Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global # _journal_coden_Cambridge 186 _publ_contact_author ; Isaia, Francesco Universit\'a di Cagliari Dipartimento di Chimica Analitica ed Inorganica S. S. 554, bivio per Sestu I-09042, Cagliari Italy ; _publ_contact_author_phone '++39 70 6754496' _publ_contact_author_email 'isia@unica.it' _publ_requested_journal 'Journal of the Chemical Society, Dalton Transition' _publ_requested_coeditor_name ? _publ_contact_letter ; ? ; #============================================================================== # 2. TITLE AND AUTHOR LIST _publ_section_title ; Oxidation of palladium powder by the tetraphenyldithioimidodiphosphine-diiodine adduct (LH-I2). Crystal structure of PdL2 ; loop_ _publ_author_name _publ_author_address 'Abbati, G. Luca' ; Universit\'a di Modena e Reggio Emilia Dipartimento di Chimica Via G. Campi, 183 I-41100 Modena Italy ; 'Aragoni, M. Carla' ; Universit\'a di Cagliari Dipartimento di Chimica Analitica ed Inorganica S. S. 554, bivio per Sestu I-09042, Cagliari Italy ; 'Arca, Massimiliano' ; Universit\'a di Cagliari Dipartimento di Chimica Analitica ed Inorganica S. S. 554, bivio per Sestu I-09042, Cagliari Italy ; 'Devillanova, Francesco A.' ; Universit\'a di Cagliari Dipartimento di Chimica Analitica ed Inorganica S. S. 554, bivio per Sestu I-09042, Cagliari Italy ; 'Fabretti, Antonio Costantino' ; Universit\'a di Modena e Reggio Emilia Dipartimento di Chimica Via G. Campi, 183 I-41100 Modena Italy ; 'Garau, Alessandra' ; Universit\'a di Cagliari Dipartimento di Chimica Analitica ed Inorganica S. S. 554, bivio per Sestu I-09042, Cagliari Italy ; 'Isaia, Francesco' ; Universit\'a di Cagliari Dipartimento di Chimica Analitica ed Inorganica S. S. 554, bivio per Sestu I-09042, Cagliari Italy ; 'Lippolis, Vito' ; Universit\'a di Cagliari Dipartimento di Chimica Analitica ed Inorganica S. S. 554, bivio per Sestu I-09042, Cagliari Italy ; 'Verani, Gaetano' ; Universit\'a di Cagliari Dipartimento di Chimica Analitica ed Inorganica S. S. 554, bivio per Sestu I-09042, Cagliari Italy ; #============================================================================== # 4. RESULTS data_135dv _database_code_CSD 153387 _audit_creation_method SHELXL-93 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety [Pd(C24H20P2S2N)2] _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C48 H40 N2 P4 Pd S4' _chemical_formula_weight 1003.41 _chemical_melting_point ? _chemical_compound_source Synthesis loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _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 8.8384(10) _cell_length_b 11.516(2) _cell_length_c 13.328(2) _cell_angle_alpha 112.140(10) _cell_angle_beta 100.220(10) _cell_angle_gamma 105.204(11) _cell_volume 1153.1(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 23 _cell_measurement_theta_min 6.53 _cell_measurement_theta_max 11.88 _exptl_crystal_description 'Elonged blocks' _exptl_crystal_colour 'Ambered red' _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.445 _exptl_crystal_density_method none _exptl_crystal_F_000 512 _exptl_absorpt_coefficient_mu 0.758 _exptl_absorpt_correction_type 'empirical, psi-scans' _exptl_absorpt_correction_T_min 0.9581 _exptl_absorpt_correction_T_max 0.9999 _exptl_special_details ; Crystal mounted on the top of a glass fiber with epoxy resin ; _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 'Enraf Nonius CAD4 automatic diffractometer' _diffrn_measurement_method 'omega-2theta scan' _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 3600 _diffrn_standards_decay_% None _diffrn_reflns_number 4550 _diffrn_reflns_av_R_equivalents 0.0205 _diffrn_reflns_av_sigmaI/netI 0.0469 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 31.37 _reflns_number_total 4385 _reflns_number_observed 4385 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'CAD-4 Software. V5.0. (Enraf-Nonius, 1989)' _computing_cell_refinement 'CAD-4 Software. V5.0. (Enraf-Nonius, 1989)' _computing_data_reduction 'SDP (Enraf-Nonius, 1985)' _computing_structure_solution 'SIR92 (Altomare et. al, 1994)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'ZORTEP (Szolnai, 1997)' _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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. All the hydrogen atoms were located on the DF map and refined isotropically. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0446P)^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 refU _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4385 _refine_ls_number_parameters 348 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0389 _refine_ls_wR_factor_all 0.0821 _refine_ls_wR_factor_obs 0.0821 _refine_ls_goodness_of_fit_all 1.046 _refine_ls_goodness_of_fit_obs 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_restrained_S_obs 1.046 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pd1 Pd 0.5000 0.5000 1.0000 0.02445(10) Uani 1 d S . P1 P 0.62200(10) 0.82831(8) 1.17169(7) 0.0287(2) Uani 1 d . . P2 P 0.58443(10) 0.68354(8) 1.29906(7) 0.0276(2) Uani 1 d . . S1 S 0.41271(10) 0.68416(8) 1.05006(7) 0.0309(2) Uani 1 d . . S2 S 0.58747(11) 0.51159(8) 1.18046(7) 0.0347(2) Uani 1 d . . N1 N 0.6635(3) 0.8188(3) 1.2893(2) 0.0335(6) Uani 1 d . . C1A C 0.5922(4) 0.9857(3) 1.2026(3) 0.0332(7) Uani 1 d . . C2A C 0.6576(6) 1.0739(4) 1.1616(4) 0.0570(11) Uani 1 d . . C3A C 0.6211(7) 1.1881(5) 1.1843(5) 0.0698(14) Uani 1 d . . C4A C 0.5192(7) 1.2154(4) 1.2475(4) 0.0655(14) Uani 1 d . . C5A C 0.4526(8) 1.1301(5) 1.2887(4) 0.074(2) Uani 1 d . . C6A C 0.4910(7) 1.0164(5) 1.2682(4) 0.0611(12) Uani 1 d . . C1B C 0.7924(4) 0.8264(3) 1.1145(3) 0.0359(7) Uani 1 d . . C2B C 0.7863(6) 0.8304(5) 1.0120(4) 0.0507(10) Uani 1 d . . C3B C 0.9153(7) 0.8234(5) 0.9672(5) 0.0691(14) Uani 1 d . . C4B C 1.0483(7) 0.8083(6) 1.0242(6) 0.076(2) Uani 1 d . . C5B C 1.0538(7) 0.8003(6) 1.1227(6) 0.079(2) Uani 1 d . . C6B C 0.9278(5) 0.8105(5) 1.1703(4) 0.0523(10) Uani 1 d . . C1C C 0.7077(4) 0.7058(3) 1.4332(3) 0.0312(7) Uani 1 d . . C2C C 0.8408(5) 0.8227(4) 1.5025(3) 0.0468(9) Uani 1 d . . C3C C 0.9410(6) 0.8346(5) 1.6016(3) 0.0594(12) Uani 1 d . . C4C C 0.9068(6) 0.7292(6) 1.6304(4) 0.0651(13) Uani 1 d . . C5C C 0.7731(7) 0.6144(6) 1.5619(4) 0.0661(13) Uani 1 d . . C6C C 0.6732(5) 0.6023(4) 1.4642(3) 0.0486(9) Uani 1 d . . C1D C 0.3790(4) 0.6611(4) 1.3109(3) 0.0360(7) Uani 1 d . . C2D C 0.2406(5) 0.5543(5) 1.2328(4) 0.0506(10) Uani 1 d . . C3D C 0.0874(6) 0.5442(6) 1.2468(5) 0.0679(14) Uani 1 d . . C4D C 0.0711(7) 0.6390(7) 1.3384(6) 0.078(2) Uani 1 d . . C5D C 0.2066(8) 0.7463(7) 1.4168(6) 0.089(2) Uani 1 d . . C6D C 0.3612(6) 0.7591(5) 1.4033(4) 0.0615(12) Uani 1 d . . H2A H 0.7412(60) 1.0655(47) 1.1254(40) 0.074(15) Uiso 1 d . . H3A H 0.6645(78) 1.2496(66) 1.1601(53) 0.122(23) Uiso 1 d . . H4A H 0.4939(55) 1.2845(48) 1.2566(38) 0.067(14) Uiso 1 d . . H5A H 0.3758(61) 1.1403(51) 1.3266(43) 0.081(16) Uiso 1 d . . H6A H 0.4486(64) 0.9603(54) 1.2995(45) 0.090(17) Uiso 1 d . . H2B H 0.6973(54) 0.8308(43) 0.9779(36) 0.055(13) Uiso 1 d . . H3B H 0.9050(55) 0.8279(44) 0.9001(39) 0.064(14) Uiso 1 d . . H4B H 1.1358(64) 0.7988(51) 0.9918(43) 0.085(16) Uiso 1 d . . H5B H 1.1393(58) 0.7903(46) 1.1613(39) 0.064(14) Uiso 1 d . . H6B H 0.9249(53) 0.8079(44) 1.2334(37) 0.055(13) Uiso 1 d . . H2C H 0.8624(45) 0.8911(39) 1.4813(31) 0.042(11) Uiso 1 d . . H3C H 1.0282(54) 0.9152(46) 1.6470(37) 0.061(13) Uiso 1 d . . H4C H 0.9774(68) 0.7363(56) 1.6980(49) 0.102(19) Uiso 1 d . . H5C H 0.7568(67) 0.5489(55) 1.5769(46) 0.090(19) Uiso 1 d . . H6C H 0.5789(58) 0.5276(48) 1.4171(39) 0.069(14) Uiso 1 d . . H2D H 0.2483(48) 0.4887(41) 1.1724(34) 0.046(11) Uiso 1 d . . H3D H -0.0049(63) 0.4711(50) 1.1925(41) 0.075(16) Uiso 1 d . . H4D H -0.0421(93) 0.6266(73) 1.3489(62) 0.155(28) Uiso 1 d . . H5D H 0.1962(70) 0.8117(57) 1.4836(47) 0.098(19) Uiso 1 d . . H6D H 0.4521(56) 0.8294(46) 1.4526(39) 0.063(14) Uiso 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 0.0274(2) 0.0216(2) 0.0250(2) 0.00994(14) 0.00825(15) 0.01024(15) P1 0.0327(4) 0.0251(4) 0.0317(4) 0.0140(3) 0.0116(4) 0.0126(3) P2 0.0314(4) 0.0278(4) 0.0259(4) 0.0130(3) 0.0096(3) 0.0121(3) S1 0.0326(4) 0.0277(4) 0.0332(4) 0.0119(3) 0.0091(3) 0.0152(3) S2 0.0500(5) 0.0304(4) 0.0284(4) 0.0143(3) 0.0112(4) 0.0207(4) N1 0.040(2) 0.0259(13) 0.0307(14) 0.0127(11) 0.0073(12) 0.0088(12) C1A 0.040(2) 0.0250(14) 0.033(2) 0.0128(13) 0.0073(14) 0.0125(13) C2A 0.075(3) 0.046(2) 0.075(3) 0.040(2) 0.039(3) 0.030(2) C3A 0.100(4) 0.048(3) 0.089(4) 0.048(3) 0.038(3) 0.036(3) C4A 0.109(4) 0.039(2) 0.060(3) 0.024(2) 0.021(3) 0.045(3) C5A 0.117(5) 0.068(3) 0.074(3) 0.034(3) 0.056(3) 0.068(3) C6A 0.097(4) 0.051(2) 0.068(3) 0.037(2) 0.049(3) 0.046(3) C1B 0.034(2) 0.031(2) 0.044(2) 0.0162(15) 0.0160(15) 0.0121(14) C2B 0.045(2) 0.063(3) 0.052(2) 0.028(2) 0.025(2) 0.020(2) C3B 0.080(4) 0.077(3) 0.069(3) 0.039(3) 0.051(3) 0.029(3) C4B 0.065(3) 0.082(4) 0.106(4) 0.048(3) 0.056(3) 0.038(3) C5B 0.051(3) 0.091(4) 0.119(5) 0.054(4) 0.043(3) 0.042(3) C6B 0.044(2) 0.062(3) 0.069(3) 0.039(2) 0.026(2) 0.028(2) C1C 0.033(2) 0.038(2) 0.0270(15) 0.0146(13) 0.0110(13) 0.0167(14) C2C 0.047(2) 0.044(2) 0.037(2) 0.013(2) 0.004(2) 0.011(2) C3C 0.047(2) 0.069(3) 0.035(2) 0.009(2) -0.003(2) 0.012(2) C4C 0.068(3) 0.092(4) 0.043(2) 0.034(3) 0.009(2) 0.039(3) C5C 0.083(4) 0.076(3) 0.052(3) 0.043(3) 0.014(2) 0.030(3) C6C 0.052(2) 0.050(2) 0.041(2) 0.025(2) 0.006(2) 0.014(2) C1D 0.036(2) 0.045(2) 0.040(2) 0.026(2) 0.0164(15) 0.019(2) C2D 0.039(2) 0.056(3) 0.060(3) 0.030(2) 0.019(2) 0.014(2) C3D 0.037(2) 0.085(4) 0.087(4) 0.051(3) 0.017(3) 0.012(3) C4D 0.049(3) 0.117(5) 0.102(4) 0.066(4) 0.038(3) 0.043(3) C5D 0.075(4) 0.123(5) 0.089(4) 0.040(4) 0.053(3) 0.060(4) C6D 0.048(3) 0.076(3) 0.058(3) 0.019(2) 0.024(2) 0.030(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 S2 2.3333(8) . ? Pd1 S2 2.3333(8) 2_667 ? Pd1 S1 2.3478(8) 2_667 ? Pd1 S1 2.3478(8) . ? P1 N1 1.597(3) . ? P1 C1A 1.803(3) . ? P1 C1B 1.806(3) . ? P1 S1 2.0255(13) . ? P2 N1 1.595(3) . ? P2 C1C 1.807(3) . ? P2 C1D 1.809(3) . ? P2 S2 2.0258(11) . ? C1A C2A 1.374(5) . ? C1A C6A 1.378(5) . ? C2A C3A 1.372(6) . ? C3A C4A 1.355(7) . ? C4A C5A 1.354(7) . ? C5A C6A 1.379(6) . ? C1B C2B 1.377(5) . ? C1B C6B 1.386(5) . ? C2B C3B 1.384(6) . ? C3B C4B 1.371(8) . ? C4B C5B 1.344(8) . ? C5B C6B 1.385(6) . ? C1C C2C 1.377(5) . ? C1C C6C 1.382(5) . ? C2C C3C 1.390(6) . ? C3C C4C 1.383(7) . ? C4C C5C 1.366(7) . ? C5C C6C 1.372(6) . ? C1D C2D 1.374(6) . ? C1D C6D 1.389(6) . ? C2D C3D 1.380(6) . ? C3D C4D 1.358(8) . ? C4D C5D 1.363(9) . ? C5D C6D 1.387(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 S2 Pd1 S2 180.0 . 2_667 ? S2 Pd1 S1 81.29(3) . 2_667 ? S2 Pd1 S1 98.71(3) 2_667 2_667 ? S2 Pd1 S1 98.71(3) . . ? S2 Pd1 S1 81.29(3) 2_667 . ? S1 Pd1 S1 180.0 2_667 . ? N1 P1 C1A 106.94(15) . . ? N1 P1 C1B 109.9(2) . . ? C1A P1 C1B 109.6(2) . . ? N1 P1 S1 115.59(11) . . ? C1A P1 S1 105.90(12) . . ? C1B P1 S1 108.75(12) . . ? N1 P2 C1C 106.0(2) . . ? N1 P2 C1D 111.8(2) . . ? C1C P2 C1D 105.26(15) . . ? N1 P2 S2 117.27(11) . . ? C1C P2 S2 105.15(11) . . ? C1D P2 S2 110.33(13) . . ? P1 S1 Pd1 99.34(4) . . ? P2 S2 Pd1 109.33(4) . . ? P2 N1 P1 122.2(2) . . ? C2A C1A C6A 118.0(3) . . ? C2A C1A P1 124.6(3) . . ? C6A C1A P1 117.3(3) . . ? C3A C2A C1A 120.7(4) . . ? C4A C3A C2A 120.4(4) . . ? C5A C4A C3A 120.2(4) . . ? C4A C5A C6A 119.9(5) . . ? C1A C6A C5A 120.8(4) . . ? C2B C1B C6B 118.7(4) . . ? C2B C1B P1 121.5(3) . . ? C6B C1B P1 119.6(3) . . ? C1B C2B C3B 120.8(5) . . ? C4B C3B C2B 119.4(5) . . ? C5B C4B C3B 120.5(5) . . ? C4B C5B C6B 120.9(5) . . ? C5B C6B C1B 119.7(5) . . ? C2C C1C C6C 119.5(3) . . ? C2C C1C P2 120.6(3) . . ? C6C C1C P2 119.8(3) . . ? C1C C2C C3C 119.9(4) . . ? C4C C3C C2C 120.0(4) . . ? C5C C4C C3C 119.7(4) . . ? C4C C5C C6C 120.6(5) . . ? C5C C6C C1C 120.4(4) . . ? C2D C1D C6D 118.6(4) . . ? C2D C1D P2 123.6(3) . . ? C6D C1D P2 117.7(3) . . ? C1D C2D C3D 120.5(5) . . ? C4D C3D C2D 120.6(5) . . ? C3D C4D C5D 119.9(5) . . ? C4D C5D C6D 120.3(5) . . ? C5D C6D C1D 120.0(5) . . ? _refine_diff_density_max 0.619 _refine_diff_density_min -0.416 _refine_diff_density_rms 0.075 #============================================================================== # End of Crystallographic Information File