# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Neil M Boag' _publ_contact_author_email N.M.BOAG@SALFORD.AC.UK _publ_section_title ; Activation of Metal-Bound n5-Pentamethylcyclopentadienyl Groups to Diels-Alder Addition of Dioxygen and Other Dienophiles ; loop_ _publ_author_name 'Neil M Boag' 'K Mohan Rao' # Attachment '2b.cif' data_2b _database_code_depnum_ccdc_archive 'CCDC 706170' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H42 I O2 P Pt' _chemical_formula_sum 'C28 H42 I O2 P Pt' _chemical_formula_weight 763.58 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' 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' I I -0.4742 1.8119 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.954(3) _cell_length_b 11.961(4) _cell_length_c 12.053(5) _cell_angle_alpha 90.00 _cell_angle_beta 93.41(3) _cell_angle_gamma 90.00 _cell_volume 1432.5(8) _cell_formula_units_Z 2 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 15 _cell_measurement_theta_min 2.66 _cell_measurement_theta_max 9.70 _exptl_crystal_description needle _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.770 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 744 _exptl_absorpt_coefficient_mu 6.053 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.667 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ; 5 reflections having 2\q between 11.59 and 17.67 degrees giving 175 \y scans used for parameter estimation ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(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 'Siemens R3m/V' _diffrn_measurement_method 'profile data from \q/2\q scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 4 _diffrn_reflns_number 3645 _diffrn_reflns_av_R_equivalents 0.0480 _diffrn_reflns_av_sigmaI/netI 0.1024 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 27.56 _reflns_number_total 3455 _reflns_number_gt 2440 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SHELXTL Plus Release 3.4 (Nicolet, 1988)' _computing_cell_refinement 'SHELXTL Plus Release 3.4 (Nicolet, 1988)' _computing_data_reduction 'SHELXTL Plus Release 3.4 (Nicolet, 1988)' _computing_structure_solution 'SHELXTL Plus Release 3.4 (Nicolet, 1988)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL Version 5.03 (Siemens, 1994)' _computing_publication_material SHELXL-97 _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. Atoms C5, C2 and C41 restrained from going non-positive definite by means of the SHELXL constraint ISOR The collected data was weak, mean (1/sigma) = 6.48, resulting in a poorly determined structure with large peaks and holes of electron density within 1 \%A of the platinum atom and large errors in the C-C distances. ; _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^)+(0.0665P)^2^+0.4385P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.017(17) _refine_ls_number_reflns 3455 _refine_ls_number_parameters 291 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.0963 _refine_ls_R_factor_gt 0.0634 _refine_ls_wR_factor_ref 0.1419 _refine_ls_wR_factor_gt 0.1260 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.037 _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 Pt Pt 0.21661(8) -0.00036(6) 0.77316(6) 0.0335(2) Uani 1 1 d . . . I I 0.24083(19) -0.15665(12) 0.61495(13) 0.0553(5) Uani 1 1 d . . . C2 C 0.227(3) 0.0696(18) 0.9318(17) 0.044(6) Uani 1 1 d U . . C21 C 0.184(2) 0.1850(18) 0.9643(18) 0.042(5) Uani 1 1 d . . . H21A H 0.1780 0.1887 1.0442 0.062 Uiso 1 1 calc R . . H21B H 0.0962 0.2017 0.9281 0.062 Uiso 1 1 calc R . . H21C H 0.2489 0.2392 0.9413 0.062 Uiso 1 1 calc R . . C3 C 0.362(2) 0.0317(18) 0.9631(18) 0.049(6) Uani 1 1 d . . . C31 C 0.487(3) 0.092(2) 0.951(2) 0.069(8) Uani 1 1 d . . . H31A H 0.5045 0.0977 0.8733 0.103 Uiso 1 1 calc R . . H31B H 0.5605 0.0521 0.9905 0.103 Uiso 1 1 calc R . . H31C H 0.4799 0.1663 0.9826 0.103 Uiso 1 1 calc R . . C4 C 0.350(3) -0.0840(16) 0.9059(17) 0.042(5) Uani 1 1 d . . . C41 C 0.471(3) -0.146(2) 0.873(2) 0.067(8) Uani 1 1 d U . . H41A H 0.5302 -0.1607 0.9380 0.100 Uiso 1 1 calc R . . H41B H 0.5180 -0.1023 0.8199 0.100 Uiso 1 1 calc R . . H41C H 0.4432 -0.2169 0.8388 0.100 Uiso 1 1 calc R . . C5 C 0.215(2) -0.1149(16) 0.9196(17) 0.029(5) Uani 1 1 d U . . C51 C 0.168(3) -0.2364(17) 0.907(2) 0.053(7) Uani 1 1 d . . . H51A H 0.1481 -0.2532 0.8295 0.080 Uiso 1 1 calc R . . H51B H 0.0881 -0.2471 0.9481 0.080 Uiso 1 1 calc R . . H51C H 0.2389 -0.2859 0.9370 0.080 Uiso 1 1 calc R . . C6 C 0.156(2) -0.0269(16) 0.9847(18) 0.044(6) Uani 1 1 d . . . C61 C 0.005(3) -0.0298(17) 0.995(2) 0.067(8) Uani 1 1 d . . . H61A H -0.0402 -0.0195 0.9222 0.101 Uiso 1 1 calc R . . H61B H -0.0206 0.0296 1.0442 0.101 Uiso 1 1 calc R . . H61C H -0.0202 -0.1014 1.0251 0.101 Uiso 1 1 calc R . . O1 O 0.3585(17) 0.007(3) 1.0860(11) 0.073(5) Uani 1 1 d . . . O2 O 0.216(2) -0.0341(14) 1.0986(12) 0.065(6) Uani 1 1 d . . . P P 0.1412(5) 0.1394(4) 0.6560(4) 0.0319(11) Uani 1 1 d . . . C71 C 0.2023(12) 0.2807(8) 0.6950(10) 0.030(4) Uani 1 1 d G . . C72 C 0.1225(10) 0.3755(10) 0.6806(11) 0.042(5) Uani 1 1 d G . . H72 H 0.0326 0.3689 0.6529 0.051 Uiso 1 1 calc R . . C73 C 0.1757(13) 0.4803(8) 0.7072(11) 0.047(6) Uani 1 1 d G . . H73 H 0.1217 0.5444 0.6975 0.056 Uiso 1 1 calc R . . C74 C 0.3087(14) 0.4901(8) 0.7481(11) 0.056(6) Uani 1 1 d G . . H74 H 0.3447 0.5610 0.7661 0.067 Uiso 1 1 calc R . . C75 C 0.3885(10) 0.3953(11) 0.7625(11) 0.044(6) Uani 1 1 d G . . H75 H 0.4784 0.4019 0.7902 0.053 Uiso 1 1 calc R . . C76 C 0.3353(12) 0.2905(9) 0.7359(11) 0.051(6) Uani 1 1 d G . . H76 H 0.3892 0.2264 0.7456 0.061 Uiso 1 1 calc R . . C81 C -0.0411(18) 0.1465(17) 0.6429(15) 0.032(4) Uani 1 1 d . . . H81 H -0.0664 0.2060 0.5884 0.038 Uiso 1 1 calc R . . C82 C -0.1027(19) 0.1770(19) 0.7535(15) 0.038(5) Uani 1 1 d . . . H82A H -0.0683 0.2499 0.7791 0.045 Uiso 1 1 calc R . . H82B H -0.0757 0.1212 0.8100 0.045 Uiso 1 1 calc R . . C83 C -0.260(2) 0.181(2) 0.7388(19) 0.057(7) Uani 1 1 d . . . H83A H -0.2969 0.1969 0.8107 0.068 Uiso 1 1 calc R . . H83B H -0.2870 0.2424 0.6878 0.068 Uiso 1 1 calc R . . C84 C -0.316(2) 0.073(2) 0.694(2) 0.065(8) Uani 1 1 d . . . H84A H -0.4141 0.0788 0.6828 0.078 Uiso 1 1 calc R . . H84B H -0.2952 0.0130 0.7473 0.078 Uiso 1 1 calc R . . C85 C -0.2567(18) 0.0436(18) 0.5824(18) 0.043(5) Uani 1 1 d . . . H85A H -0.2823 0.1011 0.5271 0.052 Uiso 1 1 calc R . . H85B H -0.2934 -0.0281 0.5553 0.052 Uiso 1 1 calc R . . C86 C -0.099(2) 0.0358(19) 0.597(2) 0.056(7) Uani 1 1 d . . . H86A H -0.0733 -0.0253 0.6480 0.067 Uiso 1 1 calc R . . H86B H -0.0623 0.0197 0.5249 0.067 Uiso 1 1 calc R . . C91 C 0.1936(19) 0.1248(19) 0.5092(16) 0.038(5) Uani 1 1 d . . . H91 H 0.1620 0.0511 0.4808 0.046 Uiso 1 1 calc R . . C92 C 0.346(2) 0.128(2) 0.5050(16) 0.044(6) Uani 1 1 d . . . H92A H 0.3791 0.2015 0.5292 0.053 Uiso 1 1 calc R . . H92B H 0.3859 0.0716 0.5558 0.053 Uiso 1 1 calc R . . C93 C 0.386(2) 0.105(3) 0.3888(19) 0.062(7) Uani 1 1 d . . . H93A H 0.3518 0.0317 0.3641 0.074 Uiso 1 1 calc R . . H93B H 0.4840 0.1045 0.3872 0.074 Uiso 1 1 calc R . . C94 C 0.327(3) 0.195(3) 0.312(2) 0.070(8) Uani 1 1 d . . . H94A H 0.3536 0.1816 0.2363 0.084 Uiso 1 1 calc R . . H94B H 0.3634 0.2683 0.3361 0.084 Uiso 1 1 calc R . . C95 C 0.173(3) 0.197(2) 0.3137(19) 0.063(7) Uani 1 1 d . . . H95A H 0.1367 0.1257 0.2846 0.076 Uiso 1 1 calc R . . H95B H 0.1368 0.2570 0.2656 0.076 Uiso 1 1 calc R . . C96 C 0.129(2) 0.215(2) 0.4332(15) 0.051(6) Uani 1 1 d . . . H96A H 0.1576 0.2890 0.4598 0.061 Uiso 1 1 calc R . . H96B H 0.0310 0.2104 0.4340 0.061 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 Pt 0.0401(4) 0.0258(3) 0.0345(3) -0.0011(5) 0.0020(3) 0.0036(6) I 0.0743(12) 0.0363(8) 0.0548(9) -0.0138(7) 0.0003(8) 0.0055(9) C2 0.063(15) 0.029(11) 0.039(11) 0.004(9) 0.001(10) 0.029(11) C21 0.044(13) 0.034(11) 0.048(12) -0.011(10) 0.005(10) 0.010(10) C3 0.048(13) 0.049(16) 0.047(12) -0.015(10) -0.017(10) -0.003(11) C31 0.056(17) 0.059(16) 0.09(2) -0.016(15) -0.017(15) 0.024(14) C4 0.066(17) 0.025(10) 0.035(11) 0.006(9) 0.003(11) 0.003(11) C41 0.065(15) 0.045(12) 0.091(17) -0.009(13) 0.008(13) 0.045(13) C5 0.032(10) 0.021(8) 0.034(9) 0.018(8) -0.010(8) -0.015(8) C51 0.064(16) 0.024(10) 0.076(17) 0.006(11) 0.038(14) -0.004(11) C6 0.057(14) 0.038(13) 0.037(11) 0.000(8) 0.010(11) 0.010(10) C61 0.088(18) 0.030(12) 0.090(17) 0.026(11) 0.058(15) 0.025(11) O1 0.082(11) 0.099(13) 0.036(7) -0.011(15) -0.013(7) 0.019(19) O2 0.104(16) 0.062(12) 0.028(8) 0.009(7) 0.008(9) 0.002(10) P 0.032(3) 0.031(3) 0.032(3) 0.001(2) 0.000(2) -0.004(2) C71 0.034(11) 0.029(9) 0.026(9) -0.006(7) 0.003(8) -0.011(9) C72 0.031(12) 0.037(11) 0.061(14) -0.011(10) 0.016(10) -0.009(10) C73 0.073(16) 0.033(15) 0.035(10) 0.011(8) 0.009(11) 0.007(10) C74 0.066(16) 0.061(15) 0.043(12) -0.013(13) 0.014(10) -0.014(17) C75 0.035(12) 0.030(10) 0.068(15) -0.027(10) 0.004(11) -0.012(10) C76 0.062(15) 0.063(15) 0.028(11) -0.005(10) -0.008(11) -0.009(13) C81 0.025(10) 0.038(10) 0.032(9) 0.005(8) -0.003(8) -0.012(9) C82 0.030(11) 0.046(11) 0.038(11) -0.018(9) 0.008(9) 0.000(10) C83 0.061(17) 0.059(15) 0.050(14) -0.006(12) -0.002(12) 0.024(13) C84 0.032(12) 0.09(2) 0.077(19) 0.020(16) 0.012(12) -0.002(13) C85 0.017(9) 0.036(10) 0.077(15) -0.008(10) 0.011(10) -0.012(8) C86 0.048(13) 0.058(16) 0.063(14) -0.013(11) 0.009(11) -0.002(11) C91 0.024(10) 0.051(13) 0.039(11) -0.008(10) -0.008(9) -0.003(10) C92 0.034(12) 0.065(15) 0.033(11) 0.007(10) -0.002(9) -0.009(12) C93 0.037(13) 0.10(2) 0.050(14) -0.024(15) 0.004(11) -0.005(14) C94 0.066(19) 0.09(2) 0.060(17) -0.008(15) 0.029(14) -0.015(17) C95 0.08(2) 0.061(16) 0.045(13) -0.005(12) -0.018(13) 0.000(15) C96 0.062(16) 0.064(15) 0.025(10) 0.008(10) -0.008(10) 0.003(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt C2 2.08(2) . ? Pt C5 2.234(18) . ? Pt C4 2.25(2) . ? Pt P 2.286(5) . ? Pt I 2.6913(17) . ? C2 C3 1.45(3) . ? C2 C21 1.50(3) . ? C2 C6 1.51(3) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C3 C31 1.45(4) . ? C3 O1 1.51(3) . ? C3 C4 1.55(3) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C31 H31C 0.9700 . ? C4 C5 1.41(3) . ? C4 C41 1.49(3) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C41 H41C 0.9700 . ? C5 C6 1.46(3) . ? C5 C51 1.53(3) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C51 H51C 0.9700 . ? C6 O2 1.47(2) . ? C6 C61 1.51(3) . ? C61 H61A 0.9700 . ? C61 H61B 0.9700 . ? C61 H61C 0.9700 . ? O1 O2 1.52(3) . ? P C81 1.814(19) . ? P C71 1.847(10) . ? P C91 1.88(2) . ? C71 C72 1.3900 . ? C71 C76 1.3900 . ? C72 C73 1.3900 . ? C72 H72 0.9400 . ? C73 C74 1.3900 . ? C73 H73 0.9400 . ? C74 C75 1.3900 . ? C74 H74 0.9400 . ? C75 C76 1.3900 . ? C75 H75 0.9400 . ? C76 H76 0.9400 . ? C81 C86 1.54(3) . ? C81 C82 1.54(3) . ? C81 H81 0.9900 . ? C82 C83 1.56(3) . ? C82 H82A 0.9800 . ? C82 H82B 0.9800 . ? C83 C84 1.50(4) . ? C83 H83A 0.9800 . ? C83 H83B 0.9800 . ? C84 C85 1.54(3) . ? C84 H84A 0.9800 . ? C84 H84B 0.9800 . ? C85 C86 1.57(3) . ? C85 H85A 0.9800 . ? C85 H85B 0.9800 . ? C86 H86A 0.9800 . ? C86 H86B 0.9800 . ? C91 C92 1.52(3) . ? C91 C96 1.53(3) . ? C91 H91 0.9900 . ? C92 C93 1.50(3) . ? C92 H92A 0.9800 . ? C92 H92B 0.9800 . ? C93 C94 1.51(4) . ? C93 H93A 0.9800 . ? C93 H93B 0.9800 . ? C94 C95 1.54(4) . ? C94 H94A 0.9800 . ? C94 H94B 0.9800 . ? C95 C96 1.55(3) . ? C95 H95A 0.9800 . ? C95 H95B 0.9800 . ? C96 H96A 0.9800 . ? C96 H96B 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 C2 Pt C5 61.5(9) . . ? C2 Pt C4 62.1(8) . . ? C5 Pt C4 36.5(8) . . ? C2 Pt P 105.6(5) . . ? C5 Pt P 156.8(6) . . ? C4 Pt P 157.2(6) . . ? C2 Pt I 158.0(5) . . ? C5 Pt I 98.0(6) . . ? C4 Pt I 97.0(5) . . ? P Pt I 96.33(14) . . ? C3 C2 C21 120(2) . . ? C3 C2 C6 95.8(17) . . ? C21 C2 C6 116.4(19) . . ? C3 C2 Pt 96.1(14) . . ? C21 C2 Pt 127.4(15) . . ? C6 C2 Pt 94.7(14) . . ? C2 C21 H21A 109.5 . . ? C2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C31 C3 C2 127(2) . . ? C31 C3 O1 105.3(18) . . ? C2 C3 O1 103.9(19) . . ? C31 C3 C4 117(2) . . ? C2 C3 C4 96.6(17) . . ? O1 C3 C4 104.7(18) . . ? C3 C31 H31A 109.5 . . ? C3 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C3 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C5 C4 C41 134(2) . . ? C5 C4 C3 103.5(19) . . ? C41 C4 C3 121(2) . . ? C5 C4 Pt 71.1(12) . . ? C41 C4 Pt 118.9(15) . . ? C3 C4 Pt 87.0(12) . . ? C4 C41 H41A 109.5 . . ? C4 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C4 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C4 C5 C6 107.0(18) . . ? C4 C5 C51 122(2) . . ? C6 C5 C51 127(2) . . ? C4 C5 Pt 72.4(11) . . ? C6 C5 Pt 90.2(12) . . ? C51 C5 Pt 121.5(16) . . ? C5 C51 H51A 109.5 . . ? C5 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C5 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C5 C6 O2 107.9(17) . . ? C5 C6 C2 96.3(17) . . ? O2 C6 C2 105.5(17) . . ? C5 C6 C61 118(2) . . ? O2 C6 C61 106(2) . . ? C2 C6 C61 122.7(18) . . ? C6 C61 H61A 109.5 . . ? C6 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C6 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C3 O1 O2 103.8(13) . . ? C6 O2 O1 102.5(15) . . ? C81 P C71 107.0(8) . . ? C81 P C91 104.7(8) . . ? C71 P C91 102.6(8) . . ? C81 P Pt 112.2(6) . . ? C71 P Pt 114.9(4) . . ? C91 P Pt 114.4(7) . . ? C72 C71 C76 120.0 . . ? C72 C71 P 122.5(7) . . ? C76 C71 P 117.4(7) . . ? C73 C72 C71 120.0 . . ? C73 C72 H72 120.0 . . ? C71 C72 H72 120.0 . . ? C74 C73 C72 120.0 . . ? C74 C73 H73 120.0 . . ? C72 C73 H73 120.0 . . ? C75 C74 C73 120.0 . . ? C75 C74 H74 120.0 . . ? C73 C74 H74 120.0 . . ? C74 C75 C76 120.0 . . ? C74 C75 H75 120.0 . . ? C76 C75 H75 120.0 . . ? C75 C76 C71 120.0 . . ? C75 C76 H76 120.0 . . ? C71 C76 H76 120.0 . . ? C86 C81 C82 110.8(17) . . ? C86 C81 P 110.1(15) . . ? C82 C81 P 112.5(12) . . ? C86 C81 H81 107.7 . . ? C82 C81 H81 107.7 . . ? P C81 H81 107.7 . . ? C81 C82 C83 110.9(16) . . ? C81 C82 H82A 109.5 . . ? C83 C82 H82A 109.5 . . ? C81 C82 H82B 109.5 . . ? C83 C82 H82B 109.5 . . ? H82A C82 H82B 108.1 . . ? C84 C83 C82 111.1(19) . . ? C84 C83 H83A 109.4 . . ? C82 C83 H83A 109.4 . . ? C84 C83 H83B 109.4 . . ? C82 C83 H83B 109.4 . . ? H83A C83 H83B 108.0 . . ? C83 C84 C85 111(2) . . ? C83 C84 H84A 109.4 . . ? C85 C84 H84A 109.4 . . ? C83 C84 H84B 109.4 . . ? C85 C84 H84B 109.4 . . ? H84A C84 H84B 108.0 . . ? C84 C85 C86 110.5(19) . . ? C84 C85 H85A 109.6 . . ? C86 C85 H85A 109.6 . . ? C84 C85 H85B 109.6 . . ? C86 C85 H85B 109.6 . . ? H85A C85 H85B 108.1 . . ? C81 C86 C85 109.9(18) . . ? C81 C86 H86A 109.7 . . ? C85 C86 H86A 109.7 . . ? C81 C86 H86B 109.7 . . ? C85 C86 H86B 109.7 . . ? H86A C86 H86B 108.2 . . ? C92 C91 C96 110.3(19) . . ? C92 C91 P 111.2(13) . . ? C96 C91 P 111.6(15) . . ? C92 C91 H91 107.9 . . ? C96 C91 H91 107.9 . . ? P C91 H91 107.9 . . ? C93 C92 C91 110.3(17) . . ? C93 C92 H92A 109.6 . . ? C91 C92 H92A 109.6 . . ? C93 C92 H92B 109.6 . . ? C91 C92 H92B 109.6 . . ? H92A C92 H92B 108.1 . . ? C92 C93 C94 109(2) . . ? C92 C93 H93A 109.9 . . ? C94 C93 H93A 109.9 . . ? C92 C93 H93B 109.9 . . ? C94 C93 H93B 109.9 . . ? H93A C93 H93B 108.3 . . ? C93 C94 C95 110(2) . . ? C93 C94 H94A 109.6 . . ? C95 C94 H94A 109.6 . . ? C93 C94 H94B 109.6 . . ? C95 C94 H94B 109.6 . . ? H94A C94 H94B 108.1 . . ? C94 C95 C96 110.5(19) . . ? C94 C95 H95A 109.5 . . ? C96 C95 H95A 109.5 . . ? C94 C95 H95B 109.5 . . ? C96 C95 H95B 109.5 . . ? H95A C95 H95B 108.1 . . ? C91 C96 C95 109(2) . . ? C91 C96 H96A 109.8 . . ? C95 C96 H96A 109.8 . . ? C91 C96 H96B 109.8 . . ? C95 C96 H96B 109.8 . . ? H96A C96 H96B 108.3 . . ? 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 C5 Pt C2 C3 70.1(14) . . . . ? C4 Pt C2 C3 28.4(14) . . . . ? P Pt C2 C3 -130.8(13) . . . . ? I Pt C2 C3 47(3) . . . . ? C5 Pt C2 C21 -155(3) . . . . ? C4 Pt C2 C21 163(3) . . . . ? P Pt C2 C21 4(2) . . . . ? I Pt C2 C21 -177.7(11) . . . . ? C5 Pt C2 C6 -26.2(12) . . . . ? C4 Pt C2 C6 -67.9(14) . . . . ? P Pt C2 C6 132.9(12) . . . . ? I Pt C2 C6 -49(3) . . . . ? C21 C2 C3 C31 -47(3) . . . . ? C6 C2 C3 C31 -172(2) . . . . ? Pt C2 C3 C31 93(2) . . . . ? C21 C2 C3 O1 75(3) . . . . ? C6 C2 C3 O1 -50(2) . . . . ? Pt C2 C3 O1 -145.0(16) . . . . ? C21 C2 C3 C4 -178(2) . . . . ? C6 C2 C3 C4 57.4(18) . . . . ? Pt C2 C3 C4 -38.0(16) . . . . ? C31 C3 C4 C5 -173.0(19) . . . . ? C2 C3 C4 C5 -35(2) . . . . ? O1 C3 C4 C5 71.1(19) . . . . ? C31 C3 C4 C41 19(3) . . . . ? C2 C3 C4 C41 157(2) . . . . ? O1 C3 C4 C41 -97(2) . . . . ? C31 C3 C4 Pt -103.3(19) . . . . ? C2 C3 C4 Pt 34.6(16) . . . . ? O1 C3 C4 Pt 140.9(14) . . . . ? C2 Pt C4 C5 79.0(15) . . . . ? P Pt C4 C5 140.7(14) . . . . ? I Pt C4 C5 -94.0(12) . . . . ? C2 Pt C4 C41 -151(2) . . . . ? C5 Pt C4 C41 130(2) . . . . ? P Pt C4 C41 -89(2) . . . . ? I Pt C4 C41 36.0(19) . . . . ? C2 Pt C4 C3 -26.4(14) . . . . ? C5 Pt C4 C3 -105.4(19) . . . . ? P Pt C4 C3 35(2) . . . . ? I Pt C4 C3 160.6(13) . . . . ? C41 C4 C5 C6 163(2) . . . . ? C3 C4 C5 C6 -3(2) . . . . ? Pt C4 C5 C6 -84.7(14) . . . . ? C41 C4 C5 C51 4(4) . . . . ? C3 C4 C5 C51 -161(2) . . . . ? Pt C4 C5 C51 117(2) . . . . ? C41 C4 C5 Pt -112(3) . . . . ? C3 C4 C5 Pt 82.0(13) . . . . ? C2 Pt C5 C4 -80.7(13) . . . . ? P Pt C5 C4 -141.5(12) . . . . ? I Pt C5 C4 90.9(12) . . . . ? C2 Pt C5 C6 27.1(13) . . . . ? C4 Pt C5 C6 107.8(18) . . . . ? P Pt C5 C6 -34(2) . . . . ? I Pt C5 C6 -161.3(12) . . . . ? C2 Pt C5 C51 162(2) . . . . ? C4 Pt C5 C51 -117(2) . . . . ? P Pt C5 C51 102(2) . . . . ? I Pt C5 C51 -25.9(18) . . . . ? C4 C5 C6 O2 -71(2) . . . . ? C51 C5 C6 O2 86(3) . . . . ? Pt C5 C6 O2 -142.4(15) . . . . ? C4 C5 C6 C2 37.8(19) . . . . ? C51 C5 C6 C2 -165(2) . . . . ? Pt C5 C6 C2 -33.8(14) . . . . ? C4 C5 C6 C61 170.0(19) . . . . ? C51 C5 C6 C61 -33(3) . . . . ? Pt C5 C6 C61 98.4(18) . . . . ? C3 C2 C6 C5 -59.9(18) . . . . ? C21 C2 C6 C5 173.0(19) . . . . ? Pt C2 C6 C5 36.8(15) . . . . ? C3 C2 C6 O2 50.7(19) . . . . ? C21 C2 C6 O2 -76(2) . . . . ? Pt C2 C6 O2 147.3(14) . . . . ? C3 C2 C6 C61 171(2) . . . . ? C21 C2 C6 C61 44(3) . . . . ? Pt C2 C6 C61 -92(2) . . . . ? C31 C3 O1 O2 168.7(19) . . . . ? C2 C3 O1 O2 33(2) . . . . ? C4 C3 O1 O2 -68(2) . . . . ? C5 C6 O2 O1 71(2) . . . . ? C2 C6 O2 O1 -31(2) . . . . ? C61 C6 O2 O1 -162.3(17) . . . . ? C3 O1 O2 C6 0(2) . . . . ? C2 Pt P C81 -86.9(10) . . . . ? C5 Pt P C81 -34.1(15) . . . . ? C4 Pt P C81 -140.9(16) . . . . ? I Pt P C81 93.8(7) . . . . ? C2 Pt P C71 35.6(9) . . . . ? C5 Pt P C71 88.4(14) . . . . ? C4 Pt P C71 -18.4(17) . . . . ? I Pt P C71 -143.8(5) . . . . ? C2 Pt P C91 153.9(10) . . . . ? C5 Pt P C91 -153.2(15) . . . . ? C4 Pt P C91 100.0(17) . . . . ? I Pt P C91 -25.4(7) . . . . ? C81 P C71 C72 -17.9(11) . . . . ? C91 P C71 C72 92.0(10) . . . . ? Pt P C71 C72 -143.1(7) . . . . ? C81 P C71 C76 164.7(9) . . . . ? C91 P C71 C76 -85.4(9) . . . . ? Pt P C71 C76 39.5(8) . . . . ? C76 C71 C72 C73 0.0 . . . . ? P C71 C72 C73 -177.3(11) . . . . ? C71 C72 C73 C74 0.0 . . . . ? C72 C73 C74 C75 0.0 . . . . ? C73 C74 C75 C76 0.0 . . . . ? C74 C75 C76 C71 0.0 . . . . ? C72 C71 C76 C75 0.0 . . . . ? P C71 C76 C75 177.5(10) . . . . ? C71 P C81 C86 173.2(14) . . . . ? C91 P C81 C86 64.7(16) . . . . ? Pt P C81 C86 -60.0(15) . . . . ? C71 P C81 C82 -62.7(16) . . . . ? C91 P C81 C82 -171.1(15) . . . . ? Pt P C81 C82 64.2(16) . . . . ? C86 C81 C82 C83 -56(2) . . . . ? P C81 C82 C83 -179.6(16) . . . . ? C81 C82 C83 C84 56(3) . . . . ? C82 C83 C84 C85 -57(3) . . . . ? C83 C84 C85 C86 58(3) . . . . ? C82 C81 C86 C85 57(2) . . . . ? P C81 C86 C85 -178.3(15) . . . . ? C84 C85 C86 C81 -57(2) . . . . ? C81 P C91 C92 175.0(16) . . . . ? C71 P C91 C92 63.4(17) . . . . ? Pt P C91 C92 -61.7(17) . . . . ? C81 P C91 C96 51.5(17) . . . . ? C71 P C91 C96 -60.1(15) . . . . ? Pt P C91 C96 174.7(13) . . . . ? C96 C91 C92 C93 -61(3) . . . . ? P C91 C92 C93 174.6(18) . . . . ? C91 C92 C93 C94 62(3) . . . . ? C92 C93 C94 C95 -60(3) . . . . ? C93 C94 C95 C96 57(3) . . . . ? C92 C91 C96 C95 57(2) . . . . ? P C91 C96 C95 -178.6(16) . . . . ? C94 C95 C96 C91 -56(3) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 3.041 _refine_diff_density_min -1.902 _refine_diff_density_rms 0.235 # Attachment '3c.cif' data_3c _database_code_depnum_ccdc_archive 'CCDC 706171' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H38 I O P Pt' _chemical_formula_sum 'C33 H38 I O P Pt' _chemical_formula_weight 803.59 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' 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' I I -0.4742 1.8119 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.490(3) _cell_length_b 15.263(4) _cell_length_c 21.282(7) _cell_angle_alpha 90.00 _cell_angle_beta 92.55(2) _cell_angle_gamma 90.00 _cell_volume 3079.5(15) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 15 _cell_measurement_theta_min 4.67 _cell_measurement_theta_max 9.84 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.733 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1560 _exptl_absorpt_coefficient_mu 5.634 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.512 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ; 80 reflections having 2\q between 11.59 and 17.67 degrees giving 284 \y scans used for parameter estimation ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Siemens R3m/V' _diffrn_measurement_method 'profile data from \q/2\q scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 7499 _diffrn_reflns_av_R_equivalents 0.0314 _diffrn_reflns_av_sigmaI/netI 0.0515 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 27.55 _reflns_number_total 7094 _reflns_number_gt 4258 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SHELXTL Plus Release 3.4 (Nicolet, 1988)' _computing_cell_refinement 'SHELXTL Plus Release 3.4 (Nicolet, 1988)' _computing_data_reduction 'SHELXTL Plus Release 3.4 (Nicolet, 1988)' _computing_structure_solution 'SHELXTL Plus Release 3.4 (Nicolet, 1988)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL Version 5.03 (Siemens, 1994)' _computing_publication_material SHELXL-97 _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^)+(0.0417P)^2^+8.6595P] 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 SHELXL _refine_ls_extinction_coef 0.00045(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7094 _refine_ls_number_parameters 341 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0886 _refine_ls_R_factor_gt 0.0488 _refine_ls_wR_factor_ref 0.1146 _refine_ls_wR_factor_gt 0.1002 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _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 Pt Pt 0.46836(3) 0.25083(2) 0.008879(13) 0.04249(10) Uani 1 1 d . . . I I 0.74067(6) 0.20477(5) -0.00161(3) 0.0725(2) Uani 1 1 d . . . P P 0.4853(2) 0.30197(16) 0.10870(9) 0.0469(5) Uani 1 1 d . . . C2 C 0.2505(8) 0.2615(5) -0.0129(3) 0.0458(19) Uani 1 1 d . . . C3 C 0.2325(8) 0.1637(6) -0.0319(3) 0.048(2) Uani 1 1 d . . . C4 C 0.3735(8) 0.1568(6) -0.0636(4) 0.0475(19) Uani 1 1 d . . . C5 C 0.3923(8) 0.2364(6) -0.0938(4) 0.051(2) Uani 1 1 d . . . C6 C 0.2655(9) 0.2946(6) -0.0803(4) 0.055(2) Uani 1 1 d . . . C21 C 0.1418(8) 0.2993(6) 0.0287(4) 0.065(3) Uani 1 1 d . . . H21A H 0.1705 0.3569 0.0421 0.098 Uiso 1 1 calc R . . H21B H 0.1330 0.2624 0.0648 0.098 Uiso 1 1 calc R . . H21C H 0.0526 0.3027 0.0057 0.098 Uiso 1 1 calc R . . C31 C 0.2086(10) 0.0995(7) 0.0207(4) 0.075(3) Uani 1 1 d . . . H31A H 0.2300 0.0413 0.0070 0.112 Uiso 1 1 calc R . . H31B H 0.1119 0.1023 0.0320 0.112 Uiso 1 1 calc R . . H31C H 0.2688 0.1143 0.0566 0.112 Uiso 1 1 calc R . . C41 C 0.4487(10) 0.0734(6) -0.0747(5) 0.074(3) Uani 1 1 d . . . H41A H 0.4037 0.0434 -0.1098 0.111 Uiso 1 1 calc R . . H41B H 0.4461 0.0373 -0.0379 0.111 Uiso 1 1 calc R . . H41C H 0.5450 0.0857 -0.0837 0.111 Uiso 1 1 calc R . . C51 C 0.4868(9) 0.2542(7) -0.1469(4) 0.073(3) Uani 1 1 d . . . H51A H 0.5717 0.2203 -0.1412 0.109 Uiso 1 1 calc R . . H51B H 0.5101 0.3154 -0.1476 0.109 Uiso 1 1 calc R . . H51C H 0.4392 0.2383 -0.1860 0.109 Uiso 1 1 calc R . . C61 C 0.2811(11) 0.3918(6) -0.0912(5) 0.080(3) Uani 1 1 d . . . H61A H 0.2037 0.4223 -0.0736 0.120 Uiso 1 1 calc R . . H61B H 0.2814 0.4032 -0.1356 0.120 Uiso 1 1 calc R . . H61C H 0.3681 0.4118 -0.0715 0.120 Uiso 1 1 calc R . . C32 C 0.1123(8) 0.1652(6) -0.0855(4) 0.057(2) Uani 1 1 d . . . H32 H 0.0199 0.1637 -0.0667 0.068 Uiso 1 1 calc R . . C33 C 0.1240(9) 0.0903(7) -0.1310(4) 0.063(3) Uani 1 1 d . . . O31 O 0.1898(7) 0.0961(5) -0.1783(3) 0.079(2) Uani 1 1 d . . . C34 C 0.0492(11) 0.0065(7) -0.1155(5) 0.083(3) Uani 1 1 d . . . H34A H 0.0674 -0.0065 -0.0713 0.099 Uiso 1 1 calc R . . H34B H -0.0516 0.0155 -0.1221 0.099 Uiso 1 1 calc R . . C35 C 0.0914(12) -0.0717(9) -0.1536(6) 0.105(4) Uani 1 1 d . . . H35A H 0.0754 -0.0593 -0.1975 0.157 Uiso 1 1 calc R . . H35B H 0.0362 -0.1215 -0.1424 0.157 Uiso 1 1 calc R . . H35C H 0.1896 -0.0840 -0.1450 0.157 Uiso 1 1 calc R . . C62 C 0.1348(9) 0.2550(7) -0.1161(4) 0.067(2) Uani 1 1 d . . . H62A H 0.0528 0.2921 -0.1117 0.080 Uiso 1 1 calc R . . H62B H 0.1519 0.2485 -0.1604 0.080 Uiso 1 1 calc R . . C71 C 0.4066(9) 0.2184(6) 0.1576(4) 0.051(2) Uani 1 1 d . . . C72 C 0.2756(9) 0.2275(7) 0.1850(4) 0.066(3) Uani 1 1 d . . . H72 H 0.2258 0.2798 0.1808 0.080 Uiso 1 1 calc R . . C73 C 0.2213(12) 0.1593(9) 0.2179(5) 0.085(4) Uani 1 1 d . . . H73 H 0.1349 0.1658 0.2364 0.102 Uiso 1 1 calc R . . C74 C 0.2923(15) 0.0823(9) 0.2239(5) 0.093(4) Uani 1 1 d . . . H74 H 0.2547 0.0362 0.2464 0.112 Uiso 1 1 calc R . . C75 C 0.4196(15) 0.0728(7) 0.1967(5) 0.090(4) Uani 1 1 d . . . H75 H 0.4684 0.0202 0.2012 0.108 Uiso 1 1 calc R . . C76 C 0.4760(11) 0.1397(7) 0.1630(4) 0.071(3) Uani 1 1 d . . . H76 H 0.5612 0.1318 0.1438 0.085 Uiso 1 1 calc R . . C81 C 0.6582(8) 0.3224(6) 0.1481(4) 0.052(2) Uani 1 1 d . . . C82 C 0.7554(9) 0.3719(6) 0.1180(4) 0.065(2) Uani 1 1 d . . . H82 H 0.7343 0.3904 0.0770 0.078 Uiso 1 1 calc R . . C83 C 0.8835(10) 0.3950(7) 0.1465(5) 0.079(3) Uani 1 1 d . . . H83 H 0.9471 0.4291 0.1252 0.095 Uiso 1 1 calc R . . C84 C 0.9154(10) 0.3671(7) 0.2064(5) 0.078(3) Uani 1 1 d . . . H84 H 1.0027 0.3800 0.2258 0.094 Uiso 1 1 calc R . . C85 C 0.8174(11) 0.3196(9) 0.2381(5) 0.095(4) Uani 1 1 d . . . H85 H 0.8375 0.3027 0.2795 0.114 Uiso 1 1 calc R . . C86 C 0.6897(9) 0.2967(8) 0.2090(4) 0.075(3) Uani 1 1 d . . . H86 H 0.6250 0.2639 0.2306 0.091 Uiso 1 1 calc R . . C91 C 0.3966(8) 0.4051(6) 0.1219(4) 0.051(2) Uani 1 1 d . . . C92 C 0.3578(10) 0.4339(7) 0.1810(4) 0.069(3) Uani 1 1 d . . . H92 H 0.3807 0.3999 0.2162 0.083 Uiso 1 1 calc R . . C93 C 0.2869(11) 0.5112(8) 0.1881(6) 0.085(3) Uani 1 1 d . . . H93 H 0.2564 0.5270 0.2275 0.101 Uiso 1 1 calc R . . C94 C 0.2610(11) 0.5648(7) 0.1380(6) 0.082(3) Uani 1 1 d . . . H94 H 0.2161 0.6182 0.1433 0.098 Uiso 1 1 calc R . . C95 C 0.3014(11) 0.5398(7) 0.0795(5) 0.079(3) Uani 1 1 d . . . H95 H 0.2816 0.5758 0.0451 0.094 Uiso 1 1 calc R . . C96 C 0.3707(9) 0.4622(7) 0.0715(5) 0.067(3) Uani 1 1 d . . . H96 H 0.4010 0.4474 0.0320 0.080 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 Pt 0.03483(14) 0.05644(18) 0.03639(15) -0.00095(17) 0.00389(10) -0.00104(16) I 0.0376(3) 0.0946(5) 0.0855(5) -0.0194(4) 0.0044(3) 0.0066(3) P 0.0397(10) 0.0631(14) 0.0378(11) -0.0034(10) 0.0009(8) -0.0028(10) C2 0.042(4) 0.061(6) 0.035(4) 0.002(4) 0.010(3) 0.004(4) C3 0.044(4) 0.075(6) 0.025(4) 0.003(4) 0.008(3) -0.013(4) C4 0.044(4) 0.063(5) 0.035(4) -0.002(4) -0.002(3) -0.005(4) C5 0.042(4) 0.074(7) 0.037(4) -0.008(4) 0.005(3) -0.009(4) C6 0.062(5) 0.058(5) 0.043(5) 0.003(4) -0.006(4) -0.007(5) C21 0.050(5) 0.077(6) 0.070(6) -0.029(5) 0.018(4) 0.001(5) C31 0.085(7) 0.095(8) 0.045(5) 0.010(5) 0.000(5) -0.033(6) C41 0.069(6) 0.075(7) 0.078(7) -0.016(6) -0.004(5) 0.010(5) C51 0.052(5) 0.119(8) 0.048(5) -0.003(6) 0.016(4) -0.022(6) C61 0.096(8) 0.078(7) 0.064(7) 0.018(6) -0.021(6) -0.003(6) C32 0.049(4) 0.080(6) 0.041(5) -0.003(4) 0.001(4) -0.013(4) C33 0.048(5) 0.098(8) 0.042(5) 0.000(5) 0.003(4) -0.023(5) O31 0.090(5) 0.106(6) 0.044(4) -0.008(4) 0.014(3) -0.035(4) C34 0.089(7) 0.104(9) 0.055(6) -0.003(6) 0.008(5) -0.043(7) C35 0.093(8) 0.118(11) 0.102(10) 0.012(9) -0.012(7) -0.037(8) C62 0.054(5) 0.092(7) 0.053(5) -0.002(6) -0.016(4) -0.005(5) C71 0.061(5) 0.058(5) 0.034(4) -0.006(4) -0.003(4) -0.011(4) C72 0.057(5) 0.100(8) 0.043(5) -0.009(5) 0.013(4) -0.023(5) C73 0.085(7) 0.125(10) 0.046(6) -0.021(7) 0.017(5) -0.045(8) C74 0.138(12) 0.094(9) 0.048(6) -0.002(6) 0.008(7) -0.048(9) C75 0.150(12) 0.066(7) 0.054(7) -0.001(6) 0.001(7) -0.006(8) C76 0.076(6) 0.094(8) 0.042(5) 0.004(5) 0.006(5) -0.011(6) C81 0.047(4) 0.067(6) 0.041(4) -0.007(4) -0.006(4) 0.004(4) C82 0.054(5) 0.083(7) 0.056(6) 0.000(5) -0.003(4) -0.010(5) C83 0.060(6) 0.089(8) 0.088(8) -0.019(6) -0.002(6) -0.011(5) C84 0.048(5) 0.102(9) 0.083(8) -0.024(7) -0.027(5) 0.008(5) C85 0.078(7) 0.144(12) 0.062(7) -0.009(7) -0.020(6) -0.010(8) C86 0.054(5) 0.121(9) 0.051(6) 0.004(6) -0.002(4) -0.011(6) C91 0.038(4) 0.065(6) 0.050(5) -0.004(4) 0.003(4) -0.006(4) C92 0.085(7) 0.078(7) 0.046(6) -0.011(5) 0.015(5) 0.000(6) C93 0.086(8) 0.088(9) 0.080(8) -0.026(7) 0.020(6) -0.002(7) C94 0.076(7) 0.069(7) 0.101(9) -0.009(7) 0.010(6) 0.013(6) C95 0.095(8) 0.069(7) 0.071(7) 0.009(6) -0.008(6) 0.013(6) C96 0.064(6) 0.082(7) 0.055(6) -0.005(5) 0.005(4) -0.006(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt C2 2.105(8) . ? Pt P 2.262(2) . ? Pt C4 2.264(8) . ? Pt C5 2.281(8) . ? Pt I 2.6969(9) . ? P C91 1.813(9) . ? P C71 1.828(9) . ? P C81 1.836(8) . ? C2 C21 1.504(10) . ? C2 C6 1.534(11) . ? C2 C3 1.553(11) . ? C3 C31 1.512(11) . ? C3 C4 1.529(10) . ? C3 C32 1.577(10) . ? C4 C5 1.389(11) . ? C4 C41 1.483(12) . ? C5 C51 1.500(10) . ? C5 C6 1.532(12) . ? C6 C61 1.510(12) . ? C6 C62 1.548(11) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C61 H61A 0.9600 . ? C61 H61B 0.9600 . ? C61 H61C 0.9600 . ? C32 C33 1.505(12) . ? C32 C62 1.537(12) . ? C32 H32 0.9800 . ? C33 O31 1.212(9) . ? C33 C34 1.506(13) . ? C34 C35 1.505(15) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C62 H62A 0.9700 . ? C62 H62B 0.9700 . ? C71 C76 1.371(13) . ? C71 C72 1.404(12) . ? C72 C73 1.367(14) . ? C72 H72 0.9300 . ? C73 C74 1.359(16) . ? C73 H73 0.9300 . ? C74 C75 1.369(16) . ? C74 H74 0.9300 . ? C75 C76 1.371(14) . ? C75 H75 0.9300 . ? C76 H76 0.9300 . ? C81 C82 1.373(11) . ? C81 C86 1.374(12) . ? C82 C83 1.380(12) . ? C82 H82 0.9300 . ? C83 C84 1.367(14) . ? C83 H83 0.9300 . ? C84 C85 1.378(14) . ? C84 H84 0.9300 . ? C85 C86 1.381(13) . ? C85 H85 0.9300 . ? C86 H86 0.9300 . ? C91 C96 1.395(12) . ? C91 C92 1.397(11) . ? C92 C93 1.370(14) . ? C92 H92 0.9300 . ? C93 C94 1.358(15) . ? C93 H93 0.9300 . ? C94 C95 1.373(14) . ? C94 H94 0.9300 . ? C95 C96 1.369(13) . ? C95 H95 0.9300 . ? C96 H96 0.9300 . ? 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 C2 Pt P 102.0(2) . . ? C2 Pt C4 62.7(3) . . ? P Pt C4 150.2(2) . . ? C2 Pt C5 62.0(3) . . ? P Pt C5 159.9(2) . . ? C4 Pt C5 35.6(3) . . ? C2 Pt I 159.6(2) . . ? P Pt I 98.01(6) . . ? C4 Pt I 97.6(2) . . ? C5 Pt I 99.2(2) . . ? C91 P C71 108.3(4) . . ? C91 P C81 101.2(4) . . ? C71 P C81 103.8(4) . . ? C91 P Pt 115.5(3) . . ? C71 P Pt 106.3(3) . . ? C81 P Pt 120.8(3) . . ? C21 C2 C6 121.3(7) . . ? C21 C2 C3 116.8(7) . . ? C6 C2 C3 95.0(6) . . ? C21 C2 Pt 126.3(6) . . ? C6 C2 Pt 95.8(5) . . ? C3 C2 Pt 94.5(5) . . ? C31 C3 C4 116.4(8) . . ? C31 C3 C2 116.7(7) . . ? C4 C3 C2 95.3(6) . . ? C31 C3 C32 114.6(7) . . ? C4 C3 C32 107.5(6) . . ? C2 C3 C32 104.0(7) . . ? C5 C4 C41 127.2(8) . . ? C5 C4 C3 106.0(7) . . ? C41 C4 C3 124.5(8) . . ? C5 C4 Pt 72.8(5) . . ? C41 C4 Pt 118.2(6) . . ? C3 C4 Pt 89.1(5) . . ? C4 C5 C51 126.9(8) . . ? C4 C5 C6 107.6(7) . . ? C51 C5 C6 122.5(8) . . ? C4 C5 Pt 71.6(5) . . ? C51 C5 Pt 122.0(6) . . ? C6 C5 Pt 89.1(5) . . ? C61 C6 C5 117.2(8) . . ? C61 C6 C2 118.8(8) . . ? C5 C6 C2 95.1(6) . . ? C61 C6 C62 112.9(8) . . ? C5 C6 C62 107.5(7) . . ? C2 C6 C62 103.1(7) . . ? C2 C21 H21A 109.5 . . ? C2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C3 C31 H31A 109.5 . . ? C3 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C3 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C4 C41 H41A 109.5 . . ? C4 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C4 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C5 C51 H51A 109.5 . . ? C5 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C5 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C6 C61 H61A 109.5 . . ? C6 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C6 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C33 C32 C62 112.9(7) . . ? C33 C32 C3 112.5(7) . . ? C62 C32 C3 102.1(6) . . ? C33 C32 H32 109.7 . . ? C62 C32 H32 109.7 . . ? C3 C32 H32 109.7 . . ? O31 C33 C32 122.3(9) . . ? O31 C33 C34 120.5(9) . . ? C32 C33 C34 117.1(8) . . ? C35 C34 C33 114.6(9) . . ? C35 C34 H34A 108.6 . . ? C33 C34 H34A 108.6 . . ? C35 C34 H34B 108.6 . . ? C33 C34 H34B 108.6 . . ? H34A C34 H34B 107.6 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C32 C62 C6 105.2(7) . . ? C32 C62 H62A 110.7 . . ? C6 C62 H62A 110.7 . . ? C32 C62 H62B 110.7 . . ? C6 C62 H62B 110.7 . . ? H62A C62 H62B 108.8 . . ? C76 C71 C72 118.9(9) . . ? C76 C71 P 116.9(7) . . ? C72 C71 P 124.0(7) . . ? C73 C72 C71 119.8(10) . . ? C73 C72 H72 120.1 . . ? C71 C72 H72 120.1 . . ? C74 C73 C72 120.7(11) . . ? C74 C73 H73 119.6 . . ? C72 C73 H73 119.6 . . ? C73 C74 C75 119.6(11) . . ? C73 C74 H74 120.2 . . ? C75 C74 H74 120.2 . . ? C74 C75 C76 121.0(12) . . ? C74 C75 H75 119.5 . . ? C76 C75 H75 119.5 . . ? C75 C76 C71 119.9(10) . . ? C75 C76 H76 120.0 . . ? C71 C76 H76 120.0 . . ? C82 C81 C86 118.4(8) . . ? C82 C81 P 119.1(6) . . ? C86 C81 P 122.3(7) . . ? C81 C82 C83 122.2(9) . . ? C81 C82 H82 118.9 . . ? C83 C82 H82 118.9 . . ? C84 C83 C82 119.0(10) . . ? C84 C83 H83 120.5 . . ? C82 C83 H83 120.5 . . ? C83 C84 C85 119.6(9) . . ? C83 C84 H84 120.2 . . ? C85 C84 H84 120.2 . . ? C84 C85 C86 120.8(10) . . ? C84 C85 H85 119.6 . . ? C86 C85 H85 119.6 . . ? C81 C86 C85 120.1(10) . . ? C81 C86 H86 120.0 . . ? C85 C86 H86 120.0 . . ? C96 C91 C92 116.8(9) . . ? C96 C91 P 119.4(7) . . ? C92 C91 P 123.7(7) . . ? C93 C92 C91 121.4(10) . . ? C93 C92 H92 119.3 . . ? C91 C92 H92 119.3 . . ? C94 C93 C92 120.3(10) . . ? C94 C93 H93 119.9 . . ? C92 C93 H93 119.9 . . ? C93 C94 C95 119.8(10) . . ? C93 C94 H94 120.1 . . ? C95 C94 H94 120.1 . . ? C96 C95 C94 120.6(10) . . ? C96 C95 H95 119.7 . . ? C94 C95 H95 119.7 . . ? C95 C96 C91 120.9(9) . . ? C95 C96 H96 119.5 . . ? C91 C96 H96 119.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.55 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.512 _refine_diff_density_min -1.648 _refine_diff_density_rms 0.149