# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _publ_contact_author_name 'Paola Deplano' _publ_contact_author_address ; Dipartimento di Chimica Inorganica ed Analitica Universita degli Studi di Cagliari Cagliari 09042 ITALY ; _publ_contact_author_email deplano@unica.it _publ_section_title ; Pd-Dissolution through a Mild and Effective One-Step Reaction and its Application for Pd-Recovery from Spent Catalytic Converters. ; loop_ _publ_author_name 'Angela Serpe' 'Francesco Bigoli' 'Maria Cristina Cabras' 'Paolo Fornasiero' 'Mauro Graziani' ; M.L.Mercuri ; 'Tiziano Montini' 'Luca Pilia' 'Emanuele F. Trogu' 'Paola Deplano' data_Me2dazdt.2I2 #(1) _database_code_depnum_ccdc_archive 'CCDC 244743' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety Me2dazdt.2I2 _chemical_formula_sum 'C7 H12 I4 N 2 S 2' _chemical_formula_weight 695.92 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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/n #(n. 13) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y, z+1/2' '-x, -y, -z' '-x-1/2, y, -z-1/2' _cell_length_a 8.680(6) _cell_length_b 7.713(7) _cell_length_c 12.740(5) _cell_angle_alpha 90.00 _cell_angle_beta 94.38(2) _cell_angle_gamma 90.00 _cell_volume 850.4(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 36 _cell_measurement_theta_min 13 _cell_measurement_theta_max 20 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.57 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.718 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 624 _exptl_absorpt_coefficient_mu 7.552 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.579 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Philips PW 1100' _diffrn_measurement_method \q/2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 1 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 2561 _diffrn_reflns_av_R_equivalents 0.0226 _diffrn_reflns_av_sigmaI/netI 0.0150 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 29.99 _reflns_number_total 2469 _reflns_number_gt 2180 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Philips PW1100 local upgrade' _computing_cell_refinement 'local programs' _computing_data_reduction 'local programs' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ZORTEP _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w==1/[\s^2^(Fo^2^)+(0.0386P)^2^+1.8798P] 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 2469 _refine_ls_number_parameters 77 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0341 _refine_ls_R_factor_gt 0.0293 _refine_ls_wR_factor_ref 0.0774 _refine_ls_wR_factor_gt 0.0755 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.392 _refine_ls_shift/su_mean 0.010 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 I1 I 1.00881(3) 0.78077(3) 0.396899(18) 0.03427(9) Uani 1 1 d . . . I2 I 1.31317(4) 0.90928(5) 0.42432(3) 0.05618(11) Uani 1 1 d . . . S S 0.70200(12) 0.67176(14) 0.38426(8) 0.0375(2) Uani 1 1 d . . . N N 0.5865(4) 0.3945(4) 0.2812(3) 0.0345(7) Uani 1 1 d . . . C1 C 0.6912(4) 0.5178(5) 0.2903(3) 0.0285(7) Uani 1 1 d . . . C2 C 0.6114(6) 0.2477(5) 0.2103(4) 0.0448(10) Uani 1 1 d . . . H2A H 0.6273 0.2915 0.1406 0.035(12) Uiso 1 1 calc R . . H2B H 0.5199 0.1749 0.2048 0.048(14) Uiso 1 1 calc R . . C3 C 0.7500 0.1398(8) 0.2500 0.0514(16) Uani 1 2 d S . . H3A H 0.7795 0.0657 0.1934 0.00(19) Uiso 0.50 1 calc PR . . H3B H 0.7205 0.0657 0.3066 0.09(14) Uiso 0.50 1 calc PR . . C4 C 0.4597(6) 0.3906(7) 0.3505(4) 0.0516(12) Uani 1 1 d . . . H4A H 0.5009 0.3791 0.4222 0.10(3) Uiso 1 1 calc R . . H4B H 0.3934 0.2938 0.3322 0.13(3) Uiso 1 1 calc R . . H4C H 0.4014 0.4962 0.3426 0.09(2) 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 I1 0.04190(15) 0.02951(13) 0.03133(13) -0.00362(9) 0.00239(9) 0.00025(10) I2 0.03950(17) 0.0655(2) 0.0637(2) -0.00702(16) 0.00491(14) -0.00798(14) S 0.0406(5) 0.0384(5) 0.0354(5) -0.0125(4) 0.0139(4) -0.0058(4) N 0.0428(18) 0.0284(15) 0.0328(15) 0.0011(12) 0.0060(13) -0.0061(13) C1 0.0340(17) 0.0269(16) 0.0251(15) 0.0034(12) 0.0060(13) -0.0008(13) C2 0.062(3) 0.0290(19) 0.044(2) -0.0093(16) 0.005(2) -0.0130(18) C3 0.076(5) 0.024(3) 0.055(4) 0.000 0.011(3) 0.000 C4 0.050(3) 0.048(3) 0.059(3) 0.001(2) 0.020(2) -0.016(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 I1 S 2.786(2) . ? I1 I2 2.8183(18) . ? S C1 1.683(4) . ? N C1 1.315(5) . ? N C4 1.463(6) . ? N C2 1.474(5) . ? C1 C1 1.502(7) 4_756 ? C2 C3 1.517(6) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C2 1.517(6) 4_756 ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 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 S I1 I2 175.07(2) . . ? C1 S I1 104.77(13) . . ? C1 N C4 120.6(4) . . ? C1 N C2 118.5(4) . . ? C4 N C2 120.4(4) . . ? N C1 C1 116.1(3) . 4_756 ? N C1 S 125.0(3) . . ? C1 C1 S 118.9(2) 4_756 . ? N C2 C3 111.5(4) . . ? N C2 H2A 109.3 . . ? C3 C2 H2A 109.3 . . ? N C2 H2B 109.3 . . ? C3 C2 H2B 109.3 . . ? H2A C2 H2B 108.0 . . ? C2 C3 C2 113.5(5) . 4_756 ? C2 C3 H3A 108.9 . . ? C2 C3 H3A 108.9 4_756 . ? C2 C3 H3B 108.9 . . ? C2 C3 H3B 108.9 4_756 . ? H3A C3 H3B 107.7 . . ? N C4 H4A 109.5 . . ? N C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 29.99 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.221 _refine_diff_density_min -1.263 _refine_diff_density_rms 0.137 #==END data_Compound_[Pd(Me2dazdt)2](I3)2 #(2) _database_code_depnum_ccdc_archive 'CCDC 244744' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Pd(Me2dazdt)2](I3)2' _chemical_formula_sum 'C14 H24 I6 N4 Pd S4' _chemical_formula_weight 1244.41 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 27.354(5) _cell_length_b 10.429(7) _cell_length_c 10.823(7) _cell_angle_alpha 90.00 _cell_angle_beta 91.36(2) _cell_angle_gamma 90.00 _cell_volume 3087(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 30 _cell_measurement_theta_min 7 _cell_measurement_theta_max 16 _exptl_crystal_description blade _exptl_crystal_colour 'pale brown' _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.678 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2256 _exptl_absorpt_coefficient_mu 6.884 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5945 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens AED' _diffrn_measurement_method \q/2\q' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 1 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 3550 _diffrn_reflns_av_R_equivalents 0.0305 _diffrn_reflns_av_sigmaI/netI 0.1266 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -2 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.49 _diffrn_reflns_theta_max 27.06 _reflns_number_total 3381 _reflns_number_gt 1082 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens AED local upgrade' _computing_cell_refinement 'local programs' _computing_data_reduction 'local programs' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ZORTEP _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w==1/[\s^2^(Fo^2^)+(0.0867P)^2^+0.0000P] where P==(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3381 _refine_ls_number_parameters 161 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1398 _refine_ls_R_factor_gt 0.0463 _refine_ls_wR_factor_ref 0.1413 _refine_ls_wR_factor_gt 0.1225 _refine_ls_goodness_of_fit_ref 0.698 _refine_ls_restrained_S_all 0.698 _refine_ls_shift/su_max 0.005 _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 I1 I 0.5000 0.39228(11) 0.2500 0.0661(3) Uani 1 2 d S . . I2 I 0.43031(3) 0.40071(9) 0.04151(8) 0.0765(3) Uani 1 1 d . . . I3 I 0.7413(3) 0.0570(6) 0.6512(6) 0.0980(15) Uani 0.50 1 d P . . I4 I 0.7496(7) 0.2708(13) 0.4843(16) 0.094(3) Uani 0.50 1 d P . . I5 I 0.7553(3) 0.4872(5) 0.3119(6) 0.0871(12) Uani 0.50 1 d P . . Pd Pd 0.5000 0.0000 0.5000 0.0553(4) Uani 1 2 d S . . S1 S 0.47113(11) 0.1820(3) 0.5960(3) 0.0658(9) Uani 1 1 d . . . S2 S 0.42513(11) -0.0292(3) 0.4033(3) 0.0732(10) Uani 1 1 d . . . N1 N 0.3772(3) 0.2397(9) 0.5998(8) 0.055(2) Uani 1 1 d . . . N2 N 0.3799(3) 0.1830(9) 0.3347(9) 0.056(2) Uani 1 1 d . . . C1 C 0.4140(4) 0.1862(9) 0.5415(9) 0.047(3) Uani 1 1 d . . . C2 C 0.4040(4) 0.1232(11) 0.4219(12) 0.059(3) Uani 1 1 d . . . C3 C 0.3622(4) 0.3130(11) 0.3535(11) 0.066(3) Uani 1 1 d . . . H3A H 0.3522 0.3483 0.2739 0.02(2) Uiso 1 1 calc R . . H3B H 0.3892 0.3648 0.3853 0.04(3) Uiso 1 1 calc R . . C4 C 0.3198(4) 0.3256(14) 0.4410(12) 0.073(4) Uani 1 1 d . . . H4A H 0.2893 0.3070 0.3970 0.05(3) Uiso 1 1 calc R . . H4B H 0.3182 0.4127 0.4721 0.23(11) Uiso 1 1 calc R . . C5 C 0.3267(4) 0.2326(12) 0.5486(11) 0.061(3) Uani 1 1 d . . . H5A H 0.3038 0.2533 0.6127 0.13(6) Uiso 1 1 calc R . . H5B H 0.3199 0.1460 0.5204 0.03(2) Uiso 1 1 calc R . . C6 C 0.3843(6) 0.3012(14) 0.7215(11) 0.075(4) Uani 1 1 d . . . H6A H 0.4057 0.2494 0.7723 0.26(12) Uiso 1 1 calc R . . H6B H 0.3533 0.3097 0.7605 0.08(4) Uiso 1 1 calc R . . H6C H 0.3985 0.3845 0.7110 0.15(7) Uiso 1 1 calc R . . C7 C 0.3704(6) 0.1305(15) 0.2104(11) 0.078(4) Uani 1 1 d . . . H7A H 0.4009 0.1106 0.1727 0.09(4) Uiso 1 1 calc R . . H7B H 0.3530 0.1927 0.1609 0.26(13) Uiso 1 1 calc R . . H7C H 0.3511 0.0540 0.2164 0.19(9) 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 I1 0.0655(7) 0.0734(8) 0.0600(7) 0.000 0.0097(5) 0.000 I2 0.0832(6) 0.0793(6) 0.0670(6) 0.0008(5) 0.0009(4) 0.0052(5) I3 0.100(2) 0.090(4) 0.104(4) -0.014(2) 0.007(2) -0.010(3) I4 0.0630(10) 0.110(8) 0.110(7) -0.042(4) 0.000(4) -0.011(5) I5 0.0788(17) 0.087(3) 0.096(3) -0.021(2) 0.005(2) -0.010(2) Pd 0.0481(7) 0.0534(7) 0.0641(8) -0.0021(6) -0.0055(6) 0.0055(6) S1 0.0530(18) 0.070(2) 0.0741(19) -0.0179(17) -0.0119(15) 0.0072(15) S2 0.0603(19) 0.066(2) 0.092(2) -0.0247(18) -0.0190(17) 0.0121(16) N1 0.051(5) 0.071(7) 0.043(5) 0.017(5) 0.001(4) 0.004(5) N2 0.060(6) 0.052(6) 0.057(6) 0.007(5) 0.005(5) 0.006(5) C1 0.077(8) 0.032(6) 0.032(6) 0.005(4) 0.002(5) 0.004(5) C2 0.031(6) 0.058(8) 0.086(8) -0.001(7) -0.002(6) -0.007(5) C3 0.063(8) 0.066(9) 0.066(8) 0.012(6) -0.017(7) 0.001(7) C4 0.031(6) 0.108(11) 0.080(9) 0.003(8) -0.007(6) 0.027(6) C5 0.040(6) 0.079(9) 0.065(7) -0.006(7) -0.004(6) 0.007(6) C6 0.099(11) 0.076(10) 0.050(8) -0.008(7) 0.000(8) 0.012(9) C7 0.082(10) 0.089(11) 0.064(8) -0.026(8) -0.002(8) 0.001(9) _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 I1 I2 2.9204(15) 2_655 ? I1 I2 2.9204(15) . ? I3 I5 0.616(7) 7_656 ? I3 I4 2.336(11) 7_656 ? I3 I4 2.881(12) . ? I4 I4 0.55(2) 7_656 ? I4 I3 2.336(11) 7_656 ? I4 I5 2.935(12) . ? I5 I3 0.616(7) 7_656 ? Pd S2 2.298(3) . ? Pd S2 2.298(3) 5_656 ? Pd S1 2.312(3) 5_656 ? Pd S1 2.312(3) . ? S1 C1 1.658(11) . ? S2 C2 1.704(12) . ? N1 C1 1.324(12) . ? N1 C6 1.474(14) . ? N1 C5 1.477(12) . ? N2 C2 1.298(13) . ? N2 C3 1.456(14) . ? N2 C7 1.470(14) . ? C1 C2 1.472(15) . ? C3 C4 1.522(16) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.523(15) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 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 I2 I1 I2 176.55(6) 2_655 . ? I5 I3 I4 165.1(16) 7_656 7_656 ? I5 I3 I4 166.7(16) 7_656 . ? I4 I3 I4 1.7(9) 7_656 . ? I4 I4 I3 171(5) 7_656 7_656 ? I4 I4 I3 7(4) 7_656 . ? I3 I4 I3 178.3(9) 7_656 . ? I4 I4 I5 174(4) 7_656 . ? I3 I4 I5 3.1(3) 7_656 . ? I3 I4 I5 178.5(8) . . ? I3 I5 I4 11.8(13) 7_656 . ? S2 Pd S2 180.0 . 5_656 ? S2 Pd S1 89.83(11) . 5_656 ? S2 Pd S1 90.17(11) 5_656 5_656 ? S2 Pd S1 90.17(11) . . ? S2 Pd S1 89.83(11) 5_656 . ? S1 Pd S1 179.999(1) 5_656 . ? C1 S1 Pd 101.0(4) . . ? C2 S2 Pd 97.1(4) . . ? C1 N1 C6 121.5(10) . . ? C1 N1 C5 121.0(9) . . ? C6 N1 C5 117.4(10) . . ? C2 N2 C3 120.7(10) . . ? C2 N2 C7 124.2(11) . . ? C3 N2 C7 115.0(10) . . ? N1 C1 C2 118.7(10) . . ? N1 C1 S1 124.3(8) . . ? C2 C1 S1 117.1(8) . . ? N2 C2 C1 120.4(10) . . ? N2 C2 S2 122.0(9) . . ? C1 C2 S2 117.6(9) . . ? N2 C3 C4 115.3(10) . . ? N2 C3 H3A 108.4 . . ? C4 C3 H3A 108.4 . . ? N2 C3 H3B 108.4 . . ? C4 C3 H3B 108.4 . . ? H3A C3 H3B 107.5 . . ? C3 C4 C5 109.7(9) . . ? C3 C4 H4A 109.7 . . ? C5 C4 H4A 109.7 . . ? C3 C4 H4B 109.7 . . ? C5 C4 H4B 109.7 . . ? H4A C4 H4B 108.2 . . ? N1 C5 C4 110.7(9) . . ? N1 C5 H5A 109.5 . . ? C4 C5 H5A 109.5 . . ? N1 C5 H5B 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 108.1 . . ? N1 C6 H6A 109.5 . . ? N1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N2 C7 H7A 109.5 . . ? N2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.06 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.388 _refine_diff_density_min -1.028 _refine_diff_density_rms 0.175 #==END