) 0.0166(7) 0.0033(6) C1 0.0495(11) 0.0672(14) 0.0547(12) -0.0091(10) 0.0159(9) -0.0024(10) C2 0.0539(12) 0.0854(18) 0.0560(14) -0.0113(12) 0.0133(11) -0.0159(12) C3 0.0772(16) 0.0729(16) 0.0589(15) -0.0214(12) 0.0196(12) -0.0220(13) C4 0.0724(14) 0.0558(14) 0.0624(14) -0.0168(11) 0.0223(12) -0.0056(11) C5 0.0591(11) 0.0373(10) 0.0436(10) 0.0017(8) 0.0181(8) -0.0018(8) C6 0.0548(10) 0.0380(10) 0.0470(10) 0.0023(8) 0.0201(8) 0.0088(8) C7 0.0473(9) 0.0408(10) 0.0414(10) 0.0049(7) 0.0142(8) 0.0069(7) C8 0.0474(10) 0.0627(13) 0.0482(11) 0.0012(10) 0.0121(9) 0.0108(10) C9 0.0537(12) 0.0730(15) 0.0539(13) 0.0071(10) 0.0167(10) 0.0240(11) C10 0.0496(11) 0.0540(13) 0.0601(13) -0.0062(10) 0.0171(10) 0.0023(9) C11 0.0517(12) 0.0559(13) 0.0706(15) 0.0049(11) 0.0231(11) 0.0109(10) C12 0.0697(14) 0.0544(13) 0.0663(15) -0.0005(11) 0.0317(12) 0.0180(11) C13 0.0709(14) 0.0509(12) 0.0514(12) -0.0060(10) 0.0222(11) 0.0088(10) C14 0.0558(10) 0.0385(9) 0.0394(10) 0.0035(7) 0.0176(8) 0.0047(8) C15 0.0538(10) 0.0421(10) 0.0371(9) 0.0012(8) 0.0111(8) 0.0012(8) C16 0.0478(9) 0.0410(10) 0.0386(9) 0.0031(7) 0.0127(7) -0.0003(7) C17 0.0493(10) 0.0585(13) 0.0498(12) -0.0013(9) 0.0115(9) 0.0018(9) C18 0.0560(12) 0.0708(14) 0.0492(12) -0.0059(11) 0.0049(10) -0.0028(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 C7 1.9897(18) . ? Pd1 C16 1.9957(18) . ? Pd1 N2 2.1793(15) . ? Pd1 N1 2.1807(15) . ? S1 C9 1.696(3) . ? S1 C6 1.7304(19) . ? S2 C18 1.704(2) . ? S2 C15 1.7305(19) . ? N1 C1 1.332(3) . ? N1 C5 1.358(2) . ? N2 C10 1.331(3) . ? N2 C14 1.361(2) . ? C1 C2 1.374(3) . ? C1 H1 0.96(3) . ? C2 C3 1.365(4) . ? C2 H2 0.88(3) . ? C3 C4 1.371(4) . ? C3 H3 0.93(3) . ? C4 C5 1.393(3) . ? C4 H4 0.91(3) . ? C5 C6 1.434(3) . ? C6 C7 1.374(3) . ? C7 C8 1.419(3) . ? C8 C9 1.361(3) . ? C8 H8 0.87(2) . ? C9 H9 0.88(2) . ? C10 C11 1.380(3) . ? C10 H10 0.88(2) . ? C11 C12 1.368(4) . ? C11 H11 0.88(2) . ? C12 C13 1.369(3) . ? C12 H12 0.93(2) . ? C13 C14 1.387(3) . ? C13 H13 0.88(3) . ? C14 C15 1.434(3) . ? C15 C16 1.376(3) . ? C16 C17 1.422(3) . ? C17 C18 1.354(3) . ? C17 H17 0.95(2) . ? C18 H18 0.98(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 C7 Pd1 C16 95.67(8) . . ? C7 Pd1 N2 176.18(7) . . ? C16 Pd1 N2 80.51(7) . . ? C7 Pd1 N1 80.62(7) . . ? C16 Pd1 N1 175.27(6) . . ? N2 Pd1 N1 103.19(6) . . ? C9 S1 C6 90.67(10) . . ? C18 S2 C15 90.40(10) . . ? C1 N1 C5 117.54(18) . . ? C1 N1 Pd1 131.27(14) . . ? C5 N1 Pd1 111.17(12) . . ? C10 N2 C14 117.23(17) . . ? C10 N2 Pd1 131.07(14) . . ? C14 N2 Pd1 111.63(12) . . ? N1 C1 C2 123.9(2) . . ? N1 C1 H1 116.0(15) . . ? C2 C1 H1 120.1(15) . . ? C3 C2 C1 118.5(2) . . ? C3 C2 H2 120.3(17) . . ? C1 C2 H2 121.2(17) . . ? C2 C3 C4 119.4(2) . . ? C2 C3 H3 121.3(16) . . ? C4 C3 H3 119.2(16) . . ? C3 C4 C5 119.6(2) . . ? C3 C4 H4 122.7(17) . . ? C5 C4 H4 117.8(17) . . ? N1 C5 C4 121.1(2) . . ? N1 C5 C6 113.19(17) . . ? C4 C5 C6 125.7(2) . . ? C7 C6 C5 122.18(17) . . ? C7 C6 S1 113.42(15) . . ? C5 C6 S1 124.10(15) . . ? C6 C7 C8 109.30(17) . . ? C6 C7 Pd1 111.98(14) . . ? C8 C7 Pd1 138.71(15) . . ? C9 C8 C7 114.4(2) . . ? C9 C8 H8 117.3(16) . . ? C7 C8 H8 128.2(16) . . ? C8 C9 S1 112.16(17) . . ? C8 C9 H9 128.7(15) . . ? S1 C9 H9 119.2(15) . . ? N2 C10 C11 124.0(2) . . ? N2 C10 H10 117.5(16) . . ? C11 C10 H10 118.5(16) . . ? C12 C11 C10 118.4(2) . . ? C12 C11 H11 123.9(16) . . ? C10 C11 H11 117.6(16) . . ? C11 C12 C13 119.1(2) . . ? C11 C12 H12 124.6(14) . . ? C13 C12 H12 116.3(14) . . ? C12 C13 C14 120.0(2) . . ? C12 C13 H13 123.5(16) . . ? C14 C13 H13 116.5(16) . . ? N2 C14 C13 121.29(19) . . ? N2 C14 C15 113.07(16) . . ? C13 C14 C15 125.63(19) . . ? C16 C15 C14 122.18(17) . . ? C16 C15 S2 113.70(15) . . ? C14 C15 S2 124.08(14) . . ? C15 C16 C17 108.98(17) . . ? C15 C16 Pd1 112.22(13) . . ? C17 C16 Pd1 138.80(15) . . ? C18 C17 C16 114.7(2) . . ? C18 C17 H17 118.6(14) . . ? C16 C17 H17 126.7(14) . . ? C17 C18 S2 112.18(17) . . ? C17 C18 H18 132.8(14) . . ? S2 C18 H18 115.0(13) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 28.36 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.307 _refine_diff_density_min -0.321 _refine_diff_density_rms 0.051 #=========================================================END data_jht054 _database_code_depnum_ccdc_archive 'CCDC 713105' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H50 Cl4 N10 P2 Pd2' _chemical_formula_weight 1255.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/c ' _symmetry_space_group_name_Hall '-P 2ybc' 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 19.0312(9) _cell_length_b 9.1873(4) _cell_length_c 16.2466(8) _cell_angle_alpha 90.00 _cell_angle_beta 102.573(2) _cell_angle_gamma 90.00 _cell_volume 2772.5(2) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9983 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 27.74 _exptl_crystal_description BLOCK _exptl_crystal_colour orange _exptl_crystal_size_min 0.16 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_max 0.48 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.504 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1268 _exptl_absorpt_coefficient_mu 0.945 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6598 _exptl_absorpt_correction_T_max 0.8635 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37279 _diffrn_reflns_av_R_equivalents 0.0335 _diffrn_reflns_av_sigmaI/netI 0.0348 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 28.31 _reflns_number_total 6824 _reflns_number_gt 5021 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0485P)^2^+1.8955P] 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 6824 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0638 _refine_ls_R_factor_gt 0.0392 _refine_ls_wR_factor_ref 0.1004 _refine_ls_wR_factor_gt 0.0893 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _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 0.260734(11) 0.91224(2) 0.491563(15) 0.03638(8) Uani 1 1 d . . . Cl1 Cl 0.14442(11) 0.60183(19) 0.40494(12) 0.1302(6) Uani 1 1 d . . . Cl2 Cl 0.07906(15) 0.3658(2) 0.47367(13) 0.1666(9) Uani 1 1 d . . . P1 P 0.36301(4) 0.80773(7) 0.56384(5) 0.03029(16) Uani 1 1 d . . . N1 N 0.30203(17) 0.9228(3) 0.38128(19) 0.0551(7) Uani 1 1 d . . . N2 N 0.33523(17) 1.0182(3) 0.35936(17) 0.0529(7) Uani 1 1 d . . . N3 N 0.3682(2) 1.1068(4) 0.3337(2) 0.0844(11) Uani 1 1 d . . . N4 N 0.15980(13) 0.9987(3) 0.43359(17) 0.0448(6) Uani 1 1 d . . . N5 N 0.10892(15) 0.9781(3) 0.4711(2) 0.0573(8) Uani 1 1 d . . . C1 C 0.20429(16) 0.8736(3) 0.5801(2) 0.0426(7) Uani 1 1 d . . . C2 C 0.22013(17) 0.8046(4) 0.6577(2) 0.0515(8) Uani 1 1 d . . . H2 H 0.2674 0.7778 0.6807 0.062 Uiso 1 1 calc R . . C3 C 0.1669(2) 0.7743(4) 0.7021(3) 0.0653(10) Uani 1 1 d . . . H3 H 0.1794 0.7271 0.7538 0.078 Uiso 1 1 calc R . . C4 C 0.0964(2) 0.8129(5) 0.6706(3) 0.0793(13) Uani 1 1 d . . . H4 H 0.0614 0.7912 0.7008 0.095 Uiso 1 1 calc R . . C5 C 0.07818(19) 0.8829(5) 0.5954(3) 0.0724(12) Uani 1 1 d . . . H5 H 0.0308 0.9113 0.5743 0.087 Uiso 1 1 calc R . . C6 C 0.13090(17) 0.9122(4) 0.5497(2) 0.0518(8) Uani 1 1 d . . . C7 C 0.1389(2) 1.0668(4) 0.3523(2) 0.0578(10) Uani 1 1 d . . . C8 C 0.0761(2) 1.0270(6) 0.2977(3) 0.0863(15) Uani 1 1 d . . . H8 H 0.0464 0.9545 0.3112 0.104 Uiso 1 1 calc R . . C9 C 0.0588(4) 1.1032(9) 0.2187(4) 0.116(3) Uani 1 1 d . . . H9 H 0.0176 1.0783 0.1787 0.139 Uiso 1 1 calc R . . C10 C 0.1019(5) 1.2106(10) 0.2023(4) 0.130(3) Uani 1 1 d . . . H10 H 0.0884 1.2609 0.1516 0.156 Uiso 1 1 calc R . . C11 C 0.1638(4) 1.2484(7) 0.2562(4) 0.1084(19) Uani 1 1 d . . . H11 H 0.1927 1.3225 0.2430 0.130 Uiso 1 1 calc R . . C12 C 0.1827(3) 1.1734(5) 0.3320(3) 0.0769(12) Uani 1 1 d . . . H12 H 0.2257 1.1956 0.3694 0.092 Uiso 1 1 calc R . . C13 C 0.34987(15) 0.6118(3) 0.56131(19) 0.0340(6) Uani 1 1 d . . . C14 C 0.3449(2) 0.5430(4) 0.4839(2) 0.0522(8) Uani 1 1 d . . . H14 H 0.3504 0.5964 0.4372 0.063 Uiso 1 1 calc R . . C15 C 0.3318(3) 0.3951(4) 0.4767(3) 0.0706(12) Uani 1 1 d . . . H15 H 0.3295 0.3493 0.4252 0.085 Uiso 1 1 calc R . . C16 C 0.3221(2) 0.3153(4) 0.5441(3) 0.0610(10) Uani 1 1 d . . . H16 H 0.3129 0.2160 0.5383 0.073 Uiso 1 1 calc R . . C17 C 0.3260(2) 0.3813(3) 0.6197(2) 0.0551(9) Uani 1 1 d . . . H17 H 0.3186 0.3273 0.6655 0.066 Uiso 1 1 calc R . . C18 C 0.34084(17) 0.5283(3) 0.6289(2) 0.0432(7) Uani 1 1 d . . . H18 H 0.3448 0.5717 0.6815 0.052 Uiso 1 1 calc R . . C19 C 0.39718(14) 0.8614(3) 0.67273(18) 0.0336(6) Uani 1 1 d . . . C20 C 0.37451(17) 0.9896(3) 0.7036(2) 0.0433(7) Uani 1 1 d . . . H20 H 0.3386 1.0448 0.6697 0.052 Uiso 1 1 calc R . . C21 C 0.4046(2) 1.0361(4) 0.7840(2) 0.0580(10) Uani 1 1 d . . . H21 H 0.3894 1.1229 0.8039 0.070 Uiso 1 1 calc R . . C22 C 0.4570(2) 0.9545(4) 0.8347(2) 0.0589(10) Uani 1 1 d . . . H22 H 0.4769 0.9857 0.8893 0.071 Uiso 1 1 calc R . . C23 C 0.48022(18) 0.8278(4) 0.8058(2) 0.0555(9) Uani 1 1 d . . . H23 H 0.5158 0.7731 0.8406 0.067 Uiso 1 1 calc R . . C24 C 0.45088(16) 0.7809(4) 0.7251(2) 0.0472(8) Uani 1 1 d . . . H24 H 0.4671 0.6949 0.7054 0.057 Uiso 1 1 calc R . . C25 C 0.44175(15) 0.8333(3) 0.51753(19) 0.0356(6) Uani 1 1 d . . . H25A H 0.4795 0.7676 0.5449 0.043 Uiso 1 1 calc R . . H25B H 0.4288 0.8074 0.4583 0.043 Uiso 1 1 calc R . . C26 C 0.47112(15) 0.9892(3) 0.52551(19) 0.0357(6) Uani 1 1 d . . . H26A H 0.4319 1.0568 0.5058 0.043 Uiso 1 1 calc R . . H26B H 0.4914 1.0104 0.5844 0.043 Uiso 1 1 calc R . . C27 C 0.1334(3) 0.5166(7) 0.4956(4) 0.116(2) Uani 1 1 d . . . H27A H 0.1801 0.4876 0.5286 0.139 Uiso 1 1 calc R . . H27B H 0.1123 0.5844 0.5290 0.139 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 0.03194(12) 0.03365(12) 0.04389(14) 0.00465(10) 0.00900(9) 0.00007(9) Cl1 0.1343(14) 0.1191(13) 0.1266(14) 0.0066(10) 0.0055(11) -0.0316(10) Cl2 0.269(3) 0.1131(13) 0.1315(15) -0.0228(12) 0.0739(17) -0.0603(16) P1 0.0287(3) 0.0262(3) 0.0376(4) 0.0004(3) 0.0110(3) -0.0017(3) N1 0.0600(18) 0.0583(18) 0.0485(17) 0.0037(14) 0.0153(14) -0.0020(15) N2 0.0662(19) 0.0570(18) 0.0363(15) 0.0063(14) 0.0125(13) 0.0034(16) N3 0.111(3) 0.082(3) 0.066(2) 0.015(2) 0.030(2) -0.022(2) N4 0.0375(13) 0.0421(15) 0.0521(16) 0.0014(12) 0.0037(12) 0.0056(11) N5 0.0419(15) 0.0583(18) 0.071(2) 0.0064(16) 0.0105(14) 0.0090(14) C1 0.0338(15) 0.0393(16) 0.058(2) 0.0063(14) 0.0176(14) 0.0001(12) C2 0.0392(16) 0.0530(19) 0.067(2) 0.0133(17) 0.0211(16) 0.0020(14) C3 0.057(2) 0.071(3) 0.077(3) 0.024(2) 0.0338(19) 0.0034(19) C4 0.053(2) 0.091(3) 0.107(4) 0.028(3) 0.044(2) 0.007(2) C5 0.0362(18) 0.082(3) 0.106(3) 0.022(3) 0.031(2) 0.0111(18) C6 0.0356(16) 0.0513(19) 0.070(2) 0.0084(18) 0.0149(16) 0.0067(14) C7 0.055(2) 0.064(2) 0.050(2) -0.0038(18) 0.0026(17) 0.0254(18) C8 0.059(2) 0.120(4) 0.069(3) -0.025(3) -0.008(2) 0.028(3) C9 0.092(4) 0.176(7) 0.064(3) -0.023(4) -0.018(3) 0.056(4) C10 0.157(7) 0.162(7) 0.066(4) 0.024(4) 0.015(4) 0.082(6) C11 0.143(5) 0.102(4) 0.082(4) 0.034(3) 0.028(4) 0.031(4) C12 0.092(3) 0.072(3) 0.065(3) 0.021(2) 0.012(2) 0.011(2) C13 0.0314(13) 0.0283(14) 0.0441(16) -0.0007(12) 0.0117(12) -0.0001(10) C14 0.068(2) 0.0412(17) 0.052(2) -0.0060(15) 0.0241(17) -0.0153(16) C15 0.104(3) 0.042(2) 0.074(3) -0.0229(19) 0.037(2) -0.022(2) C16 0.078(3) 0.0291(16) 0.077(3) -0.0047(17) 0.020(2) -0.0115(16) C17 0.073(2) 0.0310(16) 0.060(2) 0.0098(15) 0.0108(18) -0.0065(15) C18 0.0541(18) 0.0325(15) 0.0426(17) 0.0006(13) 0.0096(14) -0.0032(14) C19 0.0334(14) 0.0316(13) 0.0383(15) -0.0030(12) 0.0133(12) -0.0062(11) C20 0.0506(17) 0.0338(15) 0.0493(19) -0.0004(14) 0.0189(14) 0.0008(13) C21 0.082(3) 0.0416(18) 0.059(2) -0.0165(17) 0.032(2) -0.0137(18) C22 0.070(2) 0.066(2) 0.0418(19) -0.0104(18) 0.0146(18) -0.029(2) C23 0.0481(19) 0.063(2) 0.051(2) 0.0041(18) 0.0007(16) -0.0082(17) C24 0.0389(16) 0.0464(18) 0.055(2) -0.0046(16) 0.0075(14) 0.0023(14) C25 0.0367(14) 0.0305(14) 0.0441(17) -0.0013(12) 0.0186(13) -0.0014(11) C26 0.0361(14) 0.0312(14) 0.0427(16) -0.0040(12) 0.0151(12) -0.0063(11) C27 0.132(5) 0.095(4) 0.103(4) -0.018(4) -0.011(4) -0.004(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C1 2.006(3) . ? Pd1 N4 2.102(2) . ? Pd1 N1 2.109(3) . ? Pd1 P1 2.2571(7) . ? Cl1 C27 1.720(7) . ? Cl2 C27 1.719(6) . ? P1 C19 1.815(3) . ? P1 C13 1.816(3) . ? P1 C25 1.832(3) . ? N1 N2 1.180(4) . ? N2 N3 1.159(4) . ? N4 N5 1.266(4) . ? N4 C7 1.436(4) . ? N5 C6 1.393(5) . ? C1 C2 1.384(5) . ? C1 C6 1.421(4) . ? C2 C3 1.393(5) . ? C2 H2 0.9300 . ? C3 C4 1.375(5) . ? C3 H3 0.9300 . ? C4 C5 1.358(6) . ? C4 H4 0.9300 . ? C5 C6 1.398(5) . ? C5 H5 0.9300 . ? C7 C12 1.373(6) . ? C7 C8 1.374(6) . ? C8 C9 1.436(8) . ? C8 H8 0.9300 . ? C9 C10 1.346(10) . ? C9 H9 0.9300 . ? C10 C11 1.352(9) . ? C10 H10 0.9300 . ? C11 C12 1.388(6) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C18 1.381(4) . ? C13 C14 1.392(5) . ? C14 C15 1.382(5) . ? C14 H14 0.9300 . ? C15 C16 1.363(5) . ? C15 H15 0.9300 . ? C16 C17 1.357(5) . ? C16 H16 0.9300 . ? C17 C18 1.381(4) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C20 1.386(4) . ? C19 C24 1.392(4) . ? C20 C21 1.374(5) . ? C20 H20 0.9300 . ? C21 C22 1.371(6) . ? C21 H21 0.9300 . ? C22 C23 1.364(5) . ? C22 H22 0.9300 . ? C23 C24 1.378(5) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 C26 1.532(4) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C26 1.527(5) 3_676 ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pd1 N4 78.96(12) . . ? C1 Pd1 N1 166.94(12) . . ? N4 Pd1 N1 94.31(11) . . ? C1 Pd1 P1 95.01(9) . . ? N4 Pd1 P1 173.79(8) . . ? N1 Pd1 P1 91.32(9) . . ? C19 P1 C13 108.05(14) . . ? C19 P1 C25 102.34(13) . . ? C13 P1 C25 103.81(13) . . ? C19 P1 Pd1 118.49(10) . . ? C13 P1 Pd1 108.11(9) . . ? C25 P1 Pd1 114.92(10) . . ? N2 N1 Pd1 127.9(3) . . ? N3 N2 N1 175.9(4) . . ? N5 N4 C7 114.8(3) . . ? N5 N4 Pd1 116.6(2) . . ? C7 N4 Pd1 128.3(2) . . ? N4 N5 C6 113.5(3) . . ? C2 C1 C6 115.7(3) . . ? C2 C1 Pd1 133.6(2) . . ? C6 C1 Pd1 110.2(2) . . ? C1 C2 C3 121.6(3) . . ? C1 C2 H2 119.2 . . ? C3 C2 H2 119.2 . . ? C4 C3 C2 121.2(4) . . ? C4 C3 H3 119.4 . . ? C2 C3 H3 119.4 . . ? C5 C4 C3 119.6(4) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? C4 C5 C6 119.8(3) . . ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? N5 C6 C5 117.6(3) . . ? N5 C6 C1 120.2(3) . . ? C5 C6 C1 122.1(3) . . ? C12 C7 C8 121.5(4) . . ? C12 C7 N4 118.1(3) . . ? C8 C7 N4 120.4(4) . . ? C7 C8 C9 116.5(6) . . ? C7 C8 H8 121.7 . . ? C9 C8 H8 121.7 . . ? C10 C9 C8 120.2(6) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C9 C10 C11 122.9(6) . . ? C9 C10 H10 118.6 . . ? C11 C10 H10 118.6 . . ? C10 C11 C12 118.0(6) . . ? C10 C11 H11 121.0 . . ? C12 C11 H11 121.0 . . ? C7 C12 C11 120.9(5) . . ? C7 C12 H12 119.5 . . ? C11 C12 H12 119.5 . . ? C18 C13 C14 118.0(3) . . ? C18 C13 P1 124.9(2) . . ? C14 C13 P1 116.9(2) . . ? C15 C14 C13 119.9(3) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C16 C15 C14 120.9(4) . . ? C16 C15 H15 119.5 . . ? C14 C15 H15 119.5 . . ? C17 C16 C15 119.8(3) . . ? C17 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? C16 C17 C18 120.3(3) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C13 C18 C17 121.0(3) . . ? C13 C18 H18 119.5 . . ? C17 C18 H18 119.5 . . ? C20 C19 C24 118.4(3) . . ? C20 C19 P1 120.7(2) . . ? C24 C19 P1 120.7(2) . . ? C21 C20 C19 120.7(3) . . ? C21 C20 H20 119.7 . . ? C19 C20 H20 119.7 . . ? C22 C21 C20 120.0(3) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C23 C22 C21 120.5(3) . . ? C23 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? C22 C23 C24 120.0(3) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C23 C24 C19 120.5(3) . . ? C23 C24 H24 119.8 . . ? C19 C24 H24 119.8 . . ? C26 C25 P1 113.64(19) . . ? C26 C25 H25A 108.8 . . ? P1 C25 H25A 108.8 . . ? C26 C25 H25B 108.8 . . ? P1 C25 H25B 108.8 . . ? H25A C25 H25B 107.7 . . ? C26 C26 C25 111.6(3) 3_676 . ? C26 C26 H26A 109.3 3_676 . ? C25 C26 H26A 109.3 . . ? C26 C26 H26B 109.3 3_676 . ? C25 C26 H26B 109.3 . . ? H26A C26 H26B 108.0 . . ? Cl2 C27 Cl1 111.7(3) . . ? Cl2 C27 H27A 109.3 . . ? Cl1 C27 H27A 109.3 . . ? Cl2 C27 H27B 109.3 . . ? Cl1 C27 H27B 109.3 . . ? H27A C27 H27B 107.9 . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.827 _refine_diff_density_min -0.872 _refine_diff_density_rms 0.077 #=========================================================END data_jht073 _database_code_depnum_ccdc_archive 'CCDC 713106' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H44 Cl4 N8 P2 Pd2' _chemical_formula_weight 981.31 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.5919(14) _cell_length_b 16.830(2) _cell_length_c 10.5581(13) _cell_angle_alpha 90.00 _cell_angle_beta 101.612(5) _cell_angle_gamma 90.00 _cell_volume 2017.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9066 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 28.37 _exptl_crystal_description BLOCK _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.615 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 988 _exptl_absorpt_coefficient_mu 1.272 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7016 _exptl_absorpt_correction_T_max 0.7851 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30424 _diffrn_reflns_av_R_equivalents 0.0261 _diffrn_reflns_av_sigmaI/netI 0.0241 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 28.40 _reflns_number_total 4960 _reflns_number_gt 4031 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0654P)^2^+2.2164P] 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 4960 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0548 _refine_ls_R_factor_gt 0.0408 _refine_ls_wR_factor_ref 0.1197 _refine_ls_wR_factor_gt 0.1093 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _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 0.70399(2) 0.033890(14) 0.42171(2) 0.03415(10) Uani 1 1 d . . . P1 P 0.85215(8) -0.00663(5) 0.32896(8) 0.03458(19) Uani 1 1 d . . . N1 N 0.7188(3) -0.0550(2) 0.5496(3) 0.0510(8) Uani 1 1 d . . . N2 N 0.6581(3) 0.12989(19) 0.2914(3) 0.0500(8) Uani 1 1 d . . . N3 N 0.6220(3) 0.1229(2) 0.1811(4) 0.0513(8) Uani 1 1 d . . . N4 N 0.5840(5) 0.1200(3) 0.0709(4) 0.0877(15) Uani 1 1 d . . . C1 C 0.6025(3) 0.08067(19) 0.5467(3) 0.0312(6) Uani 1 1 d . . . C2 C 0.5555(3) 0.1537(2) 0.5375(4) 0.0499(9) Uani 1 1 d . . . H2 H 0.5544 0.1834 0.4629 0.060 Uiso 1 1 calc R . . C3 C 0.5085(4) 0.1858(3) 0.6373(5) 0.0583(11) Uani 1 1 d . . . H3 H 0.4778 0.2371 0.6300 0.070 Uiso 1 1 calc R . . C4 C 0.5073(4) 0.1426(3) 0.7446(5) 0.0648(12) Uani 1 1 d . . . H4 H 0.4759 0.1638 0.8117 0.078 Uiso 1 1 calc R . . C5 C 0.5535(4) 0.0661(3) 0.7539(4) 0.0613(11) Uani 1 1 d . . . H5 H 0.5513 0.0351 0.8263 0.074 Uiso 1 1 calc R . . C6 C 0.6029(3) 0.0363(2) 0.6541(4) 0.0460(9) Uani 1 1 d . . . C7 C 0.6607(3) -0.0404(2) 0.6526(4) 0.0442(8) Uani 1 1 d . . . C8 C 0.6567(4) -0.0983(3) 0.7468(4) 0.0583(11) Uani 1 1 d . . . H8 H 0.6179 -0.0876 0.8139 0.070 Uiso 1 1 calc R . . C9 C 0.7095(4) -0.1704(3) 0.7410(5) 0.0656(12) Uani 1 1 d . . . H9 H 0.7084 -0.2081 0.8052 0.079 Uiso 1 1 calc R . . C10 C 0.7643(4) -0.1874(3) 0.6394(5) 0.0630(11) Uani 1 1 d . . . H10 H 0.7988 -0.2369 0.6344 0.076 Uiso 1 1 calc R . . C11 C 0.7679(4) -0.1307(2) 0.5450(4) 0.0493(9) Uani 1 1 d . . . H11 H 0.8041 -0.1434 0.4766 0.059 Uiso 1 1 calc R . . C12 C 0.9850(3) -0.03173(19) 0.4472(4) 0.0388(7) Uani 1 1 d . . . H12A H 0.9738 -0.0824 0.4867 0.047 Uiso 1 1 calc R . . H12B H 1.0505 -0.0372 0.4033 0.047 Uiso 1 1 calc R . . C13 C 0.9019(3) 0.0713(2) 0.2330(4) 0.0462(8) Uani 1 1 d . . . H13A H 0.8365 0.0860 0.1643 0.055 Uiso 1 1 calc R . . H13B H 0.9218 0.1176 0.2878 0.055 Uiso 1 1 calc R . . C14 C 1.0063(4) 0.0518(3) 0.1726(4) 0.0633(12) Uani 1 1 d . . . H14A H 1.0251 0.0969 0.1250 0.095 Uiso 1 1 calc R . . H14B H 0.9872 0.0074 0.1151 0.095 Uiso 1 1 calc R . . H14C H 1.0729 0.0386 0.2393 0.095 Uiso 1 1 calc R . . C15 C 0.8283(4) -0.0923(2) 0.2209(4) 0.0502(9) Uani 1 1 d . . . H15A H 0.9030 -0.1081 0.2004 0.060 Uiso 1 1 calc R . . H15B H 0.7995 -0.1363 0.2650 0.060 Uiso 1 1 calc R . . C16 C 0.7412(5) -0.0754(3) 0.0962(4) 0.0670(12) Uani 1 1 d . . . H16A H 0.7316 -0.1222 0.0430 0.101 Uiso 1 1 calc R . . H16B H 0.7703 -0.0327 0.0509 0.101 Uiso 1 1 calc R . . H16C H 0.6667 -0.0606 0.1156 0.101 Uiso 1 1 calc R . . Cl1 Cl 0.8466(3) 0.1433(3) 0.8344(5) 0.266(3) Uani 1 1 d . . . Cl2 Cl 0.9226(5) 0.25647(18) 1.0210(4) 0.327(4) Uani 1 1 d . . . C17 C 0.8071(8) 0.2137(4) 0.9211(9) 0.128(3) Uani 1 1 d . . . H17A H 0.7537 0.1921 0.9722 0.153 Uiso 1 1 calc R . . H17B H 0.7649 0.2539 0.8642 0.153 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 0.03564(15) 0.03479(15) 0.03169(16) 0.00095(9) 0.00601(10) 0.00065(9) P1 0.0376(4) 0.0356(4) 0.0295(4) -0.0020(3) 0.0042(3) 0.0023(3) N1 0.0488(18) 0.0560(19) 0.0481(19) 0.0053(15) 0.0095(15) -0.0047(15) N2 0.060(2) 0.0425(16) 0.048(2) 0.0070(14) 0.0113(16) 0.0094(14) N3 0.0565(19) 0.0491(18) 0.052(2) 0.0085(15) 0.0187(16) 0.0112(15) N4 0.117(4) 0.098(4) 0.042(2) 0.006(2) 0.003(2) 0.030(3) C1 0.0279(14) 0.0366(15) 0.0287(15) -0.0037(12) 0.0045(12) -0.0007(11) C2 0.0440(19) 0.051(2) 0.056(2) -0.0082(18) 0.0147(17) -0.0012(16) C3 0.049(2) 0.056(2) 0.072(3) -0.018(2) 0.017(2) 0.0013(18) C4 0.057(2) 0.088(3) 0.054(3) -0.024(2) 0.020(2) -0.001(2) C5 0.059(3) 0.088(3) 0.041(2) -0.004(2) 0.0187(19) -0.003(2) C6 0.0366(18) 0.060(2) 0.041(2) -0.0052(16) 0.0073(15) -0.0076(15) C7 0.0392(18) 0.056(2) 0.0358(19) 0.0041(15) 0.0025(15) -0.0081(15) C8 0.052(2) 0.081(3) 0.043(2) 0.013(2) 0.0112(18) -0.011(2) C9 0.068(3) 0.067(3) 0.061(3) 0.027(2) 0.010(2) -0.007(2) C10 0.069(3) 0.047(2) 0.070(3) 0.017(2) 0.009(2) -0.006(2) C11 0.056(2) 0.0399(18) 0.051(2) 0.0049(16) 0.0102(17) -0.0045(16) C12 0.0393(18) 0.0380(17) 0.0368(19) -0.0045(14) 0.0021(14) 0.0056(13) C13 0.050(2) 0.051(2) 0.041(2) 0.0085(16) 0.0138(16) 0.0018(16) C14 0.055(2) 0.087(3) 0.052(3) 0.006(2) 0.020(2) 0.001(2) C15 0.058(2) 0.049(2) 0.041(2) -0.0124(16) 0.0025(17) 0.0050(17) C16 0.077(3) 0.074(3) 0.042(2) -0.013(2) -0.005(2) -0.006(2) Cl1 0.118(2) 0.332(6) 0.326(5) -0.185(5) -0.006(2) 0.061(3) Cl2 0.515(8) 0.1007(18) 0.260(4) 0.049(2) -0.171(5) -0.115(3) C17 0.145(7) 0.077(4) 0.167(8) 0.033(5) 0.042(6) 0.020(5) _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 2.000(3) . ? Pd1 C1 2.091(3) . ? Pd1 N2 2.119(3) . ? Pd1 P1 2.2473(9) . ? P1 C13 1.821(4) . ? P1 C15 1.825(4) . ? P1 C12 1.826(4) . ? N1 C11 1.401(5) . ? N1 C7 1.411(5) . ? N2 N3 1.161(5) . ? N3 N4 1.159(5) . ? C1 C2 1.340(5) . ? C1 C6 1.356(5) . ? C2 C3 1.390(5) . ? C2 H2 0.9300 . ? C3 C4 1.349(7) . ? C3 H3 0.9300 . ? C4 C5 1.391(7) . ? C4 H4 0.9300 . ? C5 C6 1.390(6) . ? C5 H5 0.9300 . ? C6 C7 1.457(6) . ? C7 C8 1.400(6) . ? C8 C9 1.366(7) . ? C8 H8 0.9300 . ? C9 C10 1.381(7) . ? C9 H9 0.9300 . ? C10 C11 1.386(6) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 C12 1.533(7) 3_756 ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.514(5) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C16 1.516(6) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? Cl1 C17 1.619(8) . ? Cl2 C17 1.689(10) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? 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 C1 80.69(13) . . ? N1 Pd1 N2 170.09(13) . . ? C1 Pd1 N2 91.33(13) . . ? N1 Pd1 P1 95.62(10) . . ? C1 Pd1 P1 164.97(9) . . ? N2 Pd1 P1 93.57(9) . . ? C13 P1 C15 104.25(19) . . ? C13 P1 C12 103.23(18) . . ? C15 P1 C12 104.20(17) . . ? C13 P1 Pd1 112.28(13) . . ? C15 P1 Pd1 118.66(14) . . ? C12 P1 Pd1 112.70(12) . . ? C11 N1 C7 116.5(3) . . ? C11 N1 Pd1 129.6(3) . . ? C7 N1 Pd1 113.6(3) . . ? N3 N2 Pd1 124.5(3) . . ? N4 N3 N2 176.5(4) . . ? C2 C1 C6 119.9(3) . . ? C2 C1 Pd1 124.8(3) . . ? C6 C1 Pd1 114.4(2) . . ? C1 C2 C3 121.2(4) . . ? C1 C2 H2 119.4 . . ? C3 C2 H2 119.4 . . ? C4 C3 C2 119.9(4) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C3 C4 C5 119.3(4) . . ? C3 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? C6 C5 C4 119.5(4) . . ? C6 C5 H5 120.3 . . ? C4 C5 H5 120.3 . . ? C1 C6 C5 120.2(4) . . ? C1 C6 C7 113.8(3) . . ? C5 C6 C7 126.0(4) . . ? C8 C7 N1 121.0(4) . . ? C8 C7 C6 121.9(4) . . ? N1 C7 C6 117.0(3) . . ? C9 C8 C7 120.5(4) . . ? C9 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? C8 C9 C10 119.9(4) . . ? C8 C9 H9 120.1 . . ? C10 C9 H9 120.1 . . ? C9 C10 C11 120.1(4) . . ? C9 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? C10 C11 N1 122.0(4) . . ? C10 C11 H11 119.0 . . ? N1 C11 H11 119.0 . . ? C12 C12 P1 111.9(3) 3_756 . ? C12 C12 H12A 109.2 3_756 . ? P1 C12 H12A 109.2 . . ? C12 C12 H12B 109.2 3_756 . ? P1 C12 H12B 109.2 . . ? H12A C12 H12B 107.9 . . ? C14 C13 P1 116.6(3) . . ? C14 C13 H13A 108.1 . . ? P1 C13 H13A 108.1 . . ? C14 C13 H13B 108.1 . . ? P1 C13 H13B 108.1 . . ? H13A C13 H13B 107.3 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 P1 112.7(3) . . ? C16 C15 H15A 109.1 . . ? P1 C15 H15A 109.1 . . ? C16 C15 H15B 109.1 . . ? P1 C15 H15B 109.1 . . ? H15A C15 H15B 107.8 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Cl1 C17 Cl2 112.8(6) . . ? Cl1 C17 H17A 109.0 . . ? Cl2 C17 H17A 109.0 . . ? Cl1 C17 H17B 109.0 . . ? Cl2 C17 H17B 109.0 . . ? H17A C17 H17B 107.8 . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 28.40 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 1.409 _refine_diff_density_min -1.107 _refine_diff_density_rms 0.099 #=========================================================END data_lke236 _database_code_depnum_ccdc_archive 'CCDC 713107' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H38 N5 P Pd' _chemical_formula_weight 545.97 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' 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 'P2(1)/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 12.0749(17) _cell_length_b 10.950(3) _cell_length_c 20.463(5) _cell_angle_alpha 90.00 _cell_angle_beta 100.344(12) _cell_angle_gamma 90.00 _cell_volume 2661.7(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 21 _cell_measurement_theta_min 7.33 _cell_measurement_theta_max 12.56 _exptl_crystal_description 'BLOCK ' _exptl_crystal_colour 'YELLOW ' _exptl_crystal_size_max 0.74 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.38 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.362 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1136 _exptl_absorpt_coefficient_mu 0.778 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7523 _exptl_absorpt_correction_T_max 0.9313 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 4920 _diffrn_reflns_av_R_equivalents 0.0376 _diffrn_reflns_av_sigmaI/netI 0.0551 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 25.03 _reflns_number_total 4683 _reflns_number_gt 3501 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _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^)+(0.0298P)^2^+2.0588P] 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 4683 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0631 _refine_ls_R_factor_gt 0.0396 _refine_ls_wR_factor_ref 0.0957 _refine_ls_wR_factor_gt 0.0853 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _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 0.02416(2) 0.77221(3) 0.191646(16) 0.04512(12) Uani 1 1 d . . . P1 P -0.09642(9) 0.64561(9) 0.12709(5) 0.0472(3) Uani 1 1 d . . . N1 N 0.1536(3) 0.8743(3) 0.2609(2) 0.0596(10) Uani 1 1 d . . . N2 N -0.1818(2) 0.9185(3) 0.20751(14) 0.0361(7) Uani 1 1 d . . . N3 N 0.1645(3) 0.6988(4) 0.1533(3) 0.0836(14) Uani 1 1 d . . . N4 N 0.1733(4) 0.6755(4) 0.0982(3) 0.0804(13) Uani 1 1 d . . . N5 N 0.1860(5) 0.6477(7) 0.0457(3) 0.129(2) Uani 1 1 d . . . C1 C 0.2204(4) 0.7802(5) 0.3027(3) 0.0876(18) Uani 1 1 d . . . H1A H 0.1719 0.7342 0.3259 0.131 Uiso 1 1 calc R . . H1B H 0.2781 0.8191 0.3342 0.131 Uiso 1 1 calc R . . H1C H 0.2545 0.7264 0.2750 0.131 Uiso 1 1 calc R . . C2 C 0.2292(4) 0.9445(5) 0.2255(3) 0.0859(18) Uani 1 1 d . . . H2A H 0.1865 1.0057 0.1983 0.129 Uiso 1 1 calc R . . H2B H 0.2633 0.8902 0.1980 0.129 Uiso 1 1 calc R . . H2C H 0.2868 0.9831 0.2572 0.129 Uiso 1 1 calc R . . C3 C 0.1064(3) 0.9629(4) 0.3048(2) 0.0576(12) Uani 1 1 d . . . H3A H 0.1675 0.9978 0.3365 0.069 Uiso 1 1 calc R . . H3B H 0.0688 1.0288 0.2779 0.069 Uiso 1 1 calc R . . C4 C 0.0244(4) 0.9022(4) 0.3415(2) 0.0557(11) Uani 1 1 d . . . C5 C 0.0413(5) 0.9025(5) 0.4107(3) 0.0809(16) Uani 1 1 d . . . H5 H 0.1048 0.9403 0.4347 0.097 Uiso 1 1 calc R . . C6 C -0.0343(6) 0.8482(6) 0.4436(3) 0.0932(19) Uani 1 1 d . . . H6 H -0.0222 0.8503 0.4898 0.112 Uiso 1 1 calc R . . C7 C -0.1277(6) 0.7907(5) 0.4096(3) 0.0834(17) Uani 1 1 d . . . H7 H -0.1779 0.7521 0.4325 0.100 Uiso 1 1 calc R . . C8 C -0.1470(4) 0.7904(4) 0.3398(2) 0.0591(12) Uani 1 1 d . . . H8 H -0.2104 0.7517 0.3163 0.071 Uiso 1 1 calc R . . C9 C -0.0725(3) 0.8473(3) 0.30615(19) 0.0428(9) Uani 1 1 d . . . C10 C -0.0963(3) 0.8542(3) 0.23168(18) 0.0369(8) Uani 1 1 d . . . C11 C -0.2214(3) 0.9403(3) 0.13905(18) 0.0360(8) Uani 1 1 d . . . C12 C -0.3348(3) 0.9073(4) 0.11380(18) 0.0413(9) Uani 1 1 d . . . C13 C -0.3748(3) 0.9244(4) 0.0465(2) 0.0525(10) Uani 1 1 d . . . H13 H -0.4461 0.8959 0.0279 0.063 Uiso 1 1 calc R . . C14 C -0.3108(4) 0.9826(4) 0.0071(2) 0.0568(11) Uani 1 1 d . . . H14 H -0.3389 0.9922 -0.0380 0.068 Uiso 1 1 calc R . . C15 C -0.2059(3) 1.0270(4) 0.0332(2) 0.0522(11) Uani 1 1 d . . . H15 H -0.1658 1.0709 0.0062 0.063 Uiso 1 1 calc R . . C16 C -0.1586(3) 1.0070(3) 0.09985(19) 0.0402(9) Uani 1 1 d . . . C17 C -0.4124(3) 0.8641(4) 0.1602(2) 0.0508(10) Uani 1 1 d . . . H17 H -0.3660 0.8263 0.1991 0.061 Uiso 1 1 calc R . . C18 C -0.4689(4) 0.9782(5) 0.1836(2) 0.0712(14) Uani 1 1 d . . . H18A H -0.4121 1.0357 0.2025 0.107 Uiso 1 1 calc R . . H18B H -0.5126 0.9551 0.2164 0.107 Uiso 1 1 calc R . . H18C H -0.5171 1.0150 0.1464 0.107 Uiso 1 1 calc R . . C19 C -0.5026(4) 0.7723(5) 0.1301(2) 0.0673(13) Uani 1 1 d . . . H19A H -0.5473 0.7505 0.1626 0.101 Uiso 1 1 calc R . . H19B H -0.4671 0.7005 0.1165 0.101 Uiso 1 1 calc R . . H19C H -0.5499 0.8082 0.0922 0.101 Uiso 1 1 calc R . . C20 C -0.0457(3) 1.0635(4) 0.1304(2) 0.0479(10) Uani 1 1 d . . . H20 H -0.0023 1.0013 0.1584 0.058 Uiso 1 1 calc R . . C21 C -0.0631(4) 1.1717(4) 0.1753(3) 0.0785(15) Uani 1 1 d . . . H21A H -0.1073 1.1457 0.2074 0.118 Uiso 1 1 calc R . . H21B H -0.1016 1.2363 0.1488 0.118 Uiso 1 1 calc R . . H21C H 0.0087 1.2006 0.1979 0.118 Uiso 1 1 calc R . . C22 C 0.0240(5) 1.1049(8) 0.0805(3) 0.136(3) Uani 1 1 d . . . H22A H 0.0935 1.1392 0.1033 0.204 Uiso 1 1 calc R . . H22B H -0.0167 1.1656 0.0519 0.204 Uiso 1 1 calc R . . H22C H 0.0398 1.0364 0.0544 0.204 Uiso 1 1 calc R . . C23 C -0.1329(5) 0.6895(4) 0.0407(2) 0.0705(14) Uani 1 1 d . . . H23A H -0.0658 0.7111 0.0244 0.106 Uiso 1 1 calc R . . H23B H -0.1830 0.7582 0.0366 0.106 Uiso 1 1 calc R . . H23C H -0.1693 0.6223 0.0153 0.106 Uiso 1 1 calc R . . C24 C -0.0336(4) 0.4950(4) 0.1211(3) 0.0718(14) Uani 1 1 d . . . H24A H 0.0387 0.5040 0.1084 0.108 Uiso 1 1 calc R . . H24B H -0.0818 0.4471 0.0884 0.108 Uiso 1 1 calc R . . H24C H -0.0249 0.4548 0.1634 0.108 Uiso 1 1 calc R . . C25 C -0.2292(4) 0.6080(4) 0.1512(2) 0.0661(13) Uani 1 1 d . . . H25A H -0.2162 0.5835 0.1970 0.099 Uiso 1 1 calc R . . H25B H -0.2642 0.5423 0.1241 0.099 Uiso 1 1 calc R . . H25C H -0.2775 0.6782 0.1454 0.099 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 0.03310(16) 0.03408(16) 0.0667(2) -0.00442(16) 0.00504(13) 0.00196(14) P1 0.0517(6) 0.0335(5) 0.0538(7) 0.0000(5) 0.0024(5) -0.0026(5) N1 0.0333(17) 0.039(2) 0.100(3) -0.0083(19) -0.0055(18) 0.0024(15) N2 0.0257(14) 0.0375(17) 0.0449(18) 0.0033(14) 0.0055(13) -0.0038(13) N3 0.053(2) 0.083(3) 0.114(4) -0.032(3) 0.014(3) 0.019(2) N4 0.058(3) 0.075(3) 0.111(4) -0.002(3) 0.023(3) 0.008(2) N5 0.109(4) 0.184(7) 0.103(4) 0.000(5) 0.041(4) 0.020(4) C1 0.056(3) 0.063(3) 0.127(5) -0.012(3) -0.030(3) 0.015(3) C2 0.037(2) 0.075(4) 0.145(5) -0.017(4) 0.015(3) -0.013(2) C3 0.042(2) 0.044(2) 0.079(3) -0.012(2) -0.008(2) -0.0044(19) C4 0.059(3) 0.040(2) 0.059(3) 0.000(2) -0.014(2) 0.007(2) C5 0.094(4) 0.069(3) 0.064(3) 0.000(3) -0.028(3) 0.004(3) C6 0.136(6) 0.088(4) 0.045(3) 0.004(3) -0.011(3) -0.001(4) C7 0.124(5) 0.069(4) 0.059(3) 0.016(3) 0.020(3) -0.008(3) C8 0.071(3) 0.055(3) 0.049(3) 0.005(2) 0.004(2) -0.005(2) C9 0.045(2) 0.035(2) 0.045(2) 0.0041(17) -0.0023(18) 0.0029(17) C10 0.0317(18) 0.0308(19) 0.047(2) 0.0007(16) 0.0046(16) -0.0052(15) C11 0.0320(18) 0.034(2) 0.042(2) -0.0008(16) 0.0079(16) 0.0020(15) C12 0.0354(19) 0.045(2) 0.043(2) 0.0034(18) 0.0061(17) 0.0011(16) C13 0.039(2) 0.063(3) 0.052(3) 0.002(2) -0.0002(19) 0.001(2) C14 0.054(3) 0.069(3) 0.045(2) 0.012(2) 0.001(2) 0.008(2) C15 0.054(2) 0.056(3) 0.053(3) 0.010(2) 0.025(2) 0.007(2) C16 0.0354(19) 0.037(2) 0.049(2) 0.0033(17) 0.0119(17) 0.0060(16) C17 0.033(2) 0.067(3) 0.051(2) 0.009(2) 0.0028(17) -0.0107(19) C18 0.047(2) 0.100(4) 0.072(3) -0.024(3) 0.022(2) -0.016(3) C19 0.051(2) 0.078(3) 0.071(3) 0.002(3) 0.007(2) -0.021(2) C20 0.043(2) 0.050(2) 0.055(2) 0.006(2) 0.0188(19) -0.0064(18) C21 0.073(3) 0.050(3) 0.109(4) -0.011(3) 0.009(3) -0.001(3) C22 0.088(4) 0.248(10) 0.080(4) -0.009(5) 0.035(3) -0.091(5) C23 0.097(4) 0.053(3) 0.058(3) 0.005(2) 0.006(3) -0.004(3) C24 0.087(3) 0.034(2) 0.088(4) -0.003(2) -0.001(3) 0.005(2) C25 0.057(3) 0.054(3) 0.083(3) 0.007(2) 0.002(2) -0.013(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C10 2.005(4) . ? Pd1 N3 2.147(4) . ? Pd1 N1 2.215(3) . ? Pd1 P1 2.2574(11) . ? P1 C25 1.807(4) . ? P1 C23 1.808(5) . ? P1 C24 1.829(4) . ? N1 C2 1.478(6) . ? N1 C1 1.482(6) . ? N1 C3 1.502(5) . ? N2 C10 1.274(4) . ? N2 C11 1.417(4) . ? N3 N4 1.179(6) . ? N4 N5 1.154(7) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 C4 1.501(6) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.393(6) . ? C4 C9 1.397(5) . ? C5 C6 1.365(8) . ? C5 H5 0.9300 . ? C6 C7 1.367(8) . ? C6 H6 0.9300 . ? C7 C8 1.406(6) . ? C7 H7 0.9300 . ? C8 C9 1.376(6) . ? C8 H8 0.9300 . ? C9 C10 1.501(5) . ? C11 C16 1.404(5) . ? C11 C12 1.421(5) . ? C12 C13 1.388(5) . ? C12 C17 1.524(5) . ? C13 C14 1.371(6) . ? C13 H13 0.9300 . ? C14 C15 1.372(6) . ? C14 H14 0.9300 . ? C15 C16 1.398(5) . ? C15 H15 0.9300 . ? C16 C20 1.525(5) . ? C17 C19 1.528(5) . ? C17 C18 1.540(6) . ? C17 H17 0.9800 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 C22 1.505(6) . ? C20 C21 1.537(6) . ? C20 H20 0.9800 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? 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 Pd1 N3 174.15(15) . . ? C10 Pd1 N1 89.57(13) . . ? N3 Pd1 N1 84.85(16) . . ? C10 Pd1 P1 94.32(10) . . ? N3 Pd1 P1 91.42(13) . . ? N1 Pd1 P1 172.44(9) . . ? C25 P1 C23 104.8(2) . . ? C25 P1 C24 102.2(2) . . ? C23 P1 C24 101.8(2) . . ? C25 P1 Pd1 119.36(17) . . ? C23 P1 Pd1 115.30(17) . . ? C24 P1 Pd1 111.20(17) . . ? C2 N1 C1 108.9(4) . . ? C2 N1 C3 107.0(3) . . ? C1 N1 C3 109.2(4) . . ? C2 N1 Pd1 112.1(3) . . ? C1 N1 Pd1 105.4(3) . . ? C3 N1 Pd1 114.1(2) . . ? C10 N2 C11 125.7(3) . . ? N4 N3 Pd1 130.0(4) . . ? N5 N4 N3 176.3(6) . . ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 N1 111.6(3) . . ? C4 C3 H3A 109.3 . . ? N1 C3 H3A 109.3 . . ? C4 C3 H3B 109.3 . . ? N1 C3 H3B 109.3 . . ? H3A C3 H3B 108.0 . . ? C5 C4 C9 118.9(5) . . ? C5 C4 C3 121.2(4) . . ? C9 C4 C3 119.9(4) . . ? C6 C5 C4 120.8(5) . . ? C6 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? C5 C6 C7 120.9(5) . . ? C5 C6 H6 119.5 . . ? C7 C6 H6 119.5 . . ? C6 C7 C8 119.2(5) . . ? C6 C7 H7 120.4 . . ? C8 C7 H7 120.4 . . ? C9 C8 C7 120.2(5) . . ? C9 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? C8 C9 C4 119.8(4) . . ? C8 C9 C10 120.5(3) . . ? C4 C9 C10 119.6(4) . . ? N2 C10 C9 114.6(3) . . ? N2 C10 Pd1 133.3(3) . . ? C9 C10 Pd1 111.8(2) . . ? C16 C11 N2 122.1(3) . . ? C16 C11 C12 120.6(3) . . ? N2 C11 C12 116.6(3) . . ? C13 C12 C11 117.9(3) . . ? C13 C12 C17 121.0(3) . . ? C11 C12 C17 120.9(3) . . ? C14 C13 C12 120.9(4) . . ? C14 C13 H13 119.5 . . ? C12 C13 H13 119.5 . . ? C13 C14 C15 121.0(4) . . ? C13 C14 H14 119.5 . . ? C15 C14 H14 119.5 . . ? C14 C15 C16 120.8(4) . . ? C14 C15 H15 119.6 . . ? C16 C15 H15 119.6 . . ? C15 C16 C11 118.1(3) . . ? C15 C16 C20 121.0(3) . . ? C11 C16 C20 120.8(3) . . ? C12 C17 C19 115.3(4) . . ? C12 C17 C18 107.3(3) . . ? C19 C17 C18 109.7(3) . . ? C12 C17 H17 108.1 . . ? C19 C17 H17 108.1 . . ? C18 C17 H17 108.1 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C22 C20 C16 114.3(4) . . ? C22 C20 C21 109.1(5) . . ? C16 C20 C21 110.4(3) . . ? C22 C20 H20 107.6 . . ? C16 C20 H20 107.6 . . ? C21 C20 H20 107.6 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? P1 C23 H23A 109.5 . . ? P1 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? P1 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? P1 C24 H24A 109.5 . . ? P1 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? P1 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? P1 C25 H25A 109.5 . . ? P1 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? P1 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.469 _refine_diff_density_min -0.493 _refine_diff_density_rms 0.068 #=========================================================END data_kmy166 _database_code_depnum_ccdc_archive 'CCDC 713108' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H51 N3 P2 Pd S' _chemical_formula_weight 666.15 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' P P 0.1023 0.0942 '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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 9.354(2) _cell_length_b 9.495(2) _cell_length_c 11.390(2) _cell_angle_alpha 69.850(17) _cell_angle_beta 68.533(16) _cell_angle_gamma 76.593(19) _cell_volume 877.3(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 6.64 _cell_measurement_theta_max 12.52 _exptl_crystal_description 'BLOCK ' _exptl_crystal_colour 'RED ' _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.261 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 350 _exptl_absorpt_coefficient_mu 0.702 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6555 _exptl_absorpt_correction_T_max 0.8998 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 3629 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0324 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 25.01 _reflns_number_total 3629 _reflns_number_gt 3536 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _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^)+(0.0469P)^2^+0.0104P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00 _refine_ls_number_reflns 3629 _refine_ls_number_parameters 343 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0288 _refine_ls_R_factor_gt 0.0277 _refine_ls_wR_factor_ref 0.0703 _refine_ls_wR_factor_gt 0.0693 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.041 _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 0.06631(3) 0.12061(3) 0.75085(3) 0.03879(9) Uani 1 1 d . . . S1 S 0.5072(3) 0.4031(2) 0.5644(2) 0.0768(6) Uani 1 1 d . . . P1 P -0.0375(2) 0.29501(18) 0.87134(18) 0.0455(5) Uani 1 1 d . . . P2 P 0.16855(18) -0.05703(18) 0.63207(16) 0.0424(4) Uani 1 1 d . . . N1 N 0.2639(7) 0.2300(7) 0.6618(6) 0.0546(16) Uani 1 1 d . . . N2 N -0.0517(4) -0.1524(4) 1.0158(3) 0.0476(8) Uani 1 1 d . . . N3 N -0.0739(6) -0.2751(5) 1.1054(4) 0.0585(11) Uani 1 1 d . . . C1 C 0.3656(5) 0.3010(5) 0.6200(4) 0.0471(10) Uani 1 1 d . . . C2 C -0.1321(7) 0.0242(7) 0.8332(7) 0.0436(15) Uani 1 1 d . . . C3 C -0.2477(6) 0.0797(5) 0.7711(4) 0.0533(10) Uani 1 1 d . . . H3 H -0.2323 0.1639 0.6976 0.064 Uiso 1 1 calc R . . C4 C -0.3837(6) 0.0148(6) 0.8144(5) 0.0602(11) Uani 1 1 d . . . H4 H -0.4563 0.0534 0.7696 0.072 Uiso 1 1 calc R . . C5 C -0.4091(8) -0.1111(8) 0.9280(8) 0.0662(18) Uani 1 1 d . . . H5 H -0.5006 -0.1544 0.9605 0.079 Uiso 1 1 calc R . . C6 C -0.2986(6) -0.1690(5) 0.9899(5) 0.0536(10) Uani 1 1 d . . . H6 H -0.3139 -0.2541 1.0626 0.064 Uiso 1 1 calc R . . C7 C -0.1626(5) -0.1015(4) 0.9452(4) 0.0421(8) Uani 1 1 d . . . C8 C 0.0293(7) -0.3222(6) 1.1807(5) 0.0580(13) Uani 1 1 d . . . C9 C 0.1442(7) -0.2417(7) 1.1660(6) 0.0638(14) Uani 1 1 d . . . H9 H 0.1573 -0.1491 1.1018 0.077 Uiso 1 1 calc R . . C10 C 0.2398(7) -0.2958(7) 1.2448(5) 0.0739(15) Uani 1 1 d . . . H10 H 0.3181 -0.2416 1.2318 0.089 Uiso 1 1 calc R . . C11 C 0.2170(9) -0.4322(9) 1.3434(6) 0.081(2) Uani 1 1 d . . . H11 H 0.2783 -0.4693 1.3986 0.097 Uiso 1 1 calc R . . C12 C 0.1022(11) -0.5118(9) 1.3582(7) 0.097(3) Uani 1 1 d . . . H12 H 0.0886 -0.6038 1.4231 0.116 Uiso 1 1 calc R . . C13 C 0.0070(10) -0.4592(8) 1.2800(7) 0.089(2) Uani 1 1 d . . . H13 H -0.0707 -0.5140 1.2930 0.107 Uiso 1 1 calc R . . C14 C -0.0803(10) 0.4828(8) 0.7621(8) 0.060(2) Uani 1 1 d . . . H14A H -0.1176 0.5556 0.8124 0.072 Uiso 1 1 calc R . . H14B H 0.0145 0.5131 0.6930 0.072 Uiso 1 1 calc R . . C15 C -0.1990(11) 0.4867(9) 0.7003(9) 0.073(3) Uani 1 1 d . . . H15A H -0.2939 0.4560 0.7693 0.088 Uiso 1 1 calc R . . H15B H -0.1616 0.4149 0.6492 0.088 Uiso 1 1 calc R . . C16 C -0.2343(14) 0.6463(10) 0.6096(12) 0.098(3) Uani 1 1 d . . . H16A H -0.3103 0.6438 0.5723 0.147 Uiso 1 1 calc R . . H16B H -0.1411 0.6763 0.5402 0.147 Uiso 1 1 calc R . . H16C H -0.2734 0.7174 0.6602 0.147 Uiso 1 1 calc R . . C17 C -0.2147(9) 0.2603(9) 1.0125(8) 0.0578(18) Uani 1 1 d . . . H17A H -0.2950 0.2508 0.9817 0.069 Uiso 1 1 calc R . . H17B H -0.1948 0.1644 1.0748 0.069 Uiso 1 1 calc R . . C18 C -0.2765(13) 0.3832(12) 1.0857(10) 0.089(3) Uani 1 1 d . . . H18A H -0.1982 0.3912 1.1193 0.107 Uiso 1 1 calc R . . H18B H -0.2955 0.4798 1.0238 0.107 Uiso 1 1 calc R . . C19 C -0.4222(12) 0.3498(14) 1.1972(11) 0.111(3) Uani 1 1 d . . . H19A H -0.4496 0.4227 1.2453 0.167 Uiso 1 1 calc R . . H19B H -0.4067 0.2504 1.2547 0.167 Uiso 1 1 calc R . . H19C H -0.5039 0.3549 1.1633 0.167 Uiso 1 1 calc R . . C20 C 0.1041(9) 0.3230(7) 0.9353(7) 0.0537(17) Uani 1 1 d . . . H20A H 0.1894 0.3677 0.8618 0.064 Uiso 1 1 calc R . . H20B H 0.0558 0.3937 0.9871 0.064 Uiso 1 1 calc R . . C21 C 0.1679(9) 0.1764(9) 1.0205(8) 0.0676(18) Uani 1 1 d . . . H21A H 0.0833 0.1347 1.0965 0.081 Uiso 1 1 calc R . . H21B H 0.2111 0.1038 0.9702 0.081 Uiso 1 1 calc R . . C22 C 0.2921(12) 0.1979(10) 1.0678(10) 0.088(3) Uani 1 1 d . . . H22A H 0.3273 0.1024 1.1205 0.132 Uiso 1 1 calc R . . H22B H 0.2496 0.2678 1.1195 0.132 Uiso 1 1 calc R . . H22C H 0.3775 0.2369 0.9931 0.132 Uiso 1 1 calc R . . C23 C 0.2133(8) -0.2447(7) 0.7367(6) 0.0450(15) Uani 1 1 d . . . H23A H 0.1180 -0.2801 0.8019 0.054 Uiso 1 1 calc R . . H23B H 0.2583 -0.3139 0.6832 0.054 Uiso 1 1 calc R . . C24 C 0.3266(9) -0.2465(9) 0.8078(8) 0.0587(19) Uani 1 1 d . . . H24A H 0.4213 -0.2100 0.7424 0.070 Uiso 1 1 calc R . . H24B H 0.2811 -0.1774 0.8615 0.070 Uiso 1 1 calc R . . C25 C 0.3658(10) -0.3987(8) 0.8931(9) 0.070(2) Uani 1 1 d . . . H25A H 0.4402 -0.3933 0.9307 0.105 Uiso 1 1 calc R . . H25B H 0.4085 -0.4685 0.8413 0.105 Uiso 1 1 calc R . . H25C H 0.2738 -0.4326 0.9623 0.105 Uiso 1 1 calc R . . C26 C 0.3524(9) -0.0179(9) 0.4976(7) 0.0552(18) Uani 1 1 d . . . H26A H 0.3335 0.0770 0.4338 0.066 Uiso 1 1 calc R . . H26B H 0.4255 -0.0044 0.5340 0.066 Uiso 1 1 calc R . . C27 C 0.4258(10) -0.1348(11) 0.4272(9) 0.0697(19) Uani 1 1 d . . . H27A H 0.3534 -0.1468 0.3893 0.084 Uiso 1 1 calc R . . H27B H 0.4427 -0.2302 0.4913 0.084 Uiso 1 1 calc R . . C28 C 0.5796(10) -0.1039(12) 0.3177(8) 0.088(3) Uani 1 1 d . . . H28A H 0.6199 -0.1883 0.2820 0.133 Uiso 1 1 calc R . . H28B H 0.6521 -0.0895 0.3530 0.133 Uiso 1 1 calc R . . H28C H 0.5633 -0.0145 0.2493 0.133 Uiso 1 1 calc R . . C29 C 0.0421(9) -0.0840(8) 0.5535(7) 0.0536(17) Uani 1 1 d . . . H29A H 0.0911 -0.1649 0.5128 0.064 Uiso 1 1 calc R . . H29B H -0.0543 -0.1143 0.6201 0.064 Uiso 1 1 calc R . . C30 C 0.0072(10) 0.0599(9) 0.4487(7) 0.073(2) Uani 1 1 d . . . H30A H -0.0238 0.1449 0.4850 0.088 Uiso 1 1 calc R . . H30B H 0.1003 0.0796 0.3741 0.088 Uiso 1 1 calc R . . C31 C -0.1208(12) 0.0454(12) 0.4023(9) 0.098(3) Uani 1 1 d . . . H31A H -0.1421 0.1383 0.3390 0.147 Uiso 1 1 calc R . . H31B H -0.2128 0.0245 0.4762 0.147 Uiso 1 1 calc R . . H31C H -0.0883 -0.0355 0.3623 0.147 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 0.03673(14) 0.03807(13) 0.04443(13) -0.01049(9) -0.01418(9) -0.00945(9) S1 0.0664(12) 0.0755(11) 0.0914(11) -0.0058(9) -0.0268(9) -0.0383(9) P1 0.0460(11) 0.0394(10) 0.0567(11) -0.0169(8) -0.0184(10) -0.0068(8) P2 0.0401(10) 0.0466(10) 0.0446(10) -0.0148(8) -0.0126(9) -0.0116(8) N1 0.056(4) 0.054(4) 0.064(4) -0.024(3) -0.017(3) -0.018(3) N2 0.047(2) 0.0508(18) 0.0431(16) -0.0109(14) -0.0121(15) -0.0097(16) N3 0.065(3) 0.053(2) 0.056(3) -0.0041(19) -0.023(2) -0.016(2) C1 0.045(2) 0.046(2) 0.053(2) -0.0147(18) -0.018(2) -0.006(2) C2 0.036(4) 0.044(3) 0.054(3) -0.012(3) -0.016(3) -0.011(3) C3 0.052(3) 0.050(2) 0.056(2) -0.0090(18) -0.020(2) -0.006(2) C4 0.042(2) 0.075(3) 0.071(3) -0.023(2) -0.021(2) -0.011(2) C5 0.042(3) 0.073(4) 0.087(4) -0.020(3) -0.019(3) -0.020(3) C6 0.047(3) 0.055(2) 0.060(2) -0.0119(19) -0.015(2) -0.019(2) C7 0.038(2) 0.044(2) 0.0467(19) -0.0160(16) -0.0107(18) -0.0079(17) C8 0.064(3) 0.053(3) 0.054(3) -0.014(2) -0.018(2) -0.004(3) C9 0.077(4) 0.057(3) 0.061(3) -0.011(2) -0.034(3) -0.005(3) C10 0.072(4) 0.093(4) 0.069(3) -0.023(3) -0.039(3) -0.006(3) C11 0.086(5) 0.092(5) 0.058(4) -0.020(3) -0.033(4) 0.020(4) C12 0.113(6) 0.077(4) 0.080(4) 0.007(3) -0.038(4) -0.007(5) C13 0.106(6) 0.067(4) 0.073(4) 0.010(3) -0.032(4) -0.011(4) C14 0.060(5) 0.045(4) 0.078(5) -0.013(3) -0.029(4) -0.008(4) C15 0.082(6) 0.053(5) 0.092(6) -0.003(4) -0.050(5) -0.010(4) C16 0.115(9) 0.064(5) 0.132(8) -0.006(5) -0.081(7) -0.006(6) C17 0.050(4) 0.057(4) 0.061(4) -0.025(3) -0.006(3) -0.004(3) C18 0.090(6) 0.093(5) 0.094(6) -0.063(5) -0.011(5) -0.001(5) C19 0.085(6) 0.139(9) 0.104(7) -0.065(6) -0.012(5) 0.015(6) C20 0.054(4) 0.046(3) 0.068(4) -0.020(3) -0.022(3) -0.010(3) C21 0.072(4) 0.061(3) 0.069(4) -0.008(3) -0.029(3) -0.013(3) C22 0.102(6) 0.079(5) 0.103(6) -0.014(4) -0.069(5) -0.005(4) C23 0.047(4) 0.042(3) 0.049(3) -0.016(3) -0.015(3) -0.007(3) C24 0.049(4) 0.057(4) 0.078(5) -0.019(4) -0.026(4) -0.013(3) C25 0.067(5) 0.061(5) 0.090(5) -0.019(4) -0.041(4) 0.001(4) C26 0.056(4) 0.058(4) 0.057(4) -0.017(3) -0.017(3) -0.018(3) C27 0.060(4) 0.090(5) 0.067(4) -0.039(4) -0.007(3) -0.020(3) C28 0.068(5) 0.122(7) 0.073(4) -0.046(5) -0.005(4) -0.008(5) C29 0.057(4) 0.065(4) 0.054(3) -0.023(3) -0.025(3) -0.014(3) C30 0.083(5) 0.080(4) 0.065(4) -0.007(3) -0.038(4) -0.020(4) C31 0.093(6) 0.123(7) 0.081(4) -0.010(4) -0.053(4) -0.009(5) _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 C2 2.021(6) . ? Pd1 N1 2.078(6) . ? Pd1 P1 2.3266(19) . ? Pd1 P2 2.3382(19) . ? S1 C1 1.629(5) . ? P1 C20 1.832(8) . ? P1 C17 1.838(7) . ? P1 C14 1.842(8) . ? P2 C23 1.824(7) . ? P2 C29 1.827(7) . ? P2 C26 1.848(8) . ? N1 C1 1.153(7) . ? N2 N3 1.257(6) . ? N2 C7 1.437(6) . ? N3 C8 1.418(8) . ? C2 C7 1.406(7) . ? C2 C3 1.408(8) . ? C3 C4 1.392(7) . ? C3 H3 0.9300 . ? C4 C5 1.414(9) . ? C4 H4 0.9300 . ? C5 C6 1.368(9) . ? C5 H5 0.9300 . ? C6 C7 1.403(6) . ? C6 H6 0.9300 . ? C8 C9 1.388(9) . ? C8 C13 1.397(8) . ? C9 C10 1.388(8) . ? C9 H9 0.9300 . ? C10 C11 1.391(9) . ? C10 H10 0.9300 . ? C11 C12 1.381(13) . ? C11 H11 0.9300 . ? C12 C13 1.380(11) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 C15 1.505(12) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.553(11) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C18 1.548(13) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.492(13) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 C21 1.531(10) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.524(12) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 C24 1.546(10) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.488(10) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 C27 1.484(14) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.531(11) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 C30 1.534(11) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 C31 1.524(13) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? 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 Pd1 N1 177.0(3) . . ? C2 Pd1 P1 91.2(2) . . ? N1 Pd1 P1 87.50(18) . . ? C2 Pd1 P2 88.1(2) . . ? N1 Pd1 P2 93.19(18) . . ? P1 Pd1 P2 179.23(8) . . ? C20 P1 C17 105.7(4) . . ? C20 P1 C14 104.0(3) . . ? C17 P1 C14 105.9(4) . . ? C20 P1 Pd1 111.3(3) . . ? C17 P1 Pd1 118.9(3) . . ? C14 P1 Pd1 109.8(3) . . ? C23 P2 C29 104.8(3) . . ? C23 P2 C26 104.3(4) . . ? C29 P2 C26 104.4(4) . . ? C23 P2 Pd1 111.8(2) . . ? C29 P2 Pd1 115.4(3) . . ? C26 P2 Pd1 115.0(3) . . ? C1 N1 Pd1 172.9(5) . . ? N3 N2 C7 114.4(4) . . ? N2 N3 C8 114.9(5) . . ? N1 C1 S1 178.4(5) . . ? C7 C2 C3 116.0(5) . . ? C7 C2 Pd1 125.2(4) . . ? C3 C2 Pd1 118.7(4) . . ? C4 C3 C2 123.3(5) . . ? C4 C3 H3 118.4 . . ? C2 C3 H3 118.4 . . ? C3 C4 C5 118.5(5) . . ? C3 C4 H4 120.8 . . ? C5 C4 H4 120.8 . . ? C6 C5 C4 119.8(6) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? C5 C6 C7 120.8(5) . . ? C5 C6 H6 119.6 . . ? C7 C6 H6 119.6 . . ? C6 C7 C2 121.6(4) . . ? C6 C7 N2 121.6(3) . . ? C2 C7 N2 116.8(4) . . ? C9 C8 C13 118.9(7) . . ? C9 C8 N3 125.5(5) . . ? C13 C8 N3 115.6(6) . . ? C10 C9 C8 121.7(6) . . ? C10 C9 H9 119.2 . . ? C8 C9 H9 119.2 . . ? C9 C10 C11 119.1(7) . . ? C9 C10 H10 120.5 . . ? C11 C10 H10 120.5 . . ? C12 C11 C10 119.1(7) . . ? C12 C11 H11 120.4 . . ? C10 C11 H11 120.4 . . ? C13 C12 C11 122.2(7) . . ? C13 C12 H12 118.9 . . ? C11 C12 H12 118.9 . . ? C12 C13 C8 118.9(8) . . ? C12 C13 H13 120.5 . . ? C8 C13 H13 120.5 . . ? C15 C14 P1 113.0(5) . . ? C15 C14 H14A 109.0 . . ? P1 C14 H14A 109.0 . . ? C15 C14 H14B 109.0 . . ? P1 C14 H14B 109.0 . . ? H14A C14 H14B 107.8 . . ? C14 C15 C16 112.1(7) . . ? C14 C15 H15A 109.2 . . ? C16 C15 H15A 109.2 . . ? C14 C15 H15B 109.2 . . ? C16 C15 H15B 109.2 . . ? H15A C15 H15B 107.9 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 P1 115.3(6) . . ? C18 C17 H17A 108.4 . . ? P1 C17 H17A 108.4 . . ? C18 C17 H17B 108.4 . . ? P1 C17 H17B 108.4 . . ? H17A C17 H17B 107.5 . . ? C19 C18 C17 112.6(8) . . ? C19 C18 H18A 109.1 . . ? C17 C18 H18A 109.1 . . ? C19 C18 H18B 109.1 . . ? C17 C18 H18B 109.1 . . ? H18A C18 H18B 107.8 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 P1 113.2(5) . . ? C21 C20 H20A 108.9 . . ? P1 C20 H20A 108.9 . . ? C21 C20 H20B 108.9 . . ? P1 C20 H20B 108.9 . . ? H20A C20 H20B 107.7 . . ? C22 C21 C20 113.4(7) . . ? C22 C21 H21A 108.9 . . ? C20 C21 H21A 108.9 . . ? C22 C21 H21B 108.9 . . ? C20 C21 H21B 108.9 . . ? H21A C21 H21B 107.7 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 P2 112.6(4) . . ? C24 C23 H23A 109.1 . . ? P2 C23 H23A 109.1 . . ? C24 C23 H23B 109.1 . . ? P2 C23 H23B 109.1 . . ? H23A C23 H23B 107.8 . . ? C25 C24 C23 113.6(6) . . ? C25 C24 H24A 108.9 . . ? C23 C24 H24A 108.9 . . ? C25 C24 H24B 108.9 . . ? C23 C24 H24B 108.9 . . ? H24A C24 H24B 107.7 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C27 C26 P2 116.1(5) . . ? C27 C26 H26A 108.3 . . ? P2 C26 H26A 108.3 . . ? C27 C26 H26B 108.3 . . ? P2 C26 H26B 108.3 . . ? H26A C26 H26B 107.4 . . ? C26 C27 C28 116.1(8) . . ? C26 C27 H27A 108.3 . . ? C28 C27 H27A 108.3 . . ? C26 C27 H27B 108.3 . . ? C28 C27 H27B 108.3 . . ? H27A C27 H27B 107.4 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 P2 112.1(5) . . ? C30 C29 H29A 109.2 . . ? P2 C29 H29A 109.2 . . ? C30 C29 H29B 109.2 . . ? P2 C29 H29B 109.2 . . ? H29A C29 H29B 107.9 . . ? C31 C30 C29 111.6(7) . . ? C31 C30 H30A 109.3 . . ? C29 C30 H30A 109.3 . . ? C31 C30 H30B 109.3 . . ? C29 C30 H30B 109.3 . . ? H30A C30 H30B 108.0 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 0.446 _refine_diff_density_min -0.535 _refine_diff_density_rms 0.046 #=========================================================END data_JHT180 _database_code_depnum_ccdc_archive 'CCDC 727728' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H31 N5 P2 Pd S2' _chemical_formula_weight 561.95 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' P P 0.1023 0.0942 '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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/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 14.0772(2) _cell_length_b 11.9202(2) _cell_length_c 15.9738(3) _cell_angle_alpha 90.00 _cell_angle_beta 107.5900(10) _cell_angle_gamma 90.00 _cell_volume 2555.12(7) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9362 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 23.55 _exptl_crystal_description BLOCK _exptl_crystal_colour colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.461 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1152 _exptl_absorpt_coefficient_mu 1.030 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7901 _exptl_absorpt_correction_T_max 0.8525 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 142684 _diffrn_reflns_av_R_equivalents 0.0520 _diffrn_reflns_av_sigmaI/netI 0.0305 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 28.42 _reflns_number_total 6392 _reflns_number_gt 4669 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0388P)^2^+1.2706P] 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 6392 _refine_ls_number_parameters 262 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0606 _refine_ls_R_factor_gt 0.0347 _refine_ls_wR_factor_ref 0.0851 _refine_ls_wR_factor_gt 0.0752 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _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 0.698718(15) 0.138212(16) 0.887497(12) 0.03642(7) Uani 1 1 d . . . S1 S 0.81571(6) -0.16843(6) 0.77635(5) 0.04945(19) Uani 1 1 d . . . S2 S 0.62437(7) 0.28046(7) 0.95380(5) 0.0562(2) Uani 1 1 d . . . P1 P 0.86240(6) 0.19144(7) 0.95392(5) 0.04932(19) Uani 1 1 d . . . P2 P 0.54114(6) 0.07493(8) 0.81306(6) 0.0564(2) Uani 1 1 d . . . N1 N 0.8007(2) -0.2620(2) 0.93470(17) 0.0581(7) Uani 1 1 d . . . N2 N 0.7207(2) 0.1621(2) 1.10334(18) 0.0553(6) Uani 1 1 d . . . N3 N 0.7264(2) 0.1697(3) 1.18903(18) 0.0656(7) Uani 1 1 d . . . N4 N 0.6737(2) 0.2517(3) 1.20269(17) 0.0661(8) Uani 1 1 d . . . N5 N 0.63247(18) 0.3006(2) 1.12451(15) 0.0488(6) Uani 1 1 d . . . C1 C 0.8004(2) -0.0549(2) 0.70972(19) 0.0520(7) Uani 1 1 d . . . H1 H 0.8133 -0.0552 0.6559 0.062 Uiso 1 1 calc R . . C2 C 0.7675(2) 0.0361(2) 0.74321(18) 0.0484(7) Uani 1 1 d . . . H2 H 0.7551 0.1048 0.7144 0.058 Uiso 1 1 calc R . . C3 C 0.75359(19) 0.0166(2) 0.82703(16) 0.0385(6) Uani 1 1 d . . . C4 C 0.77730(19) -0.0919(2) 0.85355(17) 0.0376(6) Uani 1 1 d . . . C5 C 0.7746(2) -0.1536(2) 0.93239(18) 0.0417(6) Uani 1 1 d . . . C6 C 0.7501(2) -0.1044(3) 1.00204(19) 0.0511(7) Uani 1 1 d . . . H6 H 0.7330 -0.0288 1.0000 0.061 Uiso 1 1 calc R . . C7 C 0.7513(3) -0.1681(3) 1.0736(2) 0.0648(9) Uani 1 1 d . . . H7 H 0.7349 -0.1363 1.1206 0.078 Uiso 1 1 calc R . . C8 C 0.7767(3) -0.2787(3) 1.0755(2) 0.0746(11) Uani 1 1 d . . . H8 H 0.7779 -0.3237 1.1233 0.090 Uiso 1 1 calc R . . C9 C 0.8005(3) -0.3218(3) 1.0046(3) 0.0739(10) Uani 1 1 d . . . H9 H 0.8175 -0.3973 1.0058 0.089 Uiso 1 1 calc R . . C10 C 0.9290(2) 0.1061(3) 1.0459(2) 0.0673(9) Uani 1 1 d . . . H10A H 0.9234 0.0286 1.0287 0.101 Uiso 1 1 calc R . . H10B H 0.9012 0.1166 1.0933 0.101 Uiso 1 1 calc R . . H10C H 0.9980 0.1275 1.0647 0.101 Uiso 1 1 calc R . . C11 C 0.8827(3) 0.3327(3) 0.9982(3) 0.0822(12) Uani 1 1 d . . . H11A H 0.8499 0.3855 0.9533 0.123 Uiso 1 1 calc R . . H11B H 0.9529 0.3484 1.0179 0.123 Uiso 1 1 calc R . . H11C H 0.8561 0.3391 1.0467 0.123 Uiso 1 1 calc R . . C12 C 0.9413(3) 0.1885(4) 0.8831(3) 0.0757(10) Uani 1 1 d . . . H12A H 0.9114 0.2325 0.8315 0.114 Uiso 1 1 calc R . . H12B H 0.9490 0.1125 0.8663 0.114 Uiso 1 1 calc R . . H12C H 1.0055 0.2191 0.9138 0.114 Uiso 1 1 calc R . . C13 C 0.4508(3) 0.1827(4) 0.7658(3) 0.1028(15) Uani 1 1 d . . . H13A H 0.4531 0.2393 0.8091 0.154 Uiso 1 1 calc R . . H13B H 0.3854 0.1502 0.7466 0.154 Uiso 1 1 calc R . . H13C H 0.4659 0.2158 0.7165 0.154 Uiso 1 1 calc R . . C14 C 0.4843(4) 0.0059(6) 0.8865(4) 0.150(3) Uani 1 1 d . . . H14A H 0.4901 0.0529 0.9366 0.224 Uiso 1 1 calc R . . H14B H 0.5174 -0.0641 0.9055 0.224 Uiso 1 1 calc R . . H14C H 0.4151 -0.0076 0.8564 0.224 Uiso 1 1 calc R . . C15 C 0.5249(4) -0.0201(6) 0.7232(4) 0.174(3) Uani 1 1 d . . . H15A H 0.5704 -0.0818 0.7412 0.262 Uiso 1 1 calc R . . H15B H 0.5379 0.0183 0.6750 0.262 Uiso 1 1 calc R . . H15C H 0.4578 -0.0478 0.7053 0.262 Uiso 1 1 calc R . . C16 C 0.6616(2) 0.2450(2) 1.06292(17) 0.0398(6) Uani 1 1 d . . . C17 C 0.5636(3) 0.3964(3) 1.1139(2) 0.0669(9) Uani 1 1 d . . . H17 H 0.5555 0.4286 1.0557 0.080 Uiso 1 1 calc R . . C18 C 0.4654(5) 0.3569(5) 1.1148(7) 0.207(4) Uani 1 1 d . . . H18A H 0.4421 0.3001 1.0708 0.311 Uiso 1 1 calc R . . H18B H 0.4193 0.4186 1.1028 0.311 Uiso 1 1 calc R . . H18C H 0.4703 0.3262 1.1716 0.311 Uiso 1 1 calc R . . C19 C 0.6041(6) 0.4818(5) 1.1766(6) 0.256(6) Uani 1 1 d . . . H19A H 0.6678 0.5046 1.1721 0.384 Uiso 1 1 calc R . . H19B H 0.6121 0.4534 1.2346 0.384 Uiso 1 1 calc R . . H19C H 0.5598 0.5451 1.1657 0.384 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 0.04263(12) 0.03657(12) 0.03092(11) -0.00129(8) 0.01239(8) 0.00652(9) S1 0.0642(5) 0.0394(4) 0.0485(4) -0.0089(3) 0.0227(4) 0.0039(3) S2 0.0780(6) 0.0562(5) 0.0395(4) 0.0042(3) 0.0253(4) 0.0259(4) P1 0.0459(4) 0.0490(4) 0.0494(4) -0.0084(4) 0.0089(3) 0.0010(3) P2 0.0444(4) 0.0605(5) 0.0597(5) -0.0033(4) 0.0088(4) -0.0001(4) N1 0.0786(19) 0.0414(14) 0.0513(15) -0.0003(12) 0.0153(14) 0.0028(13) N2 0.0577(16) 0.0558(15) 0.0528(16) 0.0086(12) 0.0173(13) 0.0119(12) N3 0.0675(19) 0.077(2) 0.0491(16) 0.0140(14) 0.0125(14) 0.0080(16) N4 0.0726(19) 0.087(2) 0.0387(15) 0.0030(14) 0.0169(13) 0.0032(17) N5 0.0551(15) 0.0562(15) 0.0379(13) -0.0029(11) 0.0183(11) 0.0039(12) C1 0.072(2) 0.0493(17) 0.0431(16) -0.0084(13) 0.0296(15) -0.0045(15) C2 0.068(2) 0.0399(15) 0.0425(16) 0.0012(12) 0.0238(15) 0.0013(14) C3 0.0430(15) 0.0394(14) 0.0345(14) -0.0062(11) 0.0141(12) 0.0005(11) C4 0.0409(14) 0.0364(13) 0.0368(14) -0.0052(11) 0.0140(11) -0.0001(11) C5 0.0440(15) 0.0403(15) 0.0382(14) -0.0017(11) 0.0087(12) -0.0001(12) C6 0.0603(19) 0.0500(16) 0.0454(17) 0.0068(13) 0.0195(14) 0.0084(14) C7 0.074(2) 0.076(2) 0.0460(19) 0.0090(16) 0.0219(17) 0.0043(18) C8 0.104(3) 0.066(2) 0.051(2) 0.0202(18) 0.019(2) -0.002(2) C9 0.102(3) 0.0463(18) 0.068(2) 0.0154(18) 0.018(2) 0.0042(19) C10 0.0489(19) 0.084(2) 0.062(2) 0.0012(18) 0.0073(16) 0.0137(17) C11 0.081(3) 0.061(2) 0.093(3) -0.023(2) 0.010(2) -0.0083(19) C12 0.062(2) 0.091(3) 0.079(3) -0.005(2) 0.027(2) -0.014(2) C13 0.067(3) 0.104(3) 0.115(4) -0.003(3) -0.006(2) 0.025(2) C14 0.098(4) 0.177(6) 0.169(6) 0.069(5) 0.034(4) -0.044(4) C15 0.075(3) 0.230(7) 0.179(6) -0.151(6) -0.021(3) 0.020(4) C16 0.0410(15) 0.0436(15) 0.0390(14) -0.0017(12) 0.0184(12) 0.0001(12) C17 0.079(2) 0.071(2) 0.056(2) -0.0102(17) 0.0278(18) 0.0249(19) C18 0.096(4) 0.138(6) 0.413(14) -0.035(7) 0.113(7) 0.029(4) C19 0.227(8) 0.086(4) 0.339(12) -0.111(6) -0.089(8) 0.057(5) _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 C3 2.020(2) . ? Pd1 P2 2.3042(9) . ? Pd1 P1 2.3151(8) . ? Pd1 S2 2.4005(7) . ? S1 C1 1.695(3) . ? S1 C4 1.746(3) . ? S2 C16 1.715(3) . ? P1 C10 1.800(3) . ? P1 C12 1.810(3) . ? P1 C11 1.816(3) . ? P2 C15 1.788(5) . ? P2 C13 1.804(4) . ? P2 C14 1.805(5) . ? N1 C9 1.325(4) . ? N1 C5 1.342(4) . ? N2 C16 1.327(4) . ? N2 N3 1.350(4) . ? N3 N4 1.285(4) . ? N4 N5 1.341(3) . ? N5 C16 1.348(3) . ? N5 C17 1.475(4) . ? C1 C2 1.352(4) . ? C1 H1 0.9300 . ? C2 C3 1.429(4) . ? C2 H2 0.9300 . ? C3 C4 1.371(4) . ? C4 C5 1.469(4) . ? C5 C6 1.390(4) . ? C6 C7 1.369(4) . ? C6 H6 0.9300 . ? C7 C8 1.365(5) . ? C7 H7 0.9300 . ? C8 C9 1.373(5) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C17 C19 1.421(7) . ? C17 C18 1.465(7) . ? C17 H17 0.9800 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? 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 C3 Pd1 P2 88.05(8) . . ? C3 Pd1 P1 86.81(8) . . ? P2 Pd1 P1 174.75(3) . . ? C3 Pd1 S2 176.78(8) . . ? P2 Pd1 S2 88.79(3) . . ? P1 Pd1 S2 96.34(3) . . ? C1 S1 C4 91.06(13) . . ? C16 S2 Pd1 103.56(9) . . ? C10 P1 C12 103.45(18) . . ? C10 P1 C11 102.98(19) . . ? C12 P1 C11 101.9(2) . . ? C10 P1 Pd1 114.83(13) . . ? C12 P1 Pd1 114.98(13) . . ? C11 P1 Pd1 116.77(14) . . ? C15 P2 C13 102.3(3) . . ? C15 P2 C14 105.0(3) . . ? C13 P2 C14 101.6(3) . . ? C15 P2 Pd1 119.41(17) . . ? C13 P2 Pd1 115.45(16) . . ? C14 P2 Pd1 111.1(2) . . ? C9 N1 C5 118.1(3) . . ? C16 N2 N3 106.2(2) . . ? N4 N3 N2 111.3(3) . . ? N3 N4 N5 106.4(2) . . ? N4 N5 C16 109.0(2) . . ? N4 N5 C17 121.9(2) . . ? C16 N5 C17 129.1(3) . . ? C2 C1 S1 112.7(2) . . ? C2 C1 H1 123.7 . . ? S1 C1 H1 123.7 . . ? C1 C2 C3 113.6(3) . . ? C1 C2 H2 123.2 . . ? C3 C2 H2 123.2 . . ? C4 C3 C2 110.7(2) . . ? C4 C3 Pd1 128.45(19) . . ? C2 C3 Pd1 120.8(2) . . ? C3 C4 C5 132.1(2) . . ? C3 C4 S1 111.93(19) . . ? C5 C4 S1 115.95(19) . . ? N1 C5 C6 121.1(3) . . ? N1 C5 C4 115.4(2) . . ? C6 C5 C4 123.5(2) . . ? C7 C6 C5 119.4(3) . . ? C7 C6 H6 120.3 . . ? C5 C6 H6 120.3 . . ? C8 C7 C6 119.4(3) . . ? C8 C7 H7 120.3 . . ? C6 C7 H7 120.3 . . ? C7 C8 C9 118.1(3) . . ? C7 C8 H8 120.9 . . ? C9 C8 H8 120.9 . . ? N1 C9 C8 123.8(3) . . ? N1 C9 H9 118.1 . . ? C8 C9 H9 118.1 . . ? P1 C10 H10A 109.5 . . ? P1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? P1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? P1 C11 H11A 109.5 . . ? P1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? P1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? P1 C12 H12A 109.5 . . ? P1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? P1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? P2 C13 H13A 109.5 . . ? P2 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? P2 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? P2 C14 H14A 109.5 . . ? P2 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? P2 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? P2 C15 H15A 109.5 . . ? P2 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? P2 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N2 C16 N5 107.2(2) . . ? N2 C16 S2 129.2(2) . . ? N5 C16 S2 123.6(2) . . ? C19 C17 C18 113.7(6) . . ? C19 C17 N5 111.3(4) . . ? C18 C17 N5 109.8(4) . . ? C19 C17 H17 107.2 . . ? C18 C17 H17 107.2 . . ? N5 C17 H17 107.2 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 28.42 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.578 _refine_diff_density_min -0.378 _refine_diff_density_rms 0.072