# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full J.Mater.Chem. _journal_coden_Cambridge 1145 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Simon Higgins' _publ_contact_author_email SHIGGINS@LIVERPOOL.AC.UK _publ_section_title ; Synthesis and characterization of monomeric and polymeric Pd(II) and Pt(II) complexes of 3,4-ethylenedioxythiophene-functionalized phosphine ligands ; loop_ _publ_author_name 'Simon Higgins' 'John Bacsa' 'Wolfgang Haiss' 'Richard Nichols' 'R. M. G. Rajapakse' ; K.Velauthamurty ; 'Harm van Zalinge' data_kugpd30 _database_code_depnum_ccdc_archive 'CCDC 699407' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common kugpd30 _chemical_melting_point ? _chemical_formula_moiety 'C36 H30 Cl2 O4 P2 Pd S2, C H Cl3' _chemical_formula_sum 'C37 H31 Cl5 O4 P2 Pd S2' _chemical_formula_weight 949.37 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' Cl Cl 0.1484 0.1585 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.602(4) _cell_length_b 12.373(4) _cell_length_c 15.379(6) _cell_angle_alpha 72.451(7) _cell_angle_beta 89.477(6) _cell_angle_gamma 65.076(5) _cell_volume 1891(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1482 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 27.7 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.658 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 956 _exptl_absorpt_coefficient_mu 1.073 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9002 _exptl_absorpt_correction_T_max 0.9893 _exptl_absorpt_process_details 'SADABS-2008/1 (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker D8 diffractometer with APEX detector' _diffrn_measurement_method '\w scans with a narrow frame width' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8515 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1013 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 21.03 _reflns_number_total 3161 _reflns_number_gt 2669 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART v.5.632 (Bruker, 2005)' _computing_cell_refinement 'SAINT v6.45a (Bruker, 2005)' _computing_data_reduction 'SAINT v6.45a (Bruker, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0001P)^2^+46.7224P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3161 _refine_ls_number_parameters 259 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1292 _refine_ls_R_factor_gt 0.1087 _refine_ls_wR_factor_ref 0.2138 _refine_ls_wR_factor_gt 0.2043 _refine_ls_goodness_of_fit_ref 1.280 _refine_ls_restrained_S_all 1.280 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags Pd1 Pd Uani 0.00000 0.00000 0.50000 1.000 0.0151(8) . . Cl1 Cl Uani -0.0989(5) -0.0974(4) 0.4458(4) 1.000 0.0235(19) . . S1 S Uani 0.1037(5) 0.1551(5) 0.3212(4) 1.000 0.0269(19) . . P1 P Uani -0.1434(5) 0.1994(5) 0.4025(4) 1.000 0.0164(19) . . O1 O Uiso -0.2222(13) 0.4379(12) 0.2040(9) 1.000 0.033(4) . . O2 O Uiso -0.0187(13) 0.4367(13) 0.0939(10) 1.000 0.037(4) . . C1 C Uiso -0.0605(17) 0.2493(17) 0.3129(13) 1.000 0.019(5) . . C2 C Uiso 0.1166(19) 0.2458(17) 0.2160(13) 1.000 0.025(5) . . C3 C Uiso 0.0033(19) 0.3459(18) 0.1775(14) 1.000 0.027(5) . . C4 C Uiso -0.152(2) 0.509(2) 0.0556(17) 1.000 0.049(7) . . C5 C Uiso -0.234(3) 0.539(2) 0.1231(19) 1.000 0.064(8) . . C6 C Uiso -0.0984(16) 0.3499(16) 0.2323(12) 1.000 0.012(4) . . C7 C Uiso -0.2158(17) 0.3166(16) 0.4614(13) 1.000 0.014(5) . . C8 C Uiso -0.2587(18) 0.4432(17) 0.4157(15) 1.000 0.024(5) . . C9 C Uiso -0.3254(19) 0.530(2) 0.4599(15) 1.000 0.032(6) . . C10 C Uiso -0.3497(19) 0.4852(19) 0.5478(14) 1.000 0.030(6) . . C11 C Uiso -0.3075(18) 0.3619(17) 0.5924(15) 1.000 0.025(5) . . C12 C Uiso -0.2393(17) 0.2762(18) 0.5505(14) 1.000 0.020(5) . . C13 C Uiso -0.2842(17) 0.2091(17) 0.3436(14) 1.000 0.018(5) . . C14 C Uiso -0.285(2) 0.1950(18) 0.2578(15) 1.000 0.033(6) . . C15 C Uiso -0.3868(18) 0.1926(17) 0.2182(15) 1.000 0.026(5) . . C16 C Uiso -0.495(2) 0.2122(18) 0.2599(15) 1.000 0.029(6) . . C17 C Uiso -0.498(2) 0.2248(18) 0.3451(15) 1.000 0.030(6) . . C18 C Uiso -0.3915(18) 0.2239(17) 0.3855(14) 1.000 0.023(5) . . Pd2 Pd Uani 0.50000 0.00000 0.00000 1.000 0.0177(8) . . Cl2 Cl Uani 0.4256(5) 0.1731(4) 0.0481(4) 1.000 0.0230(19) . . S2 S Uani 0.1579(5) 0.1611(5) 0.0020(4) 1.000 0.0359(19) . . P2 P Uani 0.3966(5) -0.0793(5) 0.1140(4) 1.000 0.0204(19) . . O3 O Uiso -0.1024(14) 0.0713(13) 0.1153(10) 1.000 0.040(4) . . O4 O Uiso 0.1546(12) -0.1132(12) 0.2006(9) 1.000 0.029(4) . . C19 C Uiso 0.2255(18) 0.0186(17) 0.0915(13) 1.000 0.019(5) . . C20 C Uiso 0.006(2) 0.179(2) 0.0178(15) 1.000 0.035(6) . . C21 C Uiso 0.0057(18) 0.0830(17) 0.0865(13) 1.000 0.019(5) . . C22 C Uiso -0.072(3) -0.049(2) 0.1791(18) 1.000 0.063(8) . . C23 C Uiso 0.040(2) -0.105(2) 0.2404(18) 1.000 0.060(8) . . C24 C Uiso 0.1319(18) -0.0102(18) 0.1301(14) 1.000 0.025(5) . . C25 C Uiso 0.4047(18) -0.2328(17) 0.1213(14) 1.000 0.021(5) . . C26 C Uiso 0.348(2) -0.244(2) 0.0479(16) 1.000 0.041(6) . . C27 C Uiso 0.3567(19) -0.3564(18) 0.0483(15) 1.000 0.030(6) . . C28 C Uiso 0.424(2) -0.465(2) 0.1251(15) 1.000 0.042(6) . . C29 C Uiso 0.471(2) -0.4511(19) 0.1980(15) 1.000 0.033(6) . . C30 C Uiso 0.4679(19) -0.3388(18) 0.1971(15) 1.000 0.029(6) . . C31 C Uiso 0.4595(18) -0.0926(17) 0.2266(13) 1.000 0.018(5) . . C32 C Uiso 0.5844(19) -0.1154(17) 0.2437(14) 1.000 0.027(5) . . C33 C Uiso 0.635(2) -0.1223(17) 0.3273(14) 1.000 0.026(5) . . C34 C Uiso 0.5569(18) -0.0992(17) 0.3940(15) 1.000 0.025(5) . . C35 C Uiso 0.433(2) -0.0750(18) 0.3756(15) 1.000 0.029(5) . . C36 C Uiso 0.3809(19) -0.0701(17) 0.2970(14) 1.000 0.022(5) . . Cl1S Cl Uani -0.0884(6) 0.6366(6) 0.3060(6) 1.000 0.073(3) . . Cl2S Cl Uani 0.1659(7) 0.5288(8) 0.2577(5) 1.000 0.071(3) . . Cl3S Cl Uani 0.0965(7) 0.3879(6) 0.4178(5) 1.000 0.070(3) . . C1S C Uiso 0.071(2) 0.538(2) 0.3476(17) 1.000 0.047(7) . . H2 H Uiso 0.19330 0.22780 0.18880 1.000 0.0300 calc R H4A H Uiso -0.16400 0.58750 0.00740 1.000 0.0590 calc R H4B H Uiso -0.17760 0.45960 0.02630 1.000 0.0590 calc R H5A H Uiso -0.32330 0.58160 0.09280 1.000 0.0770 calc R H5B H Uiso -0.21790 0.60090 0.14310 1.000 0.0770 calc R H8 H Uiso -0.24300 0.47130 0.35420 1.000 0.0290 calc R H9 H Uiso -0.35320 0.61800 0.43020 1.000 0.0380 calc R H10 H Uiso -0.39800 0.54360 0.57780 1.000 0.0360 calc R H11 H Uiso -0.32510 0.33400 0.65330 1.000 0.0300 calc R H12 H Uiso -0.20790 0.18870 0.58270 1.000 0.0240 calc R H14 H Uiso -0.21300 0.18680 0.22620 1.000 0.0390 calc R H15 H Uiso -0.38320 0.17720 0.16120 1.000 0.0310 calc R H16 H Uiso -0.56900 0.21700 0.22950 1.000 0.0350 calc R H17 H Uiso -0.57080 0.23410 0.37590 1.000 0.0360 calc R H18 H Uiso -0.39300 0.23380 0.44440 1.000 0.0280 calc R H20 H Uiso -0.06930 0.24850 -0.01820 1.000 0.0420 calc R H22A H Uiso -0.14470 -0.04200 0.21510 1.000 0.0760 calc R H22B H Uiso -0.06630 -0.10630 0.14430 1.000 0.0760 calc R H23A H Uiso 0.05390 -0.19080 0.27710 1.000 0.0720 calc R H23B H Uiso 0.02720 -0.05640 0.28340 1.000 0.0720 calc R H26 H Uiso 0.30280 -0.17130 -0.00390 1.000 0.0500 calc R H27 H Uiso 0.31760 -0.36210 -0.00300 1.000 0.0360 calc R H28 H Uiso 0.43500 -0.54580 0.12520 1.000 0.0500 calc R H29 H Uiso 0.50830 -0.52170 0.25250 1.000 0.0400 calc R H30 H Uiso 0.50870 -0.33410 0.24810 1.000 0.0350 calc R H32 H Uiso 0.63770 -0.12690 0.19690 1.000 0.0320 calc R H33 H Uiso 0.72350 -0.14260 0.33870 1.000 0.0310 calc R H34 H Uiso 0.58880 -0.10030 0.45100 1.000 0.0300 calc R H35 H Uiso 0.37920 -0.06060 0.42190 1.000 0.0350 calc R H36 H Uiso 0.29310 -0.05190 0.28780 1.000 0.0260 calc R H1S H Uiso 0.09970 0.57650 0.38640 1.000 0.0570 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 Pd1 0.0105(12) 0.0135(12) 0.0155(15) -0.0041(11) 0.0012(11) -0.0004(10) Cl1 0.020(3) 0.023(3) 0.026(4) -0.011(3) 0.000(3) -0.006(2) S1 0.026(3) 0.028(3) 0.019(4) -0.006(3) 0.009(3) -0.006(3) P1 0.016(3) 0.017(3) 0.014(4) -0.004(3) 0.007(3) -0.006(2) Pd2 0.0148(13) 0.0189(12) 0.0156(16) -0.0057(11) 0.0072(11) -0.0041(10) Cl2 0.028(3) 0.021(3) 0.021(4) -0.017(3) 0.013(3) -0.005(2) S2 0.021(3) 0.039(3) 0.031(4) -0.001(3) -0.001(3) -0.005(3) P2 0.014(3) 0.021(3) 0.020(4) -0.007(3) 0.004(3) -0.002(2) Cl1S 0.037(4) 0.056(4) 0.119(7) -0.020(5) 0.008(4) -0.019(3) Cl2S 0.049(4) 0.108(6) 0.073(6) -0.050(5) 0.024(4) -0.038(4) Cl3S 0.052(4) 0.055(4) 0.095(6) -0.018(4) -0.012(4) -0.021(4) _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; 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 Pd1 Cl1 2.292(6) . . yes Pd1 P1 2.336(6) . . yes Pd1 Cl1 2.292(6) . 2_556 yes Pd1 P1 2.336(6) . 2_556 yes Pd2 P2 2.322(6) . . yes Pd2 Cl2 2.295(5) . 2_655 yes Pd2 Cl2 2.295(5) . . yes Pd2 P2 2.322(6) . 2_655 yes Cl1S C1S 1.72(3) . . yes Cl2S C1S 1.76(3) . . yes Cl3S C1S 1.74(3) . . yes S1 C1 1.75(2) . . yes S1 C2 1.72(2) . . yes S2 C19 1.74(2) . . yes S2 C20 1.71(3) . . yes P1 C1 1.78(2) . . yes P1 C7 1.84(2) . . yes P1 C13 1.82(2) . . yes P2 C19 1.81(2) . . yes P2 C25 1.83(2) . . yes P2 C31 1.82(2) . . yes O1 C5 1.43(3) . . yes O1 C6 1.36(2) . . yes O2 C3 1.37(3) . . yes O2 C4 1.44(3) . . yes O3 C21 1.38(3) . . yes O3 C22 1.41(3) . . yes O4 C23 1.44(3) . . yes O4 C24 1.33(2) . . yes C1 C6 1.38(3) . . no C2 C3 1.35(3) . . no C3 C6 1.44(3) . . no C4 C5 1.43(4) . . no C7 C8 1.37(3) . . no C7 C12 1.38(3) . . no C8 C9 1.39(3) . . no C9 C10 1.37(3) . . no C10 C11 1.34(3) . . no C11 C12 1.36(3) . . no C13 C14 1.38(3) . . no C13 C18 1.37(3) . . no C14 C15 1.35(3) . . no C15 C16 1.37(3) . . no C16 C17 1.36(3) . . no C17 C18 1.38(3) . . no C2 H2 0.9500 . . no C4 H4B 0.9900 . . no C4 H4A 0.9800 . . no C5 H5A 0.9800 . . no C5 H5B 0.9900 . . no C8 H8 0.9500 . . no C9 H9 0.9500 . . no C10 H10 0.9500 . . no C11 H11 0.9500 . . no C12 H12 0.9500 . . no C14 H14 0.9500 . . no C15 H15 0.9500 . . no C16 H16 0.9500 . . no C17 H17 0.9500 . . no C18 H18 0.9500 . . no C19 C24 1.36(3) . . no C20 C21 1.33(3) . . no C21 C24 1.43(3) . . no C22 C23 1.39(4) . . no C25 C30 1.38(3) . . no C25 C26 1.38(3) . . no C26 C27 1.35(3) . . no C27 C28 1.41(3) . . no C28 C29 1.34(3) . . no C29 C30 1.37(3) . . no C31 C36 1.43(3) . . no C31 C32 1.37(3) . . no C32 C33 1.38(3) . . no C33 C34 1.38(3) . . no C34 C35 1.35(3) . . no C35 C36 1.33(3) . . no C20 H20 0.9500 . . no C22 H22B 0.9900 . . no C22 H22A 0.9900 . . no C23 H23B 0.9900 . . no C23 H23A 0.9800 . . no C26 H26 0.9500 . . no C27 H27 0.9500 . . no C28 H28 0.9500 . . no C29 H29 0.9500 . . no C30 H30 0.9500 . . no C32 H32 0.9500 . . no C33 H33 0.9500 . . no C34 H34 0.9500 . . no C35 H35 0.9500 . . no C36 H36 0.9500 . . no C1S H1S 1.0000 . . no 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 Pd1 P1 92.2(2) . . . yes Cl1 Pd1 Cl1 180.00 . . 2_556 yes Cl1 Pd1 P1 87.8(2) . . 2_556 yes Cl1 Pd1 P1 87.8(2) 2_556 . . yes P1 Pd1 P1 180.00 . . 2_556 yes Cl1 Pd1 P1 92.2(2) 2_556 . 2_556 yes Cl2 Pd2 Cl2 180.00 . . 2_655 yes Cl2 Pd2 P2 94.3(2) . . 2_655 yes Cl2 Pd2 P2 94.3(2) 2_655 . . yes P2 Pd2 P2 180.00 . . 2_655 yes Cl2 Pd2 P2 85.7(2) 2_655 . 2_655 yes Cl2 Pd2 P2 85.7(2) . . . yes C1 S1 C2 93.5(10) . . . yes C19 S2 C20 92.2(11) . . . yes Pd1 P1 C1 107.6(7) . . . yes Pd1 P1 C7 113.9(7) . . . yes Pd1 P1 C13 116.6(7) . . . yes C1 P1 C7 111.6(10) . . . yes C1 P1 C13 104.9(10) . . . yes C7 P1 C13 101.8(10) . . . yes Pd2 P2 C25 115.5(7) . . . yes Pd2 P2 C31 110.8(7) . . . yes Pd2 P2 C19 111.1(7) . . . yes C19 P2 C31 110.0(10) . . . yes C25 P2 C31 107.7(10) . . . yes C19 P2 C25 101.4(10) . . . yes C5 O1 C6 111.9(19) . . . yes C3 O2 C4 114.0(18) . . . yes C21 O3 C22 112(2) . . . yes C23 O4 C24 111.4(17) . . . yes P1 C1 C6 133.6(17) . . . yes S1 C1 P1 117.7(11) . . . yes S1 C1 C6 108.7(15) . . . yes S1 C2 C3 110.9(17) . . . yes O2 C3 C6 121.0(19) . . . yes C2 C3 C6 113.5(18) . . . no O2 C3 C2 126(2) . . . yes O2 C4 C5 113(2) . . . yes O1 C5 C4 118(2) . . . yes O1 C6 C3 123.4(16) . . . yes C1 C6 C3 113.4(18) . . . no O1 C6 C1 123.0(18) . . . yes P1 C7 C12 118.4(15) . . . yes P1 C7 C8 121.5(15) . . . yes C8 C7 C12 119.7(19) . . . no C7 C8 C9 120(2) . . . no C8 C9 C10 118(2) . . . no C9 C10 C11 122(2) . . . no C10 C11 C12 120(2) . . . no C7 C12 C11 120(2) . . . no P1 C13 C14 121.9(17) . . . yes P1 C13 C18 120.5(16) . . . yes C14 C13 C18 118(2) . . . no C13 C14 C15 121(2) . . . no C14 C15 C16 120(2) . . . no C15 C16 C17 121(2) . . . no C16 C17 C18 118(2) . . . no C13 C18 C17 122(2) . . . no S1 C2 H2 124.00 . . . no C3 C2 H2 125.00 . . . no O2 C4 H4B 109.00 . . . no O2 C4 H4A 110.00 . . . no H4A C4 H4B 108.00 . . . no C5 C4 H4A 109.00 . . . no C5 C4 H4B 109.00 . . . no O1 C5 H5A 108.00 . . . no C4 C5 H5B 107.00 . . . no O1 C5 H5B 108.00 . . . no C4 C5 H5A 108.00 . . . no H5A C5 H5B 107.00 . . . no C9 C8 H8 120.00 . . . no C7 C8 H8 120.00 . . . no C10 C9 H9 121.00 . . . no C8 C9 H9 121.00 . . . no C9 C10 H10 119.00 . . . no C11 C10 H10 119.00 . . . no C10 C11 H11 120.00 . . . no C12 C11 H11 120.00 . . . no C7 C12 H12 120.00 . . . no C11 C12 H12 120.00 . . . no C13 C14 H14 120.00 . . . no C15 C14 H14 119.00 . . . no C14 C15 H15 120.00 . . . no C16 C15 H15 120.00 . . . no C15 C16 H16 120.00 . . . no C17 C16 H16 119.00 . . . no C16 C17 H17 121.00 . . . no C18 C17 H17 121.00 . . . no C13 C18 H18 119.00 . . . no C17 C18 H18 119.00 . . . no S2 C19 P2 121.5(12) . . . yes S2 C19 C24 110.1(16) . . . yes P2 C19 C24 128.0(16) . . . yes S2 C20 C21 111.9(18) . . . yes O3 C21 C20 125(2) . . . yes O3 C21 C24 121.8(18) . . . yes C20 C21 C24 113(2) . . . no O3 C22 C23 117(3) . . . yes O4 C23 C22 116(2) . . . yes O4 C24 C19 124(2) . . . yes O4 C24 C21 124(2) . . . yes C19 C24 C21 112.7(19) . . . no P2 C25 C26 119.2(16) . . . yes P2 C25 C30 122.1(16) . . . yes C26 C25 C30 119(2) . . . no C25 C26 C27 121(2) . . . no C26 C27 C28 120(2) . . . no C27 C28 C29 118(2) . . . no C28 C29 C30 123(2) . . . no C25 C30 C29 119(2) . . . no P2 C31 C32 119.8(16) . . . yes P2 C31 C36 122.6(17) . . . yes C32 C31 C36 117.4(19) . . . no C31 C32 C33 122(2) . . . no C32 C33 C34 120(2) . . . no C33 C34 C35 118(2) . . . no C34 C35 C36 125(2) . . . no C31 C36 C35 119(2) . . . no S2 C20 H20 124.00 . . . no C21 C20 H20 124.00 . . . no O3 C22 H22A 108.00 . . . no O3 C22 H22B 108.00 . . . no C23 C22 H22A 108.00 . . . no C23 C22 H22B 108.00 . . . no H22A C22 H22B 107.00 . . . no O4 C23 H23A 108.00 . . . no O4 C23 H23B 108.00 . . . no C22 C23 H23A 109.00 . . . no C22 C23 H23B 108.00 . . . no H23A C23 H23B 107.00 . . . no C25 C26 H26 119.00 . . . no C27 C26 H26 119.00 . . . no C26 C27 H27 120.00 . . . no C28 C27 H27 120.00 . . . no C27 C28 H28 121.00 . . . no C29 C28 H28 121.00 . . . no C28 C29 H29 119.00 . . . no C30 C29 H29 118.00 . . . no C25 C30 H30 120.00 . . . no C29 C30 H30 120.00 . . . no C31 C32 H32 119.00 . . . no C33 C32 H32 119.00 . . . no C32 C33 H33 120.00 . . . no C34 C33 H33 120.00 . . . no C33 C34 H34 121.00 . . . no C35 C34 H34 121.00 . . . no C34 C35 H35 118.00 . . . no C36 C35 H35 117.00 . . . no C31 C36 H36 120.00 . . . no C35 C36 H36 121.00 . . . no Cl1S C1S Cl2S 111.4(14) . . . yes Cl1S C1S Cl3S 112.9(14) . . . yes Cl2S C1S Cl3S 110.8(13) . . . yes Cl1S C1S H1S 107.00 . . . no Cl2S C1S H1S 107.00 . . . no Cl3S C1S H1S 107.00 . . . no 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 Cl1 Pd1 P1 C1 -106.2(7) . . . . no Cl1 Pd1 P1 C7 129.4(8) . . . . no Cl1 Pd1 P1 C13 11.2(8) . . . . no Cl1 Pd1 P1 C1 73.8(7) 2_556 . . . no Cl1 Pd1 P1 C7 -50.6(8) 2_556 . . . no Cl1 Pd1 P1 C13 -168.8(8) 2_556 . . . no Cl2 Pd2 P2 C31 -59.4(7) . . . . no Cl2 Pd2 P2 C19 63.1(7) . . . . no Cl2 Pd2 P2 C25 177.9(8) . . . . no Cl2 Pd2 P2 C31 120.6(7) 2_655 . . . no Cl2 Pd2 P2 C19 -116.9(7) 2_655 . . . no Cl2 Pd2 P2 C25 -2.2(8) 2_655 . . . no C2 S1 C1 P1 175.8(13) . . . . no C2 S1 C1 C6 -2.9(16) . . . . no C1 S1 C2 C3 2.4(18) . . . . no C20 S2 C19 P2 172.5(14) . . . . no C19 S2 C20 C21 -0.2(18) . . . . no C20 S2 C19 C24 -0.2(17) . . . . no Pd1 P1 C1 C6 171.9(19) . . . . no Pd1 P1 C1 S1 -6.4(14) . . . . no C13 P1 C1 S1 -131.1(12) . . . . no C7 P1 C1 S1 119.4(12) . . . . no C7 P1 C1 C6 -62(2) . . . . no C1 P1 C13 C14 28(2) . . . . no C1 P1 C13 C18 -155.4(17) . . . . no C7 P1 C13 C14 144.7(18) . . . . no C7 P1 C13 C18 -38.9(19) . . . . no C13 P1 C7 C8 -80(2) . . . . no C13 P1 C7 C12 93.0(18) . . . . no C13 P1 C1 C6 47(2) . . . . no Pd1 P1 C7 C8 153.7(16) . . . . no Pd1 P1 C7 C12 -33.3(19) . . . . no C1 P1 C7 C8 32(2) . . . . no C1 P1 C7 C12 -155.5(17) . . . . no Pd1 P1 C13 C18 85.7(18) . . . . no Pd1 P1 C13 C14 -90.7(18) . . . . no C31 P2 C19 C24 -73(2) . . . . no C31 P2 C19 S2 116.3(13) . . . . no Pd2 P2 C19 S2 -6.7(15) . . . . no Pd2 P2 C19 C24 164.5(17) . . . . no C25 P2 C19 S2 -130.0(13) . . . . no C25 P2 C19 C24 41(2) . . . . no C31 P2 C25 C30 -9(2) . . . . no Pd2 P2 C31 C32 -30.2(19) . . . . no Pd2 P2 C25 C26 -64(2) . . . . no Pd2 P2 C25 C30 115.1(18) . . . . no C19 P2 C25 C26 57(2) . . . . no C19 P2 C25 C30 -125(2) . . . . no C31 P2 C25 C26 172.1(19) . . . . no C19 P2 C31 C32 -153.4(17) . . . . no C19 P2 C31 C36 21(2) . . . . no Pd2 P2 C31 C36 144.6(16) . . . . no C25 P2 C31 C36 -88.3(19) . . . . no C25 P2 C31 C32 97.0(18) . . . . no C5 O1 C6 C1 174(2) . . . . no C6 O1 C5 C4 37(3) . . . . no C5 O1 C6 C3 -12(3) . . . . no C3 O2 C4 C5 40(3) . . . . no C4 O2 C3 C2 161(2) . . . . no C4 O2 C3 C6 -18(3) . . . . no C22 O3 C21 C24 -10(3) . . . . no C21 O3 C22 C23 36(3) . . . . no C22 O3 C21 C20 171(2) . . . . no C24 O4 C23 C22 39(3) . . . . no C23 O4 C24 C21 -13(3) . . . . no C23 O4 C24 C19 166(2) . . . . no S1 C1 C6 C3 3(2) . . . . no S1 C1 C6 O1 177.2(15) . . . . no P1 C1 C6 O1 -1(3) . . . . no P1 C1 C6 C3 -175.7(17) . . . . no S1 C2 C3 O2 179.8(17) . . . . no S1 C2 C3 C6 -1(2) . . . . no O2 C3 C6 C1 178.1(19) . . . . no C2 C3 C6 O1 -175.6(19) . . . . no O2 C3 C6 O1 4(3) . . . . no C2 C3 C6 C1 -1(3) . . . . no O2 C4 C5 O1 -52(3) . . . . no P1 C7 C8 C9 173.1(18) . . . . no C8 C7 C12 C11 2(3) . . . . no P1 C7 C12 C11 -171.6(17) . . . . no C12 C7 C8 C9 0(3) . . . . no C7 C8 C9 C10 -2(3) . . . . no C8 C9 C10 C11 2(4) . . . . no C9 C10 C11 C12 -1(4) . . . . no C10 C11 C12 C7 -1(3) . . . . no P1 C13 C14 C15 174.7(17) . . . . no C14 C13 C18 C17 0(3) . . . . no C18 C13 C14 C15 -2(3) . . . . no P1 C13 C18 C17 -176.4(17) . . . . no C13 C14 C15 C16 4(3) . . . . no C14 C15 C16 C17 -5(3) . . . . no C15 C16 C17 C18 3(3) . . . . no C16 C17 C18 C13 -1(3) . . . . no S2 C19 C24 O4 -179.5(16) . . . . no S2 C19 C24 C21 0(2) . . . . no P2 C19 C24 O4 9(3) . . . . no P2 C19 C24 C21 -171.6(15) . . . . no S2 C20 C21 O3 179.9(16) . . . . no S2 C20 C21 C24 0(2) . . . . no O3 C21 C24 O4 0(3) . . . . no O3 C21 C24 C19 179.9(18) . . . . no C20 C21 C24 O4 179(2) . . . . no C20 C21 C24 C19 -1(3) . . . . no O3 C22 C23 O4 -53(3) . . . . no P2 C25 C26 C27 176.8(19) . . . . no C30 C25 C26 C27 -2(4) . . . . no P2 C25 C30 C29 -179.6(18) . . . . no C26 C25 C30 C29 -1(3) . . . . no C25 C26 C27 C28 1(4) . . . . no C26 C27 C28 C29 4(4) . . . . no C27 C28 C29 C30 -7(4) . . . . no C28 C29 C30 C25 6(4) . . . . no P2 C31 C32 C33 178.0(16) . . . . no C36 C31 C32 C33 3(3) . . . . no P2 C31 C36 C35 -176.3(17) . . . . no C32 C31 C36 C35 -1(3) . . . . no C31 C32 C33 C34 -4(3) . . . . no C32 C33 C34 C35 3(3) . . . . no C33 C34 C35 C36 -1(3) . . . . no C34 C35 C36 C31 1(3) . . . . no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag C4 H4A O2 0.9800 2.5900 3.13(3) 114.00 2_565 yes C8 H8 O1 0.9500 2.4600 3.30(3) 147.00 . yes C14 H14 O3 0.9500 2.5500 3.29(3) 136.00 . yes C22 H22B S2 0.9900 2.8700 3.77(3) 152.00 2_555 yes C26 H26 O3 0.9500 2.5000 3.28(3) 140.00 2_555 yes C36 H36 S1 0.9500 2.7700 3.36(2) 121.00 . yes C36 H36 O4 0.9500 2.5800 3.33(3) 137.00 . yes _diffrn_measured_fraction_theta_max 0.771 _diffrn_reflns_theta_full 21.03 _diffrn_measured_fraction_theta_full 0.771 _refine_diff_density_max 0.891 _refine_diff_density_min -0.870 _refine_diff_density_rms 0.144 # Attachment 'kugpt30s.cif' data_kugpt30s _database_code_depnum_ccdc_archive 'CCDC 699408' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H30 Cl2 O4 P2 Pt S2, (C4 H10 O)' _chemical_formula_sum 'C40 H40 Cl2 O5 P2 Pt S2' _chemical_formula_weight 992.77 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' Cl Cl 0.1484 0.1585 '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' P P 0.1023 0.0942 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.379(2) _cell_length_b 12.109(2) _cell_length_c 15.524(3) _cell_angle_alpha 72.370(4) _cell_angle_beta 89.055(5) _cell_angle_gamma 66.038(5) _cell_volume 1848.9(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100 _cell_measurement_reflns_used 343 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 13.74 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.733 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 988 _exptl_absorpt_coefficient_mu 4.068 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6865 _exptl_absorpt_correction_T_max 0.9605 _exptl_absorpt_process_details 'SADABS V2008-1 (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 ? _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 100003 _diffrn_reflns_av_R_equivalents 0.0326 _diffrn_reflns_av_sigmaI/netI 0.0719 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 26.02 _reflns_number_total 6965 _reflns_number_gt 4981 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART v.5.632 (Bruker, 2005)' _computing_cell_refinement 'SAINT v6.45a (Bruker, 2005)' _computing_data_reduction 'SAINT v6.45a (Bruker, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 2001)' _computing_publication_material 'PLATON (Spek, 2003)' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0534P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7165 _refine_ls_number_parameters 426 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0623 _refine_ls_R_factor_gt 0.0403 _refine_ls_wR_factor_ref 0.0955 _refine_ls_wR_factor_gt 0.0901 _refine_ls_goodness_of_fit_ref 0.916 _refine_ls_restrained_S_all 0.916 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags Pt1 Pt Uani 0.00000 0.00000 0.50000 1.000 0.0198(1) . . Cl1 Cl Uani -0.10790(14) -0.09939(13) 0.45130(9) 1.000 0.0265(4) . . S1 S Uani 0.10728(15) 0.15748(16) 0.31877(10) 1.000 0.0336(5) . . P1 P Uani -0.13985(14) 0.19929(13) 0.40439(9) 1.000 0.0212(4) . . O1 O Uani -0.2187(4) 0.4416(4) 0.2097(3) 1.000 0.0432(14) . . O2 O Uani -0.0171(4) 0.4404(4) 0.0942(3) 1.000 0.0356(12) . . C1 C Uani -0.0559(5) 0.2544(5) 0.3151(4) 1.000 0.0245(17) . . C2 C Uani 0.1174(6) 0.2486(6) 0.2139(4) 1.000 0.0364(19) . . C3 C Uani 0.0038(6) 0.3488(6) 0.1762(4) 1.000 0.0310(19) . . C4 C Uani -0.1531(5) 0.5108(6) 0.0586(4) 1.000 0.047(2) . . C5B C Uiso -0.2224(10) 0.5531(6) 0.1352(5) 0.671(16) 0.030(2) . . C6 C Uani -0.0967(6) 0.3528(5) 0.2348(4) 1.000 0.0261(17) . . C7 C Uani -0.2136(5) 0.3180(5) 0.4623(4) 1.000 0.0235(17) . . C8 C Uani -0.2648(6) 0.4462(6) 0.4152(4) 1.000 0.033(2) . . C9 C Uani -0.3341(7) 0.5321(6) 0.4608(5) 1.000 0.041(2) . . C10 C Uani -0.3484(6) 0.4894(6) 0.5504(5) 1.000 0.038(2) . . C11 C Uani -0.2963(6) 0.3580(6) 0.5974(4) 1.000 0.0319(19) . . C12 C Uani -0.2286(6) 0.2733(5) 0.5532(4) 1.000 0.0265(17) . . C13 C Uani -0.2809(5) 0.2061(5) 0.3468(3) 1.000 0.0214(17) . . C14 C Uani -0.2776(6) 0.1890(6) 0.2618(4) 1.000 0.0308(19) . . C15 C Uani -0.3825(6) 0.1862(6) 0.2215(4) 1.000 0.0316(19) . . C16 C Uani -0.4933(6) 0.1994(5) 0.2648(4) 1.000 0.0281(17) . . C17 C Uani -0.4972(6) 0.2169(5) 0.3495(4) 1.000 0.0292(17) . . C18 C Uani -0.3931(5) 0.2204(5) 0.3902(4) 1.000 0.0236(17) . . C5A C Uiso -0.2611(8) 0.5383(14) 0.1186(5) 0.329(16) 0.030(2) . . Pt2 Pt Uani 0.50000 0.00000 0.00000 1.000 0.0219(1) . . Cl2 Cl Uani 0.42529(14) 0.17398(13) 0.05058(9) 1.000 0.0283(4) . . S2 S Uani 0.15578(16) 0.15619(16) 0.00523(11) 1.000 0.0371(5) . . P2 P Uani 0.39612(14) -0.08411(14) 0.11177(10) 1.000 0.0233(4) . . O3 O Uani -0.1061(4) 0.0577(5) 0.1220(3) 1.000 0.0478(19) . . O4 O Uani 0.1524(4) -0.1263(4) 0.2047(3) 1.000 0.0360(14) . . C19 C Uani 0.2248(6) 0.0120(6) 0.0948(4) 1.000 0.0297(17) . . C20 C Uani 0.0036(6) 0.1715(6) 0.0224(4) 1.000 0.039(2) . . C21 C Uani 0.0021(6) 0.0724(7) 0.0915(4) 1.000 0.036(2) . . C22 C Uani -0.0824(4) -0.0570(6) 0.1882(5) 1.000 0.070(3) . . C23A C Uiso 0.0398(6) -0.1072(11) 0.2528(5) 0.618(11) 0.044(2) . . C24 C Uani 0.1306(6) -0.0197(6) 0.1336(4) 1.000 0.0308(19) . . C25 C Uani 0.4041(6) -0.2386(6) 0.1195(4) 1.000 0.0303(17) . . C26 C Uani 0.3495(6) -0.2496(6) 0.0440(4) 1.000 0.0312(19) . . C27 C Uani 0.3598(7) -0.3637(6) 0.0412(5) 1.000 0.042(2) . . C28 C Uani 0.4204(7) -0.4726(6) 0.1171(5) 1.000 0.043(2) . . C29 C Uani 0.4713(6) -0.4655(6) 0.1927(5) 1.000 0.039(2) . . C30 C Uani 0.4648(6) -0.3475(6) 0.1941(4) 1.000 0.0307(17) . . C31 C Uani 0.4600(6) -0.0965(5) 0.2235(4) 1.000 0.0281(17) . . C32 C Uani 0.5927(6) -0.1304(6) 0.2408(4) 1.000 0.0306(17) . . C33 C Uani 0.6417(6) -0.1357(6) 0.3229(4) 1.000 0.0317(19) . . C34 C Uani 0.5641(7) -0.1105(6) 0.3883(4) 1.000 0.0310(19) . . C35 C Uani 0.4364(7) -0.0796(6) 0.3731(4) 1.000 0.0334(19) . . C36 C Uani 0.3817(6) -0.0736(6) 0.2898(4) 1.000 0.0299(17) . . C23B C Uiso 0.0500(5) -0.1692(7) 0.2178(13) 0.382(11) 0.044(2) . . H5B1 H Uiso -0.18000 0.59720 0.15850 0.671(16) 0.0360 calc . H5B2 H Uiso -0.31350 0.61390 0.11180 0.671(16) 0.0360 calc . H4A H Uiso -0.17150 0.46510 0.02120 1.000 0.0560 calc R H4B H Uiso -0.16320 0.59460 0.01600 1.000 0.0560 calc R H8 H Uiso -0.25350 0.47630 0.35300 1.000 0.0400 calc R H9 H Uiso -0.37150 0.62130 0.42880 1.000 0.0490 calc R H10 H Uiso -0.39360 0.54860 0.58100 1.000 0.0460 calc R H11 H Uiso -0.30790 0.32760 0.65950 1.000 0.0380 calc R H12 H Uiso -0.19200 0.18410 0.58500 1.000 0.0320 calc R H14 H Uiso -0.20250 0.17920 0.23160 1.000 0.0360 calc R H15 H Uiso -0.37930 0.17500 0.16340 1.000 0.0380 calc R H16 H Uiso -0.56520 0.19650 0.23690 1.000 0.0340 calc R H17 H Uiso -0.57250 0.22650 0.37940 1.000 0.0350 calc R H18 H Uiso -0.39690 0.23250 0.44810 1.000 0.0280 calc R H2 H Uiso 0.19430 0.23070 0.18520 1.000 0.0440 calc R H5A1 H Uiso -0.28560 0.62410 0.12390 0.329(16) 0.0360 calc . H5A2 H Uiso -0.33830 0.53780 0.09050 0.329(16) 0.0360 calc . H22A H Uiso -0.07470 -0.12090 0.15850 1.000 0.0830 calc R H22B H Uiso -0.15710 -0.04600 0.22370 1.000 0.0830 calc R H23A H Uiso 0.03080 -0.04560 0.28510 0.618(11) 0.0520 calc . H23B H Uiso 0.05160 -0.18920 0.29890 0.618(11) 0.0520 calc . H26 H Uiso 0.30410 -0.17500 -0.00660 1.000 0.0370 calc R H27 H Uiso 0.32600 -0.36980 -0.01190 1.000 0.0500 calc R H28 H Uiso 0.42620 -0.55260 0.11590 1.000 0.0510 calc R H29 H Uiso 0.51120 -0.53980 0.24440 1.000 0.0470 calc R H30 H Uiso 0.50220 -0.34250 0.24630 1.000 0.0360 calc R H32 H Uiso 0.64840 -0.14960 0.19600 1.000 0.0370 calc R H33 H Uiso 0.73150 -0.15740 0.33420 1.000 0.0380 calc R H34 H Uiso 0.59960 -0.11450 0.44470 1.000 0.0380 calc R H35 H Uiso 0.38260 -0.06160 0.41910 1.000 0.0400 calc R H36 H Uiso 0.29220 -0.05400 0.28010 1.000 0.0350 calc R H20 H Uiso -0.07230 0.24170 -0.01260 1.000 0.0470 calc R H23C H Uiso 0.05630 -0.21770 0.28300 0.382(11) 0.0520 calc . H23D H Uiso 0.06040 -0.22720 0.18210 0.382(11) 0.0520 calc . 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 0.0219(2) 0.0140(2) 0.0178(2) -0.0026(1) 0.0027(1) -0.0039(1) Cl1 0.0293(8) 0.0193(7) 0.0276(7) -0.0058(6) 0.0000(6) -0.0081(6) S1 0.0256(8) 0.0357(9) 0.0283(8) -0.0075(7) 0.0081(6) -0.0044(7) P1 0.0222(8) 0.0151(7) 0.0196(7) -0.0024(6) 0.0048(6) -0.0037(6) O1 0.031(3) 0.030(2) 0.036(2) 0.012(2) 0.017(2) 0.002(2) O2 0.032(2) 0.035(2) 0.028(2) 0.0006(19) 0.0155(19) -0.011(2) C1 0.023(3) 0.019(3) 0.026(3) -0.004(2) 0.002(2) -0.006(2) C2 0.023(3) 0.047(4) 0.026(3) -0.008(3) 0.009(3) -0.005(3) C3 0.037(4) 0.035(3) 0.026(3) -0.013(3) 0.013(3) -0.018(3) C4 0.032(4) 0.038(4) 0.047(4) 0.000(3) 0.010(3) -0.003(3) C6 0.026(3) 0.022(3) 0.030(3) -0.007(2) 0.010(3) -0.011(3) C7 0.021(3) 0.020(3) 0.030(3) -0.010(2) 0.006(2) -0.008(2) C8 0.036(4) 0.025(3) 0.037(4) -0.007(3) 0.010(3) -0.014(3) C9 0.046(4) 0.018(3) 0.048(4) -0.005(3) 0.008(3) -0.007(3) C10 0.033(4) 0.034(4) 0.056(4) -0.030(3) 0.011(3) -0.011(3) C11 0.034(4) 0.033(3) 0.026(3) -0.008(3) 0.012(3) -0.013(3) C12 0.030(3) 0.018(3) 0.024(3) -0.004(2) 0.004(2) -0.005(3) C13 0.023(3) 0.010(3) 0.020(3) -0.002(2) -0.001(2) 0.002(2) C14 0.035(4) 0.030(3) 0.026(3) -0.011(3) 0.008(3) -0.011(3) C15 0.044(4) 0.029(3) 0.022(3) -0.009(3) 0.002(3) -0.015(3) C16 0.025(3) 0.022(3) 0.034(3) -0.004(3) -0.005(3) -0.010(3) C17 0.033(3) 0.020(3) 0.026(3) -0.002(2) 0.006(3) -0.007(3) C18 0.027(3) 0.014(3) 0.024(3) -0.002(2) 0.002(2) -0.006(2) Pt2 0.0229(2) 0.0191(2) 0.0174(2) -0.0019(1) 0.0050(1) -0.0057(1) Cl2 0.0335(8) 0.0218(7) 0.0247(7) -0.0062(6) 0.0083(6) -0.0081(6) S2 0.0314(9) 0.0312(9) 0.0335(9) -0.0027(7) -0.0002(7) -0.0039(7) P2 0.0232(8) 0.0216(8) 0.0192(7) -0.0028(6) 0.0059(6) -0.0067(6) O3 0.028(3) 0.074(4) 0.037(3) -0.020(3) 0.009(2) -0.016(2) O4 0.033(2) 0.049(3) 0.023(2) -0.0013(19) 0.0073(18) -0.022(2) C19 0.029(3) 0.029(3) 0.023(3) -0.006(3) 0.003(3) -0.006(3) C20 0.027(4) 0.036(4) 0.043(4) -0.016(3) 0.001(3) 0.001(3) C21 0.025(3) 0.047(4) 0.034(4) -0.019(3) 0.003(3) -0.008(3) C22 0.041(5) 0.055(5) 0.108(7) -0.024(5) 0.030(5) -0.018(4) C24 0.027(3) 0.034(4) 0.024(3) -0.009(3) 0.006(3) -0.006(3) C25 0.025(3) 0.027(3) 0.032(3) -0.006(3) 0.010(3) -0.007(3) C26 0.025(3) 0.022(3) 0.038(4) -0.003(3) -0.004(3) -0.006(3) C27 0.046(4) 0.035(4) 0.043(4) -0.011(3) -0.002(3) -0.016(3) C28 0.041(4) 0.021(3) 0.062(5) -0.008(3) 0.000(4) -0.013(3) C29 0.034(4) 0.018(3) 0.046(4) 0.003(3) 0.005(3) -0.003(3) C30 0.025(3) 0.026(3) 0.025(3) 0.001(3) 0.004(2) -0.002(3) C31 0.033(3) 0.023(3) 0.020(3) -0.001(2) 0.005(3) -0.008(3) C32 0.026(3) 0.030(3) 0.033(3) -0.008(3) 0.009(3) -0.011(3) C33 0.036(4) 0.023(3) 0.029(3) 0.001(3) -0.002(3) -0.012(3) C34 0.045(4) 0.024(3) 0.020(3) 0.001(3) -0.007(3) -0.016(3) C35 0.041(4) 0.024(3) 0.029(3) -0.007(3) 0.010(3) -0.009(3) C36 0.027(3) 0.031(3) 0.022(3) -0.003(3) 0.005(2) -0.007(3) 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 Pt1 Cl1 2.3042(17) . . yes Pt1 P1 2.3126(15) . . yes Pt1 Cl1 2.3042(17) . 2_556 yes Pt1 P1 2.3126(15) . 2_556 yes Pt2 Cl2 2.3028(16) . 2_655 yes Pt2 P2 2.2989(17) . 2_655 yes Pt2 Cl2 2.3028(16) . . yes Pt2 P2 2.2989(17) . . yes S1 C2 1.700(6) . . yes S1 C1 1.738(6) . . yes S2 C20 1.691(8) . . yes S2 C19 1.747(7) . . yes P1 C13 1.810(6) . . yes P1 C7 1.832(6) . . yes P1 C1 1.787(6) . . yes P2 C25 1.802(7) . . yes P2 C19 1.792(7) . . yes P2 C31 1.832(6) . . yes O1 C5A 1.471(10) . . yes O1 C6 1.337(8) . . yes O1 C5B 1.474(9) . . yes O2 C4 1.449(8) . . yes O2 C3 1.359(8) . . yes O3 C21 1.371(9) . . yes O3 C22 1.378(9) . . yes O4 C23B 1.445(9) . . yes O4 C24 1.354(8) . . yes O4 C23A 1.444(10) . . yes C1 C6 1.364(8) . . no C2 C3 1.344(10) . . no C3 C6 1.444(10) . . no C4 C5A 1.519(13) . . no C4 C5B 1.519(10) . . no C7 C8 1.370(9) . . no C7 C12 1.385(8) . . no C8 C9 1.402(10) . . no C9 C10 1.362(10) . . no C10 C11 1.400(10) . . no C11 C12 1.372(9) . . no C13 C14 1.394(8) . . no C13 C18 1.406(8) . . no C14 C15 1.374(10) . . no C15 C16 1.393(10) . . no C16 C17 1.391(8) . . no C17 C18 1.373(9) . . no C2 H2 0.9500 . . no C4 H4A 0.9900 . . no C4 H4B 0.9900 . . no C5A H5A2 0.9900 . . no C5A H5A1 0.9900 . . no C5B H5B1 0.9900 . . no C5B H5B2 0.9900 . . no C8 H8 0.9500 . . no C9 H9 0.9500 . . no C10 H10 0.9500 . . no C11 H11 0.9500 . . no C12 H12 0.9500 . . no C14 H14 0.9500 . . no C15 H15 0.9500 . . no C16 H16 0.9500 . . no C17 H17 0.9500 . . no C18 H18 0.9500 . . no C19 C24 1.354(10) . . no C20 C21 1.352(9) . . no C21 C24 1.440(10) . . no C22 C23A 1.516(10) . . no C22 C23B 1.520(12) . . no C25 C26 1.401(9) . . no C25 C30 1.385(9) . . no C26 C27 1.353(10) . . no C27 C28 1.396(10) . . no C28 C29 1.358(11) . . no C29 C30 1.407(10) . . no C31 C32 1.401(10) . . no C31 C36 1.368(9) . . no C32 C33 1.373(9) . . no C33 C34 1.358(10) . . no C34 C35 1.350(12) . . no C35 C36 1.414(9) . . no C20 H20 0.9500 . . no C22 H22A 0.9900 . . no C22 H22B 0.9900 . . no C23A H23A 0.9900 . . no C23A H23B 0.9900 . . no C23B H23C 0.9900 . . no C23B H23D 0.9900 . . no C26 H26 0.9500 . . no C27 H27 0.9500 . . no C28 H28 0.9500 . . no C29 H29 0.9500 . . no C30 H30 0.9500 . . no C32 H32 0.9500 . . no C33 H33 0.9500 . . no C34 H34 0.9500 . . no C35 H35 0.9500 . . no C36 H36 0.9500 . . no 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 Pt1 P1 92.32(5) . . . yes Cl1 Pt1 Cl1 180.00 . . 2_556 yes Cl1 Pt1 P1 87.68(5) . . 2_556 yes Cl1 Pt1 P1 87.68(5) 2_556 . . yes P1 Pt1 P1 180.00 . . 2_556 yes Cl1 Pt1 P1 92.32(5) 2_556 . 2_556 yes Cl2 Pt2 P2 94.19(6) . . 2_655 yes Cl2 Pt2 P2 85.81(6) . . . yes Cl2 Pt2 Cl2 180.00 . . 2_655 yes Cl2 Pt2 P2 85.81(6) 2_655 . 2_655 yes Cl2 Pt2 P2 94.19(6) 2_655 . . yes P2 Pt2 P2 180.00 . . 2_655 yes C1 S1 C2 92.9(3) . . . yes C19 S2 C20 92.4(3) . . . yes Pt1 P1 C13 115.86(19) . . . yes Pt1 P1 C1 109.1(2) . . . yes Pt1 P1 C7 114.04(19) . . . yes C7 P1 C13 101.9(3) . . . yes C1 P1 C7 110.5(3) . . . yes C1 P1 C13 105.0(3) . . . yes Pt2 P2 C19 112.1(2) . . . yes C19 P2 C25 102.1(3) . . . yes Pt2 P2 C25 116.5(2) . . . yes Pt2 P2 C31 110.1(2) . . . yes C19 P2 C31 108.1(3) . . . yes C25 P2 C31 107.4(3) . . . yes C5B O1 C6 110.0(6) . . . yes C5A O1 C6 122.1(6) . . . yes C3 O2 C4 112.6(5) . . . yes C21 O3 C22 115.2(5) . . . yes C23A O4 C24 110.0(6) . . . yes C23B O4 C24 117.1(8) . . . yes S1 C1 C6 109.4(5) . . . yes P1 C1 C6 132.8(5) . . . yes S1 C1 P1 117.3(3) . . . yes S1 C2 C3 112.1(5) . . . yes O2 C3 C2 125.6(6) . . . yes O2 C3 C6 122.2(6) . . . yes C2 C3 C6 112.2(6) . . . no O2 C4 C5A 123.3(6) . . . yes O2 C4 C5B 105.9(6) . . . yes O1 C5A C4 110.3(9) . . . yes O1 C5B C4 110.1(5) . . . yes O1 C6 C1 124.1(6) . . . yes O1 C6 C3 122.5(5) . . . yes C1 C6 C3 113.4(6) . . . no C8 C7 C12 121.1(6) . . . no P1 C7 C12 117.3(4) . . . yes P1 C7 C8 121.2(5) . . . yes C7 C8 C9 118.6(6) . . . no C8 C9 C10 120.9(6) . . . no C9 C10 C11 119.9(6) . . . no C10 C11 C12 119.6(6) . . . no C7 C12 C11 120.0(6) . . . no C14 C13 C18 118.9(6) . . . no P1 C13 C14 120.9(5) . . . yes P1 C13 C18 120.1(4) . . . yes C13 C14 C15 120.3(6) . . . no C14 C15 C16 120.9(6) . . . no C15 C16 C17 119.1(6) . . . no C16 C17 C18 120.6(6) . . . no C13 C18 C17 120.4(5) . . . no S1 C2 H2 124.00 . . . no C3 C2 H2 124.00 . . . no O2 C4 H4B 107.00 . . . no C5B C4 H4A 130.00 . . . no O2 C4 H4A 107.00 . . . no H4A C4 H4B 106.00 . . . no C5A C4 H4A 106.00 . . . no C5B C4 H4B 100.00 . . . no C5A C4 H4B 107.00 . . . no O1 C5A H5A2 110.00 . . . no C4 C5A H5A1 110.00 . . . no O1 C5A H5A1 110.00 . . . no H5A1 C5A H5A2 108.00 . . . no C4 C5A H5A2 110.00 . . . no O1 C5B H5B2 110.00 . . . no O1 C5B H5B1 110.00 . . . no C4 C5B H5B2 110.00 . . . no H5B1 C5B H5B2 108.00 . . . no C4 C5B H5B1 110.00 . . . no C9 C8 H8 121.00 . . . no C7 C8 H8 121.00 . . . no C10 C9 H9 120.00 . . . no C8 C9 H9 120.00 . . . no C9 C10 H10 120.00 . . . no C11 C10 H10 120.00 . . . no C10 C11 H11 120.00 . . . no C12 C11 H11 120.00 . . . no C7 C12 H12 120.00 . . . no C11 C12 H12 120.00 . . . no C13 C14 H14 120.00 . . . no C15 C14 H14 120.00 . . . no C14 C15 H15 120.00 . . . no C16 C15 H15 120.00 . . . no C17 C16 H16 120.00 . . . no C15 C16 H16 120.00 . . . no C16 C17 H17 120.00 . . . no C18 C17 H17 120.00 . . . no C17 C18 H18 120.00 . . . no C13 C18 H18 120.00 . . . no S2 C19 P2 120.6(4) . . . yes S2 C19 C24 110.0(5) . . . yes P2 C19 C24 128.5(5) . . . yes S2 C20 C21 112.3(5) . . . yes O3 C21 C20 126.1(7) . . . yes O3 C21 C24 121.7(6) . . . yes C20 C21 C24 112.2(7) . . . no O3 C22 C23A 113.0(6) . . . yes O3 C22 C23B 124.3(7) . . . yes O4 C23A C22 111.4(6) . . . yes O4 C23B C22 111.1(8) . . . yes O4 C24 C19 124.5(6) . . . yes C19 C24 C21 113.1(6) . . . no O4 C24 C21 122.4(6) . . . yes P2 C25 C26 117.7(5) . . . yes C26 C25 C30 118.3(6) . . . no P2 C25 C30 124.0(5) . . . yes C25 C26 C27 121.7(6) . . . no C26 C27 C28 119.4(7) . . . no C27 C28 C29 120.7(7) . . . no C28 C29 C30 119.7(7) . . . no C25 C30 C29 120.1(6) . . . no P2 C31 C32 118.6(5) . . . yes C32 C31 C36 119.6(6) . . . no P2 C31 C36 121.7(5) . . . yes C31 C32 C33 119.6(6) . . . no C32 C33 C34 121.1(7) . . . no C33 C34 C35 120.0(6) . . . no C34 C35 C36 120.9(6) . . . no C31 C36 C35 118.8(7) . . . no S2 C20 H20 124.00 . . . no C21 C20 H20 124.00 . . . no O3 C22 H22A 109.00 . . . no O3 C22 H22B 109.00 . . . no C23A C22 H22A 109.00 . . . no C23A C22 H22B 109.00 . . . no H22A C22 H22B 108.00 . . . no C23B C22 H22A 70.00 . . . no C23B C22 H22B 125.00 . . . no O4 C23A H23A 109.00 . . . no O4 C23A H23B 109.00 . . . no C22 C23A H23A 109.00 . . . no C22 C23A H23B 109.00 . . . no H23A C23A H23B 108.00 . . . no C22 C23B H23C 109.00 . . . no C22 C23B H23D 109.00 . . . no H23C C23B H23D 108.00 . . . no O4 C23B H23D 109.00 . . . no O4 C23B H23C 109.00 . . . no C25 C26 H26 119.00 . . . no C27 C26 H26 119.00 . . . no C28 C27 H27 120.00 . . . no C26 C27 H27 120.00 . . . no C27 C28 H28 120.00 . . . no C29 C28 H28 120.00 . . . no C28 C29 H29 120.00 . . . no C30 C29 H29 120.00 . . . no C29 C30 H30 120.00 . . . no C25 C30 H30 120.00 . . . no C33 C32 H32 120.00 . . . no C31 C32 H32 120.00 . . . no C32 C33 H33 119.00 . . . no C34 C33 H33 119.00 . . . no C33 C34 H34 120.00 . . . no C35 C34 H34 120.00 . . . no C36 C35 H35 120.00 . . . no C34 C35 H35 119.00 . . . no C35 C36 H36 121.00 . . . no C31 C36 H36 121.00 . . . no 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 Cl1 Pt1 P1 C1 -109.6(2) . . . . no Cl1 Pt1 P1 C7 126.3(2) . . . . no Cl1 Pt1 P1 C13 8.5(2) . . . . no Cl1 Pt1 P1 C1 70.4(2) 2_556 . . . no Cl1 Pt1 P1 C7 -53.7(2) 2_556 . . . no Cl1 Pt1 P1 C13 -171.5(2) 2_556 . . . no Cl2 Pt2 P2 C31 -58.7(2) . . . . no Cl2 Pt2 P2 C19 61.7(2) . . . . no Cl2 Pt2 P2 C25 178.8(3) . . . . no Cl2 Pt2 P2 C31 121.3(2) 2_655 . . . no Cl2 Pt2 P2 C19 -118.3(2) 2_655 . . . no Cl2 Pt2 P2 C25 -1.3(3) 2_655 . . . no C2 S1 C1 P1 172.0(4) . . . . no C2 S1 C1 C6 -0.4(5) . . . . no C1 S1 C2 C3 0.1(6) . . . . no C20 S2 C19 P2 170.4(4) . . . . no C19 S2 C20 C21 -0.9(6) . . . . no C20 S2 C19 C24 0.6(5) . . . . no Pt1 P1 C1 C6 167.6(6) . . . . no Pt1 P1 C1 S1 -2.6(4) . . . . no C13 P1 C1 S1 -127.3(4) . . . . no C7 P1 C1 S1 123.6(4) . . . . no C7 P1 C1 C6 -66.3(7) . . . . no C1 P1 C13 C14 30.2(6) . . . . no C1 P1 C13 C18 -154.1(5) . . . . no C7 P1 C13 C14 145.4(5) . . . . no C7 P1 C13 C18 -38.8(5) . . . . no C13 P1 C7 C8 -75.0(6) . . . . no C13 P1 C7 C12 98.0(5) . . . . no C13 P1 C1 C6 42.8(7) . . . . no Pt1 P1 C7 C8 159.5(5) . . . . no Pt1 P1 C7 C12 -27.6(6) . . . . no C1 P1 C7 C8 36.1(6) . . . . no C1 P1 C7 C12 -150.9(5) . . . . no Pt1 P1 C13 C18 85.5(5) . . . . no Pt1 P1 C13 C14 -90.2(5) . . . . no C31 P2 C19 C24 -74.2(7) . . . . no C31 P2 C19 S2 118.1(4) . . . . no Pt2 P2 C19 S2 -3.5(5) . . . . no Pt2 P2 C19 C24 164.3(5) . . . . no C25 P2 C19 S2 -128.8(4) . . . . no C25 P2 C19 C24 38.9(7) . . . . no C31 P2 C25 C30 -7.9(7) . . . . no Pt2 P2 C31 C32 -37.0(5) . . . . no Pt2 P2 C25 C26 -61.6(6) . . . . no Pt2 P2 C25 C30 116.0(6) . . . . no C19 P2 C25 C26 60.9(6) . . . . no C19 P2 C25 C30 -121.5(6) . . . . no C31 P2 C25 C26 174.5(6) . . . . no C19 P2 C31 C32 -159.8(5) . . . . no C19 P2 C31 C36 20.2(6) . . . . no Pt2 P2 C31 C36 143.0(5) . . . . no C25 P2 C31 C36 -89.3(6) . . . . no C25 P2 C31 C32 90.7(6) . . . . no C5B O1 C6 C1 162.7(6) . . . . no C6 O1 C5B C4 52.5(8) . . . . no C5B O1 C6 C3 -20.6(8) . . . . no C3 O2 C4 C5B 50.5(7) . . . . no C4 O2 C3 C2 161.4(7) . . . . no C4 O2 C3 C6 -21.1(8) . . . . no C22 O3 C21 C24 -6.9(9) . . . . no C21 O3 C22 C23A 34.8(9) . . . . no C22 O3 C21 C20 174.5(7) . . . . no C24 O4 C23A C22 50.8(10) . . . . no C23A O4 C24 C21 -23.8(9) . . . . no C23A O4 C24 C19 156.1(7) . . . . no S1 C1 C6 C3 0.5(7) . . . . no S1 C1 C6 O1 177.5(5) . . . . no P1 C1 C6 O1 6.8(10) . . . . no P1 C1 C6 C3 -170.2(5) . . . . no S1 C2 C3 O2 177.9(5) . . . . no S1 C2 C3 C6 0.2(8) . . . . no O2 C3 C6 C1 -178.3(6) . . . . no C2 C3 C6 O1 -177.5(6) . . . . no O2 C3 C6 O1 4.7(10) . . . . no C2 C3 C6 C1 -0.5(9) . . . . no O2 C4 C5B O1 -68.8(8) . . . . no P1 C7 C8 C9 172.2(6) . . . . no C8 C7 C12 C11 0.3(11) . . . . no P1 C7 C12 C11 -172.6(5) . . . . no C12 C7 C8 C9 -0.5(10) . . . . no C7 C8 C9 C10 1.2(12) . . . . no C8 C9 C10 C11 -1.7(12) . . . . no C9 C10 C11 C12 1.5(11) . . . . no C10 C11 C12 C7 -0.8(11) . . . . no P1 C13 C14 C15 175.8(5) . . . . no C14 C13 C18 C17 0.3(9) . . . . no C18 C13 C14 C15 0.0(9) . . . . no P1 C13 C18 C17 -175.6(5) . . . . no C13 C14 C15 C16 -0.5(10) . . . . no C14 C15 C16 C17 0.7(10) . . . . no C15 C16 C17 C18 -0.4(9) . . . . no C16 C17 C18 C13 -0.1(9) . . . . no S2 C19 C24 O4 179.9(5) . . . . no S2 C19 C24 C21 -0.2(7) . . . . no P2 C19 C24 O4 11.1(10) . . . . no P2 C19 C24 C21 -169.0(5) . . . . no S2 C20 C21 O3 179.6(6) . . . . no S2 C20 C21 C24 0.9(8) . . . . no O3 C21 C24 O4 0.7(10) . . . . no O3 C21 C24 C19 -179.2(6) . . . . no C20 C21 C24 O4 179.5(6) . . . . no C20 C21 C24 C19 -0.5(9) . . . . no O3 C22 C23A O4 -59.3(10) . . . . no P2 C25 C26 C27 174.9(6) . . . . no C30 C25 C26 C27 -2.9(11) . . . . no P2 C25 C30 C29 -177.2(6) . . . . no C26 C25 C30 C29 0.4(11) . . . . no C25 C26 C27 C28 3.4(12) . . . . no C26 C27 C28 C29 -1.4(12) . . . . no C27 C28 C29 C30 -1.0(12) . . . . no C28 C29 C30 C25 1.5(11) . . . . no P2 C31 C32 C33 177.7(5) . . . . no C36 C31 C32 C33 -2.4(10) . . . . no P2 C31 C36 C35 -177.4(5) . . . . no C32 C31 C36 C35 2.7(10) . . . . no C31 C32 C33 C34 1.0(10) . . . . no C32 C33 C34 C35 0.0(11) . . . . no C33 C34 C35 C36 0.3(11) . . . . no C34 C35 C36 C31 -1.7(10) . . . . no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag C8 H8 O1 0.9500 2.3800 3.238(8) 149.00 . yes C14 H14 O3 0.9500 2.5300 3.237(8) 131.00 . yes C26 H26 O3 0.9500 2.5100 3.331(8) 145.00 2_555 yes C36 H36 S1 0.9500 2.8000 3.377(7) 120.00 . yes C36 H36 O4 0.9500 2.5500 3.307(9) 137.00 . yes _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 2.348 _refine_diff_density_min -1.082 _refine_diff_density_rms 0.147 # Attachment 'nfpdm.cif' data_nfpdm _database_code_depnum_ccdc_archive 'CCDC 701459' _audit_creation_method ; SHELXL-97, PLATON and text editor ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Pd 2+, (C19 H17 O2 S P)2, (Cl 1-)2' _chemical_formula_sum 'C38 H34 Cl2 O4 P2 Pd S2' _chemical_formula_weight 858.01 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' Cl Cl 0.1484 0.1585 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,-z _cell_length_a 9.244(5) _cell_length_b 10.182(5) _cell_length_c 10.679(6) _cell_angle_alpha 107.001(8) _cell_angle_beta 96.758(9) _cell_angle_gamma 106.538(8) _cell_volume 899.0(8) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2110 _cell_measurement_theta_min 0.89 _cell_measurement_theta_max 27.5 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.585 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 436 _exptl_absorpt_coefficient_mu 0.911 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6588 _exptl_absorpt_correction_T_max 0.9144 _exptl_absorpt_process_details 'SADABS V2008-1 (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 ? _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 5198 _diffrn_reflns_av_R_equivalents 0.0298 _diffrn_reflns_av_sigmaI/netI 0.0671 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 27.10 _reflns_number_total 3759 _reflns_number_gt 3054 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART v.5.632 (Bruker, 2005)' _computing_cell_refinement 'SAINT v6.45a (Bruker, 2005)' _computing_data_reduction 'SAINT v6.45a (Bruker, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 2001)' _computing_publication_material 'PLATON (Spek, 2003)' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0622P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3759 _refine_ls_number_parameters 223 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0537 _refine_ls_R_factor_gt 0.0417 _refine_ls_wR_factor_ref 0.1080 _refine_ls_wR_factor_gt 0.1035 _refine_ls_goodness_of_fit_ref 0.984 _refine_ls_restrained_S_all 0.984 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags Pd1 Pd Uani 0.00000 1.00000 0.00000 1.000 0.0207(1) . . Cl1 Cl Uani -0.24390(9) 0.83464(10) -0.06105(8) 1.000 0.0307(3) . . S1 S Uani 0.46576(10) 0.65604(10) 0.10110(9) 1.000 0.0297(3) . . P1 P Uani -0.02630(9) 1.03855(9) 0.21834(8) 1.000 0.0217(3) . . O1 O Uani 0.0578(3) 0.5373(3) 0.1742(3) 1.000 0.0341(8) . . O2 O Uani 0.1711(3) 0.8461(3) 0.2146(2) 1.000 0.0285(8) . . C1 C Uani 0.3041(4) 0.5374(4) 0.1196(4) 1.000 0.0325(12) . . C2 C Uani 0.3985(4) 0.8004(4) 0.1472(3) 1.000 0.0276(10) . . C3 C Uani 0.2569(4) 0.7562(4) 0.1741(3) 1.000 0.0255(10) . . C4 C Uani 0.2012(4) 0.6058(4) 0.1578(3) 1.000 0.0285(11) . . C5 C Uani 0.0091(4) 0.7648(4) 0.1891(4) 1.000 0.0348(11) . . C6 C Uani -0.0156(4) 0.6378(4) 0.2377(4) 1.000 0.0378(12) . . C7 C Uani -0.0693(4) 0.8683(4) 0.2578(3) 1.000 0.0246(10) . . C8 C Uani 0.1271(4) 1.1789(4) 0.3548(3) 1.000 0.0260(10) . . C9 C Uani 0.1412(5) 1.3230(4) 0.3740(4) 1.000 0.0405(12) . . C10 C Uani 0.2504(5) 1.4334(5) 0.4786(5) 1.000 0.0490(16) . . C11 C Uani 0.3472(4) 1.4008(4) 0.5661(4) 1.000 0.0342(11) . . C12 C Uani 0.3375(4) 1.2598(4) 0.5443(3) 1.000 0.0305(10) . . C13 C Uani 0.2295(4) 1.1483(4) 0.4385(3) 1.000 0.0274(10) . . C14 C Uani -0.1900(3) 1.0984(4) 0.2519(3) 1.000 0.0227(9) . . C15 C Uani -0.2413(4) 1.0998(4) 0.3681(3) 1.000 0.0300(11) . . C16 C Uani -0.3630(4) 1.1485(4) 0.3974(3) 1.000 0.0307(11) . . C17 C Uani -0.4333(4) 1.1986(4) 0.3062(4) 1.000 0.0306(11) . . C18 C Uani -0.3807(4) 1.2020(4) 0.1925(4) 1.000 0.0333(11) . . C19 C Uani -0.2593(4) 1.1495(4) 0.1621(3) 1.000 0.0297(11) . . H1 H Uiso 0.28800 0.43730 0.10520 1.000 0.0390 calc R H2 H Uiso 0.45300 0.89720 0.15290 1.000 0.0330 calc R H5 H Uiso -0.03460 0.72750 0.09030 1.000 0.0420 calc R H6A H Uiso 0.02550 0.67450 0.33590 1.000 0.0450 calc R H6B H Uiso -0.12800 0.58550 0.22040 1.000 0.0450 calc R H7A H Uiso -0.03730 0.89380 0.35610 1.000 0.0300 calc R H7B H Uiso -0.18250 0.81740 0.23180 1.000 0.0300 calc R H9 H Uiso 0.07510 1.34540 0.31450 1.000 0.0480 calc R H10 H Uiso 0.25980 1.53210 0.49140 1.000 0.0590 calc R H11 H Uiso 0.41980 1.47670 0.64080 1.000 0.0410 calc R H12 H Uiso 0.40570 1.23790 0.60250 1.000 0.0370 calc R H13 H Uiso 0.22540 1.05040 0.42280 1.000 0.0330 calc R H15 H Uiso -0.19210 1.06640 0.42970 1.000 0.0360 calc R H16 H Uiso -0.39790 1.14800 0.47750 1.000 0.0370 calc R H17 H Uiso -0.51830 1.23040 0.32360 1.000 0.0360 calc R H18 H Uiso -0.42660 1.24020 0.13350 1.000 0.0400 calc R H19 H Uiso -0.22510 1.14890 0.08150 1.000 0.0360 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 Pd1 0.0153(2) 0.0265(2) 0.0234(2) 0.0124(2) 0.0067(1) 0.0068(2) Cl1 0.0203(4) 0.0349(5) 0.0331(5) 0.0132(4) 0.0062(3) 0.0021(4) S1 0.0255(4) 0.0343(5) 0.0315(5) 0.0095(4) 0.0059(4) 0.0154(4) P1 0.0179(4) 0.0271(5) 0.0243(4) 0.0132(4) 0.0072(3) 0.0082(4) O1 0.0297(13) 0.0283(14) 0.0516(16) 0.0203(12) 0.0150(12) 0.0114(11) O2 0.0230(12) 0.0255(13) 0.0401(14) 0.0123(11) 0.0108(10) 0.0100(10) C1 0.031(2) 0.030(2) 0.039(2) 0.0122(16) 0.0061(16) 0.0142(17) C2 0.0204(17) 0.0314(19) 0.0291(17) 0.0085(15) 0.0039(14) 0.0084(15) C3 0.0227(17) 0.0299(19) 0.0241(16) 0.0092(14) 0.0009(13) 0.0110(15) C4 0.0253(18) 0.0309(19) 0.0331(18) 0.0153(15) 0.0068(14) 0.0105(15) C5 0.0254(18) 0.037(2) 0.048(2) 0.0223(18) 0.0118(16) 0.0097(16) C6 0.031(2) 0.035(2) 0.057(2) 0.0245(19) 0.0165(18) 0.0135(17) C7 0.0181(16) 0.0293(19) 0.0319(17) 0.0173(15) 0.0100(13) 0.0074(14) C8 0.0209(16) 0.0335(19) 0.0249(16) 0.0118(14) 0.0067(13) 0.0086(15) C9 0.037(2) 0.037(2) 0.045(2) 0.0188(18) -0.0040(18) 0.0090(18) C10 0.048(3) 0.029(2) 0.061(3) 0.014(2) -0.001(2) 0.0061(19) C11 0.0277(19) 0.043(2) 0.0288(18) 0.0123(16) 0.0071(15) 0.0070(17) C12 0.0204(17) 0.048(2) 0.0237(17) 0.0122(16) 0.0080(14) 0.0114(16) C13 0.0240(17) 0.036(2) 0.0280(17) 0.0139(15) 0.0108(14) 0.0134(15) C14 0.0176(16) 0.0243(17) 0.0273(16) 0.0081(13) 0.0055(13) 0.0093(14) C15 0.0283(18) 0.040(2) 0.0281(17) 0.0163(16) 0.0074(14) 0.0156(16) C16 0.0309(19) 0.037(2) 0.0283(17) 0.0115(15) 0.0155(15) 0.0134(17) C17 0.0235(17) 0.033(2) 0.0354(19) 0.0088(15) 0.0086(14) 0.0120(16) C18 0.0290(19) 0.046(2) 0.0363(19) 0.0204(17) 0.0107(15) 0.0216(17) C19 0.0265(18) 0.044(2) 0.0271(17) 0.0178(16) 0.0112(14) 0.0164(17) _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; 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 Pd1 Cl1 2.2791(16) . . yes Pd1 P1 2.3027(15) . . yes Pd1 Cl1 2.2791(16) . 2_575 yes Pd1 P1 2.3027(15) . 2_575 yes S1 C1 1.707(4) . . yes S1 C2 1.720(4) . . yes P1 C7 1.848(4) . . yes P1 C8 1.822(4) . . yes P1 C14 1.821(3) . . yes O1 C4 1.369(5) . . yes O1 C6 1.437(5) . . yes O2 C3 1.384(5) . . yes O2 C5 1.438(5) . . yes C1 C4 1.363(6) . . no C2 C3 1.352(6) . . no C3 C4 1.419(6) . . no C5 C6 1.499(6) . . no C5 C7 1.511(6) . . no C8 C9 1.386(6) . . no C8 C13 1.387(5) . . no C9 C10 1.373(7) . . no C10 C11 1.392(6) . . no C11 C12 1.360(6) . . no C12 C13 1.379(5) . . no C14 C15 1.377(5) . . no C14 C19 1.392(5) . . no C15 C16 1.385(6) . . no C16 C17 1.401(5) . . no C17 C18 1.366(6) . . no C18 C19 1.406(6) . . no C1 H1 0.9500 . . no C2 H2 0.9500 . . no C5 H5 1.0000 . . no C6 H6A 0.9900 . . no C6 H6B 0.9900 . . no C7 H7A 0.9900 . . no C7 H7B 0.9900 . . no C9 H9 0.9500 . . no C10 H10 0.9500 . . no C11 H11 0.9500 . . no C12 H12 0.9500 . . no C13 H13 0.9500 . . no C15 H15 0.9500 . . no C16 H16 0.9500 . . no C17 H17 0.9500 . . no C18 H18 0.9500 . . no C19 H19 0.9500 . . no 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 Pd1 P1 86.45(3) . . . yes Cl1 Pd1 Cl1 180.00 . . 2_575 yes Cl1 Pd1 P1 93.55(3) . . 2_575 yes Cl1 Pd1 P1 93.55(3) 2_575 . . yes P1 Pd1 P1 180.00 . . 2_575 yes Cl1 Pd1 P1 86.45(3) 2_575 . 2_575 yes C1 S1 C2 92.9(2) . . . yes Pd1 P1 C7 111.76(11) . . . yes Pd1 P1 C8 119.50(12) . . . yes Pd1 P1 C14 112.77(11) . . . yes C7 P1 C8 107.37(16) . . . yes C7 P1 C14 103.46(18) . . . yes C8 P1 C14 100.30(17) . . . yes C4 O1 C6 112.8(3) . . . yes C3 O2 C5 111.9(3) . . . yes S1 C1 C4 110.8(3) . . . yes S1 C2 C3 110.1(3) . . . yes O2 C3 C2 124.6(4) . . . yes O2 C3 C4 121.6(3) . . . yes C2 C3 C4 113.8(4) . . . no O1 C4 C1 124.3(4) . . . yes O1 C4 C3 123.3(3) . . . yes C1 C4 C3 112.4(4) . . . no O2 C5 C6 111.0(3) . . . yes O2 C5 C7 107.7(3) . . . yes C6 C5 C7 111.6(3) . . . no O1 C6 C5 112.9(3) . . . yes P1 C7 C5 114.5(3) . . . yes P1 C8 C9 117.6(3) . . . yes P1 C8 C13 123.3(3) . . . yes C9 C8 C13 119.1(3) . . . no C8 C9 C10 120.3(4) . . . no C9 C10 C11 120.0(4) . . . no C10 C11 C12 119.8(4) . . . no C11 C12 C13 120.6(4) . . . no C8 C13 C12 120.1(4) . . . no P1 C14 C15 120.6(3) . . . yes P1 C14 C19 119.6(2) . . . yes C15 C14 C19 119.7(3) . . . no C14 C15 C16 121.6(3) . . . no C15 C16 C17 118.4(3) . . . no C16 C17 C18 120.6(4) . . . no C17 C18 C19 120.6(4) . . . no C14 C19 C18 119.0(3) . . . no S1 C1 H1 125.00 . . . no C4 C1 H1 125.00 . . . no S1 C2 H2 125.00 . . . no C3 C2 H2 125.00 . . . no O2 C5 H5 109.00 . . . no C6 C5 H5 109.00 . . . no C7 C5 H5 109.00 . . . no O1 C6 H6A 109.00 . . . no O1 C6 H6B 109.00 . . . no C5 C6 H6A 109.00 . . . no C5 C6 H6B 109.00 . . . no H6A C6 H6B 108.00 . . . no P1 C7 H7A 109.00 . . . no P1 C7 H7B 109.00 . . . no C5 C7 H7A 109.00 . . . no C5 C7 H7B 109.00 . . . no H7A C7 H7B 108.00 . . . no C8 C9 H9 120.00 . . . no C10 C9 H9 120.00 . . . no C9 C10 H10 120.00 . . . no C11 C10 H10 120.00 . . . no C10 C11 H11 120.00 . . . no C12 C11 H11 120.00 . . . no C11 C12 H12 120.00 . . . no C13 C12 H12 120.00 . . . no C8 C13 H13 120.00 . . . no C12 C13 H13 120.00 . . . no C14 C15 H15 119.00 . . . no C16 C15 H15 119.00 . . . no C15 C16 H16 121.00 . . . no C17 C16 H16 121.00 . . . no C16 C17 H17 120.00 . . . no C18 C17 H17 120.00 . . . no C17 C18 H18 120.00 . . . no C19 C18 H18 120.00 . . . no C14 C19 H19 121.00 . . . no C18 C19 H19 121.00 . . . no 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 Cl1 Pd1 P1 C7 57.48(14) . . . . no Cl1 Pd1 P1 C8 -175.99(15) . . . . no Cl1 Pd1 P1 C14 -58.59(14) . . . . no Cl1 Pd1 P1 C7 -122.52(14) 2_575 . . . no Cl1 Pd1 P1 C8 4.01(15) 2_575 . . . no Cl1 Pd1 P1 C14 121.41(14) 2_575 . . . no C2 S1 C1 C4 0.9(3) . . . . no C1 S1 C2 C3 -0.5(3) . . . . no Pd1 P1 C7 C5 35.1(3) . . . . no C8 P1 C7 C5 -97.8(3) . . . . no C14 P1 C7 C5 156.7(3) . . . . no Pd1 P1 C8 C9 74.2(3) . . . . no Pd1 P1 C8 C13 -105.4(3) . . . . no C7 P1 C8 C9 -157.3(3) . . . . no C7 P1 C8 C13 23.2(4) . . . . no C14 P1 C8 C9 -49.5(3) . . . . no C14 P1 C8 C13 130.9(3) . . . . no Pd1 P1 C14 C15 167.5(3) . . . . no Pd1 P1 C14 C19 -15.5(3) . . . . no C7 P1 C14 C15 46.5(3) . . . . no C7 P1 C14 C19 -136.4(3) . . . . no C8 P1 C14 C15 -64.3(3) . . . . no C8 P1 C14 C19 112.8(3) . . . . no C6 O1 C4 C1 169.5(3) . . . . no C6 O1 C4 C3 -13.0(5) . . . . no C4 O1 C6 C5 40.3(4) . . . . no C5 O2 C3 C2 158.9(3) . . . . no C5 O2 C3 C4 -21.5(4) . . . . no C3 O2 C5 C6 47.9(4) . . . . no C3 O2 C5 C7 170.4(3) . . . . no S1 C1 C4 O1 176.7(3) . . . . no S1 C1 C4 C3 -1.1(4) . . . . no S1 C2 C3 O2 179.7(2) . . . . no S1 C2 C3 C4 0.0(3) . . . . no O2 C3 C4 O1 3.2(5) . . . . no O2 C3 C4 C1 -179.0(3) . . . . no C2 C3 C4 O1 -177.1(3) . . . . no C2 C3 C4 C1 0.7(4) . . . . no O2 C5 C6 O1 -59.8(4) . . . . no C7 C5 C6 O1 -179.9(3) . . . . no O2 C5 C7 P1 51.3(3) . . . . no C6 C5 C7 P1 173.3(3) . . . . no P1 C8 C9 C10 177.3(4) . . . . no C13 C8 C9 C10 -3.1(6) . . . . no P1 C8 C13 C12 -176.5(3) . . . . no C9 C8 C13 C12 3.9(6) . . . . no C8 C9 C10 C11 -0.2(7) . . . . no C9 C10 C11 C12 2.7(7) . . . . no C10 C11 C12 C13 -1.9(6) . . . . no C11 C12 C13 C8 -1.4(6) . . . . no P1 C14 C15 C16 178.3(3) . . . . no C19 C14 C15 C16 1.2(6) . . . . no P1 C14 C19 C18 -176.9(3) . . . . no C15 C14 C19 C18 0.1(6) . . . . no C14 C15 C16 C17 -0.7(6) . . . . no C15 C16 C17 C18 -1.3(6) . . . . no C16 C17 C18 C19 2.7(6) . . . . no C17 C18 C19 C14 -2.1(6) . . . . no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag C1 H1 Cl1 0.9500 2.5700 3.519(5) 179.00 2_565 yes C13 H13 O2 0.9500 2.4400 3.150(5) 131.00 . yes _diffrn_measured_fraction_theta_max 0.949 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_full 0.949 _refine_diff_density_max 1.409 _refine_diff_density_min -0.760 _refine_diff_density_rms 0.113