# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 1145/210 data_vkj84 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H32 Pd2 S2' _chemical_formula_weight 501.34 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' 'S' 'S' 0.1246 0.1234 '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' _symmetry_cell_setting ORTHORHOMBIC _symmetry_space_group_name_H-M C221 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, -z' '-x, -y, z+1/2' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, -z' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' _cell_length_a 12.369(3) _cell_length_b 13.674(2) _cell_length_c 12.3800(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2093.8(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12 _cell_measurement_theta_max 15 _exptl_crystal_description PLATE _exptl_crystal_colour YELLOW _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.590 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1008 _exptl_absorpt_coefficient_mu 1.908 _exptl_absorpt_correction_type 'PSI SCAN' _exptl_absorpt_correction_T_min 0.85 _exptl_absorpt_correction_T_max 0.99 _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 'CAD4 DIFFRACTOMETER' _diffrn_measurement_method 'OMEGA TWOTHETA' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '1 HOUR' _diffrn_standards_decay_% 1 _diffrn_reflns_number 2053 _diffrn_reflns_av_R_equivalents 0.0173 _diffrn_reflns_av_sigmaI/netI 0.0100 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 24.97 _reflns_number_total 1845 _reflns_number_gt 1697 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 PROGRAMS' _computing_cell_refinement 'CAD4 PROGRAMS' _computing_data_reduction MOLEN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _computing_publication_material 'SHELXL-97 (Sheldrick,1997)' _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 w=1/[\s^2^(Fo^2^)+(0.0140P)^2^+3.7750P] 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 0.00174(10) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.33(17) _refine_ls_number_reflns 1845 _refine_ls_number_parameters 108 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0213 _refine_ls_R_factor_gt 0.0184 _refine_ls_wR_factor_ref 0.0470 _refine_ls_wR_factor_gt 0.0448 _refine_ls_goodness_of_fit_ref 1.189 _refine_ls_restrained_S_all 1.189 _refine_ls_shift/su_max 0.583 _refine_ls_shift/su_mean 0.107 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd 0.115029(16) -0.00028(5) 0.372993(16) 0.03937(10) Uani 1 d . . . S1 S 0.03939(6) 0.10853(5) 0.5003(2) 0.04239(17) Uani 1 d . . . C1 C 0.0950(3) 0.2341(3) 0.5057(12) 0.0516(11) Uani 1 d . . . C2 C 0.0551(10) 0.2853(6) 0.3959(8) 0.067(3) Uani 1 d . . . H2A H 0.0882 0.2534 0.3352 0.101 Uiso 1 calc R . . H2B H 0.0755 0.3531 0.3965 0.101 Uiso 1 calc R . . H2C H -0.0221 0.2801 0.3903 0.101 Uiso 1 calc R . . C3 C 0.2186(3) 0.2337(3) 0.5014(14) 0.0648(11) Uani 1 d . . . H3A H 0.2421 0.1994 0.4380 0.097 Uiso 1 calc R . . H3B H 0.2466 0.2017 0.5645 0.097 Uiso 1 calc R . . H3C H 0.2446 0.2998 0.4990 0.097 Uiso 1 calc R . . C4 C 0.0482(13) 0.2835(6) 0.5970(9) 0.080(3) Uani 1 d . . . H4A H -0.0292 0.2790 0.5933 0.120 Uiso 1 calc R . . H4B H 0.0693 0.3511 0.5961 0.120 Uiso 1 calc R . . H4C H 0.0731 0.2535 0.6625 0.120 Uiso 1 calc R . . C5 C 0.2383(3) 0.0037(9) 0.2517(2) 0.0481(8) Uani 1 d . . . C6 C 0.3531(3) 0.0041(9) 0.2928(3) 0.0697(14) Uani 1 d . . . H6A H 0.3807 -0.0615 0.2931 0.104 Uiso 1 calc R . . H6B H 0.3546 0.0299 0.3649 0.104 Uiso 1 calc R . . H6C H 0.3969 0.0441 0.2466 0.104 Uiso 1 calc R . . C7 C 0.1832(10) 0.0884(6) 0.2453(8) 0.051(2) Uani 1 d . . . C8 C 0.1747(13) -0.0846(8) 0.2390(10) 0.062(3) Uani 1 d . . . H7A H 0.108(3) 0.090(3) 0.191(3) 0.023(10) Uiso 1 d . . . H7B H 0.213(4) 0.153(3) 0.253(4) 0.021(11) Uiso 1 d . . . H8A H 0.151(8) -0.087(7) 0.199(6) 0.11(4) Uiso 1 d . . . H8B H 0.214(8) -0.128(6) 0.269(7) 0.10(4) 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 Pd 0.03559(13) 0.04545(14) 0.03706(14) -0.0002(4) -0.00010(8) 0.0009(5) S1 0.0377(3) 0.0443(4) 0.0452(4) -0.0002(13) 0.0050(17) 0.0050(3) C1 0.0557(18) 0.0434(16) 0.056(3) 0.009(5) -0.011(5) 0.0036(14) C2 0.069(6) 0.063(5) 0.069(6) 0.024(4) -0.008(4) 0.022(5) C3 0.059(2) 0.062(2) 0.073(2) 0.001(7) 0.023(6) -0.0123(18) C4 0.096(8) 0.048(4) 0.096(8) -0.012(5) -0.003(6) -0.001(5) C5 0.0441(16) 0.060(2) 0.0399(14) -0.004(6) 0.0082(12) -0.003(8) C6 0.0435(17) 0.075(3) 0.091(3) 0.027(6) 0.0050(18) 0.001(6) C7 0.042(4) 0.070(5) 0.043(4) 0.014(4) 0.006(4) -0.003(4) C8 0.072(8) 0.065(5) 0.048(5) -0.009(5) 0.004(5) 0.000(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 Pd C5 2.140(3) . ? Pd C8 2.150(11) . ? Pd C7 2.163(9) . ? Pd S1 2.351(2) 2_556 ? Pd S1 2.361(2) . ? Pd Pd 3.1447(6) 2_556 ? S1 C1 1.851(4) . ? S1 Pd 2.351(2) 2_556 ? C1 C4 1.439(16) . ? C1 C3 1.529(5) . ? C1 C2 1.607(14) . ? C5 C7 1.345(13) . ? C5 C8 1.449(15) . ? C5 C6 1.508(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 Pd C8 39.5(4) . . ? C5 Pd C7 36.4(4) . . ? C8 Pd C7 66.6(2) . . ? C5 Pd S1 140.1(3) . 2_556 ? C8 Pd S1 108.3(3) . 2_556 ? C7 Pd S1 174.6(3) . 2_556 ? C5 Pd S1 137.3(3) . . ? C8 Pd S1 171.4(4) . . ? C7 Pd S1 106.8(3) . . ? S1 Pd S1 78.09(3) 2_556 . ? C5 Pd Pd 134.54(9) . 2_556 ? C8 Pd Pd 140.6(4) . 2_556 ? C7 Pd Pd 136.8(3) . 2_556 ? S1 Pd Pd 48.26(5) 2_556 2_556 ? S1 Pd Pd 48.00(5) . 2_556 ? C1 S1 Pd 114.3(3) . 2_556 ? C1 S1 Pd 117.5(4) . . ? Pd S1 Pd 83.74(3) 2_556 . ? C4 C1 C3 115.6(10) . . ? C4 C1 C2 109.6(3) . . ? C3 C1 C2 106.2(10) . . ? C4 C1 S1 108.3(7) . . ? C3 C1 S1 111.6(3) . . ? C2 C1 S1 105.0(7) . . ? C7 C5 C8 115.8(5) . . ? C7 C5 C6 119.6(12) . . ? C8 C5 C6 123.4(13) . . ? C7 C5 Pd 72.7(5) . . ? C8 C5 Pd 70.6(5) . . ? C6 C5 Pd 115.7(2) . . ? C5 C7 Pd 70.9(4) . . ? C5 C8 Pd 69.9(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 Pd S1 C1 -0.4(4) . . . . ? C8 Pd S1 C1 -64(2) . . . . ? C7 Pd S1 C1 -24.7(5) . . . . ? S1 Pd S1 C1 157.7(4) 2_556 . . . ? Pd Pd S1 C1 114.2(3) 2_556 . . . ? C5 Pd S1 Pd -114.6(2) . . . 2_556 ? C8 Pd S1 Pd -178(2) . . . 2_556 ? C7 Pd S1 Pd -138.9(3) . . . 2_556 ? S1 Pd S1 Pd 43.48(5) 2_556 . . 2_556 ? Pd S1 C1 C4 -76.8(7) 2_556 . . . ? Pd S1 C1 C4 -172.5(7) . . . . ? Pd S1 C1 C3 51.5(12) 2_556 . . . ? Pd S1 C1 C3 -44.3(12) . . . . ? Pd S1 C1 C2 166.1(5) 2_556 . . . ? Pd S1 C1 C2 70.3(5) . . . . ? C8 Pd C5 C7 126.4(5) . . . . ? S1 Pd C5 C7 173.2(5) 2_556 . . . ? S1 Pd C5 C7 -41.5(6) . . . . ? Pd Pd C5 C7 -113.0(6) 2_556 . . . ? C7 Pd C5 C8 -126.4(5) . . . . ? S1 Pd C5 C8 46.9(7) 2_556 . . . ? S1 Pd C5 C8 -167.9(6) . . . . ? Pd Pd C5 C8 120.7(7) 2_556 . . . ? C8 Pd C5 C6 -118.6(14) . . . . ? C7 Pd C5 C6 115.1(14) . . . . ? S1 Pd C5 C6 -71.7(12) 2_556 . . . ? S1 Pd C5 C6 73.5(12) . . . . ? Pd Pd C5 C6 2.1(14) 2_556 . . . ? C8 C5 C7 Pd 57.6(4) . . . . ? C6 C5 C7 Pd -110.2(4) . . . . ? C8 Pd C7 C5 -33.9(4) . . . . ? S1 Pd C7 C5 -53(4) 2_556 . . . ? S1 Pd C7 C5 152.0(4) . . . . ? Pd Pd C7 C5 106.4(4) 2_556 . . . ? C7 C5 C8 Pd -58.7(4) . . . . ? C6 C5 C8 Pd 108.6(5) . . . . ? C7 Pd C8 C5 31.4(4) . . . . ? S1 Pd C8 C5 -150.5(5) 2_556 . . . ? S1 Pd C8 C5 72(3) . . . . ? Pd Pd C8 C5 -105.1(5) 2_556 . . . ? _diffrn_measured_fraction_theta_max 0.499 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 0.499 _refine_diff_density_max 0.668 _refine_diff_density_min -0.253 _refine_diff_density_rms 0.048