Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Yong-Joo Kim.' 'Xiaohong Chang.' 'Hyun Sue Huh.' 'Mi-Young Kim.' 'Lee,Soon W.' _publ_contact_author_name 'Yong-Joo Kim' _publ_contact_author_address ; Department of Chemistry Kangnung Natiopnal University Kangnung 210-702 SOUTH KOREA ; _publ_contact_author_email YJKIM@KANGNUNG.AC.KR _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Dinuclear palladium-azido complexes containing thiophene derivatives: reactivity toward organic isocyanides and isothiocyanates ; # Attachment 'yjk-1-3.CIF' data_cxh309 _database_code_depnum_ccdc_archive 'CCDC 628104' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H46 N8 P4 Pd2 S2' _chemical_formula_weight 919.55 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 'C2/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 28.363(4) _cell_length_b 11.0249(14) _cell_length_c 15.054(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.081(13) _cell_angle_gamma 90.00 _cell_volume 4660.7(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 27 _cell_measurement_theta_min 2.70 _cell_measurement_theta_max 12.49 _exptl_crystal_description 'BLOCK ' _exptl_crystal_colour 'ORANGE ' _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.310 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1864 _exptl_absorpt_coefficient_mu 1.026 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6863 _exptl_absorpt_correction_T_max 0.9102 _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_% ? _diffrn_reflns_number 4109 _diffrn_reflns_av_R_equivalents 0.0322 _diffrn_reflns_av_sigmaI/netI 0.0760 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 25.05 _reflns_number_total 4025 _reflns_number_gt 2484 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1191P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00023(13) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4025 _refine_ls_number_parameters 194 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1216 _refine_ls_R_factor_gt 0.0697 _refine_ls_wR_factor_ref 0.2104 _refine_ls_wR_factor_gt 0.1747 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _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 0.63479(2) 0.72730(7) 0.41734(5) 0.0568(3) Uani 1 1 d . . . S1 S 0.55742(7) 0.3778(2) 0.47522(15) 0.0547(6) Uani 1 1 d . . . P1 P 0.60833(9) 0.6921(3) 0.26673(18) 0.0695(7) Uani 1 1 d . . . P2 P 0.65750(13) 0.7635(4) 0.5672(2) 0.0957(11) Uani 1 1 d . . . N1 N 0.6425(3) 0.2760(9) 0.4354(6) 0.078(2) Uani 1 1 d . . . N2 N 0.6733(5) 0.8816(10) 0.3902(8) 0.118(4) Uani 1 1 d . . . N3 N 0.6899(4) 0.9196(8) 0.3339(7) 0.088(3) Uani 1 1 d . . . N4 N 0.7087(8) 0.9606(12) 0.2835(12) 0.204(10) Uani 1 1 d . . . C1 C 0.5235(3) 0.5073(8) 0.4864(6) 0.050(2) Uani 1 1 d . . . C2 C 0.5481(3) 0.6075(8) 0.4715(6) 0.051(2) Uani 1 1 d . . . H2 H 0.5356 0.6850 0.4753 0.062 Uiso 1 1 calc R . . C3 C 0.5949(3) 0.5864(8) 0.4493(6) 0.050(2) Uani 1 1 d . . . C4 C 0.6049(3) 0.4670(8) 0.4494(5) 0.052(2) Uani 1 1 d . . . C5 C 0.6465(3) 0.3972(9) 0.4292(6) 0.055(2) Uani 1 1 d . . . C6 C 0.6876(3) 0.4515(10) 0.4045(7) 0.076(3) Uani 1 1 d . . . H6 H 0.6905 0.5354 0.4022 0.091 Uiso 1 1 calc R . . C7 C 0.7240(3) 0.3757(11) 0.3834(7) 0.075(3) Uani 1 1 d . . . H7 H 0.7517 0.4090 0.3670 0.090 Uiso 1 1 calc R . . C8 C 0.7191(4) 0.2570(12) 0.3868(9) 0.089(4) Uani 1 1 d . . . H8 H 0.7428 0.2066 0.3709 0.107 Uiso 1 1 calc R . . C9 C 0.6792(4) 0.2079(10) 0.4137(9) 0.093(4) Uani 1 1 d . . . H9 H 0.6770 0.1240 0.4173 0.112 Uiso 1 1 calc R . . C10 C 0.5716(7) 0.8168(17) 0.2174(11) 0.145(6) Uani 1 1 d . . . H10A H 0.5455 0.8292 0.2507 0.217 Uiso 1 1 calc R . . H10B H 0.5595 0.7977 0.1562 0.217 Uiso 1 1 calc R . . H10C H 0.5904 0.8893 0.2192 0.217 Uiso 1 1 calc R . . C11 C 0.6563(5) 0.6779(17) 0.1991(9) 0.124(5) Uani 1 1 d . . . H11A H 0.6766 0.6116 0.2210 0.186 Uiso 1 1 calc R . . H11B H 0.6745 0.7517 0.2028 0.186 Uiso 1 1 calc R . . H11C H 0.6431 0.6631 0.1378 0.186 Uiso 1 1 calc R . . C12 C 0.5727(4) 0.5578(14) 0.2372(7) 0.104(4) Uani 1 1 d . . . H12A H 0.5895 0.4875 0.2624 0.156 Uiso 1 1 calc R . . H12B H 0.5667 0.5500 0.1730 0.156 Uiso 1 1 calc R . . H12C H 0.5429 0.5648 0.2603 0.156 Uiso 1 1 calc R . . C13 C 0.7158(5) 0.8246(16) 0.5959(10) 0.124(5) Uiso 1 1 d . . . H13A H 0.7310 0.8305 0.5429 0.185 Uiso 1 1 calc R . . H13B H 0.7342 0.7724 0.6386 0.185 Uiso 1 1 calc R . . H13C H 0.7137 0.9037 0.6216 0.185 Uiso 1 1 calc R . . C14 C 0.6365(10) 0.676(3) 0.6492(19) 0.245(12) Uiso 1 1 d . . . H14A H 0.6060 0.6429 0.6259 0.368 Uiso 1 1 calc R . . H14B H 0.6336 0.7254 0.7006 0.368 Uiso 1 1 calc R . . H14C H 0.6585 0.6109 0.6664 0.368 Uiso 1 1 calc R . . C15 C 0.6170(14) 0.835(4) 0.614(3) 0.332(19) Uiso 1 1 d . . . H15A H 0.6151 0.9179 0.5934 0.498 Uiso 1 1 calc R . . H15B H 0.6255 0.8340 0.6780 0.498 Uiso 1 1 calc R . . H15C H 0.5868 0.7966 0.5979 0.498 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 0.0563(4) 0.0541(5) 0.0646(5) -0.0045(3) 0.0243(3) -0.0159(3) S1 0.0498(12) 0.0511(13) 0.0664(14) -0.0002(10) 0.0195(10) -0.0093(9) P1 0.0663(16) 0.0831(19) 0.0615(16) 0.0049(13) 0.0165(13) -0.0089(13) P2 0.093(2) 0.127(3) 0.0717(18) -0.0255(18) 0.0260(16) -0.055(2) N1 0.077(6) 0.067(5) 0.096(7) 0.002(5) 0.033(5) 0.005(4) N2 0.159(10) 0.093(8) 0.118(9) -0.020(6) 0.075(8) -0.071(7) N3 0.115(8) 0.054(5) 0.108(7) 0.006(5) 0.056(6) -0.016(5) N4 0.34(2) 0.088(9) 0.230(17) 0.009(10) 0.210(19) -0.047(12) C1 0.041(4) 0.059(5) 0.054(5) -0.005(4) 0.013(4) -0.003(4) C2 0.049(5) 0.044(5) 0.065(5) -0.002(4) 0.020(4) -0.008(4) C3 0.033(4) 0.061(6) 0.057(5) -0.009(4) 0.015(4) -0.011(4) C4 0.054(5) 0.054(5) 0.049(5) -0.001(4) 0.012(4) -0.012(4) C5 0.040(5) 0.065(6) 0.063(6) -0.004(4) 0.014(4) -0.004(4) C6 0.063(6) 0.075(7) 0.093(8) 0.004(6) 0.027(6) -0.012(5) C7 0.049(5) 0.083(8) 0.096(8) 0.006(6) 0.025(5) 0.012(5) C8 0.080(7) 0.096(10) 0.098(9) 0.009(7) 0.033(7) 0.031(7) C9 0.099(9) 0.057(7) 0.132(11) -0.005(6) 0.047(8) 0.021(6) C10 0.166(16) 0.125(13) 0.137(14) 0.034(11) -0.001(12) 0.031(12) C11 0.120(11) 0.174(15) 0.089(9) -0.024(10) 0.055(8) -0.037(11) C12 0.097(9) 0.155(13) 0.057(7) -0.012(7) 0.004(6) -0.035(8) _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 2.019(8) . ? Pd1 N2 2.093(9) . ? Pd1 P2 2.293(3) . ? Pd1 P1 2.319(3) . ? S1 C1 1.743(9) . ? S1 C4 1.755(8) . ? P1 C12 1.813(13) . ? P1 C11 1.817(12) . ? P1 C10 1.819(16) . ? P2 C15 1.63(4) . ? P2 C14 1.74(3) . ? P2 C13 1.782(15) . ? N1 C5 1.345(12) . ? N1 C9 1.360(13) . ? N2 N3 1.108(12) . ? N3 N4 1.088(13) . ? C1 C2 1.341(11) . ? C1 C1 1.458(15) 5_666 ? C2 C3 1.435(10) . ? C3 C4 1.346(12) . ? C4 C5 1.477(12) . ? C5 C6 1.405(12) . ? C6 C7 1.400(14) . ? C7 C8 1.318(15) . ? C8 C9 1.367(17) . ? 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 N2 175.7(4) . . ? C3 Pd1 P2 89.4(2) . . ? N2 Pd1 P2 88.2(3) . . ? C3 Pd1 P1 89.4(2) . . ? N2 Pd1 P1 93.0(3) . . ? P2 Pd1 P1 177.44(11) . . ? C1 S1 C4 90.8(4) . . ? C12 P1 C11 103.2(7) . . ? C12 P1 C10 104.4(8) . . ? C11 P1 C10 105.5(8) . . ? C12 P1 Pd1 118.0(4) . . ? C11 P1 Pd1 113.4(5) . . ? C10 P1 Pd1 111.1(6) . . ? C15 P2 C14 68.5(17) . . ? C15 P2 C13 113.4(16) . . ? C14 P2 C13 115.9(12) . . ? C15 P2 Pd1 113.0(14) . . ? C14 P2 Pd1 121.7(10) . . ? C13 P2 Pd1 115.3(5) . . ? C5 N1 C9 117.1(9) . . ? N3 N2 Pd1 138.2(9) . . ? N4 N3 N2 174.4(18) . . ? C2 C1 C1 130.9(10) . 5_666 ? C2 C1 S1 110.6(6) . . ? C1 C1 S1 118.4(9) 5_666 . ? C1 C2 C3 115.2(8) . . ? C4 C3 C2 111.1(7) . . ? C4 C3 Pd1 128.9(6) . . ? C2 C3 Pd1 119.9(6) . . ? C3 C4 C5 133.1(7) . . ? C3 C4 S1 112.4(6) . . ? C5 C4 S1 114.5(7) . . ? N1 C5 C6 121.6(9) . . ? N1 C5 C4 115.1(7) . . ? C6 C5 C4 123.3(9) . . ? C7 C6 C5 118.1(10) . . ? C8 C7 C6 119.9(10) . . ? C7 C8 C9 120.1(10) . . ? N1 C9 C8 123.1(11) . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.987 _refine_diff_density_min -0.606 _refine_diff_density_rms 0.129 #=========================================================END data_332 _database_code_depnum_ccdc_archive 'CCDC 628105' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H62 N6 P2 Pd2 S2' _chemical_formula_weight 1085.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Orthorhombic _symmetry_space_group_name_H-M 'Pbca ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z+1/2' 'x+1/2, -y, -z+1/2' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, y-1/2, -z-1/2' '-x-1/2, y, z-1/2' 'x-1/2, -y-1/2, z' _cell_length_a 39.276(8) _cell_length_b 8.758(2) _cell_length_c 14.875(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5116.7(19) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 29 _cell_measurement_theta_min 4.95 _cell_measurement_theta_max 13.82 _exptl_crystal_description 'block ' _exptl_crystal_colour 'orange ' _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.410 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2232 _exptl_absorpt_coefficient_mu 0.886 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4390 _exptl_absorpt_correction_T_max 0.4970 _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_% ? _diffrn_reflns_number 4485 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0414 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 46 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 25.01 _reflns_number_total 4485 _reflns_number_gt 3323 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0458P)^2^+5.1500P] 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 0.00023(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4485 _refine_ls_number_parameters 281 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0610 _refine_ls_R_factor_gt 0.0389 _refine_ls_wR_factor_ref 0.1053 _refine_ls_wR_factor_gt 0.0917 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.002 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 0.411485(7) 0.12826(3) 0.39627(2) 0.04399(13) Uani 1 1 d . . . S1 S 0.51731(3) 0.28396(13) 0.44325(8) 0.0536(3) Uani 1 1 d . . . P1 P 0.37435(3) 0.31154(14) 0.42947(9) 0.0576(3) Uani 1 1 d . . . N1 N 0.45071(8) -0.0296(4) 0.3647(2) 0.0465(8) Uani 1 1 d . . . N2 N 0.37482(9) -0.0296(4) 0.3573(3) 0.0582(9) Uani 1 1 d . . . N3 N 0.32082(10) -0.1229(5) 0.4094(3) 0.0709(12) Uani 1 1 d . . . C1 C 0.45143(9) 0.2550(4) 0.4323(3) 0.0443(9) Uani 1 1 d . . . C2 C 0.45857(10) 0.3991(4) 0.4708(3) 0.0487(10) Uani 1 1 d . . . H2 H 0.4415 0.4665 0.4882 0.058 Uiso 1 1 calc R . . C3 C 0.49234(10) 0.4321(4) 0.4808(3) 0.0488(10) Uani 1 1 d . . . C4 C 0.48144(10) 0.1801(5) 0.4153(3) 0.0461(9) Uani 1 1 d . . . C5 C 0.48239(11) 0.0266(5) 0.3801(3) 0.0500(10) Uani 1 1 d . . . C6 C 0.51046(12) -0.0614(5) 0.3618(3) 0.0622(12) Uani 1 1 d . . . H6 H 0.5322 -0.0227 0.3722 0.075 Uiso 1 1 calc R . . C7 C 0.50664(14) -0.2065(6) 0.3281(3) 0.0715(14) Uani 1 1 d . . . H7 H 0.5256 -0.2662 0.3152 0.086 Uiso 1 1 calc R . . C8 C 0.47429(13) -0.2620(6) 0.3137(3) 0.0662(13) Uani 1 1 d . . . H8 H 0.4710 -0.3604 0.2918 0.079 Uiso 1 1 calc R . . C9 C 0.44686(12) -0.1696(5) 0.3323(3) 0.0577(11) Uani 1 1 d . . . H9 H 0.4250 -0.2063 0.3219 0.069 Uiso 1 1 calc R . . C10 C 0.34988(12) -0.0770(5) 0.3876(3) 0.0540(11) Uani 1 1 d . . . C11 C 0.31167(10) -0.2233(5) 0.4793(3) 0.0552(11) Uani 1 1 d . . . C12 C 0.28307(11) -0.3159(5) 0.4632(3) 0.0597(12) Uani 1 1 d . . . C13 C 0.27264(13) -0.4128(6) 0.5288(4) 0.0759(15) Uani 1 1 d . . . H13 H 0.2540 -0.4757 0.5184 0.091 Uiso 1 1 calc R . . C14 C 0.28898(16) -0.4202(7) 0.6099(4) 0.0829(16) Uani 1 1 d . . . H14 H 0.2818 -0.4897 0.6532 0.099 Uiso 1 1 calc R . . C15 C 0.31602(14) -0.3248(6) 0.6273(4) 0.0735(14) Uani 1 1 d . . . H15 H 0.3264 -0.3282 0.6834 0.088 Uiso 1 1 calc R . . C16 C 0.32801(11) -0.2241(5) 0.5631(3) 0.0566(11) Uani 1 1 d . . . C17 C 0.26487(12) -0.3045(7) 0.3722(4) 0.0737(14) Uani 1 1 d . . . H17 H 0.2664 -0.1980 0.3524 0.088 Uiso 1 1 calc R . . C18 C 0.22729(16) -0.3440(9) 0.3790(5) 0.114(2) Uani 1 1 d . . . H18A H 0.2166 -0.2793 0.4228 0.171 Uiso 1 1 calc R . . H18B H 0.2248 -0.4488 0.3968 0.171 Uiso 1 1 calc R . . H18C H 0.2166 -0.3290 0.3216 0.171 Uiso 1 1 calc R . . C19 C 0.28188(16) -0.4005(8) 0.3024(4) 0.110(2) Uani 1 1 d . . . H19A H 0.3055 -0.3734 0.2987 0.166 Uiso 1 1 calc R . . H19B H 0.2712 -0.3835 0.2452 0.166 Uiso 1 1 calc R . . H19C H 0.2799 -0.5063 0.3184 0.166 Uiso 1 1 calc R . . C20 C 0.35737(12) -0.1195(6) 0.5859(3) 0.0657(13) Uani 1 1 d . . . H20 H 0.3564 -0.0333 0.5439 0.079 Uiso 1 1 calc R . . C21 C 0.35574(16) -0.0543(7) 0.6801(4) 0.0968(19) Uani 1 1 d . . . H21A H 0.3749 0.0118 0.6898 0.145 Uiso 1 1 calc R . . H21B H 0.3563 -0.1360 0.7230 0.145 Uiso 1 1 calc R . . H21C H 0.3350 0.0028 0.6871 0.145 Uiso 1 1 calc R . . C22 C 0.39150(14) -0.1976(8) 0.5723(5) 0.098(2) Uani 1 1 d . . . H22A H 0.4095 -0.1274 0.5863 0.147 Uiso 1 1 calc R . . H22B H 0.3936 -0.2299 0.5109 0.147 Uiso 1 1 calc R . . H22C H 0.3930 -0.2848 0.6112 0.147 Uiso 1 1 calc R . . C23 C 0.38117(12) 0.4926(5) 0.3742(4) 0.0700(14) Uani 1 1 d . . . H23A H 0.3825 0.4770 0.3104 0.105 Uiso 1 1 calc R . . H23B H 0.4021 0.5368 0.3952 0.105 Uiso 1 1 calc R . . H23C H 0.3626 0.5601 0.3877 0.105 Uiso 1 1 calc R . . C24 C 0.33044(13) 0.2719(7) 0.4001(5) 0.102(2) Uani 1 1 d . . . H24A H 0.3236 0.1764 0.4263 0.153 Uiso 1 1 calc R . . H24B H 0.3283 0.2660 0.3359 0.153 Uiso 1 1 calc R . . H24C H 0.3161 0.3521 0.4225 0.153 Uiso 1 1 calc R . . C25 C 0.37212(15) 0.3547(6) 0.5489(4) 0.0838(17) Uani 1 1 d . . . H25A H 0.3684 0.2621 0.5820 0.126 Uiso 1 1 calc R . . H25B H 0.3537 0.4241 0.5598 0.126 Uiso 1 1 calc R . . H25C H 0.3931 0.4006 0.5679 0.126 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 0.04096(18) 0.04019(19) 0.0508(2) -0.00519(14) -0.00149(14) -0.00957(13) S1 0.0394(5) 0.0538(6) 0.0678(7) -0.0078(5) -0.0070(5) -0.0052(5) P1 0.0448(6) 0.0491(6) 0.0789(8) -0.0076(6) -0.0018(6) -0.0039(5) N1 0.053(2) 0.0390(18) 0.0474(19) -0.0020(15) -0.0015(16) -0.0050(15) N2 0.047(2) 0.060(2) 0.068(2) -0.015(2) 0.0041(19) -0.0211(19) N3 0.051(2) 0.084(3) 0.078(3) 0.019(2) -0.013(2) -0.026(2) C1 0.041(2) 0.041(2) 0.051(2) 0.0007(19) -0.0055(18) -0.0064(17) C2 0.046(2) 0.041(2) 0.059(3) -0.0070(19) -0.010(2) -0.0039(18) C3 0.045(2) 0.043(2) 0.058(3) -0.002(2) -0.0121(19) -0.0064(18) C4 0.042(2) 0.046(2) 0.050(2) -0.0026(18) -0.0069(18) -0.0068(18) C5 0.059(3) 0.047(2) 0.044(2) -0.0017(19) -0.0031(19) -0.003(2) C6 0.056(3) 0.063(3) 0.067(3) -0.013(3) 0.002(2) 0.001(2) C7 0.079(4) 0.066(3) 0.069(3) -0.013(3) 0.006(3) 0.020(3) C8 0.085(3) 0.055(3) 0.059(3) -0.014(2) 0.002(3) 0.002(3) C9 0.071(3) 0.049(2) 0.053(3) -0.009(2) -0.005(2) -0.006(2) C10 0.062(3) 0.048(2) 0.052(3) -0.004(2) -0.011(2) -0.010(2) C11 0.042(2) 0.059(3) 0.065(3) 0.001(2) 0.003(2) -0.002(2) C12 0.045(2) 0.062(3) 0.072(3) -0.001(2) 0.004(2) -0.005(2) C13 0.063(3) 0.082(4) 0.083(4) 0.007(3) 0.010(3) -0.020(3) C14 0.089(4) 0.082(4) 0.078(4) 0.013(3) 0.019(3) -0.016(3) C15 0.081(4) 0.075(3) 0.065(3) 0.000(3) 0.004(3) 0.002(3) C16 0.052(2) 0.058(3) 0.060(3) 0.000(2) 0.005(2) 0.004(2) C17 0.047(3) 0.077(3) 0.097(4) -0.002(3) -0.004(3) -0.015(3) C18 0.071(4) 0.142(7) 0.129(6) 0.006(5) -0.016(4) -0.027(4) C19 0.087(4) 0.154(6) 0.090(4) -0.016(4) -0.022(4) 0.019(4) C20 0.061(3) 0.071(3) 0.065(3) -0.009(3) -0.013(2) -0.002(3) C21 0.106(5) 0.101(5) 0.084(4) -0.029(4) -0.015(4) 0.008(4) C22 0.060(3) 0.107(5) 0.128(5) -0.029(4) -0.009(3) -0.004(3) C23 0.063(3) 0.056(3) 0.090(4) 0.004(3) -0.023(3) 0.002(2) C24 0.044(3) 0.073(4) 0.187(7) -0.022(4) -0.011(4) 0.001(3) C25 0.094(4) 0.068(3) 0.090(4) -0.012(3) 0.028(3) 0.001(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 1.995(4) . ? Pd1 N2 2.078(3) . ? Pd1 N1 2.122(3) . ? Pd1 P1 2.2242(13) . ? S1 C3 1.719(4) . ? S1 C4 1.727(4) . ? P1 C23 1.806(5) . ? P1 C24 1.813(5) . ? P1 C25 1.819(6) . ? N1 C9 1.326(5) . ? N1 C5 1.358(5) . ? N2 C10 1.155(5) . ? N3 C10 1.253(6) . ? N3 C11 1.408(6) . ? C1 C4 1.372(6) . ? C1 C2 1.414(5) . ? C2 C3 1.366(5) . ? C3 C3 1.450(7) 5_666 ? C4 C5 1.443(6) . ? C5 C6 1.373(6) . ? C6 C7 1.374(7) . ? C7 C8 1.377(7) . ? C8 C9 1.376(6) . ? C11 C16 1.403(6) . ? C11 C12 1.406(6) . ? C12 C13 1.357(7) . ? C12 C17 1.533(7) . ? C13 C14 1.368(7) . ? C14 C15 1.375(8) . ? C15 C16 1.383(7) . ? C16 C20 1.511(6) . ? C17 C19 1.494(8) . ? C17 C18 1.520(7) . ? C20 C21 1.515(7) . ? C20 C22 1.518(7) . ? 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 171.74(16) . . ? C1 Pd1 N1 81.42(14) . . ? N2 Pd1 N1 90.46(14) . . ? C1 Pd1 P1 93.13(12) . . ? N2 Pd1 P1 95.03(11) . . ? N1 Pd1 P1 174.30(9) . . ? C3 S1 C4 90.59(19) . . ? C23 P1 C24 101.5(3) . . ? C23 P1 C25 105.6(2) . . ? C24 P1 C25 103.3(3) . . ? C23 P1 Pd1 115.80(18) . . ? C24 P1 Pd1 115.6(2) . . ? C25 P1 Pd1 113.48(19) . . ? C9 N1 C5 120.1(4) . . ? C9 N1 Pd1 126.9(3) . . ? C5 N1 Pd1 113.1(3) . . ? C10 N2 Pd1 135.9(3) . . ? C10 N3 C11 128.6(4) . . ? C4 C1 C2 109.3(3) . . ? C4 C1 Pd1 111.1(3) . . ? C2 C1 Pd1 139.6(3) . . ? C3 C2 C1 115.2(4) . . ? C2 C3 C3 128.3(5) . 5_666 ? C2 C3 S1 111.0(3) . . ? C3 C3 S1 120.7(4) 5_666 . ? C1 C4 C5 122.3(4) . . ? C1 C4 S1 113.9(3) . . ? C5 C4 S1 123.8(3) . . ? N1 C5 C6 119.9(4) . . ? N1 C5 C4 112.0(4) . . ? C6 C5 C4 128.0(4) . . ? C5 C6 C7 120.3(5) . . ? C8 C7 C6 118.9(5) . . ? C7 C8 C9 118.9(4) . . ? N1 C9 C8 121.9(4) . . ? N2 C10 N3 171.4(5) . . ? C16 C11 C12 120.9(4) . . ? C16 C11 N3 122.9(4) . . ? C12 C11 N3 116.0(4) . . ? C13 C12 C11 118.7(5) . . ? C13 C12 C17 122.3(4) . . ? C11 C12 C17 119.0(4) . . ? C12 C13 C14 121.5(5) . . ? C13 C14 C15 120.0(5) . . ? C16 C15 C14 121.4(5) . . ? C15 C16 C11 117.5(4) . . ? C15 C16 C20 119.5(5) . . ? C11 C16 C20 123.0(4) . . ? C19 C17 C18 110.6(5) . . ? C19 C17 C12 111.6(5) . . ? C18 C17 C12 112.3(5) . . ? C21 C20 C16 113.8(4) . . ? C21 C20 C22 109.3(5) . . ? C16 C20 C22 111.8(4) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.372 _refine_diff_density_min -0.824 _refine_diff_density_rms 0.070 #=========================================================END data_465 _database_code_depnum_ccdc_archive 'CCDC 628106' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H62 Cl4 N4 P4 Pd2 S2' _chemical_formula_weight 1141.54 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.5056(17) _cell_length_b 12.325(2) _cell_length_c 13.107(4) _cell_angle_alpha 87.887(17) _cell_angle_beta 76.69(2) _cell_angle_gamma 81.063(16) _cell_volume 1320.9(5) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 27 _cell_measurement_theta_min 5.02 _cell_measurement_theta_max 12.43 _exptl_crystal_description 'block ' _exptl_crystal_colour 'yellow ' _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.435 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 582 _exptl_absorpt_coefficient_mu 1.114 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4721 _exptl_absorpt_correction_T_max 0.8289 _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_% ? _diffrn_reflns_number 4962 _diffrn_reflns_av_R_equivalents 0.0296 _diffrn_reflns_av_sigmaI/netI 0.0513 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4624 _reflns_number_gt 3598 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0620P)^2^+1.1307P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4624 _refine_ls_number_parameters 255 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0655 _refine_ls_R_factor_gt 0.0463 _refine_ls_wR_factor_ref 0.1251 _refine_ls_wR_factor_gt 0.1135 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _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 0.67451(5) 0.67646(3) 0.80055(3) 0.04785(15) Uani 1 1 d . . . P1 P 0.49329(19) 0.83311(11) 0.78454(11) 0.0591(4) Uani 1 1 d . . . P2 P 0.83752(17) 0.51140(12) 0.81741(11) 0.0591(4) Uani 1 1 d . . . S1 S 0.63647(16) 0.60225(11) 0.57226(10) 0.0537(3) Uani 1 1 d . . . N1 N 0.7810(7) 0.7535(5) 0.8973(4) 0.0874(17) Uani 1 1 d . . . N2 N 0.9117(7) 0.8002(5) 1.0307(4) 0.0816(16) Uani 1 1 d . . . C1 C 0.5727(6) 0.5994(4) 0.7074(4) 0.0472(11) Uani 1 1 d . . . C2 C 0.4546(6) 0.5345(4) 0.7318(4) 0.0564(13) Uani 1 1 d . . . H2 H 0.4025 0.5220 0.8008 0.068 Uiso 1 1 calc R . . C3 C 0.4155(7) 0.4874(4) 0.6469(4) 0.0566(13) Uani 1 1 d . . . H3 H 0.3368 0.4413 0.6548 0.068 Uiso 1 1 calc R . . C4 C 0.5034(6) 0.5155(4) 0.5524(4) 0.0455(11) Uani 1 1 d . . . C5 C 0.8346(7) 0.7758(4) 0.9658(4) 0.0621(14) Uani 1 1 d . . . C6 C 0.8597(7) 0.8197(4) 1.1377(4) 0.0578(13) Uani 1 1 d . . . C7 C 0.7171(7) 0.7886(4) 1.2022(5) 0.0682(15) Uani 1 1 d . . . C8 C 0.6884(10) 0.8062(6) 1.3116(6) 0.089(2) Uani 1 1 d . . . H8 H 0.5957 0.7856 1.3561 0.107 Uiso 1 1 calc R . . C9 C 0.7957(12) 0.8533(7) 1.3524(6) 0.101(2) Uani 1 1 d . . . H9 H 0.7764 0.8628 1.4245 0.121 Uiso 1 1 calc R . . C10 C 0.9299(10) 0.8862(5) 1.2893(6) 0.084(2) Uani 1 1 d . . . H10 H 0.9993 0.9203 1.3185 0.101 Uiso 1 1 calc R . . C11 C 0.9652(7) 0.8699(4) 1.1825(5) 0.0647(15) Uani 1 1 d . . . C12 C 0.5964(9) 0.7400(6) 1.1585(7) 0.094(2) Uani 1 1 d . . . H12A H 0.5454 0.7941 1.1169 0.142 Uiso 1 1 calc R . . H12B H 0.5146 0.7169 1.2150 0.142 Uiso 1 1 calc R . . H12C H 0.6515 0.6779 1.1156 0.142 Uiso 1 1 calc R . . C13 C 1.1142(8) 0.9069(6) 1.1151(6) 0.091(2) Uani 1 1 d . . . H13A H 1.1655 0.9460 1.1571 0.137 Uiso 1 1 calc R . . H13B H 1.0838 0.9543 1.0608 0.137 Uiso 1 1 calc R . . H13C H 1.1891 0.8441 1.0840 0.137 Uiso 1 1 calc R . . C14 C 0.5420(12) 0.8993(7) 0.6610(6) 0.128(3) Uani 1 1 d . . . H14A H 0.5507 0.8479 0.6060 0.191 Uiso 1 1 calc R . . H14B H 0.6441 0.9262 0.6533 0.191 Uiso 1 1 calc R . . H14C H 0.4574 0.9597 0.6570 0.191 Uiso 1 1 calc R . . C15 C 0.2822(9) 0.8168(6) 0.7994(7) 0.104(3) Uani 1 1 d . . . H15A H 0.2452 0.7807 0.8647 0.157 Uiso 1 1 calc R . . H15B H 0.2719 0.7733 0.7427 0.157 Uiso 1 1 calc R . . H15C H 0.2170 0.8877 0.7987 0.157 Uiso 1 1 calc R . . C16 C 0.4798(9) 0.9368(5) 0.8819(6) 0.095(2) Uani 1 1 d . . . H16A H 0.4517 0.9057 0.9508 0.143 Uiso 1 1 calc R . . H16B H 0.3973 0.9972 0.8744 0.143 Uiso 1 1 calc R . . H16C H 0.5833 0.9623 0.8723 0.143 Uiso 1 1 calc R . . C17 C 0.9014(10) 0.4193(6) 0.7065(6) 0.113(3) Uani 1 1 d . . . H17A H 0.8073 0.4067 0.6825 0.170 Uiso 1 1 calc R . . H17B H 0.9561 0.3508 0.7270 0.170 Uiso 1 1 calc R . . H17C H 0.9746 0.4516 0.6510 0.170 Uiso 1 1 calc R . . C18 C 0.7380(9) 0.4290(6) 0.9238(7) 0.097(2) Uani 1 1 d . . . H18A H 0.6998 0.4727 0.9863 0.145 Uiso 1 1 calc R . . H18B H 0.8146 0.3669 0.9362 0.145 Uiso 1 1 calc R . . H18C H 0.6470 0.4039 0.9051 0.145 Uiso 1 1 calc R . . C19 C 1.0284(7) 0.5240(6) 0.8504(6) 0.0809(19) Uani 1 1 d . . . H19A H 1.0079 0.5713 0.9101 0.121 Uiso 1 1 calc R . . H19B H 1.0984 0.5546 0.7919 0.121 Uiso 1 1 calc R . . H19C H 1.0806 0.4528 0.8667 0.121 Uiso 1 1 calc R . . C20 C 0.1822(18) 0.7405(12) 0.5058(12) 0.211(8) Uani 1 1 d . . . H20A H 0.2763 0.6938 0.5217 0.253 Uiso 1 1 calc R . . H20B H 0.1607 0.7130 0.4428 0.253 Uiso 1 1 calc R . . Cl1 Cl 0.0080(5) 0.7376(5) 0.6127(4) 0.240(2) Uani 1 1 d . . . Cl2 Cl 0.2205(5) 0.8674(4) 0.4866(4) 0.2073(18) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0543(2) 0.0481(2) 0.0478(2) -0.01609(15) -0.02656(17) -0.00209(16) P1 0.0743(9) 0.0450(7) 0.0622(8) -0.0113(6) -0.0284(7) 0.0004(6) P2 0.0600(8) 0.0608(8) 0.0604(8) -0.0151(6) -0.0314(7) 0.0089(6) S1 0.0635(8) 0.0621(8) 0.0450(7) -0.0071(6) -0.0216(6) -0.0230(6) N1 0.091(4) 0.095(4) 0.090(4) -0.041(3) -0.052(3) -0.001(3) N2 0.087(4) 0.116(4) 0.062(3) 0.000(3) -0.035(3) -0.047(3) C1 0.054(3) 0.047(3) 0.045(3) -0.013(2) -0.022(2) 0.000(2) C2 0.061(3) 0.065(3) 0.049(3) -0.012(2) -0.016(2) -0.021(3) C3 0.066(3) 0.065(3) 0.047(3) -0.010(2) -0.019(3) -0.025(3) C4 0.048(3) 0.043(2) 0.052(3) -0.008(2) -0.023(2) -0.008(2) C5 0.073(4) 0.055(3) 0.068(3) -0.014(3) -0.037(3) -0.008(3) C6 0.072(4) 0.053(3) 0.059(3) -0.002(2) -0.036(3) -0.008(3) C7 0.066(4) 0.048(3) 0.090(4) 0.011(3) -0.023(3) -0.003(3) C8 0.093(5) 0.080(5) 0.077(5) 0.002(4) 0.008(4) 0.001(4) C9 0.136(7) 0.092(5) 0.066(4) -0.018(4) -0.018(5) 0.005(5) C10 0.116(6) 0.073(4) 0.072(4) -0.021(3) -0.047(4) 0.002(4) C11 0.080(4) 0.055(3) 0.067(4) -0.010(3) -0.039(3) -0.002(3) C12 0.082(5) 0.087(5) 0.125(6) 0.020(4) -0.033(4) -0.034(4) C13 0.086(5) 0.111(5) 0.097(5) -0.005(4) -0.042(4) -0.042(4) C14 0.173(9) 0.092(6) 0.091(6) 0.020(4) -0.013(6) 0.032(6) C15 0.087(5) 0.085(5) 0.150(7) -0.030(5) -0.054(5) 0.009(4) C16 0.112(6) 0.064(4) 0.117(6) -0.038(4) -0.047(5) 0.010(4) C17 0.141(7) 0.096(5) 0.103(5) -0.053(4) -0.071(5) 0.059(5) C18 0.094(5) 0.080(5) 0.127(6) 0.018(4) -0.047(5) -0.012(4) C19 0.061(4) 0.093(5) 0.095(5) -0.006(4) -0.042(3) 0.004(3) C20 0.222(15) 0.193(13) 0.230(16) -0.144(13) -0.105(13) 0.045(12) Cl1 0.133(3) 0.373(6) 0.229(4) 0.125(4) -0.055(3) -0.089(4) Cl2 0.222(4) 0.213(4) 0.227(4) 0.076(3) -0.102(3) -0.096(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 1.992(4) . ? Pd1 N1 2.053(5) . ? Pd1 P2 2.3111(15) . ? Pd1 P1 2.3113(15) . ? P1 C14 1.777(8) . ? P1 C15 1.803(7) . ? P1 C16 1.812(6) . ? P2 C19 1.804(6) . ? P2 C17 1.807(6) . ? P2 C18 1.820(8) . ? S1 C1 1.730(5) . ? S1 C4 1.739(4) . ? N1 C5 1.155(6) . ? N2 C5 1.258(6) . ? N2 C6 1.387(7) . ? C1 C2 1.354(7) . ? C2 C3 1.401(6) . ? C3 C4 1.355(7) . ? C4 C4 1.455(9) 2_666 ? C6 C11 1.405(7) . ? C6 C7 1.408(8) . ? C7 C8 1.417(10) . ? C7 C12 1.493(9) . ? C8 C9 1.366(11) . ? C9 C10 1.355(11) . ? C10 C11 1.378(9) . ? C11 C13 1.493(9) . ? C20 Cl2 1.645(15) . ? C20 Cl1 1.794(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pd1 N1 179.1(2) . . ? C1 Pd1 P2 87.75(14) . . ? N1 Pd1 P2 91.37(16) . . ? C1 Pd1 P1 88.50(14) . . ? N1 Pd1 P1 92.37(16) . . ? P2 Pd1 P1 175.11(6) . . ? C14 P1 C15 103.7(5) . . ? C14 P1 C16 105.8(4) . . ? C15 P1 C16 102.2(4) . . ? C14 P1 Pd1 113.5(3) . . ? C15 P1 Pd1 116.8(3) . . ? C16 P1 Pd1 113.5(2) . . ? C19 P2 C17 102.6(4) . . ? C19 P2 C18 103.7(3) . . ? C17 P2 C18 104.4(4) . . ? C19 P2 Pd1 114.7(2) . . ? C17 P2 Pd1 118.4(2) . . ? C18 P2 Pd1 111.5(2) . . ? C1 S1 C4 94.1(2) . . ? C5 N1 Pd1 164.3(6) . . ? C5 N2 C6 130.3(6) . . ? C2 C1 S1 107.6(3) . . ? C2 C1 Pd1 130.1(4) . . ? S1 C1 Pd1 122.2(3) . . ? C1 C2 C3 116.1(5) . . ? C4 C3 C2 113.6(5) . . ? C3 C4 C4 129.7(6) . 2_666 ? C3 C4 S1 108.7(3) . . ? C4 C4 S1 121.6(5) 2_666 . ? N1 C5 N2 171.9(7) . . ? N2 C6 C11 115.3(5) . . ? N2 C6 C7 125.0(5) . . ? C11 C6 C7 119.6(5) . . ? C6 C7 C8 118.1(6) . . ? C6 C7 C12 122.0(6) . . ? C8 C7 C12 119.9(6) . . ? C9 C8 C7 120.5(7) . . ? C10 C9 C8 121.0(7) . . ? C9 C10 C11 121.1(7) . . ? C10 C11 C6 119.7(6) . . ? C10 C11 C13 119.8(6) . . ? C6 C11 C13 120.5(5) . . ? Cl2 C20 Cl1 109.4(6) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.666 _refine_diff_density_min -0.772 _refine_diff_density_rms 0.080