Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2002 data_pr9818 _database_code_CSD 148650 _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Raithby, Paul' 'Al-Mandhary, Muna R.A.' 'Al-Suti, Mohammad' 'Feeder, Neil' 'Friend, Richard' 'Khan, Muhammad S.' 'Kohler, Anna' 'Nahar, Saifun' 'Wilson, Paul J.' _publ_contact_author_name 'Prof Paul Raithby' _publ_contact_author_address ; Department of Chemistry University of Bath Claverton Down Bath Avon BA2 7AY UNITED KINGDOM ; _publ_contact_author_email 'P.R.RAITHBY@BATH.AC.UK' _publ_section_title ; Synthesis, Characterisation and Electronic Properties of a Series of Platinum)II) Poly-ynes containing Novel thienyl-pyridine Liner Groups ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H25 N S2 Si2' _chemical_formula_weight 435.74 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' 'Si' 'Si' 0.0817 0.0704 '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 P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.605(3) _cell_length_b 5.744(2) _cell_length_c 11.719(2) _cell_angle_alpha 90.00 _cell_angle_beta 96.420(10) _cell_angle_gamma 90.00 _cell_volume 1177.6(5) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 3641 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 25.19 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.229 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 460 _exptl_absorpt_coefficient_mu 0.337 _exptl_absorpt_correction_type 'Interframe scaling' _exptl_absorpt_correction_T_min 0.8770 _exptl_absorpt_correction_T_max 0.9671 _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'R-Axis IIc' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3641 _diffrn_reflns_av_R_equivalents 0.0627 _diffrn_reflns_av_sigmaI/netI 0.1217 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 25.19 _reflns_number_total 1999 _reflns_number_gt 1397 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Rigaku Axis II control package' _computing_cell_refinement 'Rigaku Axis II control package' _computing_data_reduction TeXsan _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1991)' _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^)+(0.0511P)^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 SHELXL _refine_ls_extinction_coef 0.112(8) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1999 _refine_ls_number_parameters 131 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0781 _refine_ls_R_factor_gt 0.0550 _refine_ls_wR_factor_ref 0.1365 _refine_ls_wR_factor_gt 0.1255 _refine_ls_goodness_of_fit_ref 0.995 _refine_ls_restrained_S_all 0.995 _refine_ls_shift/su_max 0.202 _refine_ls_shift/su_mean 0.028 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 S1 S 0.84409(5) 0.25963(14) 0.26071(7) 0.0468(3) Uani 1 d . . . Si1 Si 0.64400(5) 0.57825(17) -0.10298(7) 0.0456(3) Uani 1 d . . . C1 C 0.5831(2) 0.7411(7) -0.0109(3) 0.0653(11) Uani 1 d . . . H1A H 0.5420 0.8199 -0.0594 0.078 Uiso 1 calc R . . H1B H 0.6142 0.8569 0.0345 0.078 Uiso 1 calc R . . H1C H 0.5610 0.6325 0.0408 0.078 Uiso 1 calc R . . C2 C 0.6977(2) 0.7818(6) -0.1863(3) 0.0572(10) Uani 1 d . . . H2A H 0.6621 0.8645 -0.2424 0.069 Uiso 1 calc R . . H2B H 0.7344 0.6943 -0.2265 0.069 Uiso 1 calc R . . H2C H 0.7252 0.8945 -0.1340 0.069 Uiso 1 calc R . . C3 C 0.5863(2) 0.3782(7) -0.2023(3) 0.0660(11) Uani 1 d . . . H3A H 0.5471 0.4673 -0.2497 0.079 Uiso 1 calc R . . H3B H 0.5617 0.2615 -0.1578 0.079 Uiso 1 calc R . . H3C H 0.6197 0.3002 -0.2519 0.079 Uiso 1 calc R . . C4 C 0.7116(2) 0.4009(6) -0.0079(3) 0.0506(9) Uani 1 d . . . C5 C 0.7555(2) 0.2844(6) 0.0541(3) 0.0485(8) Uani 1 d . . . C6 C 0.8090(2) 0.1512(6) 0.1274(2) 0.0467(8) Uani 1 d . . . C7 C 0.8399(2) -0.0625(6) 0.1090(3) 0.0526(9) Uani 1 d . . . H7 H 0.8273 -0.1517 0.0412 0.063 Uiso 1 calc R . . C8 C 0.8924(2) -0.1352(6) 0.2019(3) 0.0537(9) Uani 1 d . . . H8 H 0.9188 -0.2795 0.2027 0.064 Uiso 1 calc R . . C9 C 0.90187(18) 0.0199(5) 0.2905(3) 0.0440(8) Uani 1 d . . . C10 C 0.95196(18) 0.0083(6) 0.3992(3) 0.0441(8) Uani 1 d . . . C12 C 0.95706(19) 0.1950(6) 0.4695(3) 0.0564(9) Uani 0.50 d P . 1 H12 H 0.9275 0.3302 0.4495 0.068 Uiso 0.50 calc PR . 1 C11 C 0.9948(2) -0.1890(6) 0.4299(3) 0.0573(10) Uani 0.50 d P . 1 H11 H 0.9908 -0.3212 0.3809 0.069 Uiso 0.50 calc PR . 1 N1 N 0.95706(19) 0.1950(6) 0.4695(3) 0.0564(9) Uani 0.50 d P . 2 C11' C 0.9948(2) -0.1890(6) 0.4299(3) 0.0573(10) Uani 0.50 d P . 2 H11' H 0.9908 -0.3212 0.3809 0.069 Uiso 0.50 calc PR . 2 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 S1 0.0544(6) 0.0365(5) 0.0495(5) 0.0046(4) 0.0054(4) 0.0125(4) Si1 0.0518(6) 0.0431(6) 0.0415(5) 0.0012(4) 0.0036(4) -0.0007(4) C1 0.065(3) 0.076(3) 0.057(2) 0.0004(19) 0.0129(18) 0.008(2) C2 0.070(3) 0.052(2) 0.0517(19) -0.0004(16) 0.0129(17) 0.0036(19) C3 0.074(3) 0.057(2) 0.062(2) 0.0008(18) -0.0135(19) -0.002(2) C4 0.057(2) 0.053(2) 0.0412(16) 0.0012(16) 0.0023(15) -0.0008(19) C5 0.056(2) 0.048(2) 0.0415(17) -0.0016(15) 0.0071(15) -0.0061(18) C6 0.052(2) 0.0431(19) 0.0459(17) 0.0044(15) 0.0097(14) 0.0002(17) C7 0.059(2) 0.043(2) 0.0575(19) -0.0039(15) 0.0112(17) -0.0005(18) C8 0.052(2) 0.039(2) 0.073(2) 0.0054(17) 0.0209(18) 0.0085(17) C9 0.0421(19) 0.0350(17) 0.0563(18) 0.0091(15) 0.0124(15) 0.0087(15) C10 0.0427(19) 0.0389(17) 0.0529(18) 0.0120(15) 0.0153(15) 0.0040(15) C12 0.055(2) 0.0473(17) 0.068(2) 0.0172(16) 0.0140(17) 0.0169(16) C11 0.063(3) 0.045(2) 0.066(2) 0.0140(17) 0.0155(19) 0.0187(19) N1 0.055(2) 0.0473(17) 0.068(2) 0.0172(16) 0.0140(17) 0.0169(16) C11' 0.063(3) 0.045(2) 0.066(2) 0.0140(17) 0.0155(19) 0.0187(19) _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 S1 C9 1.724(3) . ? S1 C6 1.731(3) . ? Si1 C4 1.844(4) . ? Si1 C2 1.850(3) . ? Si1 C3 1.855(4) . ? Si1 C1 1.856(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.202(5) . ? C5 C6 1.424(5) . ? C6 C7 1.370(4) . ? C7 C8 1.411(5) . ? C7 H7 0.9500 . ? C8 C9 1.365(4) . ? C8 H8 0.9500 . ? C9 C10 1.467(4) . ? C10 C12 1.349(4) . ? C10 C11 1.386(4) . ? C12 C11 1.373(5) 3_756 ? C12 H12 0.9500 . ? C11 C12 1.373(5) 3_756 ? C11 H11 0.9500 . ? 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 C9 S1 C6 92.23(16) . . ? C4 Si1 C2 109.53(17) . . ? C4 Si1 C3 107.95(17) . . ? C2 Si1 C3 109.68(17) . . ? C4 Si1 C1 107.64(16) . . ? C2 Si1 C1 110.52(18) . . ? C3 Si1 C1 111.45(19) . . ? Si1 C1 H1A 109.5 . . ? Si1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Si1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si1 C3 H3A 109.5 . . ? Si1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Si1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C5 C4 Si1 179.7(4) . . ? C4 C5 C6 178.5(4) . . ? C7 C6 C5 129.3(3) . . ? C7 C6 S1 110.9(3) . . ? C5 C6 S1 119.8(2) . . ? C6 C7 C8 112.4(3) . . ? C6 C7 H7 123.8 . . ? C8 C7 H7 123.8 . . ? C9 C8 C7 114.1(3) . . ? C9 C8 H8 123.0 . . ? C7 C8 H8 123.0 . . ? C8 C9 C10 129.9(3) . . ? C8 C9 S1 110.4(3) . . ? C10 C9 S1 119.7(2) . . ? C12 C10 C11 119.6(3) . . ? C12 C10 C9 119.1(3) . . ? C11 C10 C9 121.3(3) . . ? C10 C12 C11 119.8(3) . 3_756 ? C10 C12 H12 120.1 . . ? C11 C12 H12 120.1 3_756 . ? C12 C11 C10 120.6(3) 3_756 . ? C12 C11 H11 119.7 3_756 . ? C10 C11 H11 119.7 . . ? 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 C2 Si1 C4 C5 -147(49) . . . . ? C3 Si1 C4 C5 -28(49) . . . . ? C1 Si1 C4 C5 93(49) . . . . ? Si1 C4 C5 C6 172(100) . . . . ? C4 C5 C6 C7 -118(13) . . . . ? C4 C5 C6 S1 61(13) . . . . ? C9 S1 C6 C7 1.1(3) . . . . ? C9 S1 C6 C5 -178.5(3) . . . . ? C5 C6 C7 C8 178.7(3) . . . . ? S1 C6 C7 C8 -0.8(4) . . . . ? C6 C7 C8 C9 0.0(4) . . . . ? C7 C8 C9 C10 -178.6(3) . . . . ? C7 C8 C9 S1 0.9(4) . . . . ? C6 S1 C9 C8 -1.1(2) . . . . ? C6 S1 C9 C10 178.4(3) . . . . ? C8 C9 C10 C12 173.5(3) . . . . ? S1 C9 C10 C12 -5.9(4) . . . . ? C8 C9 C10 C11 -5.5(5) . . . . ? S1 C9 C10 C11 175.1(2) . . . . ? C11 C10 C12 C11 0.7(5) . . . 3_756 ? C9 C10 C12 C11 -178.3(3) . . . 3_756 ? C12 C10 C11 C12 -0.7(5) . . . 3_756 ? C9 C10 C11 C12 178.3(3) . . . 3_756 ? _diffrn_measured_fraction_theta_max 0.855 _diffrn_reflns_theta_full 25.19 _diffrn_measured_fraction_theta_full 0.855 _refine_diff_density_max 0.268 _refine_diff_density_min -0.306 _refine_diff_density_rms 0.070