# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_requested_category FM _publ_contact_author_name 'Evamarie Hey-Hawkins' _publ_contact_author_email hey@rz.uni-leipzig.de loop_ _publ_author_name A.Hildebrand I.Sarosi P.Lonnecke L.Silaghi-Dumitrescu ; I.Silaghi-Dumitrescu ; E.Hey-Hawkins data_c2100fin _database_code_depnum_ccdc_archive 'CCDC 858607' #TrackingRef '- Compound_1_c2100fin.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H26 Cl2 Ni P2 S2' _chemical_formula_weight 726.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ni Ni 0.3393 1.1124 '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' S S 0.1246 0.1234 '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' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 13.650(3) _cell_length_b 18.542(4) _cell_length_c 13.989(3) _cell_angle_alpha 90.00 _cell_angle_beta 111.879(4) _cell_angle_gamma 90.00 _cell_volume 3285.4(11) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 3383 _cell_measurement_theta_min 2.70 _cell_measurement_theta_max 28.23 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.468 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1488 _exptl_absorpt_coefficient_mu 1.005 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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 CCD area detector' _diffrn_measurement_method '\W scans' _diffrn_detector_area_resol_mean 81.92 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8640 _diffrn_reflns_av_R_equivalents 0.0528 _diffrn_reflns_av_sigmaI/netI 0.0601 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 28.53 _reflns_number_total 4050 _reflns_number_gt 2950 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SIR92 (Giacovazzo 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP3 for Windows (L. J. Farrugia, 1997)' _computing_publication_material 'WINGX (L.J. Farrugia,1999)' _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^ > 2\s(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^)+(0.0592P)^2^+5.1061P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4050 _refine_ls_number_parameters 261 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0947 _refine_ls_R_factor_gt 0.0631 _refine_ls_wR_factor_ref 0.1478 _refine_ls_wR_factor_gt 0.1362 _refine_ls_goodness_of_fit_ref 1.116 _refine_ls_restrained_S_all 1.117 _refine_ls_shift/su_max 0.000 _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 Ni1 Ni 0.0000 0.33220(3) 0.7500 0.02674(18) Uani 1 2 d S . . S1 S 0.03436(10) 0.41856(5) 0.66250(8) 0.0530(3) Uani 1 1 d . . . P1 P 0.05003(7) 0.25507(4) 0.66222(6) 0.0261(2) Uani 1 1 d . . . C1 C 0.0834(3) 0.3029(2) 0.5661(3) 0.0302(7) Uani 1 1 d . . . C2 C 0.0758(3) 0.3782(2) 0.5704(3) 0.0346(8) Uani 1 1 d . . . C3 C 0.1003(4) 0.4199(3) 0.4987(3) 0.0481(10) Uani 1 1 d . . . C4 C 0.1302(3) 0.3872(3) 0.4253(3) 0.0509(11) Uani 1 1 d . . . C5 C 0.1389(3) 0.3128(3) 0.4218(3) 0.0494(11) Uani 1 1 d . . . C6 C 0.1164(3) 0.2710(2) 0.4933(3) 0.0415(9) Uani 1 1 d . . . C7 C 0.1620(3) 0.19729(18) 0.7299(2) 0.0283(7) Uani 1 1 d . . . C8 C 0.1359(3) 0.12401(18) 0.7069(3) 0.0316(7) Uani 1 1 d . . . C9 C 0.2135(3) 0.0717(2) 0.7515(3) 0.0412(9) Uani 1 1 d . . . C10 C 0.3136(3) 0.0936(2) 0.8160(3) 0.0469(10) Uani 1 1 d . . . C11 C 0.3383(3) 0.1659(2) 0.8376(3) 0.0431(9) Uani 1 1 d . . . C12 C 0.2617(3) 0.2179(2) 0.7947(3) 0.0339(8) Uani 1 1 d . . . C13 C -0.0301(3) 0.17798(18) 0.6007(3) 0.0291(7) Uani 1 1 d . . . C14 C 0.0262(3) 0.11271(19) 0.6351(3) 0.0325(8) Uani 1 1 d . . . C15 C -0.0246(4) 0.0474(2) 0.5985(3) 0.0455(10) Uani 1 1 d . . . C16 C -0.1271(4) 0.0476(3) 0.5297(4) 0.0545(12) Uani 1 1 d . . . C17 C -0.1828(3) 0.1112(3) 0.4949(3) 0.0501(11) Uani 1 1 d . . . C18 C -0.1337(3) 0.1769(2) 0.5315(3) 0.0397(9) Uani 1 1 d . . . H3 H 0.090(4) 0.465(3) 0.501(4) 0.057(14) Uiso 1 1 d . . . H4 H 0.148(3) 0.416(2) 0.378(3) 0.051(12) Uiso 1 1 d . . . H5 H 0.160(3) 0.291(3) 0.372(4) 0.057(13) Uiso 1 1 d . . . H6 H 0.128(3) 0.223(3) 0.498(3) 0.055(13) Uiso 1 1 d . . . H9 H 0.190(3) 0.023(2) 0.726(3) 0.048(12) Uiso 1 1 d . . . H10 H 0.367(3) 0.061(2) 0.844(3) 0.046(12) Uiso 1 1 d . . . H11 H 0.410(3) 0.179(2) 0.881(3) 0.034(10) Uiso 1 1 d . . . H12 H 0.279(3) 0.265(2) 0.810(3) 0.034(10) Uiso 1 1 d . . . H15 H 0.014(3) 0.004(2) 0.626(3) 0.048(12) Uiso 1 1 d . . . H16 H -0.156(4) 0.003(3) 0.505(4) 0.079(17) Uiso 1 1 d . . . H17 H -0.252(3) 0.110(2) 0.445(3) 0.041(11) Uiso 1 1 d . . . H18 H -0.168(3) 0.218(2) 0.509(3) 0.045(12) Uiso 1 1 d . . . Cl1 Cl 0.3775(9) 0.3794(6) 0.6906(8) 0.080(2) Uani 0.50 1 d PD A -1 Cl2 Cl 0.6056(8) 0.3738(7) 0.7956(9) 0.102(3) Uani 0.50 1 d PD A -1 C19 C 0.4834(8) 0.3366(6) 0.7881(9) 0.100(6) Uani 0.50 1 d PD A -1 H19A H 0.4823 0.2848 0.7733 0.121 Uiso 0.50 1 calc PR A -1 H19B H 0.4754 0.3425 0.8544 0.121 Uiso 0.50 1 calc PR A -1 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 Ni1 0.0362(3) 0.0181(3) 0.0305(3) 0.000 0.0178(3) 0.000 S1 0.1007(9) 0.0224(5) 0.0549(7) 0.0020(4) 0.0510(7) -0.0044(5) P1 0.0316(5) 0.0214(4) 0.0287(4) 0.0021(3) 0.0152(4) 0.0035(3) C1 0.0295(16) 0.0355(19) 0.0287(17) 0.0046(14) 0.0142(14) 0.0017(14) C2 0.0367(19) 0.035(2) 0.0337(19) 0.0061(15) 0.0156(16) -0.0042(15) C3 0.060(3) 0.041(3) 0.049(2) 0.009(2) 0.027(2) -0.011(2) C4 0.052(3) 0.065(3) 0.044(2) 0.017(2) 0.027(2) -0.006(2) C5 0.045(2) 0.071(3) 0.044(2) 0.008(2) 0.031(2) 0.006(2) C6 0.047(2) 0.045(2) 0.040(2) 0.0057(18) 0.0251(18) 0.0128(19) C7 0.0330(17) 0.0303(17) 0.0255(16) 0.0032(14) 0.0153(14) 0.0039(14) C8 0.0370(19) 0.0272(17) 0.0361(18) -0.0006(14) 0.0199(15) 0.0028(14) C9 0.049(2) 0.030(2) 0.050(2) 0.0066(17) 0.0250(19) 0.0087(17) C10 0.045(2) 0.053(3) 0.045(2) 0.016(2) 0.0206(19) 0.022(2) C11 0.0317(19) 0.059(3) 0.038(2) 0.0076(19) 0.0120(16) 0.0034(18) C12 0.0368(19) 0.036(2) 0.0330(18) 0.0011(15) 0.0176(15) -0.0015(15) C13 0.0331(17) 0.0286(18) 0.0310(17) -0.0020(13) 0.0182(14) 0.0024(13) C14 0.0412(19) 0.0275(18) 0.0346(18) -0.0016(14) 0.0208(15) 0.0018(15) C15 0.054(3) 0.032(2) 0.056(2) -0.0083(19) 0.027(2) -0.0066(18) C16 0.059(3) 0.046(3) 0.061(3) -0.021(2) 0.026(2) -0.020(2) C17 0.038(2) 0.063(3) 0.048(2) -0.013(2) 0.014(2) -0.012(2) C18 0.036(2) 0.045(2) 0.040(2) -0.0003(17) 0.0175(17) 0.0021(17) Cl1 0.096(4) 0.042(2) 0.081(3) 0.008(2) 0.010(3) 0.011(2) Cl2 0.095(5) 0.063(5) 0.161(9) 0.001(5) 0.064(6) 0.009(4) C19 0.084(9) 0.067(7) 0.110(12) 0.035(7) -0.011(9) -0.020(7) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Ni1 P1 2.1551(9) . ? Ni1 P1 2.1551(9) 2_556 ? Ni1 S1 2.1702(11) 2_556 ? Ni1 S1 2.1702(11) . ? S1 C2 1.756(4) . ? P1 C1 1.804(3) . ? P1 C13 1.811(3) . ? P1 C7 1.817(3) . ? C1 C6 1.391(5) . ? C1 C2 1.403(5) . ? C2 C3 1.403(5) . ? C3 C4 1.379(6) . ? C3 H3 0.86(5) . ? C4 C5 1.387(7) . ? C4 H4 0.96(5) . ? C5 C6 1.386(6) . ? C5 H5 0.94(5) . ? C6 H6 0.90(5) . ? C7 C12 1.379(5) . ? C7 C8 1.411(5) . ? C8 C9 1.399(5) . ? C8 C14 1.474(5) . ? C9 C10 1.388(6) . ? C9 H9 0.97(4) . ? C10 C11 1.389(6) . ? C10 H10 0.91(4) . ? C11 C12 1.383(5) . ? C11 H11 0.97(4) . ? C12 H12 0.91(4) . ? C13 C18 1.384(5) . ? C13 C14 1.418(5) . ? C14 C15 1.395(5) . ? C15 C16 1.371(6) . ? C15 H15 0.96(4) . ? C16 C17 1.390(7) . ? C16 H16 0.92(5) . ? C17 C18 1.394(6) . ? C17 H17 0.94(4) . ? C18 H18 0.90(4) . ? Cl1 C19 1.764(5) . ? Cl2 C19 1.772(5) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? 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 P1 Ni1 P1 96.85(5) . 2_556 ? P1 Ni1 S1 172.72(4) . 2_556 ? P1 Ni1 S1 89.28(4) 2_556 2_556 ? P1 Ni1 S1 89.28(4) . . ? P1 Ni1 S1 172.72(4) 2_556 . ? S1 Ni1 S1 84.91(6) 2_556 . ? C2 S1 Ni1 107.18(12) . . ? C1 P1 C13 108.00(16) . . ? C1 P1 C7 106.30(15) . . ? C13 P1 C7 91.38(15) . . ? C1 P1 Ni1 108.66(12) . . ? C13 P1 Ni1 122.09(11) . . ? C7 P1 Ni1 118.56(11) . . ? C6 C1 C2 120.2(3) . . ? C6 C1 P1 125.3(3) . . ? C2 C1 P1 114.4(3) . . ? C3 C2 C1 118.5(4) . . ? C3 C2 S1 121.2(3) . . ? C1 C2 S1 120.3(3) . . ? C4 C3 C2 120.3(4) . . ? C4 C3 H3 124(3) . . ? C2 C3 H3 115(3) . . ? C3 C4 C5 121.1(4) . . ? C3 C4 H4 120(3) . . ? C5 C4 H4 119(3) . . ? C6 C5 C4 119.1(4) . . ? C6 C5 H5 121(3) . . ? C4 C5 H5 120(3) . . ? C5 C6 C1 120.7(4) . . ? C5 C6 H6 121(3) . . ? C1 C6 H6 118(3) . . ? C12 C7 C8 121.4(3) . . ? C12 C7 P1 127.7(3) . . ? C8 C7 P1 110.9(2) . . ? C9 C8 C7 118.7(3) . . ? C9 C8 C14 127.8(3) . . ? C7 C8 C14 113.5(3) . . ? C10 C9 C8 119.1(4) . . ? C10 C9 H9 128(2) . . ? C8 C9 H9 113(2) . . ? C9 C10 C11 121.6(4) . . ? C9 C10 H10 122(3) . . ? C11 C10 H10 117(3) . . ? C12 C11 C10 119.7(4) . . ? C12 C11 H11 121(2) . . ? C10 C11 H11 119(2) . . ? C7 C12 C11 119.5(4) . . ? C7 C12 H12 122(2) . . ? C11 C12 H12 119(2) . . ? C18 C13 C14 120.6(3) . . ? C18 C13 P1 128.5(3) . . ? C14 C13 P1 110.9(2) . . ? C15 C14 C13 119.0(3) . . ? C15 C14 C8 127.8(3) . . ? C13 C14 C8 113.2(3) . . ? C16 C15 C14 119.5(4) . . ? C16 C15 H15 123(3) . . ? C14 C15 H15 117(3) . . ? C15 C16 C17 122.1(4) . . ? C15 C16 H16 116(3) . . ? C17 C16 H16 122(3) . . ? C16 C17 C18 119.2(4) . . ? C16 C17 H17 120(3) . . ? C18 C17 H17 121(3) . . ? C13 C18 C17 119.7(4) . . ? C13 C18 H18 120(3) . . ? C17 C18 H18 120(3) . . ? Cl1 C19 Cl2 110.6(5) . . ? Cl1 C19 H19A 109.5 . . ? Cl2 C19 H19A 109.5 . . ? Cl1 C19 H19B 109.5 . . ? Cl2 C19 H19B 109.5 . . ? H19A C19 H19B 108.1 . . ? _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 28.53 _diffrn_measured_fraction_theta_full 0.963 _refine_diff_density_max 0.433 _refine_diff_density_min -0.810 _refine_diff_density_rms 0.094 # Attachment '- Compound_2_s024_fin.cif' data_s024_fin _database_code_depnum_ccdc_archive 'CCDC 858608' #TrackingRef '- Compound_2_s024_fin.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H26 Cl2 P2 Pd S2' _chemical_formula_weight 773.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Pd Pd -0.9988 1.0072 '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' S S 0.1246 0.1234 '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' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 13.7556(10) _cell_length_b 18.8379(16) _cell_length_c 14.0750(10) _cell_angle_alpha 90.00 _cell_angle_beta 112.827(8) _cell_angle_gamma 90.00 _cell_volume 3361.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 208(2) _cell_measurement_reflns_used 7997 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 30.3 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.529 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1560 _exptl_absorpt_coefficient_mu 0.957 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.6897 _exptl_absorpt_correction_T_max 0.7828 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 208(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 'Stoe IPDS area detector' _diffrn_measurement_method '\f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33423 _diffrn_reflns_av_R_equivalents 0.0392 _diffrn_reflns_av_sigmaI/netI 0.0242 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 30.27 _reflns_number_total 4858 _reflns_number_gt 4055 _reflns_threshold_expression >2\s(I) _computing_data_collection 'STOE IPDS software' _computing_cell_refinement 'STOE IPDS software' _computing_data_reduction 'STOE IPDS software, STOE X-RED' _computing_structure_solution SHELXS-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP3 for Windows (L. J. Farrugia, 1997)' _computing_publication_material 'WINGX (L.J. Farrugia,1999)' _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^ > 2\s(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^)+(0.0461P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4858 _refine_ls_number_parameters 261 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0307 _refine_ls_R_factor_gt 0.0251 _refine_ls_wR_factor_ref 0.0666 _refine_ls_wR_factor_gt 0.0654 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.001 _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 Pd1 Pd 0.0000 0.331066(7) 0.7500 0.02215(5) Uani 1 2 d S . . S1 S 0.03800(5) 0.41978(2) 0.65630(4) 0.04726(13) Uani 1 1 d . . . P1 P 0.05008(3) 0.252518(18) 0.65665(3) 0.02249(8) Uani 1 1 d . . . C1 C 0.08298(12) 0.30169(9) 0.56281(13) 0.0299(3) Uani 1 1 d . . . C2 C 0.07650(13) 0.37581(9) 0.56626(13) 0.0332(3) Uani 1 1 d . . . C3 C 0.10074(17) 0.41611(11) 0.49390(15) 0.0452(5) Uani 1 1 d . . . C4 C 0.12931(18) 0.38291(14) 0.42162(17) 0.0536(6) Uani 1 1 d . . . C5 C 0.13730(18) 0.30938(15) 0.41976(18) 0.0532(5) Uani 1 1 d . . . C6 C 0.11454(16) 0.26892(12) 0.49078(16) 0.0436(4) Uani 1 1 d . . . C7 C 0.16049(12) 0.19461(8) 0.72455(11) 0.0250(3) Uani 1 1 d . . . C8 C 0.13239(13) 0.12287(8) 0.70295(13) 0.0300(3) Uani 1 1 d . . . C9 C 0.20871(17) 0.07083(10) 0.75006(16) 0.0422(4) Uani 1 1 d . . . C10 C 0.30962(16) 0.09130(12) 0.81564(16) 0.0480(5) Uani 1 1 d . . . C11 C 0.33636(15) 0.16191(12) 0.83624(15) 0.0440(4) Uani 1 1 d . . . C12 C 0.26139(13) 0.21465(10) 0.79094(12) 0.0328(3) Uani 1 1 d . . . C13 C -0.03240(12) 0.17742(8) 0.59426(12) 0.0272(3) Uani 1 1 d . . . C14 C 0.02215(14) 0.11311(8) 0.62949(13) 0.0316(3) Uani 1 1 d . . . C15 C -0.03009(18) 0.04875(10) 0.59429(19) 0.0487(5) Uani 1 1 d . . . C16 C -0.1345(2) 0.04999(13) 0.5236(2) 0.0601(6) Uani 1 1 d . . . C17 C -0.18719(18) 0.11294(14) 0.48845(18) 0.0545(6) Uani 1 1 d . . . C18 C -0.13687(14) 0.17796(11) 0.52421(14) 0.0391(4) Uani 1 1 d . . . H3 H 0.0996(19) 0.4688(13) 0.4948(19) 0.054(7) Uiso 1 1 d . . . H4 H 0.1412(18) 0.4112(13) 0.3753(19) 0.052(6) Uiso 1 1 d . . . H5 H 0.154(2) 0.2818(15) 0.368(2) 0.072(8) Uiso 1 1 d . . . H6 H 0.119(2) 0.2183(15) 0.490(2) 0.062(7) Uiso 1 1 d . . . H9 H 0.191(2) 0.0231(13) 0.7346(19) 0.058(7) Uiso 1 1 d . . . H10 H 0.360(2) 0.0536(14) 0.843(2) 0.062(7) Uiso 1 1 d . . . H11 H 0.406(2) 0.1718(13) 0.880(2) 0.059(7) Uiso 1 1 d . . . H12 H 0.2777(17) 0.2630(12) 0.8067(17) 0.042(6) Uiso 1 1 d . . . H15 H -0.001(2) 0.0053(16) 0.611(2) 0.071(8) Uiso 1 1 d . . . H16 H -0.171(2) 0.0075(18) 0.497(2) 0.090(10) Uiso 1 1 d . . . H17 H -0.252(2) 0.1134(15) 0.447(2) 0.074(9) Uiso 1 1 d . . . H18 H -0.1719(17) 0.2205(11) 0.5009(17) 0.040(6) Uiso 1 1 d . . . Cl1 Cl 0.3895(4) 0.3769(2) 0.7015(5) 0.146(2) Uani 0.50 1 d PD A -1 Cl2 Cl 0.6196(3) 0.37941(18) 0.8068(2) 0.0943(14) Uani 0.50 1 d PD A -1 C19 C 0.4987(5) 0.3376(4) 0.7900(7) 0.177(8) Uani 0.50 1 d PD A -1 H19A H 0.5015 0.2883 0.7691 0.212 Uiso 0.50 1 calc PR A -1 H19B H 0.4915 0.3367 0.8566 0.212 Uiso 0.50 1 calc PR A -1 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 0.02736(8) 0.01671(7) 0.02380(8) 0.000 0.01148(6) 0.000 S1 0.0840(4) 0.02182(18) 0.0464(3) 0.00442(16) 0.0368(3) -0.00641(19) P1 0.02471(17) 0.02217(16) 0.02269(18) 0.00262(12) 0.01151(15) 0.00363(12) C1 0.0262(7) 0.0384(8) 0.0271(7) 0.0087(6) 0.0126(6) 0.0035(6) C2 0.0322(8) 0.0383(8) 0.0284(8) 0.0086(6) 0.0109(6) -0.0061(6) C3 0.0496(10) 0.0490(10) 0.0372(9) 0.0132(8) 0.0172(8) -0.0135(8) C4 0.0467(11) 0.0794(15) 0.0401(11) 0.0213(10) 0.0228(9) -0.0096(10) C5 0.0486(11) 0.0809(16) 0.0421(11) 0.0124(10) 0.0307(10) 0.0088(11) C6 0.0440(10) 0.0547(11) 0.0411(10) 0.0096(8) 0.0264(9) 0.0137(8) C7 0.0271(7) 0.0274(6) 0.0233(6) 0.0033(5) 0.0129(6) 0.0059(5) C8 0.0361(8) 0.0272(7) 0.0314(8) 0.0028(6) 0.0183(7) 0.0062(6) C9 0.0512(10) 0.0310(8) 0.0496(10) 0.0086(7) 0.0254(9) 0.0141(7) C10 0.0438(10) 0.0554(11) 0.0453(10) 0.0168(9) 0.0180(9) 0.0262(9) C11 0.0295(8) 0.0655(13) 0.0328(9) 0.0077(8) 0.0075(7) 0.0125(8) C12 0.0300(7) 0.0414(8) 0.0270(7) 0.0022(6) 0.0111(6) 0.0027(6) C13 0.0277(7) 0.0323(7) 0.0248(7) -0.0035(5) 0.0135(6) -0.0008(5) C14 0.0378(8) 0.0281(7) 0.0344(8) -0.0044(6) 0.0200(7) -0.0016(6) C15 0.0572(12) 0.0315(8) 0.0612(13) -0.0118(8) 0.0270(10) -0.0068(8) C16 0.0594(13) 0.0548(12) 0.0685(15) -0.0267(11) 0.0274(12) -0.0261(11) C17 0.0370(10) 0.0775(15) 0.0453(11) -0.0177(10) 0.0119(9) -0.0180(10) C18 0.0291(8) 0.0553(10) 0.0326(8) -0.0023(7) 0.0117(7) -0.0003(7) Cl1 0.135(3) 0.074(2) 0.257(5) -0.026(3) 0.106(3) -0.025(2) Cl2 0.120(3) 0.0499(14) 0.0834(14) -0.0118(11) 0.0073(15) -0.0147(14) C19 0.168(9) 0.088(5) 0.154(10) 0.051(5) -0.069(9) -0.067(6) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Pd1 P1 2.2567(4) . ? Pd1 P1 2.2567(4) 2_556 ? Pd1 S1 2.3110(5) 2_556 ? Pd1 S1 2.3110(5) . ? S1 C2 1.759(2) . ? P1 C1 1.8087(17) . ? P1 C7 1.8121(14) . ? P1 C13 1.8129(15) . ? C1 C6 1.392(3) . ? C1 C2 1.401(2) . ? C2 C3 1.410(2) . ? C3 C4 1.375(3) . ? C3 H3 0.99(2) . ? C4 C5 1.390(4) . ? C4 H4 0.91(3) . ? C5 C6 1.386(3) . ? C5 H5 1.00(3) . ? C6 H6 0.96(3) . ? C7 C12 1.391(2) . ? C7 C8 1.406(2) . ? C8 C9 1.401(2) . ? C8 C14 1.478(2) . ? C9 C10 1.390(3) . ? C9 H9 0.94(2) . ? C10 C11 1.381(3) . ? C10 H10 0.96(3) . ? C11 C12 1.395(2) . ? C11 H11 0.93(3) . ? C12 H12 0.94(2) . ? C13 C18 1.392(2) . ? C13 C14 1.410(2) . ? C14 C15 1.398(2) . ? C15 C16 1.395(3) . ? C15 H15 0.90(3) . ? C16 C17 1.377(4) . ? C16 H16 0.94(3) . ? C17 C18 1.401(3) . ? C17 H17 0.86(3) . ? C18 H18 0.93(2) . ? Cl1 C19 1.705(4) . ? Cl2 C19 1.771(5) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? 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 P1 Pd1 P1 98.06(2) . 2_556 ? P1 Pd1 S1 173.813(17) . 2_556 ? P1 Pd1 S1 87.373(17) 2_556 2_556 ? P1 Pd1 S1 87.373(17) . . ? P1 Pd1 S1 173.813(17) 2_556 . ? S1 Pd1 S1 87.37(3) 2_556 . ? C2 S1 Pd1 105.58(6) . . ? C1 P1 C7 107.31(7) . . ? C1 P1 C13 109.44(8) . . ? C7 P1 C13 91.42(7) . . ? C1 P1 Pd1 107.98(6) . . ? C7 P1 Pd1 118.05(5) . . ? C13 P1 Pd1 121.24(5) . . ? C6 C1 C2 120.61(16) . . ? C6 C1 P1 122.79(14) . . ? C2 C1 P1 116.60(13) . . ? C1 C2 C3 118.38(17) . . ? C1 C2 S1 122.37(12) . . ? C3 C2 S1 119.25(15) . . ? C4 C3 C2 120.3(2) . . ? C4 C3 H3 118.3(15) . . ? C2 C3 H3 121.3(15) . . ? C3 C4 C5 120.95(19) . . ? C3 C4 H4 116.6(16) . . ? C5 C4 H4 122.4(16) . . ? C6 C5 C4 119.5(2) . . ? C6 C5 H5 115.2(17) . . ? C4 C5 H5 125.1(17) . . ? C5 C6 C1 120.2(2) . . ? C5 C6 H6 120.4(17) . . ? C1 C6 H6 119.4(17) . . ? C12 C7 C8 121.66(14) . . ? C12 C7 P1 127.19(12) . . ? C8 C7 P1 111.15(11) . . ? C9 C8 C7 118.52(16) . . ? C9 C8 C14 128.39(16) . . ? C7 C8 C14 113.08(13) . . ? C10 C9 C8 119.48(18) . . ? C10 C9 H9 121.7(15) . . ? C8 C9 H9 118.8(16) . . ? C11 C10 C9 121.50(16) . . ? C11 C10 H10 122.1(16) . . ? C9 C10 H10 116.3(16) . . ? C10 C11 C12 120.04(17) . . ? C10 C11 H11 116.9(15) . . ? C12 C11 H11 123.0(15) . . ? C7 C12 C11 118.79(17) . . ? C7 C12 H12 120.3(13) . . ? C11 C12 H12 120.9(14) . . ? C18 C13 C14 121.17(15) . . ? C18 C13 P1 128.14(13) . . ? C14 C13 P1 110.64(11) . . ? C15 C14 C13 119.35(17) . . ? C15 C14 C8 127.02(16) . . ? C13 C14 C8 113.62(13) . . ? C16 C15 C14 118.9(2) . . ? C16 C15 H15 115.9(18) . . ? C14 C15 H15 125.1(18) . . ? C17 C16 C15 121.53(19) . . ? C17 C16 H16 118(2) . . ? C15 C16 H16 121(2) . . ? C16 C17 C18 120.4(2) . . ? C16 C17 H17 121(2) . . ? C18 C17 H17 118(2) . . ? C13 C18 C17 118.59(19) . . ? C13 C18 H18 120.6(13) . . ? C17 C18 H18 120.8(13) . . ? Cl1 C19 Cl2 114.8(3) . . ? Cl1 C19 H19A 108.6 . . ? Cl2 C19 H19A 108.6 . . ? Cl1 C19 H19B 108.6 . . ? Cl2 C19 H19B 108.6 . . ? H19A C19 H19B 107.5 . . ? _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 30.27 _diffrn_measured_fraction_theta_full 0.963 _refine_diff_density_max 0.788 _refine_diff_density_min -0.608 _refine_diff_density_rms 0.069 # Attachment '- Compound_3_c1750fin.cif' data_c1750fin _database_code_depnum_ccdc_archive 'CCDC 858609' #TrackingRef '- Compound_3_c1750fin.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H26 Cl2 P2 Pt S2' _chemical_formula_weight 862.63 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Pt Pt -1.7033 8.3905 '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' S S 0.1246 0.1234 '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' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 13.714(5) _cell_length_b 18.770(5) _cell_length_c 13.998(4) _cell_angle_alpha 90.00 _cell_angle_beta 112.904(7) _cell_angle_gamma 90.00 _cell_volume 3319.3(18) _cell_formula_units_Z 4 _cell_measurement_temperature 210(2) _cell_measurement_reflns_used 978 _cell_measurement_theta_min 2.68 _cell_measurement_theta_max 28.42 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.726 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1688 _exptl_absorpt_coefficient_mu 4.637 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 210(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 CCD area detector' _diffrn_measurement_method '\W scans' _diffrn_detector_area_resol_mean 81.92 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16932 _diffrn_reflns_av_R_equivalents 0.0358 _diffrn_reflns_av_sigmaI/netI 0.0341 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 29.37 _reflns_number_total 4233 _reflns_number_gt 3640 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP3 for Windows (L. J. Farrugia, 1997)' _computing_publication_material 'WINGX (L.J. Farrugia,1999)' _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^ > 2\s(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^)+(0.0240P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4233 _refine_ls_number_parameters 261 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0332 _refine_ls_R_factor_gt 0.0226 _refine_ls_wR_factor_ref 0.0450 _refine_ls_wR_factor_gt 0.0430 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.005 _refine_ls_shift/su_max 0.001 _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 0.0000 0.331236(7) 0.7500 0.02200(5) Uani 1 2 d S . . S1 S 0.03910(7) 0.42034(4) 0.65670(6) 0.04215(18) Uani 1 1 d . . . P1 P 0.05038(5) 0.25281(3) 0.65785(5) 0.02267(13) Uani 1 1 d . . . C1 C 0.08312(19) 0.30169(15) 0.56351(19) 0.0283(5) Uani 1 1 d . . . C2 C 0.0773(2) 0.37587(15) 0.5664(2) 0.0324(6) Uani 1 1 d . . . C3 C 0.1015(2) 0.41586(18) 0.4933(2) 0.0415(7) Uani 1 1 d . . . C4 C 0.1304(2) 0.3824(2) 0.4218(2) 0.0487(8) Uani 1 1 d . . . C5 C 0.1379(3) 0.3088(2) 0.4198(2) 0.0492(8) Uani 1 1 d . . . C6 C 0.1147(2) 0.26839(18) 0.4909(2) 0.0390(7) Uani 1 1 d . . . C7 C 0.16102(19) 0.19512(13) 0.72582(18) 0.0236(5) Uani 1 1 d . . . C8 C 0.1331(2) 0.12351(13) 0.70356(19) 0.0283(5) Uani 1 1 d . . . C9 C 0.2096(2) 0.07138(16) 0.7506(2) 0.0394(7) Uani 1 1 d . . . C10 C 0.3099(2) 0.09185(18) 0.8165(2) 0.0431(7) Uani 1 1 d . . . C11 C 0.3366(2) 0.16249(18) 0.8375(2) 0.0406(7) Uani 1 1 d . . . C12 C 0.2617(2) 0.21497(16) 0.79229(19) 0.0312(6) Uani 1 1 d . . . C13 C -0.03188(19) 0.17763(14) 0.59535(18) 0.0267(5) Uani 1 1 d . . . C14 C 0.0226(2) 0.11309(14) 0.6300(2) 0.0296(6) Uani 1 1 d . . . C15 C -0.0294(3) 0.04936(17) 0.5942(3) 0.0439(7) Uani 1 1 d . . . C16 C -0.1336(3) 0.0500(2) 0.5237(3) 0.0517(8) Uani 1 1 d . . . C17 C -0.1864(3) 0.1133(2) 0.4895(2) 0.0481(8) Uani 1 1 d . . . C18 C -0.1362(2) 0.17802(18) 0.5257(2) 0.0362(6) Uani 1 1 d . . . H3 H 0.095(2) 0.4691(17) 0.495(2) 0.052(9) Uiso 1 1 d . . . H4 H 0.145(2) 0.4117(15) 0.372(2) 0.036(7) Uiso 1 1 d . . . H5 H 0.159(3) 0.2856(18) 0.375(2) 0.056(10) Uiso 1 1 d . . . H6 H 0.119(2) 0.2140(18) 0.494(2) 0.043(8) Uiso 1 1 d . . . H9 H 0.186(2) 0.0226(16) 0.733(2) 0.042(8) Uiso 1 1 d . . . H10 H 0.359(2) 0.0597(17) 0.844(2) 0.047(9) Uiso 1 1 d . . . H11 H 0.408(3) 0.1737(16) 0.884(3) 0.056(10) Uiso 1 1 d . . . H12 H 0.277(2) 0.2648(16) 0.804(2) 0.032(7) Uiso 1 1 d . . . H15 H 0.007(2) 0.0063(17) 0.615(2) 0.038(8) Uiso 1 1 d . . . H16 H -0.169(2) 0.0039(18) 0.494(2) 0.050(8) Uiso 1 1 d . . . H17 H -0.252(2) 0.1151(16) 0.444(2) 0.041(8) Uiso 1 1 d . . . H18 H -0.168(2) 0.2221(16) 0.506(2) 0.040(8) Uiso 1 1 d . . . Cl1 Cl 0.3737(6) 0.3791(4) 0.6902(5) 0.0793(14) Uani 0.50 1 d PD A -1 Cl2 Cl 0.6017(6) 0.3782(5) 0.7945(7) 0.119(3) Uani 0.50 1 d PD A -1 C19 C 0.4820(6) 0.3411(4) 0.7912(6) 0.101(4) Uani 0.50 1 d PD A -1 H19A H 0.4823 0.2895 0.7810 0.121 Uiso 0.50 1 calc PR A -1 H19B H 0.4755 0.3499 0.8575 0.121 Uiso 0.50 1 calc PR A -1 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 0.02410(7) 0.01905(7) 0.02321(7) 0.000 0.00958(5) 0.000 S1 0.0689(5) 0.0224(3) 0.0428(4) 0.0036(3) 0.0301(4) -0.0052(3) P1 0.0232(3) 0.0239(3) 0.0218(3) 0.0020(2) 0.0098(3) 0.0024(3) C1 0.0223(12) 0.0375(14) 0.0247(12) 0.0068(11) 0.0088(10) 0.0014(11) C2 0.0286(13) 0.0380(16) 0.0281(13) 0.0068(11) 0.0084(11) -0.0039(12) C3 0.0406(16) 0.0452(19) 0.0377(16) 0.0109(14) 0.0141(13) -0.0101(15) C4 0.0427(17) 0.070(2) 0.0376(17) 0.0178(16) 0.0205(14) -0.0077(16) C5 0.0434(18) 0.075(2) 0.0396(17) 0.0082(16) 0.0278(15) 0.0054(16) C6 0.0379(16) 0.0487(19) 0.0341(15) 0.0075(13) 0.0182(13) 0.0113(14) C7 0.0245(12) 0.0266(12) 0.0215(11) 0.0024(9) 0.0107(10) 0.0048(10) C8 0.0336(14) 0.0259(13) 0.0292(13) 0.0026(10) 0.0163(11) 0.0054(11) C9 0.0465(17) 0.0309(16) 0.0443(16) 0.0058(13) 0.0215(14) 0.0116(14) C10 0.0387(17) 0.0480(19) 0.0417(16) 0.0142(14) 0.0146(14) 0.0225(16) C11 0.0312(14) 0.059(2) 0.0297(13) 0.0057(14) 0.0094(12) 0.0105(15) C12 0.0293(14) 0.0380(16) 0.0259(13) 0.0033(11) 0.0102(11) 0.0034(12) C13 0.0268(12) 0.0326(14) 0.0238(11) -0.0026(10) 0.0131(10) 0.0006(11) C14 0.0335(14) 0.0284(14) 0.0308(13) -0.0033(11) 0.0170(11) 0.0007(11) C15 0.0506(19) 0.0320(16) 0.0530(19) -0.0088(14) 0.0245(16) -0.0036(15) C16 0.051(2) 0.049(2) 0.055(2) -0.0198(17) 0.0198(17) -0.0187(17) C17 0.0318(17) 0.069(2) 0.0398(17) -0.0139(16) 0.0096(14) -0.0128(17) C18 0.0286(13) 0.0500(19) 0.0299(13) 0.0000(13) 0.0113(11) -0.0010(14) Cl1 0.088(3) 0.047(2) 0.0780(19) 0.0128(15) 0.0053(18) 0.0045(19) Cl2 0.093(4) 0.077(3) 0.182(7) 0.027(4) 0.050(5) 0.012(3) C19 0.075(7) 0.078(6) 0.102(8) 0.028(5) -0.016(6) -0.031(5) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 P1 2.2365(7) 2_556 ? Pt1 P1 2.2365(7) . ? Pt1 S1 2.3098(8) 2_556 ? Pt1 S1 2.3098(8) . ? S1 C2 1.757(3) . ? P1 C1 1.803(3) . ? P1 C7 1.805(2) . ? P1 C13 1.806(3) . ? C1 C2 1.396(4) . ? C1 C6 1.398(4) . ? C2 C3 1.408(4) . ? C3 C4 1.366(5) . ? C3 H3 1.00(3) . ? C4 C5 1.385(5) . ? C4 H4 0.97(3) . ? C5 C6 1.383(4) . ? C5 H5 0.89(3) . ? C6 H6 1.02(3) . ? C7 C12 1.382(4) . ? C7 C8 1.399(4) . ? C8 C9 1.398(4) . ? C8 C14 1.477(4) . ? C9 C10 1.380(5) . ? C9 H9 0.97(3) . ? C10 C11 1.377(4) . ? C10 H10 0.88(3) . ? C11 C12 1.386(4) . ? C11 H11 0.97(3) . ? C12 H12 0.96(3) . ? C13 C18 1.382(4) . ? C13 C14 1.407(3) . ? C14 C15 1.383(4) . ? C15 C16 1.385(5) . ? C15 H15 0.93(3) . ? C16 C17 1.376(5) . ? C16 H16 1.00(3) . ? C17 C18 1.391(4) . ? C17 H17 0.87(3) . ? C18 H18 0.93(3) . ? Cl1 C19 1.755(5) . ? Cl2 C19 1.768(5) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? 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 P1 Pt1 P1 97.68(4) 2_556 . ? P1 Pt1 S1 87.63(3) 2_556 2_556 ? P1 Pt1 S1 173.98(3) . 2_556 ? P1 Pt1 S1 173.98(2) 2_556 . ? P1 Pt1 S1 87.63(3) . . ? S1 Pt1 S1 87.22(4) 2_556 . ? C2 S1 Pt1 105.24(9) . . ? C1 P1 C7 107.07(11) . . ? C1 P1 C13 109.24(12) . . ? C7 P1 C13 91.44(12) . . ? C1 P1 Pt1 107.97(9) . . ? C7 P1 Pt1 118.42(8) . . ? C13 P1 Pt1 121.25(8) . . ? C2 C1 C6 120.3(2) . . ? C2 C1 P1 116.96(19) . . ? C6 C1 P1 122.8(2) . . ? C1 C2 C3 118.6(3) . . ? C1 C2 S1 122.07(19) . . ? C3 C2 S1 119.3(2) . . ? C4 C3 C2 120.3(3) . . ? C4 C3 H3 121.7(18) . . ? C2 C3 H3 118.0(18) . . ? C3 C4 C5 121.2(3) . . ? C3 C4 H4 117.8(17) . . ? C5 C4 H4 121.0(17) . . ? C6 C5 C4 119.5(3) . . ? C6 C5 H5 117(2) . . ? C4 C5 H5 123(2) . . ? C5 C6 C1 120.1(3) . . ? C5 C6 H6 123.3(17) . . ? C1 C6 H6 116.6(17) . . ? C12 C7 C8 121.6(2) . . ? C12 C7 P1 127.4(2) . . ? C8 C7 P1 110.97(18) . . ? C9 C8 C7 118.5(2) . . ? C9 C8 C14 127.9(3) . . ? C7 C8 C14 113.6(2) . . ? C10 C9 C8 119.4(3) . . ? C10 C9 H9 125.3(17) . . ? C8 C9 H9 115.3(18) . . ? C11 C10 C9 121.6(3) . . ? C11 C10 H10 118(2) . . ? C9 C10 H10 120(2) . . ? C10 C11 C12 119.9(3) . . ? C10 C11 H11 118.0(19) . . ? C12 C11 H11 122(2) . . ? C7 C12 C11 119.0(3) . . ? C7 C12 H12 118.2(16) . . ? C11 C12 H12 122.8(17) . . ? C18 C13 C14 120.8(3) . . ? C18 C13 P1 128.1(2) . . ? C14 C13 P1 111.00(18) . . ? C15 C14 C13 119.4(3) . . ? C15 C14 C8 127.7(3) . . ? C13 C14 C8 112.9(2) . . ? C14 C15 C16 119.6(3) . . ? C14 C15 H15 120.0(18) . . ? C16 C15 H15 120.3(18) . . ? C17 C16 C15 120.9(3) . . ? C17 C16 H16 119.9(18) . . ? C15 C16 H16 119.0(18) . . ? C16 C17 C18 120.5(3) . . ? C16 C17 H17 123(2) . . ? C18 C17 H17 117(2) . . ? C13 C18 C17 118.8(3) . . ? C13 C18 H18 117.1(19) . . ? C17 C18 H18 124.1(18) . . ? Cl1 C19 Cl2 110.3(4) . . ? Cl1 C19 H19A 109.6 . . ? Cl2 C19 H19A 109.6 . . ? Cl1 C19 H19B 109.6 . . ? Cl2 C19 H19B 109.6 . . ? H19A C19 H19B 108.1 . . ? _diffrn_measured_fraction_theta_max 0.927 _diffrn_reflns_theta_full 29.37 _diffrn_measured_fraction_theta_full 0.927 _refine_diff_density_max 0.815 _refine_diff_density_min -0.719 _refine_diff_density_rms 0.098 # Attachment '- Compound_4_s051_fin.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2011-12-13 at 18:05:17 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.4 # Request file : c:\xray\wingx\files\archive.reqdat # CIF files read : s051_fin s051_stoe_ipds1 alg_ipds data_s051_fin _database_code_depnum_ccdc_archive 'CCDC 858610' #TrackingRef '- Compound_4_s051_fin.cif' _audit_creation_date 2011-12-13T18:05:17-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C57 H42 Cl6 I3 P3 Pt3 S3' _chemical_formula_weight 2094.67 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.3684(14) _cell_length_b 15.6461(15) _cell_length_c 16.5751(16) _cell_angle_alpha 92.430(12) _cell_angle_beta 110.037(11) _cell_angle_gamma 115.556(11) _cell_volume 3077.6(5) _cell_formula_units_Z 2 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 27.9 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour orange-yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 2.26 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1944 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 1 -1 0.066 0 -1 1 0.052 -1 1 1 0.096 -6 3 2 0.099 -4 0 -1 0.143 2 -5 -6 0.206 -1 0 1 0.057 -1 1 -2 0.125 1 0 -2 0.191 6 -1 0 0.061 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 8.784 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.2433 _exptl_absorpt_correction_T_max 0.408 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS area detector' _diffrn_measurement_method '\f scans' _diffrn_reflns_av_R_equivalents 0.0633 _diffrn_reflns_av_unetI/netI 0.0865 _diffrn_reflns_number 30977 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 28 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.941 _diffrn_measured_fraction_theta_max 0.919 _reflns_number_total 13682 _reflns_number_gt 9589 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'STOE IPDS software' _computing_cell_refinement 'STOE IPDS software' _computing_data_reduction 'STOE IPDS software, STOE X-RED' _computing_structure_solution ; SIR92 A. Altomare, G. Cascarano, C. Giacovazzo and A. Guagliardi, J. Appl. Crystallogr. 1993, 26, 343-350. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP3 for Windows (L. J. Farrugia, 1997)' _computing_publication_material 'WINGX (L.J. Farrugia,1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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^)+(0.0436P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 13682 _refine_ls_number_parameters 676 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0569 _refine_ls_R_factor_gt 0.038 _refine_ls_wR_factor_ref 0.0893 _refine_ls_wR_factor_gt 0.086 _refine_ls_goodness_of_fit_ref 0.881 _refine_ls_restrained_S_all 0.883 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.735 _refine_diff_density_min -2.343 _refine_diff_density_rms 0.201 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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' S S 0.1246 0.1234 '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' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.20215(2) 0.36026(2) 0.758246(18) 0.02034(7) Uani 1 1 d . . . Pt2 Pt 0.19631(2) 0.36044(2) 0.985735(18) 0.02165(7) Uani 1 1 d . . . Pt3 Pt -0.04756(2) 0.22746(2) 0.760977(19) 0.02277(7) Uani 1 1 d . . . I1 I 0.11413(5) 0.29025(4) 0.58861(4) 0.04138(14) Uani 1 1 d . . . I2 I 0.35946(5) 0.34662(6) 1.10584(4) 0.0544(2) Uani 1 1 d . . . I3 I -0.23052(5) 0.24563(6) 0.69636(5) 0.05611(19) Uani 1 1 d . . . S1 S 0.31091(14) 0.42111(14) 0.90463(12) 0.0234(4) Uani 1 1 d . . . S2 S 0.04985(13) 0.37061(13) 0.87995(11) 0.0208(4) Uani 1 1 d . . . S3 S 0.11304(14) 0.21112(14) 0.79886(12) 0.0235(4) Uani 1 1 d . . . P1 P 0.25775(15) 0.51116(14) 0.73978(13) 0.0232(4) Uani 1 1 d . . . P2 P 0.08811(15) 0.30630(15) 1.05996(12) 0.0233(4) Uani 1 1 d . . . P3 P -0.13437(16) 0.09181(16) 0.65760(14) 0.0290(4) Uani 1 1 d . . . C1 C 0.3455(6) 0.5914(6) 0.8486(5) 0.0274(16) Uani 1 1 d . . . C2 C 0.3616(5) 0.5496(6) 0.9215(5) 0.0253(16) Uani 1 1 d . . . C3 C 0.4246(6) 0.6075(7) 1.0045(5) 0.0328(19) Uani 1 1 d . . . H3 H 0.436 0.5788 1.0532 0.039 Uiso 1 1 calc R . . C4 C 0.4707(7) 0.7050(7) 1.0180(6) 0.042(2) Uani 1 1 d . . . H4 H 0.514 0.7431 1.0758 0.051 Uiso 1 1 calc R . . C5 C 0.4551(8) 0.7510(7) 0.9464(7) 0.047(2) Uani 1 1 d . . . H5 H 0.4873 0.8191 0.9562 0.056 Uiso 1 1 calc R . . C6 C 0.3907(7) 0.6929(6) 0.8609(6) 0.038(2) Uani 1 1 d . . . H6 H 0.3777 0.7214 0.8122 0.045 Uiso 1 1 calc R . . C7 C 0.3160(6) 0.5566(6) 0.6605(5) 0.0290(17) Uani 1 1 d . . . C8 C 0.2498(6) 0.5889(6) 0.6007(5) 0.0309(17) Uani 1 1 d . . . C9 C 0.2787(8) 0.6225(7) 0.5308(6) 0.044(2) Uani 1 1 d . . . H9 H 0.2375 0.6472 0.4911 0.052 Uiso 1 1 calc R . . C10 C 0.3693(8) 0.6184(7) 0.5216(6) 0.047(2) Uani 1 1 d . . . H10 H 0.3872 0.6387 0.4738 0.057 Uiso 1 1 calc R . . C11 C 0.4333(8) 0.5859(7) 0.5795(6) 0.048(2) Uani 1 1 d . . . H11 H 0.4949 0.585 0.5721 0.058 Uiso 1 1 calc R . . C12 C 0.4063(6) 0.5541(6) 0.6500(6) 0.037(2) Uani 1 1 d . . . H12 H 0.4493 0.531 0.69 0.044 Uiso 1 1 calc R . . C13 C 0.1451(6) 0.5407(6) 0.6919(5) 0.0300(17) Uani 1 1 d . . . C14 C 0.1549(6) 0.5838(6) 0.6189(5) 0.0304(17) Uani 1 1 d . . . C15 C 0.0746(8) 0.6106(7) 0.5734(6) 0.042(2) Uani 1 1 d . . . H15 H 0.0791 0.639 0.5251 0.05 Uiso 1 1 calc R . . C16 C -0.0113(8) 0.5956(7) 0.5991(6) 0.046(2) Uani 1 1 d . . . H16 H -0.0655 0.6137 0.5675 0.055 Uiso 1 1 calc R . . C17 C -0.0208(8) 0.5540(8) 0.6712(7) 0.047(2) Uani 1 1 d . . . H17 H -0.0801 0.5448 0.6879 0.056 Uiso 1 1 calc R . . C18 C 0.0591(7) 0.5264(6) 0.7177(6) 0.0353(19) Uani 1 1 d . . . H18 H 0.0542 0.4982 0.7661 0.042 Uiso 1 1 calc R . . C19 C -0.0209(6) 0.3422(5) 1.0182(5) 0.0230(15) Uani 1 1 d . . . C20 C -0.0366(6) 0.3698(5) 0.9371(5) 0.0215(15) Uani 1 1 d . . . C21 C -0.1172(6) 0.4008(6) 0.9030(5) 0.0280(17) Uani 1 1 d . . . H21 H -0.128 0.4205 0.8492 0.034 Uiso 1 1 calc R . . C22 C -0.1803(6) 0.4025(6) 0.9485(6) 0.0322(19) Uani 1 1 d . . . H22 H -0.2344 0.4234 0.9252 0.039 Uiso 1 1 calc R . . C23 C -0.1661(7) 0.3736(6) 1.0292(6) 0.0354(19) Uani 1 1 d . . . H23 H -0.2114 0.3736 1.0588 0.042 Uiso 1 1 calc R . . C24 C -0.0851(6) 0.3455(6) 1.0640(5) 0.0306(18) Uani 1 1 d . . . H24 H -0.0729 0.3284 1.1189 0.037 Uiso 1 1 calc R . . C25 C 0.0136(6) 0.1797(7) 1.0584(5) 0.0308(19) Uani 1 1 d . . . C26 C 0.0326(7) 0.1652(7) 1.1457(6) 0.038(2) Uani 1 1 d . . . C27 C -0.0247(9) 0.0713(8) 1.1560(7) 0.053(3) Uani 1 1 d . . . H27 H -0.0138 0.0596 1.2128 0.063 Uiso 1 1 calc R . . C28 C -0.0966(9) -0.0034(8) 1.0840(8) 0.057(3) Uani 1 1 d . . . H28 H -0.1348 -0.0663 1.0921 0.068 Uiso 1 1 calc R . . C29 C -0.1153(8) 0.0107(7) 0.9980(7) 0.049(2) Uani 1 1 d . . . H29 H -0.1651 -0.0419 0.9491 0.059 Uiso 1 1 calc R . . C30 C -0.0595(7) 0.1033(6) 0.9862(6) 0.039(2) Uani 1 1 d . . . H30 H -0.0713 0.1142 0.929 0.047 Uiso 1 1 calc R . . C31 C 0.1491(7) 0.3393(7) 1.1783(5) 0.035(2) Uani 1 1 d . . . C32 C 0.1123(7) 0.2558(7) 1.2135(6) 0.037(2) Uani 1 1 d . . . C33 C 0.1547(8) 0.2654(8) 1.3045(6) 0.047(2) Uani 1 1 d . . . H33 H 0.1298 0.2108 1.3287 0.056 Uiso 1 1 calc R . . C34 C 0.2341(9) 0.3565(10) 1.3592(7) 0.063(3) Uani 1 1 d . . . H34 H 0.2638 0.363 1.4205 0.076 Uiso 1 1 calc R . . C35 C 0.2697(9) 0.4373(9) 1.3244(6) 0.054(3) Uani 1 1 d . . . H35 H 0.3229 0.4987 1.362 0.064 Uiso 1 1 calc R . . C36 C 0.2271(8) 0.4280(8) 1.2344(6) 0.041(2) Uani 1 1 d . . . H36 H 0.2519 0.4834 1.2111 0.049 Uiso 1 1 calc R . . C37 C -0.0307(7) 0.0556(6) 0.6534(5) 0.0308(18) Uani 1 1 d . . . C38 C 0.0773(7) 0.1109(6) 0.7156(5) 0.0294(17) Uani 1 1 d . . . C39 C 0.1614(7) 0.0880(7) 0.7193(6) 0.036(2) Uani 1 1 d . . . H39 H 0.2353 0.126 0.7618 0.044 Uiso 1 1 calc R . . C40 C 0.1348(9) 0.0080(7) 0.6593(7) 0.050(3) Uani 1 1 d . . . H40 H 0.1908 -0.0088 0.6611 0.06 Uiso 1 1 calc R . . C41 C 0.0278(8) -0.0461(7) 0.5977(6) 0.044(2) Uani 1 1 d . . . H41 H 0.0107 -0.1001 0.5573 0.053 Uiso 1 1 calc R . . C42 C -0.0549(8) -0.0234(6) 0.5935(6) 0.038(2) Uani 1 1 d . . . H42 H -0.1282 -0.0611 0.5501 0.046 Uiso 1 1 calc R . . C43 C -0.2298(7) 0.0737(6) 0.5459(5) 0.0353(19) Uani 1 1 d . . . C44 C -0.3383(8) -0.0042(8) 0.5281(6) 0.046(2) Uani 1 1 d . . . C45 C -0.4241(8) -0.0272(9) 0.4448(8) 0.064(3) Uani 1 1 d . . . H45 H -0.4962 -0.0794 0.431 0.077 Uiso 1 1 calc R . . C46 C -0.4043(11) 0.0241(11) 0.3851(7) 0.075(4) Uani 1 1 d . . . H46 H -0.4622 0.0054 0.3288 0.09 Uiso 1 1 calc R . . C47 C -0.3023(10) 0.1035(10) 0.4030(7) 0.063(3) Uani 1 1 d . . . H47 H -0.2931 0.14 0.3601 0.075 Uiso 1 1 calc R . . C48 C -0.2117(8) 0.1309(7) 0.4838(6) 0.042(2) Uani 1 1 d . . . H48 H -0.1415 0.1851 0.4963 0.051 Uiso 1 1 calc R . . C49 C -0.2391(7) -0.0113(6) 0.6757(6) 0.0343(18) Uani 1 1 d . . . C50 C -0.3421(8) -0.0530(7) 0.6019(7) 0.045(2) Uani 1 1 d . . . C51 C -0.4338(8) -0.1321(8) 0.6039(8) 0.059(3) Uani 1 1 d . . . H51 H -0.5031 -0.1602 0.5549 0.07 Uiso 1 1 calc R . . C52 C -0.4232(11) -0.1702(9) 0.6786(9) 0.077(4) Uani 1 1 d . . . H52 H -0.4867 -0.2226 0.6806 0.092 Uiso 1 1 calc R . . C53 C -0.3202(10) -0.1320(8) 0.7506(9) 0.068(3) Uani 1 1 d . . . H53 H -0.3131 -0.1603 0.7997 0.081 Uiso 1 1 calc R . . C54 C -0.2286(8) -0.0522(7) 0.7490(7) 0.045(2) Uani 1 1 d . . . H54 H -0.1589 -0.0253 0.7977 0.054 Uiso 1 1 calc R . . Cl1 Cl 0.6460(5) 0.0062(6) 0.1253(5) 0.206(3) Uani 1 1 d D . . Cl2 Cl 0.8180(4) 0.1959(3) 0.2225(3) 0.1079(13) Uani 1 1 d D . . C55 C 0.7372(13) 0.1171(9) 0.1186(11) 0.148(9) Uani 1 1 d D . . H55A H 0.6949 0.1447 0.0792 0.178 Uiso 1 1 calc R . . H55B H 0.7869 0.1098 0.0937 0.178 Uiso 1 1 calc R . . Cl3 Cl 0.5141(7) 0.6564(6) 0.2588(4) 0.203(3) Uani 1 1 d D . . Cl4 Cl 0.6070(4) 0.7287(5) 0.4457(3) 0.1339(19) Uani 1 1 d D . . C56 C 0.6118(14) 0.7456(15) 0.3473(7) 0.157(9) Uani 1 1 d D . . H56A H 0.6064 0.8049 0.3377 0.188 Uiso 1 1 calc R . . H56B H 0.6859 0.7572 0.3507 0.188 Uiso 1 1 calc R . . Cl5 Cl 0.5830(7) 0.1635(5) 0.8353(7) 0.226(4) Uani 1 1 d D . . Cl6 Cl 0.6181(7) 0.0061(8) 0.8779(6) 0.216(4) Uani 1 1 d D . . C57 C 0.6752(14) 0.1198(15) 0.8651(19) 0.25(2) Uani 1 1 d D . . H57A H 0.7055 0.1221 0.82 0.298 Uiso 1 1 calc R . . H57B H 0.738 0.1617 0.9205 0.298 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 0.02445(13) 0.02176(15) 0.01804(14) 0.00653(12) 0.00914(11) 0.01305(11) Pt2 0.02267(13) 0.02989(17) 0.01741(14) 0.00908(13) 0.00899(11) 0.01564(12) Pt3 0.02548(13) 0.02363(16) 0.01966(15) 0.00340(13) 0.00766(11) 0.01324(12) I1 0.0586(3) 0.0335(3) 0.0223(3) 0.0075(3) 0.0109(2) 0.0175(3) I2 0.0416(3) 0.1096(6) 0.0385(3) 0.0426(4) 0.0215(3) 0.0518(4) I3 0.0404(3) 0.0704(5) 0.0465(4) -0.0176(4) -0.0057(3) 0.0373(3) S1 0.0240(8) 0.0296(10) 0.0198(9) 0.0088(9) 0.0096(7) 0.0146(8) S2 0.0230(8) 0.0257(10) 0.0183(9) 0.0069(8) 0.0087(7) 0.0150(7) S3 0.0288(8) 0.0233(10) 0.0223(9) 0.0067(8) 0.0116(7) 0.0144(8) P1 0.0276(9) 0.0210(10) 0.0226(10) 0.0083(9) 0.0107(8) 0.0121(8) P2 0.0271(9) 0.0301(11) 0.0194(10) 0.0105(9) 0.0119(8) 0.0169(8) P3 0.0322(10) 0.0268(11) 0.0231(11) 0.0013(10) 0.0077(8) 0.0127(9) C1 0.025(3) 0.031(4) 0.025(4) -0.001(4) 0.007(3) 0.014(3) C2 0.014(3) 0.030(4) 0.029(4) 0.001(4) 0.007(3) 0.009(3) C3 0.023(3) 0.045(5) 0.022(4) 0.000(4) 0.004(3) 0.014(4) C4 0.030(4) 0.047(6) 0.032(5) -0.011(5) 0.007(4) 0.008(4) C5 0.051(5) 0.028(5) 0.048(6) -0.005(5) 0.019(5) 0.009(4) C6 0.045(5) 0.031(5) 0.042(5) 0.009(5) 0.020(4) 0.021(4) C7 0.037(4) 0.023(4) 0.031(5) 0.008(4) 0.018(4) 0.014(3) C8 0.038(4) 0.031(5) 0.016(4) 0.002(4) 0.010(3) 0.010(4) C9 0.055(5) 0.030(5) 0.033(5) 0.008(5) 0.018(4) 0.008(4) C10 0.070(6) 0.045(6) 0.030(5) 0.013(5) 0.030(5) 0.021(5) C11 0.049(5) 0.052(7) 0.041(6) 0.004(5) 0.031(5) 0.013(5) C12 0.031(4) 0.034(5) 0.038(5) 0.004(4) 0.013(4) 0.010(4) C13 0.030(4) 0.025(4) 0.030(4) 0.008(4) 0.008(3) 0.013(3) C14 0.039(4) 0.026(4) 0.021(4) 0.004(4) 0.006(3) 0.015(4) C15 0.059(5) 0.033(5) 0.031(5) 0.015(4) 0.008(4) 0.028(4) C16 0.050(5) 0.051(6) 0.044(6) 0.017(5) 0.009(4) 0.036(5) C17 0.048(5) 0.059(7) 0.049(6) 0.017(5) 0.021(5) 0.038(5) C18 0.042(4) 0.041(5) 0.034(5) 0.016(4) 0.016(4) 0.028(4) C19 0.027(3) 0.022(4) 0.023(4) 0.010(3) 0.013(3) 0.013(3) C20 0.028(3) 0.018(4) 0.022(4) 0.003(3) 0.012(3) 0.013(3) C21 0.031(4) 0.026(4) 0.027(4) 0.003(4) 0.004(3) 0.020(3) C22 0.031(4) 0.034(5) 0.042(5) 0.009(4) 0.015(4) 0.024(4) C23 0.037(4) 0.037(5) 0.041(5) 0.003(4) 0.019(4) 0.022(4) C24 0.036(4) 0.035(5) 0.033(5) 0.015(4) 0.024(4) 0.020(4) C25 0.038(4) 0.049(5) 0.024(4) 0.021(4) 0.019(3) 0.031(4) C26 0.044(4) 0.058(6) 0.037(5) 0.028(5) 0.023(4) 0.037(5) C27 0.064(6) 0.056(7) 0.059(7) 0.042(6) 0.034(6) 0.037(6) C28 0.060(6) 0.045(6) 0.080(9) 0.041(7) 0.031(6) 0.032(5) C29 0.063(6) 0.026(5) 0.058(7) 0.012(5) 0.027(5) 0.019(5) C30 0.056(5) 0.031(5) 0.044(6) 0.022(5) 0.027(5) 0.026(4) C31 0.041(4) 0.052(6) 0.023(4) 0.009(4) 0.016(4) 0.030(4) C32 0.044(4) 0.056(6) 0.029(5) 0.023(5) 0.022(4) 0.032(5) C33 0.050(5) 0.069(7) 0.027(5) 0.020(5) 0.016(4) 0.032(5) C34 0.069(7) 0.102(10) 0.026(5) 0.020(7) 0.013(5) 0.051(7) C35 0.062(6) 0.065(8) 0.032(5) -0.006(6) 0.008(5) 0.039(6) C36 0.056(5) 0.054(6) 0.025(5) 0.003(5) 0.016(4) 0.037(5) C37 0.045(4) 0.032(5) 0.024(4) 0.010(4) 0.016(4) 0.024(4) C38 0.051(5) 0.025(4) 0.022(4) 0.009(4) 0.021(4) 0.021(4) C39 0.045(5) 0.042(5) 0.030(5) 0.010(4) 0.017(4) 0.026(4) C40 0.069(6) 0.043(6) 0.065(7) 0.018(6) 0.045(6) 0.035(5) C41 0.068(6) 0.037(6) 0.041(6) 0.011(5) 0.030(5) 0.031(5) C42 0.056(5) 0.028(5) 0.026(5) 0.002(4) 0.019(4) 0.016(4) C43 0.047(5) 0.032(5) 0.020(4) -0.006(4) 0.005(4) 0.021(4) C44 0.049(5) 0.050(6) 0.031(5) -0.008(5) 0.006(4) 0.025(5) C45 0.043(5) 0.063(8) 0.053(7) -0.027(7) -0.004(5) 0.017(5) C46 0.074(8) 0.104(12) 0.029(6) -0.004(7) -0.001(5) 0.046(8) C47 0.076(7) 0.091(10) 0.028(5) 0.004(6) 0.006(5) 0.057(8) C48 0.054(5) 0.051(6) 0.027(5) 0.009(5) 0.012(4) 0.033(5) C49 0.043(4) 0.020(4) 0.035(5) -0.005(4) 0.015(4) 0.013(4) C50 0.046(5) 0.027(5) 0.047(6) -0.008(5) 0.018(4) 0.007(4) C51 0.045(5) 0.040(6) 0.070(8) -0.002(6) 0.024(5) 0.003(5) C52 0.085(9) 0.051(8) 0.069(9) 0.006(7) 0.042(7) 0.003(6) C53 0.093(9) 0.031(6) 0.071(9) 0.006(6) 0.045(7) 0.014(6) C54 0.061(6) 0.024(5) 0.043(6) 0.004(5) 0.022(5) 0.014(4) Cl1 0.119(4) 0.178(7) 0.191(7) 0.019(6) 0.016(4) -0.001(4) Cl2 0.155(4) 0.086(3) 0.103(3) 0.032(3) 0.077(3) 0.055(3) C55 0.170(18) 0.132(18) 0.23(3) 0.110(19) 0.15(2) 0.091(16) Cl3 0.216(7) 0.201(8) 0.090(4) 0.009(5) 0.003(4) 0.061(6) Cl4 0.150(4) 0.203(6) 0.116(4) 0.074(4) 0.096(3) 0.105(4) C56 0.106(13) 0.24(3) 0.101(15) 0.059(17) 0.050(12) 0.055(16) Cl5 0.236(8) 0.118(5) 0.335(12) -0.023(6) 0.200(9) 0.035(5) Cl6 0.198(7) 0.295(11) 0.236(9) 0.059(8) 0.096(7) 0.177(8) C57 0.099(15) 0.46(5) 0.26(3) 0.25(4) 0.097(19) 0.16(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 P1 2.2154(19) . ? Pt1 S1 2.2710(19) . ? Pt1 S3 2.3840(18) . ? Pt1 I1 2.6100(8) . ? Pt2 P2 2.2161(18) . ? Pt2 S2 2.3049(16) . ? Pt2 S1 2.3867(17) . ? Pt2 I2 2.6041(7) . ? Pt3 P3 2.223(2) . ? Pt3 S3 2.3053(16) . ? Pt3 S2 2.428(2) . ? Pt3 I3 2.6230(7) . ? S1 C2 1.789(8) . ? S2 C20 1.798(7) . ? S3 C38 1.806(8) . ? P1 C7 1.804(8) . ? P1 C13 1.807(7) . ? P1 C1 1.817(8) . ? P2 C25 1.793(9) . ? P2 C31 1.796(8) . ? P2 C19 1.817(7) . ? P3 C49 1.793(9) . ? P3 C43 1.808(8) . ? P3 C37 1.828(7) . ? C1 C2 1.396(10) . ? C1 C6 1.407(12) . ? C2 C3 1.366(11) . ? C3 C4 1.347(13) . ? C4 C5 1.416(13) . ? C5 C6 1.400(13) . ? C7 C12 1.383(10) . ? C7 C8 1.397(10) . ? C8 C9 1.410(11) . ? C8 C14 1.465(11) . ? C9 C10 1.389(13) . ? C10 C11 1.365(13) . ? C11 C12 1.399(12) . ? C13 C18 1.374(10) . ? C13 C14 1.430(11) . ? C14 C15 1.387(10) . ? C15 C16 1.370(12) . ? C16 C17 1.405(13) . ? C17 C18 1.396(11) . ? C19 C24 1.395(9) . ? C19 C20 1.403(9) . ? C20 C21 1.400(9) . ? C21 C22 1.370(10) . ? C22 C23 1.407(11) . ? C23 C24 1.372(10) . ? C25 C30 1.377(13) . ? C25 C26 1.425(10) . ? C26 C27 1.392(13) . ? C26 C32 1.472(14) . ? C27 C28 1.362(15) . ? C28 C29 1.403(14) . ? C29 C30 1.382(12) . ? C31 C36 1.371(13) . ? C31 C32 1.418(12) . ? C32 C33 1.392(12) . ? C33 C34 1.390(16) . ? C34 C35 1.378(16) . ? C35 C36 1.378(13) . ? C37 C38 1.375(12) . ? C37 C42 1.386(12) . ? C38 C39 1.385(10) . ? C39 C40 1.387(13) . ? C40 C41 1.360(14) . ? C41 C42 1.361(12) . ? C43 C48 1.410(12) . ? C43 C44 1.421(13) . ? C44 C45 1.402(14) . ? C44 C50 1.473(14) . ? C45 C46 1.330(17) . ? C46 C47 1.371(18) . ? C47 C48 1.396(13) . ? C49 C54 1.391(12) . ? C49 C50 1.403(12) . ? C50 C51 1.377(13) . ? C51 C52 1.385(16) . ? C52 C53 1.393(17) . ? C53 C54 1.378(14) . ? Cl1 C55 1.701(12) . ? Cl2 C55 1.746(14) . ? Cl3 C56 1.672(13) . ? Cl4 C56 1.682(12) . ? Cl5 C57 1.682(12) . ? Cl6 C57 1.665(14) . ? 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 P1 Pt1 S1 88.83(7) . . ? P1 Pt1 S3 162.83(6) . . ? S1 Pt1 S3 85.48(7) . . ? P1 Pt1 I1 91.64(6) . . ? S1 Pt1 I1 168.12(4) . . ? S3 Pt1 I1 97.24(5) . . ? P2 Pt2 S2 87.76(6) . . ? P2 Pt2 S1 178.66(6) . . ? S2 Pt2 S1 91.13(6) . . ? P2 Pt2 I2 91.44(5) . . ? S2 Pt2 I2 179.08(5) . . ? S1 Pt2 I2 89.67(4) . . ? P3 Pt3 S3 87.49(7) . . ? P3 Pt3 S2 176.81(7) . . ? S3 Pt3 S2 90.80(6) . . ? P3 Pt3 I3 88.23(5) . . ? S3 Pt3 I3 172.24(5) . . ? S2 Pt3 I3 93.77(4) . . ? C2 S1 Pt1 105.8(2) . . ? C2 S1 Pt2 107.5(2) . . ? Pt1 S1 Pt2 109.32(7) . . ? C20 S2 Pt2 103.3(2) . . ? C20 S2 Pt3 111.6(3) . . ? Pt2 S2 Pt3 107.62(7) . . ? C38 S3 Pt3 105.1(3) . . ? C38 S3 Pt1 109.3(2) . . ? Pt3 S3 Pt1 89.38(6) . . ? C7 P1 C13 91.9(3) . . ? C7 P1 C1 111.4(4) . . ? C13 P1 C1 106.2(4) . . ? C7 P1 Pt1 124.1(3) . . ? C13 P1 Pt1 114.6(3) . . ? C1 P1 Pt1 107.0(3) . . ? C25 P2 C31 92.4(4) . . ? C25 P2 C19 104.6(3) . . ? C31 P2 C19 109.2(3) . . ? C25 P2 Pt2 122.4(3) . . ? C31 P2 Pt2 120.1(3) . . ? C19 P2 Pt2 106.6(2) . . ? C49 P3 C43 91.9(4) . . ? C49 P3 C37 105.3(4) . . ? C43 P3 C37 108.3(4) . . ? C49 P3 Pt3 115.2(3) . . ? C43 P3 Pt3 124.8(3) . . ? C37 P3 Pt3 109.0(3) . . ? C2 C1 C6 119.9(8) . . ? C2 C1 P1 118.3(6) . . ? C6 C1 P1 121.7(6) . . ? C3 C2 C1 120.0(8) . . ? C3 C2 S1 120.4(6) . . ? C1 C2 S1 119.3(6) . . ? C4 C3 C2 121.3(8) . . ? C3 C4 C5 121.1(9) . . ? C6 C5 C4 118.5(9) . . ? C5 C6 C1 119.2(8) . . ? C12 C7 C8 121.0(7) . . ? C12 C7 P1 128.1(6) . . ? C8 C7 P1 110.6(5) . . ? C7 C8 C9 118.9(7) . . ? C7 C8 C14 114.6(6) . . ? C9 C8 C14 126.5(8) . . ? C10 C9 C8 118.7(8) . . ? C11 C10 C9 122.3(8) . . ? C10 C11 C12 119.4(8) . . ? C7 C12 C11 119.7(8) . . ? C18 C13 C14 121.5(7) . . ? C18 C13 P1 128.1(6) . . ? C14 C13 P1 110.4(5) . . ? C15 C14 C13 118.4(7) . . ? C15 C14 C8 129.0(7) . . ? C13 C14 C8 112.5(6) . . ? C16 C15 C14 119.8(8) . . ? C15 C16 C17 121.9(7) . . ? C18 C17 C16 119.1(8) . . ? C13 C18 C17 119.2(8) . . ? C24 C19 C20 120.4(6) . . ? C24 C19 P2 123.0(5) . . ? C20 C19 P2 116.6(5) . . ? C21 C20 C19 119.0(6) . . ? C21 C20 S2 120.2(5) . . ? C19 C20 S2 120.7(5) . . ? C22 C21 C20 119.6(7) . . ? C21 C22 C23 121.6(6) . . ? C24 C23 C22 119.0(7) . . ? C23 C24 C19 120.3(7) . . ? C30 C25 C26 121.1(8) . . ? C30 C25 P2 128.1(6) . . ? C26 C25 P2 110.7(7) . . ? C27 C26 C25 118.0(10) . . ? C27 C26 C32 129.1(8) . . ? C25 C26 C32 112.9(8) . . ? C28 C27 C26 120.2(9) . . ? C27 C28 C29 121.9(9) . . ? C30 C29 C28 118.9(10) . . ? C25 C30 C29 119.9(9) . . ? C36 C31 C32 119.3(8) . . ? C36 C31 P2 130.0(7) . . ? C32 C31 P2 110.6(7) . . ? C33 C32 C31 119.5(9) . . ? C33 C32 C26 127.1(8) . . ? C31 C32 C26 113.4(7) . . ? C34 C33 C32 119.4(9) . . ? C35 C34 C33 120.7(9) . . ? C34 C35 C36 119.9(11) . . ? C31 C36 C35 121.2(10) . . ? C38 C37 C42 119.4(7) . . ? C38 C37 P3 116.2(6) . . ? C42 C37 P3 124.4(7) . . ? C37 C38 C39 120.7(8) . . ? C37 C38 S3 121.6(6) . . ? C39 C38 S3 117.6(7) . . ? C38 C39 C40 118.8(9) . . ? C41 C40 C39 120.1(8) . . ? C40 C41 C42 121.2(9) . . ? C41 C42 C37 119.8(9) . . ? C48 C43 C44 120.6(8) . . ? C48 C43 P3 128.8(7) . . ? C44 C43 P3 110.3(7) . . ? C45 C44 C43 118.2(10) . . ? C45 C44 C50 128.9(10) . . ? C43 C44 C50 112.9(8) . . ? C46 C45 C44 120.5(11) . . ? C45 C46 C47 122.2(11) . . ? C46 C47 C48 121.1(11) . . ? C47 C48 C43 117.2(10) . . ? C54 C49 C50 120.1(8) . . ? C54 C49 P3 128.8(7) . . ? C50 C49 P3 111.1(7) . . ? C51 C50 C49 119.6(10) . . ? C51 C50 C44 126.7(10) . . ? C49 C50 C44 113.6(8) . . ? C50 C51 C52 119.7(11) . . ? C51 C52 C53 121.1(11) . . ? C54 C53 C52 119.3(11) . . ? C53 C54 C49 120.1(10) . . ? Cl1 C55 Cl2 110.8(9) . . ? Cl3 C56 Cl4 117.5(11) . . ? Cl6 C57 Cl5 113.0(10) . . ? # END of CIF