# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 1145/172 data_Ptetdt _publ_requested_journal ' Journal of Materials Chemistry ' _publ_contact_author_name ' Gen-etsu Matsubayashi ' _publ_contact_author_address ; Department of Applied Chemistry Graduate School of Engineering Osaka University 1-16 Machikaneyama, Toyonaka Osaka 560-0043, Japan ; _publ_contact_author_email ' matsubayashi@ch.wani.osaka-u.ac.jp ' _publ_contact_author_fax ' +81-6-6850-5785 ' _publ_contact_author_phone ' +81-6-6850-5769 ' _publ_section_title ; Properties of Pt(II)-complexes with a sulfur-rich dithiolate ligand having long alkyl chains and of their oxidized species and X-ray crystal structure of [NBu^n^~4~]~2~[Pt{C~6~S~8~(C~10~H~21~)~2~}] ; _publ_section_exptl_refinement ; The structure of [NBu^n^~4~]~2~[Pt{C~6~S~8~(C~10~H~21~)~2~] was refined on F by full-matrix least-squares methods anisotropically for non- hydrogen atoms. Most hydrogen atoms having 1.2 times the temperature factors of the bonded carbon atoms were fixed at geometrically calculated positions. The terminal carbon atoms(C42 and C43) of one butyl group in the [NBu^n^~4~]^+^ cation are disordered having an occupancy factor of 0.5. The positions of the hydrogen atoms bonded to C41, C42 and C43 were not calculated geometrically. The final R and R~w~ values were 0.039 and 0.043 respectively. The function minimized was \Sw(|F~o~|-|F~c~|)^2^, with w=(\s^2^(F~o~)+0.0001F~o~^2^)^-1^. ; _audit_creation_date 'May 17 1999' _audit_creation_method 'from TEXRAY.INF file' _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution SHELXS86 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 1902.22 _chemical_formula_analytical ? _chemical_formula_sum 'C84 H156 N2 Pt S16 ' _chemical_formula_moiety ' C16 H36 N 1+, C16 H36 N 1+, C52 H84 Pt S16 2- ' _chemical_formula_structural ? _chemical_melting_point ? _cell_length_a 12.416(2) _cell_length_b 22.881(4) _cell_length_c 9.315(2) _cell_angle_alpha 99.93(2) _cell_angle_beta 101.19(2) _cell_angle_gamma 83.39(1) _cell_volume 2548.0(7) _cell_formula_units_Z 1 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 23 _cell_measurement_theta_min 11.4 _cell_measurement_theta_max 11.5 _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'purple' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.240 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1008 _exptl_absorpt_coefficient_mu 1.738 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.544 _exptl_absorpt_correction_T_max 0.840 _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC5R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -7.41 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 3 -1 -1 2 1 -2 2 -1 -2 _diffrn_reflns_number 12199 _reflns_number_total 11662 _reflns_number_gt 6598 _reflns_threshold_expression I>3\s(I) _diffrn_reflns_av_R_equivalents 0.027 _diffrn_reflns_av_sigmaI/netI 0.093 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 27.51 _diffrn_reflns_reduction_process 'Lp corrections applied' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Pt' 'Pt' -1.703 8.390 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 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_calc_attached_atom Pt1 Pt 0.5000 0.0000 0.0000 0.05395(8) Uani 1.00 d . S1 S 0.3974(1) 0.08333(6) -0.0774(1) 0.0671(4) Uani 1.00 d . S2 S 0.4002(1) 0.00508(6) 0.1875(1) 0.0666(4) Uani 1.00 d . S3 S 0.1998(1) 0.15615(6) 0.0255(1) 0.0719(4) Uani 1.00 d . S4 S 0.1988(1) 0.08491(6) 0.2591(1) 0.0693(4) Uani 1.00 d . S5 S 0.0116(1) 0.25131(6) 0.1550(1) 0.0761(4) Uani 1.00 d . S6 S 0.0146(1) 0.18212(6) 0.3926(1) 0.0704(4) Uani 1.00 d . S7 S -0.1116(1) 0.35839(6) 0.3008(2) 0.0921(5) Uani 1.00 d . S8 S -0.1131(1) 0.27998(6) 0.5673(1) 0.0803(5) Uani 1.00 d . N1 N -0.3126(3) 0.1127(2) 0.4661(4) 0.061(1) Uani 1.00 d . C1 C 0.3041(3) 0.0982(2) 0.0463(5) 0.061(1) Uani 1.00 d . C2 C 0.3054(3) 0.0658(2) 0.1541(4) 0.057(1) Uani 1.00 d . C3 C 0.1477(4) 0.1498(2) 0.1842(5) 0.062(1) Uani 1.00 d . C4 C 0.0724(4) 0.1895(2) 0.2388(5) 0.064(1) Uani 1.00 d . C5 C -0.0427(4) 0.2884(2) 0.3115(5) 0.065(1) Uani 1.00 d . C6 C -0.0419(3) 0.2558(2) 0.4193(5) 0.064(1) Uani 1.00 d . C7 C -0.0046(5) 0.4004(2) 0.2745(6) 0.089(2) Uani 1.00 d . C8 C 0.0788(5) 0.4191(2) 0.4112(6) 0.091(2) Uani 1.00 d . C9 C 0.1535(5) 0.4634(3) 0.3852(6) 0.098(2) Uani 1.00 d . C10 C 0.2364(5) 0.4864(3) 0.5175(7) 0.098(2) Uani 1.00 d . C11 C 0.3032(5) 0.5314(3) 0.4849(7) 0.101(2) Uani 1.00 d . C12 C 0.3878(5) 0.5563(3) 0.6124(7) 0.109(2) Uani 1.00 d . C13 C 0.4491(6) 0.6039(3) 0.5719(8) 0.119(3) Uani 1.00 d . C14 C 0.5366(6) 0.6299(3) 0.6882(8) 0.130(3) Uani 1.00 d . C15 C 0.5936(7) 0.6779(3) 0.639(1) 0.164(4) Uani 1.00 d . C16 C 0.6821(8) 0.7042(4) 0.750(1) 0.215(5) Uani 1.00 d . C17 C -0.0130(5) 0.2588(3) 0.7223(6) 0.101(2) Uani 1.00 d . C18 C 0.0855(6) 0.2930(3) 0.7625(7) 0.112(2) Uani 1.00 d . C19 C 0.0673(6) 0.3561(3) 0.8197(7) 0.119(2) Uani 1.00 d . C20 C 0.1767(7) 0.3862(4) 0.8680(8) 0.143(3) Uani 1.00 d . C21 C 0.1641(7) 0.4492(4) 0.9266(8) 0.154(3) Uani 1.00 d . C22 C 0.2722(8) 0.4788(4) 0.9747(8) 0.163(3) Uani 1.00 d . C23 C 0.2582(8) 0.5430(4) 1.0317(9) 0.173(4) Uani 1.00 d . C24 C 0.3652(8) 0.5731(4) 1.0818(8) 0.169(4) Uani 1.00 d . C25 C 0.341(1) 0.6405(5) 1.136(1) 0.266(6) Uani 1.00 d . C26 C 0.452(1) 0.6650(7) 1.185(1) 0.362(9) Uani 1.00 d . C27 C -0.4269(4) 0.1073(2) 0.4967(5) 0.074(1) Uani 1.00 d . C28 C -0.4834(4) 0.1627(3) 0.5707(6) 0.095(2) Uani 1.00 d . C29 C -0.5972(5) 0.1524(3) 0.5829(7) 0.114(2) Uani 1.00 d . C30 C -0.6622(6) 0.2045(4) 0.6550(10) 0.154(3) Uani 1.00 d . C31 C -0.2749(4) 0.0510(2) 0.3897(5) 0.066(1) Uani 1.00 d . C32 C -0.1583(4) 0.0460(2) 0.3555(5) 0.080(2) Uani 1.00 d . C33 C -0.1271(4) -0.0168(3) 0.2756(5) 0.084(2) Uani 1.00 d . C34 C -0.1283(5) -0.0654(3) 0.3627(6) 0.093(2) Uani 1.00 d . C35 C -0.2331(3) 0.1319(2) 0.6078(4) 0.063(1) Uani 1.00 d . C36 C -0.2101(4) 0.0897(2) 0.7200(5) 0.072(2) Uani 1.00 d . C37 C -0.1319(4) 0.1157(2) 0.8580(5) 0.080(2) Uani 1.00 d . C38 C -0.1118(5) 0.0751(3) 0.9757(5) 0.096(2) Uani 1.00 d . C39 C -0.3156(4) 0.1611(2) 0.3692(5) 0.074(2) Uani 1.00 d . C40 C -0.3894(5) 0.1538(3) 0.2195(6) 0.121(2) Uani 1.00 d . C41 C -0.3856(8) 0.2067(4) 0.1416(9) 0.193(5) Uani 1.00 d . C42 C -0.296(1) 0.2152(9) 0.114(2) 0.207(9) Uani 0.50 d . C43 C -0.390(1) 0.1980(7) -0.004(1) 0.162(6) Uani 0.50 d . H1 H 0.0339 0.3767 0.2033 0.1064 Uiso 1.00 calc C7 H2 H -0.0388 0.4354 0.2373 0.1064 Uiso 1.00 calc C7 H3 H 0.0408 0.4371 0.4890 0.1096 Uiso 1.00 calc C8 H4 H 0.1231 0.3848 0.4391 0.1096 Uiso 1.00 calc C8 H5 H 0.1926 0.4443 0.3095 0.1178 Uiso 1.00 calc C9 H6 H 0.1079 0.4966 0.3527 0.1178 Uiso 1.00 calc C9 H7 H 0.1984 0.5044 0.5953 0.1181 Uiso 1.00 calc C10 H8 H 0.2849 0.4538 0.5481 0.1181 Uiso 1.00 calc C10 H9 H 0.3404 0.5130 0.4066 0.1215 Uiso 1.00 calc C11 H10 H 0.2540 0.5636 0.4537 0.1215 Uiso 1.00 calc C11 H11 H 0.3518 0.5736 0.6927 0.1312 Uiso 1.00 calc C12 H12 H 0.4397 0.5248 0.6414 0.1312 Uiso 1.00 calc C12 H13 H 0.4819 0.5863 0.4889 0.1427 Uiso 1.00 calc C13 H14 H 0.3963 0.6354 0.5453 0.1427 Uiso 1.00 calc C13 H15 H 0.5048 0.6476 0.7720 0.1562 Uiso 1.00 calc C14 H16 H 0.5907 0.5989 0.7145 0.1562 Uiso 1.00 calc C14 H17 H 0.6237 0.6602 0.5542 0.1964 Uiso 1.00 calc C15 H18 H 0.5392 0.7090 0.6145 0.1964 Uiso 1.00 calc C15 H19 H 0.7382 0.6740 0.7756 0.2582 Uiso 1.00 calc C16 H20 H 0.7121 0.7331 0.7105 0.2582 Uiso 1.00 calc C16 H21 H 0.6537 0.7228 0.8358 0.2582 Uiso 1.00 calc C16 H22 H -0.0483 0.2642 0.8061 0.1214 Uiso 1.00 calc C17 H23 H 0.0108 0.2179 0.6984 0.1214 Uiso 1.00 calc C17 H24 H 0.1361 0.2751 0.8361 0.1343 Uiso 1.00 calc C18 H25 H 0.1173 0.2899 0.6763 0.1343 Uiso 1.00 calc C18 H26 H 0.0216 0.3754 0.7445 0.1424 Uiso 1.00 calc C19 H27 H 0.0315 0.3602 0.9027 0.1424 Uiso 1.00 calc C19 H28 H 0.2221 0.3663 0.9425 0.1717 Uiso 1.00 calc C20 H29 H 0.2119 0.3818 0.7844 0.1717 Uiso 1.00 calc C20 H30 H 0.1190 0.4691 0.8521 0.1847 Uiso 1.00 calc C21 H31 H 0.1287 0.4536 1.0101 0.1847 Uiso 1.00 calc C21 H32 H 0.3169 0.4594 1.0506 0.1950 Uiso 1.00 calc C22 H33 H 0.3083 0.4738 0.8918 0.1950 Uiso 1.00 calc C22 H34 H 0.2140 0.5623 0.9553 0.2079 Uiso 1.00 calc C23 H35 H 0.2213 0.5479 1.1138 0.2079 Uiso 1.00 calc C23 H36 H 0.4094 0.5552 1.1603 0.2024 Uiso 1.00 calc C24 H37 H 0.4035 0.5684 1.0011 0.2024 Uiso 1.00 calc C24 H38 H 0.2983 0.6596 1.0584 0.3197 Uiso 1.00 calc C25 H39 H 0.3020 0.6461 1.2170 0.3197 Uiso 1.00 calc C25 H40 H 0.4936 0.6451 1.2622 0.4349 Uiso 1.00 calc C26 H41 H 0.4895 0.6589 1.1038 0.4349 Uiso 1.00 calc C26 H42 H 0.4423 0.7064 1.2208 0.4349 Uiso 1.00 calc C26 H43 H -0.4726 0.0949 0.4046 0.0887 Uiso 1.00 calc C27 H44 H -0.4203 0.0776 0.5585 0.0887 Uiso 1.00 calc C27 H45 H -0.4426 0.1739 0.6671 0.1140 Uiso 1.00 calc C28 H46 H -0.4867 0.1938 0.5140 0.1140 Uiso 1.00 calc C28 H47 H -0.6364 0.1408 0.4857 0.1363 Uiso 1.00 calc C29 H48 H -0.5922 0.1209 0.6388 0.1363 Uiso 1.00 calc C29 H49 H -0.6256 0.2164 0.7535 0.1846 Uiso 1.00 calc C30 H50 H -0.6688 0.2367 0.6006 0.1846 Uiso 1.00 calc C30 H51 H -0.7335 0.1937 0.6568 0.1846 Uiso 1.00 calc C30 H52 H -0.2775 0.0228 0.4525 0.0789 Uiso 1.00 calc C31 H53 H -0.3246 0.0419 0.2992 0.0789 Uiso 1.00 calc C31 H54 H -0.1545 0.0745 0.2940 0.0959 Uiso 1.00 calc C32 H55 H -0.1077 0.0539 0.4457 0.0959 Uiso 1.00 calc C32 H56 H -0.1781 -0.0241 0.1855 0.1005 Uiso 1.00 calc C33 H57 H -0.0551 -0.0175 0.2545 0.1005 Uiso 1.00 calc C33 H58 H -0.1999 -0.0655 0.3842 0.1121 Uiso 1.00 calc C34 H59 H -0.1087 -0.1026 0.3069 0.1121 Uiso 1.00 calc C34 H60 H -0.0768 -0.0591 0.4526 0.1121 Uiso 1.00 calc C34 H61 H -0.1649 0.1369 0.5815 0.0761 Uiso 1.00 calc C35 H62 H -0.2626 0.1689 0.6539 0.0761 Uiso 1.00 calc C35 H63 H -0.2774 0.0834 0.7470 0.0860 Uiso 1.00 calc C36 H64 H -0.1773 0.0527 0.6778 0.0860 Uiso 1.00 calc C36 H65 H -0.0636 0.1203 0.8314 0.0959 Uiso 1.00 calc C37 H66 H -0.1634 0.1535 0.8972 0.0959 Uiso 1.00 calc C37 H67 H -0.1798 0.0705 1.0032 0.1147 Uiso 1.00 calc C38 H68 H -0.0801 0.0372 0.9371 0.1147 Uiso 1.00 calc C38 H69 H -0.0630 0.0921 1.0601 0.1147 Uiso 1.00 calc C38 H70 H -0.3391 0.1980 0.4231 0.0890 Uiso 1.00 calc C39 H71 H -0.2427 0.1626 0.3535 0.0890 Uiso 1.00 calc C39 H72 H -0.3653 0.1182 0.1611 0.1449 Uiso 1.00 calc C40 H73 H -0.4629 0.1514 0.2318 0.1449 Uiso 1.00 calc C40 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 Pt1 0.0482(1) 0.0600(2) 0.0551(2) -0.0156(1) 0.0038(1) 0.0113(1) S1 0.0664(7) 0.0739(9) 0.0665(7) -0.0035(6) 0.0143(6) 0.0247(6) S2 0.0657(7) 0.0697(8) 0.0714(8) -0.0044(6) 0.0176(6) 0.0248(6) S3 0.0818(9) 0.0706(9) 0.0635(7) 0.0098(7) 0.0164(6) 0.0177(6) S4 0.0750(8) 0.0690(9) 0.0696(8) -0.0016(6) 0.0264(6) 0.0140(6) S5 0.0870(9) 0.0732(9) 0.0684(8) 0.0114(7) 0.0191(7) 0.0173(6) S6 0.0810(8) 0.0583(8) 0.0771(8) -0.0034(6) 0.0290(7) 0.0094(6) S7 0.0887(10) 0.0646(9) 0.126(1) 0.0168(7) 0.0300(9) 0.0251(8) S8 0.0850(9) 0.0748(10) 0.0840(9) -0.0096(7) 0.0354(7) -0.0052(7) N1 0.064(2) 0.060(2) 0.057(2) -0.019(2) 0.000(2) 0.009(2) C1 0.063(2) 0.062(3) 0.057(2) -0.008(2) 0.006(2) 0.011(2) C2 0.059(2) 0.053(2) 0.059(2) -0.010(2) 0.007(2) 0.009(2) C3 0.066(3) 0.059(2) 0.059(2) -0.012(2) 0.008(2) 0.001(2) C4 0.068(3) 0.060(3) 0.062(2) -0.009(2) 0.010(2) 0.003(2) C5 0.063(3) 0.052(2) 0.079(3) -0.001(2) 0.017(2) 0.001(2) C6 0.058(3) 0.057(2) 0.073(3) -0.008(2) 0.010(2) -0.003(2) C7 0.113(4) 0.054(3) 0.105(4) 0.000(3) 0.025(3) 0.026(3) C8 0.107(4) 0.071(4) 0.101(4) 0.005(3) 0.033(3) 0.016(3) C9 0.116(5) 0.080(4) 0.105(4) -0.011(3) 0.032(3) 0.016(3) C10 0.109(5) 0.078(4) 0.108(4) 0.000(3) 0.027(3) 0.011(3) C11 0.114(5) 0.077(4) 0.113(4) -0.008(3) 0.030(3) 0.004(3) C12 0.111(5) 0.091(5) 0.119(5) -0.002(3) 0.019(3) 0.004(4) C13 0.125(5) 0.092(5) 0.135(5) -0.018(4) 0.012(4) 0.012(4) C14 0.129(6) 0.109(6) 0.136(6) -0.007(4) -0.005(4) 0.007(4) C15 0.157(7) 0.092(6) 0.232(9) -0.039(5) 0.000(6) 0.020(5) C16 0.165(9) 0.146(9) 0.29(1) -0.044(6) -0.055(7) 0.002(8) C17 0.136(5) 0.098(5) 0.069(3) -0.002(3) 0.027(2) 0.008(3) C18 0.128(5) 0.107(4) 0.093(4) 0.001(4) 0.010(4) 0.010(4) C19 0.143(5) 0.096(4) 0.119(5) -0.014(4) 0.021(4) 0.021(4) C20 0.164(6) 0.125(5) 0.134(6) -0.053(5) -0.011(5) 0.017(5) C21 0.221(8) 0.121(5) 0.119(6) -0.080(6) -0.020(5) 0.032(4) C22 0.219(8) 0.141(6) 0.120(6) -0.089(6) -0.042(6) 0.031(5) C23 0.236(9) 0.137(6) 0.135(6) -0.079(7) -0.056(6) 0.047(5) C24 0.227(9) 0.143(6) 0.129(6) -0.072(6) -0.036(6) 0.042(5) C25 0.44(2) 0.128(6) 0.21(1) -0.10(1) -0.07(1) 0.049(7) C26 0.50(2) 0.34(2) 0.25(1) -0.31(2) -0.09(1) 0.05(1) C27 0.063(2) 0.082(3) 0.078(3) -0.022(2) 0.001(2) 0.018(2) C28 0.080(3) 0.091(4) 0.116(5) 0.000(3) 0.022(3) 0.018(3) C29 0.080(3) 0.140(6) 0.123(5) -0.013(3) 0.022(3) 0.018(4) C30 0.109(5) 0.146(7) 0.219(9) 0.023(5) 0.080(5) 0.026(6) C31 0.075(3) 0.061(3) 0.056(3) -0.018(2) -0.004(2) 0.003(2) C32 0.081(3) 0.085(3) 0.076(3) -0.023(3) 0.018(3) 0.003(3) C33 0.089(4) 0.091(3) 0.070(3) -0.014(3) 0.018(3) 0.001(2) C34 0.100(4) 0.105(5) 0.080(4) -0.009(3) 0.013(3) 0.030(3) C35 0.065(3) 0.067(3) 0.055(2) -0.021(2) 0.000(2) 0.002(2) C36 0.084(3) 0.079(4) 0.054(2) -0.027(3) 0.004(2) 0.013(2) C37 0.082(3) 0.095(4) 0.060(3) -0.028(3) 0.002(2) 0.002(2) C38 0.112(4) 0.115(5) 0.058(3) -0.027(4) -0.006(3) 0.020(3) C39 0.094(4) 0.060(3) 0.072(3) -0.015(3) 0.012(2) 0.019(2) C40 0.144(6) 0.121(5) 0.080(4) -0.018(4) -0.025(3) 0.013(3) C41 0.30(1) 0.182(9) 0.126(6) -0.051(9) 0.003(8) 0.108(6) C42 0.29(2) 0.24(2) 0.11(1) -0.11(2) -0.03(1) 0.11(1) C43 0.21(2) 0.17(2) 0.133(6) -0.06(1) 0.054(9) 0.05(1) _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.0001|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 6598 _refine_ls_number_parameters 475 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_gt 0.039 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.043 _refine_ls_wR_factor_gt 0.043 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 1.560 _refine_ls_shift/su_max 0.027 _refine_ls_shift/su_mean 0.002 _refine_diff_density_min -0.37 _refine_diff_density_max 0.56 _atom_sites_solution_primary ' direct methods ' _atom_sites_solution_secondary ' difference Fourier map ' 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 Pt1 S1 2.310(2) 1_555 1_555 Pt1 S1 2.310(2) 1_555 2_655 Pt1 S2 2.310(1) 1_555 1_555 Pt1 S2 2.310(1) 1_555 2_655 S1 C1 1.755(5) 1_555 1_555 S2 C2 1.744(6) 1_555 1_555 S3 C1 1.751(6) 1_555 1_555 S3 C3 1.758(5) 1_555 1_555 S4 C2 1.767(5) 1_555 1_555 S4 C3 1.751(6) 1_555 1_555 S5 C4 1.756(6) 1_555 1_555 S5 C5 1.768(6) 1_555 1_555 S6 C4 1.763(5) 1_555 1_555 S6 C6 1.745(6) 1_555 1_555 S7 C5 1.736(6) 1_555 1_555 S7 C7 1.804(7) 1_555 1_555 S8 C6 1.757(6) 1_555 1_555 S8 C17 1.809(7) 1_555 1_555 N1 C27 1.524(7) 1_555 1_555 N1 C31 1.531(7) 1_555 1_555 N1 C35 1.518(6) 1_555 1_555 N1 C39 1.539(6) 1_555 1_555 C1 C2 1.345(7) 1_555 1_555 C3 C4 1.336(7) 1_555 1_555 C5 C6 1.348(7) 1_555 1_555 C7 C8 1.509(9) 1_555 1_555 C8 C9 1.527(9) 1_555 1_555 C9 C10 1.505(9) 1_555 1_555 C10 C11 1.498(9) 1_555 1_555 C11 C12 1.503(10) 1_555 1_555 C12 C13 1.53(1) 1_555 1_555 C13 C14 1.48(1) 1_555 1_555 C14 C15 1.55(1) 1_555 1_555 C15 C16 1.46(1) 1_555 1_555 C17 C18 1.48(1) 1_555 1_555 C18 C19 1.46(1) 1_555 1_555 C19 C20 1.55(1) 1_555 1_555 C20 C21 1.45(1) 1_555 1_555 C21 C22 1.53(1) 1_555 1_555 C22 C23 1.48(1) 1_555 1_555 C23 C24 1.52(1) 1_555 1_555 C24 C25 1.55(2) 1_555 1_555 C25 C26 1.51(2) 1_555 1_555 C27 C28 1.502(9) 1_555 1_555 C28 C29 1.488(9) 1_555 1_555 C29 C30 1.50(1) 1_555 1_555 C31 C32 1.529(8) 1_555 1_555 C32 C33 1.543(9) 1_555 1_555 C33 C34 1.488(8) 1_555 1_555 C35 C36 1.508(7) 1_555 1_555 C36 C37 1.528(7) 1_555 1_555 C37 C38 1.523(8) 1_555 1_555 C39 C40 1.507(8) 1_555 1_555 C40 C41 1.527(10) 1_555 1_555 C41 C42 1.23(2) 1_555 1_555 C41 C43 1.33(1) 1_555 1_555 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 S1 Pt1 S1 180.0 1_555 1_555 2_655 S1 Pt1 S2 90.55(5) 1_555 1_555 1_555 S1 Pt1 S2 89.45(5) 1_555 1_555 2_655 S1 Pt1 S2 89.45(5) 2_655 1_555 1_555 S1 Pt1 S2 90.55(5) 2_655 1_555 2_655 S2 Pt1 S2 180.0 1_555 1_555 2_655 Pt1 S1 C1 101.0(2) 1_555 1_555 1_555 Pt1 S2 C2 101.1(2) 1_555 1_555 1_555 C1 S3 C3 95.4(3) 1_555 1_555 1_555 C2 S4 C3 95.4(3) 1_555 1_555 1_555 C4 S5 C5 94.8(3) 1_555 1_555 1_555 C4 S6 C6 95.0(3) 1_555 1_555 1_555 C5 S7 C7 101.9(3) 1_555 1_555 1_555 C6 S8 C17 101.7(3) 1_555 1_555 1_555 C27 N1 C31 105.8(4) 1_555 1_555 1_555 C27 N1 C35 111.5(4) 1_555 1_555 1_555 C27 N1 C39 111.0(4) 1_555 1_555 1_555 C31 N1 C35 111.2(4) 1_555 1_555 1_555 C31 N1 C39 111.9(4) 1_555 1_555 1_555 C35 N1 C39 105.4(4) 1_555 1_555 1_555 S1 C1 S3 119.1(3) 1_555 1_555 1_555 S1 C1 C2 123.3(5) 1_555 1_555 1_555 S3 C1 C2 117.5(4) 1_555 1_555 1_555 S2 C2 S4 119.6(3) 1_555 1_555 1_555 S2 C2 C1 123.9(4) 1_555 1_555 1_555 S4 C2 C1 116.3(4) 1_555 1_555 1_555 S3 C3 S4 113.7(3) 1_555 1_555 1_555 S3 C3 C4 123.2(5) 1_555 1_555 1_555 S4 C3 C4 123.0(4) 1_555 1_555 1_555 S5 C4 S6 112.6(3) 1_555 1_555 1_555 S5 C4 C3 123.4(4) 1_555 1_555 1_555 S6 C4 C3 123.8(5) 1_555 1_555 1_555 S5 C5 S7 117.6(3) 1_555 1_555 1_555 S5 C5 C6 116.2(5) 1_555 1_555 1_555 S7 C5 C6 125.3(5) 1_555 1_555 1_555 S6 C6 S8 119.0(3) 1_555 1_555 1_555 S6 C6 C5 117.3(4) 1_555 1_555 1_555 S8 C6 C5 123.0(5) 1_555 1_555 1_555 S7 C7 C8 115.8(5) 1_555 1_555 1_555 S7 C7 H1 107.9(5) 1_555 1_555 1_555 S7 C7 H2 107.9(5) 1_555 1_555 1_555 C8 C7 H1 107.9(6) 1_555 1_555 1_555 C8 C7 H2 107.9(6) 1_555 1_555 1_555 H1 C7 H2 109.5(6) 1_555 1_555 1_555 C7 C8 C9 112.1(6) 1_555 1_555 1_555 C7 C8 H3 108.8(7) 1_555 1_555 1_555 C7 C8 H4 108.8(6) 1_555 1_555 1_555 C9 C8 H3 108.8(6) 1_555 1_555 1_555 C9 C8 H4 108.8(7) 1_555 1_555 1_555 H3 C8 H4 109.5(7) 1_555 1_555 1_555 C8 C9 C10 115.8(6) 1_555 1_555 1_555 C8 C9 H5 107.9(7) 1_555 1_555 1_555 C8 C9 H6 107.9(7) 1_555 1_555 1_555 C10 C9 H5 107.9(7) 1_555 1_555 1_555 C10 C9 H6 107.9(7) 1_555 1_555 1_555 H5 C9 H6 109.5(7) 1_555 1_555 1_555 C9 C10 C11 112.6(6) 1_555 1_555 1_555 C9 C10 H7 108.7(7) 1_555 1_555 1_555 C9 C10 H8 108.7(7) 1_555 1_555 1_555 C11 C10 H7 108.7(7) 1_555 1_555 1_555 C11 C10 H8 108.7(7) 1_555 1_555 1_555 H7 C10 H8 109.5(7) 1_555 1_555 1_555 C10 C11 C12 115.4(7) 1_555 1_555 1_555 C10 C11 H9 108.0(7) 1_555 1_555 1_555 C10 C11 H10 108.0(7) 1_555 1_555 1_555 C12 C11 H9 108.0(7) 1_555 1_555 1_555 C12 C11 H10 108.0(7) 1_555 1_555 1_555 H9 C11 H10 109.5(8) 1_555 1_555 1_555 C11 C12 C13 112.2(7) 1_555 1_555 1_555 C11 C12 H11 108.8(7) 1_555 1_555 1_555 C11 C12 H12 108.8(7) 1_555 1_555 1_555 C13 C12 H11 108.8(7) 1_555 1_555 1_555 C13 C12 H12 108.8(7) 1_555 1_555 1_555 H11 C12 H12 109.5(8) 1_555 1_555 1_555 C12 C13 C14 116.6(8) 1_555 1_555 1_555 C12 C13 H13 107.7(7) 1_555 1_555 1_555 C12 C13 H14 107.7(8) 1_555 1_555 1_555 C14 C13 H13 107.7(8) 1_555 1_555 1_555 C14 C13 H14 107.7(8) 1_555 1_555 1_555 H13 C13 H14 109.5(8) 1_555 1_555 1_555 C13 C14 C15 113.4(8) 1_555 1_555 1_555 C13 C14 H15 108.5(8) 1_555 1_555 1_555 C13 C14 H16 108.5(8) 1_555 1_555 1_555 C15 C14 H15 108.5(9) 1_555 1_555 1_555 C15 C14 H16 108.5(9) 1_555 1_555 1_555 H15 C14 H16 109.5(9) 1_555 1_555 1_555 C14 C15 C16 115(1) 1_555 1_555 1_555 C14 C15 H17 108.0(9) 1_555 1_555 1_555 C14 C15 H18 108.0(9) 1_555 1_555 1_555 C16 C15 H17 107(1) 1_555 1_555 1_555 C16 C15 H18 108.0(9) 1_555 1_555 1_555 H17 C15 H18 109(1) 1_555 1_555 1_555 C15 C16 H19 109(1) 1_555 1_555 1_555 C15 C16 H20 109(1) 1_555 1_555 1_555 C15 C16 H21 109(1) 1_555 1_555 1_555 H19 C16 H20 109(1) 1_555 1_555 1_555 H19 C16 H21 109(1) 1_555 1_555 1_555 H20 C16 H21 109(1) 1_555 1_555 1_555 S8 C17 C18 114.9(6) 1_555 1_555 1_555 S8 C17 H22 108.1(6) 1_555 1_555 1_555 S8 C17 H23 108.1(5) 1_555 1_555 1_555 C18 C17 H22 108.1(7) 1_555 1_555 1_555 C18 C17 H23 108.1(8) 1_555 1_555 1_555 H22 C17 H23 109.5(7) 1_555 1_555 1_555 C17 C18 C19 116.4(8) 1_555 1_555 1_555 C17 C18 H24 107.7(8) 1_555 1_555 1_555 C17 C18 H25 107.7(7) 1_555 1_555 1_555 C19 C18 H24 107.7(7) 1_555 1_555 1_555 C19 C18 H25 107.7(8) 1_555 1_555 1_555 H24 C18 H25 109.5(8) 1_555 1_555 1_555 C18 C19 C20 111.8(8) 1_555 1_555 1_555 C18 C19 H26 108.9(8) 1_555 1_555 1_555 C18 C19 H27 108.9(8) 1_555 1_555 1_555 C20 C19 H26 108.9(8) 1_555 1_555 1_555 C20 C19 H27 108.9(8) 1_555 1_555 1_555 H26 C19 H27 109.5(9) 1_555 1_555 1_555 C19 C20 C21 114.4(10) 1_555 1_555 1_555 C19 C20 H28 108.2(8) 1_555 1_555 1_555 C19 C20 H29 108.2(8) 1_555 1_555 1_555 C21 C20 H28 108.2(9) 1_555 1_555 1_555 C21 C20 H29 108.2(9) 1_555 1_555 1_555 H28 C20 H29 109(1) 1_555 1_555 1_555 C20 C21 C22 114(1) 1_555 1_555 1_555 C20 C21 H30 108.2(8) 1_555 1_555 1_555 C20 C21 H31 108.2(8) 1_555 1_555 1_555 C22 C21 H30 108.2(8) 1_555 1_555 1_555 C22 C21 H31 108.2(8) 1_555 1_555 1_555 H30 C21 H31 109(1) 1_555 1_555 1_555 C21 C22 C23 113(1) 1_555 1_555 1_555 C21 C22 H32 108.4(9) 1_555 1_555 1_555 C21 C22 H33 108.4(8) 1_555 1_555 1_555 C23 C22 H32 108.4(8) 1_555 1_555 1_555 C23 C22 H33 108.4(9) 1_555 1_555 1_555 H32 C22 H33 109(1) 1_555 1_555 1_555 C22 C23 C24 114(1) 1_555 1_555 1_555 C22 C23 H34 108.2(9) 1_555 1_555 1_555 C22 C23 H35 108.2(9) 1_555 1_555 1_555 C24 C23 H34 108.2(9) 1_555 1_555 1_555 C24 C23 H35 108.2(9) 1_555 1_555 1_555 H34 C23 H35 109(1) 1_555 1_555 1_555 C23 C24 C25 110(1) 1_555 1_555 1_555 C23 C24 H36 109.3(9) 1_555 1_555 1_555 C23 C24 H37 109.3(9) 1_555 1_555 1_555 C25 C24 H36 109.3(10) 1_555 1_555 1_555 C25 C24 H37 109(1) 1_555 1_555 1_555 H36 C24 H37 109(1) 1_555 1_555 1_555 C24 C25 C26 105(1) 1_555 1_555 1_555 C24 C25 H38 110(1) 1_555 1_555 1_555 C24 C25 H39 110(1) 1_555 1_555 1_555 C26 C25 H38 110(1) 1_555 1_555 1_555 C26 C25 H39 110(1) 1_555 1_555 1_555 H38 C25 H39 109(1) 1_555 1_555 1_555 C25 C26 H40 109(1) 1_555 1_555 1_555 C25 C26 H41 109(1) 1_555 1_555 1_555 C25 C26 H42 109(2) 1_555 1_555 1_555 H40 C26 H41 109(2) 1_555 1_555 1_555 H40 C26 H42 109(1) 1_555 1_555 1_555 H41 C26 H42 109(1) 1_555 1_555 1_555 N1 C27 C28 116.4(5) 1_555 1_555 1_555 N1 C27 H43 107.7(5) 1_555 1_555 1_555 N1 C27 H44 107.7(5) 1_555 1_555 1_555 C28 C27 H43 107.7(6) 1_555 1_555 1_555 C28 C27 H44 107.7(6) 1_555 1_555 1_555 H43 C27 H44 109.5(6) 1_555 1_555 1_555 C27 C28 C29 110.7(6) 1_555 1_555 1_555 C27 C28 H45 109.2(6) 1_555 1_555 1_555 C27 C28 H46 109.2(6) 1_555 1_555 1_555 C29 C28 H45 109.2(7) 1_555 1_555 1_555 C29 C28 H46 109.2(7) 1_555 1_555 1_555 H45 C28 H46 109.5(7) 1_555 1_555 1_555 C28 C29 C30 115.8(8) 1_555 1_555 1_555 C28 C29 H47 107.9(7) 1_555 1_555 1_555 C28 C29 H48 107.9(7) 1_555 1_555 1_555 C30 C29 H47 107.9(8) 1_555 1_555 1_555 C30 C29 H48 107.9(8) 1_555 1_555 1_555 H47 C29 H48 109.5(8) 1_555 1_555 1_555 C29 C30 H49 109.5(8) 1_555 1_555 1_555 C29 C30 H50 109.5(8) 1_555 1_555 1_555 C29 C30 H51 109.5(9) 1_555 1_555 1_555 H49 C30 H50 109(1) 1_555 1_555 1_555 H49 C30 H51 109.5(9) 1_555 1_555 1_555 H50 C30 H51 109.5(9) 1_555 1_555 1_555 N1 C31 C32 114.2(4) 1_555 1_555 1_555 N1 C31 H52 108.3(5) 1_555 1_555 1_555 N1 C31 H53 108.3(5) 1_555 1_555 1_555 C32 C31 H52 108.3(5) 1_555 1_555 1_555 C32 C31 H53 108.3(5) 1_555 1_555 1_555 H52 C31 H53 109.5(5) 1_555 1_555 1_555 C31 C32 C33 111.3(5) 1_555 1_555 1_555 C31 C32 H54 109.0(6) 1_555 1_555 1_555 C31 C32 H55 109.0(5) 1_555 1_555 1_555 C33 C32 H54 109.0(6) 1_555 1_555 1_555 C33 C32 H55 109.0(6) 1_555 1_555 1_555 H54 C32 H55 109.5(6) 1_555 1_555 1_555 C32 C33 C34 114.0(5) 1_555 1_555 1_555 C32 C33 H56 108.3(6) 1_555 1_555 1_555 C32 C33 H57 108.3(6) 1_555 1_555 1_555 C34 C33 H56 108.3(6) 1_555 1_555 1_555 C34 C33 H57 108.3(6) 1_555 1_555 1_555 H56 C33 H57 109.5(6) 1_555 1_555 1_555 C33 C34 H58 109.5(6) 1_555 1_555 1_555 C33 C34 H59 109.5(6) 1_555 1_555 1_555 C33 C34 H60 109.5(6) 1_555 1_555 1_555 H58 C34 H59 109.5(7) 1_555 1_555 1_555 H58 C34 H60 109.5(6) 1_555 1_555 1_555 H59 C34 H60 109.5(7) 1_555 1_555 1_555 N1 C35 C36 116.2(4) 1_555 1_555 1_555 N1 C35 H61 107.8(4) 1_555 1_555 1_555 N1 C35 H62 107.8(5) 1_555 1_555 1_555 C36 C35 H61 107.8(5) 1_555 1_555 1_555 C36 C35 H62 107.8(5) 1_555 1_555 1_555 H61 C35 H62 109.5(5) 1_555 1_555 1_555 C35 C36 C37 110.1(5) 1_555 1_555 1_555 C35 C36 H63 109.3(5) 1_555 1_555 1_555 C35 C36 H64 109.3(5) 1_555 1_555 1_555 C37 C36 H63 109.3(5) 1_555 1_555 1_555 C37 C36 H64 109.3(5) 1_555 1_555 1_555 H63 C36 H64 109.5(6) 1_555 1_555 1_555 C36 C37 C38 111.0(5) 1_555 1_555 1_555 C36 C37 H65 109.1(5) 1_555 1_555 1_555 C36 C37 H66 109.1(6) 1_555 1_555 1_555 C38 C37 H65 109.1(6) 1_555 1_555 1_555 C38 C37 H66 109.1(6) 1_555 1_555 1_555 H65 C37 H66 109.5(6) 1_555 1_555 1_555 C37 C38 H67 109.5(6) 1_555 1_555 1_555 C37 C38 H68 109.5(6) 1_555 1_555 1_555 C37 C38 H69 109.5(6) 1_555 1_555 1_555 H67 C38 H68 109.5(7) 1_555 1_555 1_555 H67 C38 H69 109.5(6) 1_555 1_555 1_555 H68 C38 H69 109.5(7) 1_555 1_555 1_555 N1 C39 C40 117.2(5) 1_555 1_555 1_555 N1 C39 H70 107.5(5) 1_555 1_555 1_555 N1 C39 H71 107.5(5) 1_555 1_555 1_555 C40 C39 H70 107.5(6) 1_555 1_555 1_555 C40 C39 H71 107.5(6) 1_555 1_555 1_555 H70 C39 H71 109.5(6) 1_555 1_555 1_555 C39 C40 C41 110.1(7) 1_555 1_555 1_555 C39 C40 H72 109.3(7) 1_555 1_555 1_555 C39 C40 H73 109.3(6) 1_555 1_555 1_555 C41 C40 H72 109.3(7) 1_555 1_555 1_555 C41 C40 H73 109.3(8) 1_555 1_555 1_555 H72 C40 H73 109.5(7) 1_555 1_555 1_555 C40 C41 C42 117(1) 1_555 1_555 1_555 C40 C41 C43 119(1) 1_555 1_555 1_555 loop_ _publ_author_name _publ_author_address ' Takeo Nakazono ' ; Department of Applied Chemistry Graduate School of Engineering Osaka University 1-16 Machikaneyama, Toyonaka Osaka 560-0043, Japan ; ' Motohiro Nakano ' ; Department of Applied Chemistry Graduate School of Engineering Osaka University 1-16 Machikaneyama, Toyonaka Osaka 560-0043, Japan ; ' Hatsue Tamura ' ; Department of Applied Chemistry Graduate School of Engineering Osaka University 1-16 Machikaneyama, Toyonaka Osaka 560-0043, Japan ; ' Gen-etsu Matsubayashi ' ; Department of Applied Chemistry Graduate School of Engineering Osaka University 1-16 Machikaneyama, Toyonaka Osaka 560-0043, Japan ; _publ_section_abstract ; Reactions of [NBu^n^~4~]~2~[PtCl~4~] with Na~2~[C~6~S~8~R~2~][C~6~S~8~R~2~^2-^ =2-{bis(alkylthio)-1,3-dithiole-2-ylidene}-1,3-dithiole-4,5-dithiolate (2-); R=C~10~H~21~, C~14~H~29~ and C~18~H~37~] in methanol afforded [NBu^n^~4~]~2~ [Pt(C~6~S~8~R~2~)~2~]. The crystal structure of [NBu^n^~4~]~2~[Pt{C~6~S~8~( C~10~H~21~)~2~] was determined by X-ray analysis. The complex crystallizes in the triclinic space group P -1 with a=12.416(2), b=22.881(4), c=9.315(2) \%A, \a=99.93(2), \b=101.19(2), \g=83.39(1)\%, V=2548.0(7) \%A^3^ and Z=1. The crystal packing structure consists of columns of anion units through association of alkyl chains, where the metal-center units are separated by the bulky tetrabutylammonium ion. These complexes exhibit oxidation potentials of -0.25 -- +0.35 V vs. SCE. They were oxidized by bromine or iodine to yield two-electron oxidized species [Pt(C~6~S~8~R~2~)~2~]^0^ with the ligand-centered oxidation. The oxidized complexes (R=C~10~H~21~ and C~14~H~29~) exhibit electrical conductivities(\s) of 1.4\\10^-2^ -- 4.9\\10^-2^ S cm^-1^ measured for compacted pellets at room temperature, while the oxidized species with R=C~18~H~37~ behaves as an insulator(\s< 10^-8^ S cm^-1^). Electronic states and molecular interactions of the complexes in the solid state are discussed based on IR, ESR, XPS, electronic absorption, and reflectance spectra, as well as DSC. ;