Supplementary Material (ESI) for Journal of Materials Chemistry This journal is (c) The Royal Society of Chemistry 2003 data_global _publ_contact_author_email SEEBER@UNIMORE.IT _publ_contact_author_name 'Dr Renato Seeber' _journal_name_full J.Mater.Chem. _journal_coden_Cambridge 1145 _publ_section_references ; Sheldrick, G.M. (1985). SHELXS86. Program for the solution of crystal structures. Univ. of Gottingen, Federal Republic of Germany. ; loop_ _publ_author_name R.Seeber M.Manassero A.Mucci F.Parenti L.Pigani M.I.Pilo ; N.Spano ; C.Zanardi data_compound_PdBSBT _database_code_CSD 204554 _audit_creation_method 'from The Personal SDP version 2.1.1' _chemical_formula_sum 'C16 H22 Cl2 Pd S4' _chemical_formula_weight 519.92 _computing_data_collection 'SMART (Bruker)' _computing_cell_refinement 'SMART (Bruker)' _computing_data_reduction 'SAINT (Bruker)' _computing_structure_solution ; SHELXS-86 (Sheldrick, 1986) as implemented in The Personal SDP ; _computing_structure_refinement ; Full-matrix least-squares (The Personal SDP, 1991) ; _computing_molecular_graphics 'The Personal SDP (1991)' _computing_publication_material 'The Personal SDP (1991)' _cell_length_a 11.937(1) _cell_length_b 10.530(1) _cell_length_c 16.956(2) _cell_angle_alpha 90 _cell_angle_beta 90.32(1) _cell_angle_gamma 90 _cell_volume 2131.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 296 _cell_measurement_reflns_used 79 _cell_measurement_theta_min 3 _cell_measurement_theta_max 23 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 2(1)/n' loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z 1/2+x,1/2-y,1/2+z -x,-y,-z 1/2-x,1/2+y,1/2-z _exptl_crystal_description prism _exptl_crystal_colour orange-red _exptl_crystal_size_max 0.360 _exptl_crystal_size_mid 0.270 _exptl_crystal_size_min 0.250 _exptl_crystal_density_diffrn 1.620 _exptl_crystal_F_000 1048 _exptl_absorpt_coefficient_mu 1.486 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details ; SADABS ; _exptl_absorpt_correction_T_min 0.901 _exptl_absorpt_correction_T_max 1.000 _diffrn_ambient_temperature 296 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'SMART CCD area detector' _diffrn_measurement_device 'SMART (Bruker)' _diffrn_measurement_method omega _diffrn_standards_number 213 _diffrn_standards_decay_% 0.00 _diffrn_reflns_number_total 24753 _diffrn_reflns_number_independent 6458 _diffrn_reflns_av_r_eqivalents 0.0197 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 26.00 _total_number_of_frames 2450 _time_per_frame_seconds 25 _frame_width_degrees 0.30 _detector_sample_distance_cm 5.00 _diffrn_reflns_reduction_process SAINT loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source PD 0 4 -1.177 1.0070 'International Tables Vol IV Table 2.2A' CL 0 8 0.1320 0.1590 'International Tables Vol IV Table 2.2A' S 0 16 0.1100 0.1240 'International Tables Vol IV Table 2.2A' C 0 64 0.0020 0.0020 'International Tables Vol IV Table 2.2A' H 0 88 0.0000 0.0000 'International Tables Vol IV Table 2.2A' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_type_symbol PD 0.60579(1) 0.50212(1) 0.069785(8) 1.00 0.03356(5) Uani PD CL1 0.74319(4) 0.38282(5) 0.00770(3) 1.00 0.0540(2) Uani CL CL2 0.51326(5) 0.31997(4) 0.10547(4) 1.00 0.0614(2) Uani CL S1 0.47937(4) 0.63199(4) 0.13051(3) 1.00 0.0355(2) Uani S S2 0.71428(4) 0.67273(5) 0.03082(3) 1.00 0.0549(2) Uani S S3 0.69163(5) 0.83611(6) 0.28661(4) 1.00 0.0513(2) Uani S S4 0.60388(5) 1.02921(5) 0.12609(4) 1.00 0.0542(2) Uani S C1 0.5597(2) 0.6888(2) 0.2110(1) 1.00 0.0397(7) Uani C C2 0.6213(2) 0.7969(2) 0.2011(1) 1.00 0.0391(7) Uani C C3 0.6369(2) 0.7091(3) 0.3349(1) 1.00 0.065(1) Uani C C4 0.5699(2) 0.6367(2) 0.2883(1) 1.00 0.0573(9) Uani C C5 0.6320(2) 0.8696(2) 0.1283(1) 1.00 0.0405(7) Uani C C6 0.6628(2) 0.8267(2) 0.0550(1) 1.00 0.0455(7) Uani C C7 0.6632(2) 0.9247(2) -0.0023(1) 1.00 0.0605(9) Uani C C8 0.6342(2) 1.0389(2) 0.0282(2) 1.00 0.067(1) Uani C C9 0.3687(2) 0.5425(2) 0.1788(1) 1.00 0.0495(8) Uani C C10 0.2838(2) 0.6292(3) 0.2159(1) 1.00 0.071(1) Uani C C11 0.1871(3) 0.5527(4) 0.2534(2) 1.00 0.123(2) Uani C C12 0.1236(3) 0.4738(4) 0.1940(3) 1.00 0.142(2) Uani C C13 0.8323(2) 0.6601(2) 0.1011(2) 1.00 0.075(1) Uani C C14A 0.9115(4) 0.7668(4) 0.1200(3) 0.50 0.056(2) Uani C C14B 0.9199(4) 0.7758(5) 0.0553(4) 0.50 0.077(3) Uani C C15A 0.9835(4) 0.7819(5) 0.0451(4) 0.50 0.084(2) Uani C C15B 1.0171(5) 0.7861(6) 0.1151(5) 0.50 0.096(4) Uani C C16 1.0876(3) 0.8861(3) 0.0734(2) 1.00 0.121(2) Uani C H1 0.6520 0.6904 0.3899 1.00 0.0765 Uiso H H2 0.5336 0.5592 0.3054 1.00 0.0627 Uiso H H3 0.6821 0.9114 -0.0573 1.00 0.0608 Uiso H H4 0.6311 1.1169 -0.0021 1.00 0.0664 Uiso H H5 0.4017 0.4894 0.2194 1.00 0.0536 Uiso H H6 0.3313 0.4894 0.1400 1.00 0.0536 Uiso H H7 0.2532 0.6851 0.1757 1.00 0.0739 Uiso H H8 0.3203 0.6795 0.2565 1.00 0.0739 Uiso H H9 0.1354 0.6116 0.2778 1.00 0.1131 Uiso H H10 0.2182 0.4967 0.2933 1.00 0.1131 Uiso H H11 0.0642 0.4279 0.2203 1.00 0.1451 Uiso H H12 0.0916 0.5289 0.1540 1.00 0.1451 Uiso H H13 0.1743 0.4139 0.1694 1.00 0.1451 Uiso H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol PD 0.03949(7) 0.02584(5) 0.03765(6) 0.00192(5) -0.00282(5) -0.00143(5) PD CL1 0.0562(3) 0.0425(2) 0.0531(2) 0.0151(2) 0.0011(2) -0.0061(2) CL CL2 0.0649(3) 0.0279(2) 0.0826(3) -0.0030(2) 0.0081(3) 0.0036(2) CL S1 0.0379(2) 0.0316(2) 0.0400(2) -0.0011(2) -0.0003(2) -0.0015(2) S S2 0.0462(2) 0.0323(2) 0.0692(3) 0.0008(2) 0.0158(2) 0.0004(2) S S3 0.0707(4) 0.0602(3) 0.0684(3) 0.0013(3) -0.0279(3) -0.0189(3) S S4 0.0570(3) 0.0282(2) 0.0830(4) 0.0002(2) -0.0007(3) -0.0050(2) S C1 0.044(1) 0.0375(9) 0.0411(8) 0.0057(8) -0.0039(8) -0.0055(7) C C2 0.044(1) 0.0381(9) 0.0489(9) 0.0040(8) -0.0085(8) -0.0092(8) C C3 0.088(2) 0.073(2) 0.048(1) 0.008(1) -0.020(1) -0.002(1) C C4 0.070(1) 0.054(1) 0.046(1) 0.004(1) -0.007(1) 0.004(1) C C5 0.039(1) 0.0272(8) 0.065(1) -0.0020(8) -0.0040(9) -0.0036(8) C C6 0.0393(9) 0.0292(8) 0.064(1) -0.0025(8) 0.0035(9) 0.0029(8) C C7 0.053(1) 0.042(1) 0.072(1) -0.005(1) 0.011(1) 0.010(1) C C8 0.053(1) 0.0344(9) 0.094(2) -0.002(1) 0.006(1) 0.014(1) C C9 0.045(1) 0.048(1) 0.053(1) -0.0054(9) 0.0065(9) 0.0012(9) C C10 0.055(1) 0.072(2) 0.075(1) 0.002(1) 0.018(1) -0.009(1) C C11 0.066(2) 0.144(3) 0.099(2) 0.008(2) 0.035(1) 0.016(2) C C12 0.074(2) 0.133(3) 0.188(4) -0.034(2) 0.027(2) 0.037(3) C C13 0.037(1) 0.048(1) 0.178(3) 0.001(1) -0.024(2) -0.017(2) C C14A 0.040(2) 0.052(2) 0.084(3) -0.003(2) 0.002(2) -0.007(2) C C14B 0.044(3) 0.075(3) 0.124(4) -0.017(2) -0.007(3) 0.012(3) C C15A 0.045(2) 0.067(3) 0.139(4) -0.018(2) 0.042(2) -0.023(3) C C15B 0.067(3) 0.075(4) 0.210(7) -0.015(3) -0.042(4) -0.005(5) C C16 0.087(2) 0.077(2) 0.191(3) -0.025(2) 0.060(2) -0.027(2) C _refine_special_details ; weight = (4*F~o~^2^)/[\s^2^(F~o~^2^)] (refinement on F^2^) \s(F~o~^2^) = [\s^2^(F~o~^2^) + (P*F~o~^2^)^2^]^(1/2)^ P = 0.0400 ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 6458 _refine_ls_number_parameters 226 _refine_ls_number_constraints 0 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.046 _refine_ls_R_factor_obs 0.046 _refine_ls_wR_factor_obs 0.071 _refine_ls_shift/esd_max 0.024 _refine_ls_shift/esd_mean 0.003 _refine_ls_goodness_of_fit_all 1.021 _refine_ls_goodness_of_fit_obs 1.021 _refine_diff_density_max 0.680 _refine_diff_density_min -.450 _refine_diff_density_esd 0.126 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag PD CL1 2.323(1) 1_555 1_555 yes PD CL2 2.296(1) 1_555 1_555 yes PD S1 2.286(1) 1_555 1_555 yes PD S2 2.313(1) 1_555 1_555 yes S1 C1 1.768(2) 1_555 1_555 yes S1 C9 1.821(2) 1_555 1_555 yes S2 C6 1.783(2) 1_555 1_555 yes S2 C13 1.845(3) 1_555 1_555 yes S3 C2 1.721(2) 1_555 1_555 yes S3 C3 1.700(3) 1_555 1_555 yes S4 C5 1.714(2) 1_555 1_555 yes S4 C8 1.703(3) 1_555 1_555 yes C1 C2 1.367(3) 1_555 1_555 yes C1 C4 1.424(3) 1_555 1_555 yes C2 C5 1.459(3) 1_555 1_555 yes C3 C4 1.355(3) 1_555 1_555 yes C3 H1 0.970 1_555 1_555 yes C4 H2 0.970 1_555 1_555 yes C5 C6 1.373(3) 1_555 1_555 yes C6 C7 1.418(3) 1_555 1_555 yes C7 C8 1.355(3) 1_555 1_555 yes C7 H3 0.970 1_555 1_555 yes C8 H4 0.970 1_555 1_555 yes C9 C10 1.505(3) 1_555 1_555 yes C9 H5 0.970 1_555 1_555 yes C9 H6 0.970 1_555 1_555 yes C10 C11 1.548(4) 1_555 1_555 yes C10 H7 0.970 1_555 1_555 yes C10 H8 0.970 1_555 1_555 yes C11 C12 1.506(6) 1_555 1_555 yes C11 H9 0.970 1_555 1_555 yes C11 H10 0.970 1_555 1_555 yes C12 H11 0.970 1_555 1_555 yes C12 H12 0.970 1_555 1_555 yes C12 H13 0.970 1_555 1_555 yes C13 C14A 1.502(5) 1_555 1_555 yes C13 C14B 1.786(6) 1_555 1_555 yes C14A C14B 1.106(8) 1_555 1_555 yes C14A C15A 1.546(7) 1_555 1_555 yes C14A C15B 1.280(8) 1_555 1_555 yes C14B C15A 0.783(7) 1_555 1_555 yes C14B C15B 1.540(10) 1_555 1_555 yes C15A C15B 1.252(11) 1_555 1_555 yes C15A C16 1.724(6) 1_555 1_555 yes C15B C16 1.524(8) 1_555 1_555 yes 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag CL1 PD CL2 90.55(2) 1_555 1_555 1_555 yes CL1 PD S1 175.78(2) 1_555 1_555 1_555 yes CL1 PD S2 83.84(2) 1_555 1_555 1_555 yes CL2 PD S1 93.51(2) 1_555 1_555 1_555 yes CL2 PD S2 174.22(2) 1_555 1_555 1_555 yes S1 PD S2 92.07(2) 1_555 1_555 1_555 yes PD S1 C1 101.2(1) 1_555 1_555 1_555 yes PD S1 C9 112.0(1) 1_555 1_555 1_555 yes C1 S1 C9 102.7(1) 1_555 1_555 1_555 yes PD S2 C6 116.5(1) 1_555 1_555 1_555 yes PD S2 C13 100.7(1) 1_555 1_555 1_555 yes C6 S2 C13 100.4(1) 1_555 1_555 1_555 yes C2 S3 C3 91.7(1) 1_555 1_555 1_555 yes C5 S4 C8 92.1(1) 1_555 1_555 1_555 yes S1 C1 C2 118.5(1) 1_555 1_555 1_555 yes S1 C1 C4 128.6(2) 1_555 1_555 1_555 yes C2 C1 C4 113.0(2) 1_555 1_555 1_555 yes S3 C2 C1 110.9(1) 1_555 1_555 1_555 yes S3 C2 C5 122.9(1) 1_555 1_555 1_555 yes C1 C2 C5 126.2(2) 1_555 1_555 1_555 yes S3 C3 C4 112.9(2) 1_555 1_555 1_555 yes S3 C3 H1 123.6 1_555 1_555 1_555 yes C4 C3 H1 123.6 1_555 1_555 1_555 yes C1 C4 C3 111.5(2) 1_555 1_555 1_555 yes C1 C4 H2 124.2 1_555 1_555 1_555 yes C3 C4 H2 124.2 1_555 1_555 1_555 yes S4 C5 C2 121.0(1) 1_555 1_555 1_555 yes S4 C5 C6 110.8(1) 1_555 1_555 1_555 yes C2 C5 C6 128.2(2) 1_555 1_555 1_555 yes S2 C6 C5 127.0(2) 1_555 1_555 1_555 yes S2 C6 C7 120.1(2) 1_555 1_555 1_555 yes C5 C6 C7 112.6(2) 1_555 1_555 1_555 yes C6 C7 C8 112.4(2) 1_555 1_555 1_555 yes C6 C7 H3 123.8 1_555 1_555 1_555 yes C8 C7 H3 123.8 1_555 1_555 1_555 yes S4 C8 C7 112.1(2) 1_555 1_555 1_555 yes S4 C8 H4 124.0 1_555 1_555 1_555 yes C7 C8 H4 124.0 1_555 1_555 1_555 yes S1 C9 C10 111.5(2) 1_555 1_555 1_555 yes S1 C9 H5 109.0 1_555 1_555 1_555 yes S1 C9 H6 109.0 1_555 1_555 1_555 yes C10 C9 H5 109.0 1_555 1_555 1_555 yes C10 C9 H6 109.0 1_555 1_555 1_555 yes H5 C9 H6 109.5 1_555 1_555 1_555 yes C9 C10 C11 111.2(2) 1_555 1_555 1_555 yes C9 C10 H7 109.0 1_555 1_555 1_555 yes C9 C10 H8 109.0 1_555 1_555 1_555 yes C11 C10 H7 109.0 1_555 1_555 1_555 yes C11 C10 H8 109.0 1_555 1_555 1_555 yes H7 C10 H8 109.5 1_555 1_555 1_555 yes C10 C11 C12 112.7(3) 1_555 1_555 1_555 yes C10 C11 H9 108.7 1_555 1_555 1_555 yes C10 C11 H10 108.7 1_555 1_555 1_555 yes C12 C11 H9 108.7 1_555 1_555 1_555 yes C12 C11 H10 108.7 1_555 1_555 1_555 yes H9 C11 H10 109.5 1_555 1_555 1_555 yes C11 C12 H11 109.5 1_555 1_555 1_555 yes C11 C12 H12 109.5 1_555 1_555 1_555 yes C11 C12 H13 109.5 1_555 1_555 1_555 yes H11 C12 H12 109.5 1_555 1_555 1_555 yes H11 C12 H13 109.5 1_555 1_555 1_555 yes H12 C12 H13 109.5 1_555 1_555 1_555 yes S2 C13 C14A 124.2(3) 1_555 1_555 1_555 yes S2 C13 C14B 96.7(2) 1_555 1_555 1_555 yes C14A C13 C14B 38.1(3) 1_555 1_555 1_555 yes C13 C14A C14B 85.0(4) 1_555 1_555 1_555 yes C13 C14A C15A 104.7(4) 1_555 1_555 1_555 yes C13 C14A C15B 136.4(5) 1_555 1_555 1_555 yes C14B C14A C15A 28.7(3) 1_555 1_555 1_555 yes C14B C14A C15B 80.0(6) 1_555 1_555 1_555 yes C15A C14A C15B 51.5(5) 1_555 1_555 1_555 yes C13 C14B C14A 56.9(4) 1_555 1_555 1_555 yes C13 C14B C15A 136.4(7) 1_555 1_555 1_555 yes C13 C14B C15B 101.7(4) 1_555 1_555 1_555 yes C14A C14B C15A 108.7(8) 1_555 1_555 1_555 yes C14A C14B C15B 54.9(5) 1_555 1_555 1_555 yes C15A C14B C15B 54.0(6) 1_555 1_555 1_555 yes C14A C15A C14B 42.7(6) 1_555 1_555 1_555 yes C14A C15A C15B 53.2(4) 1_555 1_555 1_555 yes C14A C15A C16 103.9(4) 1_555 1_555 1_555 yes C14B C15A C15B 95.7(8) 1_555 1_555 1_555 yes C14B C15A C16 133.6(7) 1_555 1_555 1_555 yes C15B C15A C16 59.1(4) 1_555 1_555 1_555 yes C14A C15B C14B 45.0(4) 1_555 1_555 1_555 yes C14A C15B C15A 75.3(5) 1_555 1_555 1_555 yes C14A C15B C16 133.3(6) 1_555 1_555 1_555 yes C14B C15B C15A 30.4(4) 1_555 1_555 1_555 yes C14B C15B C16 99.2(6) 1_555 1_555 1_555 yes C15A C15B C16 76.1(5) 1_555 1_555 1_555 yes C15A C16 C15B 44.8(4) 1_555 1_555 1_555 yes