Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Neil Robertson' 'John Clifford' 'Alice Dawson' 'James Durrant' 'Elaine A. M. Geary' 'Narukuni Hirata' 'S. Parsons' 'Lesley Yellowlees' _publ_contact_author_name 'Dr Neil Robertson' _publ_contact_author_address ; School of Chemistry University of Edinburgh King's Buildings West Mains Rd. Edinburgh EH9 3JJ UNITED KINGDOM ; _publ_contact_author_email NEIL.ROBERTSON@ED.AC.UK _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Synthesis, Structure and Properties of [Pt(2,2'-bipyridyl-5,5'-dicarboxylic acid)(3,4-toluenedithiolate)]: Tuning molecular properties for application in dye-sensitised solar cells. ; data_egippt _database_code_CSD 211901 #Note to referee: checkcif output is in _refine_special_details. _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Pt1 N2 O4 C19 H12].[NC4H36]2.C2O1H6.C4O2H8' _chemical_formula_sum 'C57 H98 N4 O7 Pt S2' _chemical_formula_weight 1210.61 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 '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' H H 0.0000 0.0000 '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 _symmetry_space_group_name_Hall '-P 2ybc' 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 16.4091(7) _cell_length_b 14.4709(6) _cell_length_c 27.5157(12) _cell_angle_alpha 90.00 _cell_angle_beta 105.5480(10) _cell_angle_gamma 90.00 _cell_volume 6294.6(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6294 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 28.7 _exptl_crystal_description purple _exptl_crystal_colour block _exptl_crystal_size_max 0.57 _exptl_crystal_size_mid 0.55 _exptl_crystal_size_min 0.45 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.277 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2536 _exptl_absorpt_coefficient_mu 2.344 _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_min 0.288 _exptl_absorpt_correction_T_max 0.350 #!062_ALERT C Rescale T(min) & T(max) by ................... 0.35 #! original values were: #!_exptl_absorpt_correction_T_min 0.823 #!_exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'CCD area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 56147 _diffrn_reflns_av_R_equivalents 0.0277 _diffrn_reflns_av_sigmaI/netI 0.0271 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 28.95 _reflns_number_total 15448 _reflns_number_gt 13231 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Checkcif output: 761_ALERT A CIF Contains no X-H Bonds .................... ? 762_ALERT A CIF Contains no X-Y-H or H-Y-H Angles ........ ? The H's were placed in calculated positions. 043_ALERT B Check Reported Molecular Weight .............. 1210.61 044_ALERT B Calculated and Reported Dx Differ ............ ? 041_ALERT C Calc. and Rep. SumFormula Strings Differ .. ? 042_ALERT C Calc. and Rep. MoietyFormula Strings Differ .. ? 068_ALERT C Reported F000 Differs from Calcd (or Missing). ? 602_ALERT C VERY LARGE Solvent Accessible VOID(S) in Structure ! 192 e/cell treated by van der Sluis-Spek method. 223_ALERT B Large Solvent/Anion H Ueq(max)/Ueq(min) . 4.54 Ratio 221_ALERT C Large Solvent/Anion C Ueq(max)/Ueq(min) . 3.64 Ratio 244_ALERT C Low Solvent U(eq) as Compared to Neighbors ... C(1S) Eigenvalues of displacement tensor for the EtOH of solvation are: 0.1400 0.0867 0.0821 O1S 0.1110 0.0743 0.0605 C1S 0.1789 0.0807 0.0763 C2S The are large and may imply some disorder in this part of the structure. 142_ALERT C su on b - Axis Small or Missing (x 100000) ... 60 Ang. 143_ALERT C su on c - Axis Small or Missing (x 100000) ... 120 Ang. 145_ALERT C su on beta Small or Missing (x 10000) ... 10 Deg. These are the values output by the cell refinement program, though s.u.s from area detector instruments are generally considered to be much underestimated. 301_ALERT C Main Residue Disorder ........................ 2.00 Perc. 366_ALERT C Short? C(sp?)-C(sp?) Bond C(15) - C(16) = 1.37 Ang. 366_ALERT C Short? C(sp?)-C(sp?) Bond C(16) - C(17) = 1.39 Ang. 366_ALERT C Short? C(sp?)-C(sp?) Bond C(17) - C(18) = 1.38 Ang. Possibly checkcif is confused by the disorder in this region: these are not abnormal aromatic CC distances. 369_ALERT C Long C(sp2)-C(sp2) Bond C(3) - C(31) = 1.53 Ang. 369_ALERT C Long C(sp2)-C(sp2) Bond C(10) - C(101) = 1.53 Ang. Pi bonding mainly in the aromatic ring & the COO- group. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0449P)^2^+1.7713P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15448 _refine_ls_number_parameters 604 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0362 _refine_ls_R_factor_gt 0.0301 _refine_ls_wR_factor_ref 0.0802 _refine_ls_wR_factor_gt 0.0781 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.084 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_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_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.764799(6) 0.450285(6) 0.254827(3) 0.02803(4) Uani 1 1 d . B . N1 N 0.86471(13) 0.45291(12) 0.31841(8) 0.0286(4) Uani 1 1 d . . . C2 C 0.94756(16) 0.44806(15) 0.32050(10) 0.0308(5) Uani 1 1 d . . . H2 H 0.9631 0.4422 0.2898 0.037 Uiso 1 1 calc R . . C3 C 1.01059(16) 0.45113(15) 0.36487(10) 0.0316(5) Uani 1 1 d . . . C31 C 1.10329(16) 0.44204(16) 0.36395(10) 0.0322(5) Uani 1 1 d . . . O311 O 1.15778(12) 0.45565(12) 0.40534(8) 0.0401(4) Uani 1 1 d . . . O312 O 1.11635(11) 0.42201(13) 0.32294(7) 0.0348(4) Uani 1 1 d . . . C4 C 0.98752(17) 0.46061(19) 0.40950(11) 0.0418(6) Uani 1 1 d . . . H4 H 1.0296 0.4642 0.4408 0.050 Uiso 1 1 calc R . . C5 C 0.90247(18) 0.4648(2) 0.40813(11) 0.0450(7) Uani 1 1 d . . . H5 H 0.8860 0.4708 0.4385 0.054 Uiso 1 1 calc R . . C6 C 0.84217(16) 0.46006(17) 0.36267(11) 0.0351(5) Uani 1 1 d . . . C7 C 0.75073(16) 0.45949(17) 0.35752(11) 0.0360(6) Uani 1 1 d . . . C8 C 0.71600(18) 0.4639(2) 0.39812(11) 0.0440(7) Uani 1 1 d . . . H8 H 0.7512 0.4702 0.4315 0.053 Uiso 1 1 calc R . . C9 C 0.62862(18) 0.45893(18) 0.38904(12) 0.0411(6) Uani 1 1 d . . . H9 H 0.6037 0.4630 0.4164 0.049 Uiso 1 1 calc R . . C10 C 0.57815(16) 0.44826(15) 0.34092(11) 0.0339(5) Uani 1 1 d . . . C101 C 0.48225(17) 0.43861(16) 0.33048(12) 0.0382(6) Uani 1 1 d . . . O101 O 0.44267(12) 0.41533(14) 0.28699(8) 0.0488(5) Uani 1 1 d . . . O102 O 0.45345(13) 0.45401(12) 0.36719(9) 0.0453(5) Uani 1 1 d . . . C11 C 0.61602(16) 0.44480(15) 0.30171(11) 0.0334(5) Uani 1 1 d . . . H11 H 0.5813 0.4377 0.2682 0.040 Uiso 1 1 calc R . . N12 N 0.70106(13) 0.45116(12) 0.30941(9) 0.0301(4) Uani 1 1 d . . . S13 S 0.64726(4) 0.44961(4) 0.19000(3) 0.03700(14) Uani 1 1 d . . . C14 C 0.6841(2) 0.43584(17) 0.13621(11) 0.0402(6) Uani 1 1 d . . . C15 C 0.6266(2) 0.4295(2) 0.08879(12) 0.0526(8) Uani 1 1 d . B . H15 H 0.5677 0.4312 0.0860 0.063 Uiso 1 1 calc R . . C16 C 0.6541(3) 0.4210(2) 0.04601(13) 0.0626(9) Uani 1 1 d . . . H161 H 0.6143 0.4177 0.0138 0.075 Uiso 0.50 1 calc PR A 1 C20B C 0.5855(6) 0.4195(6) -0.0025(2) 0.071(2) Uani 0.50 1 d P B 2 H20D H 0.5302 0.4235 0.0047 0.107 Uiso 0.50 1 calc PR B 2 H20E H 0.5888 0.3619 -0.0206 0.107 Uiso 0.50 1 calc PR B 2 H20F H 0.5925 0.4722 -0.0234 0.107 Uiso 0.50 1 calc PR B 2 C17 C 0.7404(3) 0.4171(2) 0.04995(12) 0.0643(10) Uani 1 1 d . B . H171 H 0.7597 0.4106 0.0205 0.077 Uiso 0.50 1 calc PR C 1 C20A C 0.7804(7) 0.4111(7) 0.0015(3) 0.099(3) Uani 0.50 1 d P B 2 H20A H 0.8422 0.4082 0.0134 0.148 Uiso 0.50 1 calc PR B 2 H20B H 0.7636 0.4659 -0.0198 0.148 Uiso 0.50 1 calc PR B 2 H20C H 0.7591 0.3555 -0.0182 0.148 Uiso 0.50 1 calc PR B 2 C18 C 0.7978(2) 0.4228(2) 0.09677(11) 0.0506(7) Uani 1 1 d . . . H18 H 0.8567 0.4194 0.0994 0.061 Uiso 1 1 calc R B . C19 C 0.77069(19) 0.43358(17) 0.14019(10) 0.0383(6) Uani 1 1 d . B . S21 S 0.84399(4) 0.44951(4) 0.19942(3) 0.03361(13) Uani 1 1 d . . . N4 N 0.31809(12) 0.23606(13) 0.38213(8) 0.0316(4) Uani 1 1 d . . . C411 C 0.34015(16) 0.31204(16) 0.42228(10) 0.0346(5) Uani 1 1 d . . . H41A H 0.3846 0.3518 0.4151 0.041 Uiso 1 1 calc R . . H41B H 0.2894 0.3510 0.4193 0.041 Uiso 1 1 calc R . . C412 C 0.37057(19) 0.27793(19) 0.47598(10) 0.0441(6) Uani 1 1 d . . . H41C H 0.4204 0.2374 0.4793 0.053 Uiso 1 1 calc R . . H41D H 0.3254 0.2409 0.4843 0.053 Uiso 1 1 calc R . . C413 C 0.3944(2) 0.3581(2) 0.51294(11) 0.0494(7) Uani 1 1 d . . . H41E H 0.3441 0.3977 0.5102 0.059 Uiso 1 1 calc R . . H41F H 0.4384 0.3960 0.5040 0.059 Uiso 1 1 calc R . . C414 C 0.4275(2) 0.3241(2) 0.56760(12) 0.0641(9) Uani 1 1 d . . . H41G H 0.3814 0.2945 0.5782 0.096 Uiso 1 1 calc R . . H41H H 0.4490 0.3768 0.5897 0.096 Uiso 1 1 calc R . . H41I H 0.4732 0.2795 0.5697 0.096 Uiso 1 1 calc R . . C421 C 0.39359(16) 0.17445(16) 0.38376(10) 0.0360(5) Uani 1 1 d . . . H42A H 0.3761 0.1274 0.3569 0.043 Uiso 1 1 calc R . . H42B H 0.4085 0.1414 0.4165 0.043 Uiso 1 1 calc R . . C422 C 0.47263(16) 0.22207(17) 0.37746(10) 0.0381(6) Uani 1 1 d . . . H42C H 0.4950 0.2647 0.4061 0.046 Uiso 1 1 calc R . . H42D H 0.4585 0.2588 0.3460 0.046 Uiso 1 1 calc R . . C423 C 0.53940(19) 0.1504(2) 0.37546(15) 0.0592(8) Uani 1 1 d . . . H42E H 0.5475 0.1088 0.4049 0.071 Uiso 1 1 calc R . . H42F H 0.5189 0.1126 0.3446 0.071 Uiso 1 1 calc R . . C424 C 0.6235(2) 0.1928(2) 0.37543(14) 0.0557(8) Uani 1 1 d . . . H42G H 0.6160 0.2338 0.3462 0.083 Uiso 1 1 calc R . . H42H H 0.6636 0.1437 0.3735 0.083 Uiso 1 1 calc R . . H42I H 0.6453 0.2283 0.4065 0.083 Uiso 1 1 calc R . . C431 C 0.24914(16) 0.17282(16) 0.39027(10) 0.0357(5) Uani 1 1 d . . . H43A H 0.2708 0.1410 0.4230 0.043 Uiso 1 1 calc R . . H43B H 0.2376 0.1249 0.3636 0.043 Uiso 1 1 calc R . . C432 C 0.16616(16) 0.21989(17) 0.38995(11) 0.0389(6) Uani 1 1 d . . . H43C H 0.1763 0.2672 0.4169 0.047 Uiso 1 1 calc R . . H43D H 0.1430 0.2513 0.3572 0.047 Uiso 1 1 calc R . . C433 C 0.10274(18) 0.1493(2) 0.39831(13) 0.0495(7) Uani 1 1 d . . . H43E H 0.0934 0.1019 0.3715 0.059 Uiso 1 1 calc R . . H43F H 0.1263 0.1180 0.4311 0.059 Uiso 1 1 calc R . . C434 C 0.0188(2) 0.1931(2) 0.39808(14) 0.0587(8) Uani 1 1 d . . . H43G H 0.0276 0.2393 0.4250 0.088 Uiso 1 1 calc R . . H43H H -0.0201 0.1453 0.4036 0.088 Uiso 1 1 calc R . . H43I H -0.0054 0.2229 0.3654 0.088 Uiso 1 1 calc R . . C441 C 0.28955(15) 0.28556(16) 0.33168(9) 0.0312(5) Uani 1 1 d . . . H44A H 0.2408 0.3256 0.3321 0.037 Uiso 1 1 calc R . . H44B H 0.3360 0.3262 0.3279 0.037 Uiso 1 1 calc R . . C442 C 0.26420(16) 0.22263(16) 0.28590(10) 0.0337(5) Uani 1 1 d . . . H44C H 0.2161 0.1832 0.2882 0.040 Uiso 1 1 calc R . . H44D H 0.3122 0.1819 0.2848 0.040 Uiso 1 1 calc R . . C443 C 0.23906(16) 0.2814(2) 0.23828(10) 0.0393(6) Uani 1 1 d . . . H44E H 0.2876 0.3205 0.2363 0.047 Uiso 1 1 calc R . . H44F H 0.1919 0.3227 0.2401 0.047 Uiso 1 1 calc R . . C444 C 0.21176(19) 0.2220(2) 0.19057(11) 0.0518(7) Uani 1 1 d . . . H44G H 0.2589 0.1825 0.1880 0.078 Uiso 1 1 calc R . . H44H H 0.1954 0.2622 0.1609 0.078 Uiso 1 1 calc R . . H44I H 0.1635 0.1834 0.1923 0.078 Uiso 1 1 calc R . . N2 N 0.74659(12) 0.13358(13) 0.20087(8) 0.0317(4) Uani 1 1 d . . . C211 C 0.82095(15) 0.19598(17) 0.20073(10) 0.0361(5) Uani 1 1 d . . . H21A H 0.8004 0.2469 0.1765 0.043 Uiso 1 1 calc R . . H21B H 0.8418 0.2239 0.2346 0.043 Uiso 1 1 calc R . . C212 C 0.89458(16) 0.14947(19) 0.18723(11) 0.0408(6) Uani 1 1 d . . . H21C H 0.8772 0.1299 0.1514 0.049 Uiso 1 1 calc R . . H21D H 0.9114 0.0936 0.2083 0.049 Uiso 1 1 calc R . . C213 C 0.97023(17) 0.2157(2) 0.19565(12) 0.0476(7) Uani 1 1 d . . . H21E H 1.0112 0.1908 0.1783 0.057 Uiso 1 1 calc R . . H21F H 0.9502 0.2762 0.1801 0.057 Uiso 1 1 calc R . . C214 C 1.01463(19) 0.2302(3) 0.25055(13) 0.0606(9) Uani 1 1 d . . . H21G H 0.9742 0.2535 0.2681 0.091 Uiso 1 1 calc R . . H21H H 1.0604 0.2752 0.2537 0.091 Uiso 1 1 calc R . . H21I H 1.0382 0.1714 0.2656 0.091 Uiso 1 1 calc R . . C221 C 0.77154(16) 0.05557(16) 0.23876(11) 0.0337(5) Uani 1 1 d . . . H22A H 0.8141 0.0166 0.2289 0.040 Uiso 1 1 calc R . . H22B H 0.7211 0.0167 0.2366 0.040 Uiso 1 1 calc R . . C222 C 0.80746(19) 0.0851(2) 0.29326(11) 0.0438(6) Uani 1 1 d . . . H22C H 0.7621 0.1135 0.3058 0.053 Uiso 1 1 calc R . . H22D H 0.8519 0.1322 0.2952 0.053 Uiso 1 1 calc R . . C223 C 0.84492(18) 0.0031(2) 0.32671(11) 0.0454(6) Uani 1 1 d . . . H22E H 0.8557 0.0218 0.3625 0.055 Uiso 1 1 calc R . . H22F H 0.8028 -0.0475 0.3206 0.055 Uiso 1 1 calc R . . C224 C 0.9261(2) -0.0332(2) 0.31806(14) 0.0580(8) Uani 1 1 d . . . H22G H 0.9162 -0.0519 0.2827 0.087 Uiso 1 1 calc R . . H22H H 0.9456 -0.0866 0.3400 0.087 Uiso 1 1 calc R . . H22I H 0.9693 0.0154 0.3258 0.087 Uiso 1 1 calc R . . C231 C 0.71201(15) 0.08820(17) 0.14981(10) 0.0334(5) Uani 1 1 d . . . H23A H 0.7565 0.0480 0.1431 0.040 Uiso 1 1 calc R . . H23B H 0.6640 0.0481 0.1515 0.040 Uiso 1 1 calc R . . C232 C 0.68238(18) 0.15408(19) 0.10596(10) 0.0422(6) Uani 1 1 d . . . H23C H 0.7306 0.1917 0.1021 0.051 Uiso 1 1 calc R . . H23D H 0.6391 0.1964 0.1125 0.051 Uiso 1 1 calc R . . C233 C 0.6451(2) 0.0994(2) 0.05782(11) 0.0493(7) Uani 1 1 d . . . H23E H 0.5957 0.0637 0.0616 0.059 Uiso 1 1 calc R . . H23F H 0.6878 0.0549 0.0526 0.059 Uiso 1 1 calc R . . C234 C 0.6175(2) 0.1626(3) 0.01152(13) 0.0666(9) Uani 1 1 d . . . H23G H 0.5787 0.2099 0.0177 0.100 Uiso 1 1 calc R . . H23H H 0.5889 0.1258 -0.0180 0.100 Uiso 1 1 calc R . . H23I H 0.6674 0.1925 0.0053 0.100 Uiso 1 1 calc R . . C241 C 0.68113(15) 0.19621(16) 0.21387(10) 0.0344(5) Uani 1 1 d . . . H24A H 0.7064 0.2235 0.2475 0.041 Uiso 1 1 calc R . . H24B H 0.6689 0.2476 0.1892 0.041 Uiso 1 1 calc R . . C242 C 0.59824(15) 0.15117(17) 0.21453(11) 0.0367(5) Uani 1 1 d . . . H24C H 0.6086 0.1014 0.2402 0.044 Uiso 1 1 calc R . . H24D H 0.5717 0.1233 0.1812 0.044 Uiso 1 1 calc R . . C243 C 0.53945(16) 0.22338(18) 0.22685(12) 0.0416(6) Uani 1 1 d . . . H24E H 0.5663 0.2503 0.2604 0.050 Uiso 1 1 calc R . . H24F H 0.5310 0.2738 0.2017 0.050 Uiso 1 1 calc R . . C244 C 0.45402(18) 0.1832(2) 0.22701(13) 0.0511(7) Uani 1 1 d . . . H24G H 0.4258 0.1595 0.1933 0.077 Uiso 1 1 calc R . . H24H H 0.4190 0.2315 0.2362 0.077 Uiso 1 1 calc R . . H24I H 0.4621 0.1327 0.2516 0.077 Uiso 1 1 calc R . . O1S O 0.3737(3) 0.0318(2) 0.68861(13) 0.1029(11) Uani 1 1 d . . . H1S H 0.4083 0.0435 0.7165 0.154 Uiso 1 1 calc R . . C1S C 0.3860(3) 0.0927(3) 0.65275(18) 0.0819(12) Uani 1 1 d . . . H1S1 H 0.4448 0.0867 0.6502 0.098 Uiso 1 1 calc R . . H1S2 H 0.3786 0.1566 0.6638 0.098 Uiso 1 1 calc R . . C2S C 0.3262(4) 0.0771(4) 0.60169(19) 0.112(2) Uani 1 1 d . . . H2S1 H 0.3387 0.1211 0.5776 0.168 Uiso 1 1 calc R . . H2S2 H 0.2679 0.0859 0.6036 0.168 Uiso 1 1 calc R . . H2S3 H 0.3331 0.0139 0.5906 0.168 Uiso 1 1 calc R . . 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 Pt1 0.02279(6) 0.02316(5) 0.03807(6) 0.00087(3) 0.00803(4) -0.00030(3) N1 0.0231(10) 0.0277(10) 0.0374(11) -0.0018(8) 0.0125(8) -0.0015(7) C2 0.0280(12) 0.0292(12) 0.0388(13) -0.0008(9) 0.0151(10) 0.0003(9) C3 0.0222(12) 0.0326(12) 0.0416(13) -0.0028(10) 0.0112(10) -0.0024(9) C31 0.0221(12) 0.0306(12) 0.0446(14) 0.0039(10) 0.0105(10) 0.0007(9) O311 0.0230(9) 0.0497(12) 0.0467(11) -0.0003(8) 0.0081(8) -0.0007(7) O312 0.0260(9) 0.0365(9) 0.0453(10) 0.0011(8) 0.0153(8) 0.0027(7) C4 0.0245(13) 0.0598(18) 0.0399(14) -0.0073(12) 0.0065(11) -0.0051(11) C5 0.0303(14) 0.069(2) 0.0385(14) -0.0094(13) 0.0141(11) -0.0041(12) C6 0.0232(12) 0.0421(14) 0.0428(14) -0.0025(11) 0.0138(10) -0.0015(9) C7 0.0208(12) 0.0403(14) 0.0477(15) -0.0029(11) 0.0109(11) -0.0007(9) C8 0.0306(14) 0.0615(18) 0.0430(15) -0.0056(12) 0.0156(12) -0.0034(12) C9 0.0308(14) 0.0449(15) 0.0534(17) 0.0001(12) 0.0216(12) 0.0000(10) C10 0.0235(12) 0.0258(11) 0.0554(16) 0.0025(10) 0.0156(11) 0.0020(8) C101 0.0245(13) 0.0242(12) 0.0673(19) 0.0069(11) 0.0151(12) 0.0011(9) O101 0.0281(10) 0.0463(11) 0.0697(14) 0.0027(10) 0.0094(10) -0.0040(9) O102 0.0267(10) 0.0383(10) 0.0767(15) 0.0034(9) 0.0240(10) 0.0030(7) C11 0.0243(12) 0.0229(11) 0.0518(15) 0.0005(10) 0.0080(11) -0.0006(8) N12 0.0215(10) 0.0271(10) 0.0423(11) 0.0004(8) 0.0099(8) -0.0006(7) S13 0.0292(3) 0.0315(3) 0.0459(4) 0.0066(3) 0.0024(3) -0.0017(2) C14 0.0468(17) 0.0232(12) 0.0444(15) 0.0019(10) 0.0012(12) 0.0001(10) C15 0.057(2) 0.0386(15) 0.0511(18) -0.0005(13) -0.0057(15) -0.0020(14) C16 0.083(3) 0.0460(17) 0.0453(18) -0.0068(14) -0.0054(17) -0.0014(17) C20B 0.092(6) 0.075(5) 0.035(3) -0.006(3) -0.002(3) -0.006(4) C17 0.101(3) 0.0495(18) 0.0388(16) -0.0075(14) 0.0125(18) 0.0041(19) C20A 0.142(9) 0.109(7) 0.039(4) -0.009(4) 0.017(5) 0.026(7) C18 0.068(2) 0.0376(14) 0.0462(16) -0.0054(12) 0.0150(15) 0.0033(14) C19 0.0514(17) 0.0245(12) 0.0370(13) -0.0018(10) 0.0086(12) 0.0001(10) S21 0.0320(3) 0.0329(3) 0.0361(3) -0.0006(2) 0.0094(3) -0.0010(2) N4 0.0278(10) 0.0242(9) 0.0407(11) 0.0010(8) 0.0053(8) -0.0001(8) C411 0.0295(12) 0.0263(11) 0.0461(14) -0.0034(10) 0.0071(10) -0.0007(9) C412 0.0456(16) 0.0360(14) 0.0464(15) -0.0010(11) 0.0050(12) -0.0004(11) C413 0.0516(17) 0.0440(15) 0.0466(16) -0.0068(13) 0.0027(13) 0.0043(13) C414 0.070(2) 0.064(2) 0.0502(18) -0.0071(15) 0.0021(16) 0.0080(18) C421 0.0328(13) 0.0255(11) 0.0473(14) 0.0022(10) 0.0069(11) 0.0051(9) C422 0.0326(13) 0.0315(12) 0.0482(15) -0.0005(11) 0.0076(11) 0.0048(10) C423 0.0409(16) 0.0409(16) 0.098(3) 0.0058(16) 0.0222(17) 0.0127(13) C424 0.0412(17) 0.0528(18) 0.077(2) 0.0065(16) 0.0236(16) 0.0117(14) C431 0.0342(13) 0.0269(12) 0.0458(14) 0.0012(10) 0.0104(11) -0.0058(9) C432 0.0327(13) 0.0310(12) 0.0541(16) 0.0017(11) 0.0135(11) -0.0063(10) C433 0.0440(16) 0.0416(15) 0.0670(19) 0.0002(14) 0.0219(14) -0.0110(13) C434 0.0420(17) 0.0564(19) 0.083(2) -0.0051(17) 0.0264(16) -0.0135(14) C441 0.0253(11) 0.0256(11) 0.0423(13) 0.0040(9) 0.0082(10) 0.0007(9) C442 0.0275(12) 0.0283(12) 0.0449(14) -0.0011(10) 0.0089(10) -0.0007(9) C443 0.0309(13) 0.0425(15) 0.0451(15) 0.0057(11) 0.0115(11) 0.0041(10) C444 0.0418(16) 0.066(2) 0.0449(16) 0.0005(14) 0.0072(13) -0.0005(14) N2 0.0241(10) 0.0241(10) 0.0482(12) -0.0041(8) 0.0119(8) -0.0027(7) C211 0.0261(12) 0.0304(12) 0.0539(15) -0.0064(11) 0.0141(11) -0.0090(9) C212 0.0312(13) 0.0392(14) 0.0545(16) -0.0077(12) 0.0158(12) -0.0068(11) C213 0.0303(14) 0.0460(15) 0.070(2) -0.0034(14) 0.0195(13) -0.0102(11) C214 0.0351(16) 0.068(2) 0.077(2) -0.0125(17) 0.0113(15) -0.0175(15) C221 0.0254(12) 0.0297(12) 0.0472(14) -0.0027(10) 0.0118(10) -0.0011(9) C222 0.0437(16) 0.0403(14) 0.0477(16) -0.0070(12) 0.0127(13) 0.0020(12) C223 0.0418(16) 0.0475(16) 0.0448(15) -0.0033(12) 0.0076(12) -0.0018(12) C224 0.0402(18) 0.063(2) 0.062(2) -0.0050(16) -0.0016(15) 0.0080(14) C231 0.0260(12) 0.0303(12) 0.0456(14) -0.0052(10) 0.0126(10) -0.0023(9) C232 0.0401(14) 0.0362(14) 0.0497(15) 0.0002(12) 0.0111(12) -0.0031(11) C233 0.0498(18) 0.0477(17) 0.0499(17) -0.0026(13) 0.0122(14) 0.0053(13) C234 0.072(2) 0.074(2) 0.0516(19) 0.0072(17) 0.0126(17) 0.0034(19) C241 0.0282(12) 0.0248(11) 0.0529(15) -0.0053(10) 0.0154(11) 0.0004(9) C242 0.0279(12) 0.0295(12) 0.0560(15) -0.0053(11) 0.0169(11) 0.0010(10) C243 0.0320(13) 0.0317(13) 0.0655(18) -0.0057(12) 0.0205(12) 0.0019(10) C244 0.0351(15) 0.0452(16) 0.081(2) -0.0073(15) 0.0302(15) -0.0003(12) O1S 0.123(3) 0.091(2) 0.088(2) 0.0022(19) 0.016(2) -0.019(2) C1S 0.077(3) 0.070(3) 0.106(4) -0.010(2) 0.036(3) -0.012(2) C2S 0.175(6) 0.081(3) 0.078(3) 0.000(3) 0.031(4) 0.011(4) _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 Pt1 N12 2.047(2) . ? Pt1 N1 2.052(2) . ? Pt1 S13 2.2489(7) . ? Pt1 S21 2.2528(7) . ? N1 C2 1.347(3) . ? N1 C6 1.368(3) . ? C2 C3 1.373(4) . ? C3 C4 1.385(4) . ? C3 C31 1.534(3) . ? C31 O312 1.238(3) . ? C31 O311 1.261(3) . ? C4 C5 1.387(4) . ? C5 C6 1.373(4) . ? C6 C7 1.469(3) . ? C7 N12 1.361(4) . ? C7 C8 1.385(4) . ? C8 C9 1.390(4) . ? C9 C10 1.369(4) . ? C10 C11 1.383(4) . ? C10 C101 1.528(4) . ? C101 O102 1.245(4) . ? C101 O101 1.245(4) . ? C11 N12 1.357(3) . ? S13 C14 1.754(3) . ? C14 C15 1.393(4) . ? C14 C19 1.396(4) . ? C15 C16 1.374(5) . ? C16 C17 1.393(6) . ? C16 C20B 1.499(8) . ? C17 C18 1.379(5) . ? C17 C20A 1.638(9) . ? C18 C19 1.391(4) . ? C19 S21 1.762(3) . ? N4 C421 1.517(3) . ? N4 C431 1.518(3) . ? N4 C441 1.520(3) . ? N4 C411 1.532(3) . ? C411 C412 1.510(4) . ? C412 C413 1.523(4) . ? C413 C414 1.536(4) . ? C421 C422 1.519(3) . ? C422 C423 1.520(4) . ? C423 C424 1.510(4) . ? C431 C432 1.521(4) . ? C432 C433 1.519(3) . ? C433 C434 1.515(4) . ? C441 C442 1.519(3) . ? C442 C443 1.523(4) . ? C443 C444 1.532(4) . ? N2 C231 1.516(3) . ? N2 C221 1.517(3) . ? N2 C211 1.519(3) . ? N2 C241 1.520(3) . ? C211 C212 1.514(3) . ? C212 C213 1.536(3) . ? C213 C214 1.506(4) . ? C221 C222 1.518(4) . ? C222 C223 1.527(4) . ? C223 C224 1.509(4) . ? C231 C232 1.512(4) . ? C232 C233 1.523(4) . ? C233 C234 1.535(4) . ? C241 C242 1.513(3) . ? C242 C243 1.521(3) . ? C243 C244 1.519(4) . ? O1S C1S 1.377(5) . ? C1S C2S 1.499(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 N12 Pt1 N1 79.80(8) . . ? N12 Pt1 S13 94.80(6) . . ? N1 Pt1 S13 174.55(6) . . ? N12 Pt1 S21 175.72(6) . . ? N1 Pt1 S21 95.92(6) . . ? S13 Pt1 S21 89.48(3) . . ? C2 N1 C6 118.5(2) . . ? C2 N1 Pt1 127.00(17) . . ? C6 N1 Pt1 114.54(17) . . ? N1 C2 C3 123.2(2) . . ? C2 C3 C4 118.1(2) . . ? C2 C3 C31 119.8(2) . . ? C4 C3 C31 122.1(2) . . ? O312 C31 O311 127.3(2) . . ? O312 C31 C3 116.7(2) . . ? O311 C31 C3 116.0(2) . . ? C3 C4 C5 119.5(3) . . ? C6 C5 C4 119.8(3) . . ? N1 C6 C5 120.9(2) . . ? N1 C6 C7 115.3(2) . . ? C5 C6 C7 123.8(2) . . ? N12 C7 C8 121.3(2) . . ? N12 C7 C6 115.1(2) . . ? C8 C7 C6 123.5(3) . . ? C7 C8 C9 118.7(3) . . ? C10 C9 C8 120.5(3) . . ? C9 C10 C11 118.5(2) . . ? C9 C10 C101 121.2(2) . . ? C11 C10 C101 120.4(3) . . ? O102 C101 O101 127.9(3) . . ? O102 C101 C10 115.3(3) . . ? O101 C101 C10 116.8(3) . . ? N12 C11 C10 122.3(3) . . ? C11 N12 C7 118.7(2) . . ? C11 N12 Pt1 126.23(19) . . ? C7 N12 Pt1 115.06(17) . . ? C14 S13 Pt1 104.68(10) . . ? C15 C14 C19 119.4(3) . . ? C15 C14 S13 119.9(3) . . ? C19 C14 S13 120.7(2) . . ? C16 C15 C14 120.9(3) . . ? C15 C16 C17 119.8(3) . . ? C15 C16 C20B 115.1(5) . . ? C17 C16 C20B 125.0(5) . . ? C18 C17 C16 119.7(3) . . ? C18 C17 C20A 116.2(5) . . ? C16 C17 C20A 124.0(5) . . ? C17 C18 C19 120.9(3) . . ? C18 C19 C14 119.3(3) . . ? C18 C19 S21 120.9(3) . . ? C14 C19 S21 119.8(2) . . ? C19 S21 Pt1 104.60(10) . . ? C421 N4 C431 106.04(17) . . ? C421 N4 C441 110.67(18) . . ? C431 N4 C441 111.07(18) . . ? C421 N4 C411 111.55(18) . . ? C431 N4 C411 111.59(19) . . ? C441 N4 C411 106.01(17) . . ? C412 C411 N4 115.0(2) . . ? C411 C412 C413 111.3(2) . . ? C412 C413 C414 111.7(3) . . ? N4 C421 C422 116.45(19) . . ? C421 C422 C423 109.9(2) . . ? C424 C423 C422 113.0(3) . . ? N4 C431 C432 115.52(19) . . ? C433 C432 C431 110.3(2) . . ? C434 C433 C432 112.2(2) . . ? C442 C441 N4 115.06(19) . . ? C441 C442 C443 109.2(2) . . ? C442 C443 C444 112.0(2) . . ? C231 N2 C221 106.24(18) . . ? C231 N2 C211 110.88(18) . . ? C221 N2 C211 112.04(19) . . ? C231 N2 C241 111.34(19) . . ? C221 N2 C241 111.08(19) . . ? C211 N2 C241 105.37(17) . . ? C212 C211 N2 115.5(2) . . ? C211 C212 C213 110.6(2) . . ? C214 C213 C212 113.1(2) . . ? N2 C221 C222 115.5(2) . . ? C221 C222 C223 111.3(2) . . ? C224 C223 C222 113.9(3) . . ? C232 C231 N2 115.3(2) . . ? C231 C232 C233 109.5(2) . . ? C232 C233 C234 111.9(3) . . ? C242 C241 N2 116.13(19) . . ? C241 C242 C243 109.4(2) . . ? C244 C243 C242 112.3(2) . . ? O1S C1S C2S 113.0(4) . . ? _diffrn_measured_fraction_theta_max 0.926 _diffrn_reflns_theta_full 28.95 _diffrn_measured_fraction_theta_full 0.926 _refine_diff_density_max 1.713 _refine_diff_density_min -0.634 _refine_diff_density_rms 0.095