# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_year ? _journal_page_first ? _publ_contact_author_name 'Piero Leoni' _publ_contact_author_address ; Dipartimento di Chimica e Chimica Industriale Università di Pisa Via Risorgimento 35 Pisa I-56126 ITALY ; _publ_contact_author_email LEONI@DCCI.UNIPI.IT _publ_section_title ;Unprecedented Reversible Coupling of Alkynyl and Phosphide ligands on a Dinuclear Platinum Framework ; loop_ _publ_author_name 'A. Albinati' 'Valeria Filippi' 'Piero Leoni' 'Lorella Marchetti' 'Marco Pasquali' ; V.Passarelli ; data_albi15 _database_code_depnum_ccdc_archive 'CCDC 254340' _audit_creation_method SHELXL-97 _chemical_formula_moiety 3.THF _chemical_name_common ;(Pt2(mu–P(tBu)2)(mu,eta1,eta2–C(Ph)CH2)(C=C–Ph)(CO)(PtBu2H)(Br )) ; _chemical_formula_sum 'C37 H57 Br O2 P2 Pt2' _chemical_formula_weight 1065.86 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' Br Br -0.2901 2.4595 '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 P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.9215(2) _cell_length_b 11.2562(2) _cell_length_c 22.8096(3) _cell_angle_alpha 90.00 _cell_angle_beta 104.380(1) _cell_angle_gamma 90.00 _cell_volume 3959.8(1) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 9950 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 25.4 _exptl_crystal_description polyhedron _exptl_crystal_colour yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.788 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2064 _exptl_absorpt_coefficient_mu 8.177 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.19 _exptl_absorpt_correction_T_max 0.26 _exptl_special_details ; 2142 frames were collected on a Brucker SMART CCD diffractometer with a sample to detector distance of 50.0 mm. The counting time per frame was 20 sec and the scan width per frame 0.3 deg. ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 39906 _diffrn_reflns_av_R_equivalents 0.0339 _diffrn_reflns_av_sigmaI/netI 0.0251 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 27.49 _reflns_number_total 9069 _reflns_number_gt 7694 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'SAINT and SADABS' _computing_structure_solution 'SHELXS-97 (Sheldrick,1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP for Windows 1.074(Farrugia 1997)' _computing_publication_material 'WinGX 1.64.05 (L.J. Farruggia, 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^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. A clathrated THF molecule was found towards the end of the refinement from difmaps, and refined using ADP's for all atoms. ; _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^)+(0.0286P)^2^+5.3701P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef no _refine_ls_number_reflns 9069 _refine_ls_number_parameters 422 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0324 _refine_ls_R_factor_gt 0.0232 _refine_ls_wR_factor_ref 0.0567 _refine_ls_wR_factor_gt 0.0530 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _refine_ls_shift/su_max 0.225 _refine_ls_shift/su_mean 0.192 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 0.937284(9) 0.865620(12) 0.161971(6) 0.02308(4) Uani 1 1 d . . . Pt2 Pt 0.840850(10) 0.728391(13) 0.021210(6) 0.02899(4) Uani 1 1 d . . . Br1 Br 0.87496(4) 0.75400(5) -0.08028(2) 0.05704(14) Uani 1 1 d . . . P2 P 1.05129(6) 0.99623(8) 0.20180(4) 0.02534(18) Uani 1 1 d . . . P1 P 0.82823(6) 0.72962(8) 0.11924(4) 0.02506(18) Uani 1 1 d . . . C1 C 0.7455(3) 0.6291(4) -0.01529(17) 0.0364(9) Uani 1 1 d . . . O1 O 0.6903(2) 0.5683(3) -0.03885(14) 0.0511(8) Uani 1 1 d . . . C10 C 0.9292(2) 0.8320(3) 0.24514(16) 0.0291(8) Uani 1 1 d . . . C11 C 0.9190(3) 0.8197(4) 0.29580(17) 0.0327(8) Uani 1 1 d . . . C12 C 0.9065(3) 0.8076(4) 0.35588(17) 0.0341(8) Uani 1 1 d . . . C13 C 0.9607(3) 0.8658(4) 0.40483(19) 0.0469(11) Uani 1 1 d . . . H13 H 1.0059 0.9154 0.3984 0.061 Uiso 1 1 calc R . . C14 C 0.9496(3) 0.8520(5) 0.4625(2) 0.0563(13) Uani 1 1 d . . . H14 H 0.9878 0.8909 0.4956 0.073 Uiso 1 1 calc R . . C15 C 0.8841(4) 0.7830(5) 0.4726(2) 0.0562(14) Uani 1 1 d . . . H15 H 0.8765 0.7748 0.5124 0.073 Uiso 1 1 calc R . . C16 C 0.8293(4) 0.7253(4) 0.4252(2) 0.0535(13) Uani 1 1 d . . . H16 H 0.7839 0.6770 0.4323 0.070 Uiso 1 1 calc R . . C17 C 0.8399(3) 0.7373(4) 0.3673(2) 0.0444(10) Uani 1 1 d . . . H17 H 0.8015 0.6972 0.3347 0.058 Uiso 1 1 calc R . . C2 C 0.9267(3) 0.9538(3) 0.07265(17) 0.0338(8) Uani 1 1 d . . . H2A H 0.8682 0.9834 0.0522 0.044 Uiso 1 1 calc R . . H2B H 0.9728 1.0122 0.0716 0.044 Uiso 1 1 calc R . . C3 C 0.9441(3) 0.8384(3) 0.05878(16) 0.0315(8) Uani 1 1 d . . . C4 C 1.0335(3) 0.7982(4) 0.05892(18) 0.0376(9) Uani 1 1 d . . . C5 C 1.1007(3) 0.8792(5) 0.0589(2) 0.0500(12) Uani 1 1 d . . . H5 H 1.0901 0.9623 0.0586 0.065 Uiso 1 1 calc R . . C6 C 1.1831(4) 0.8366(7) 0.0592(3) 0.0742(18) Uani 1 1 d . . . H6 H 1.2282 0.8911 0.0583 0.096 Uiso 1 1 calc R . . C7 C 1.1999(4) 0.7159(7) 0.0608(3) 0.088(2) Uani 1 1 d . . . H7 H 1.2569 0.6883 0.0626 0.115 Uiso 1 1 calc R . . C8 C 1.1350(4) 0.6368(6) 0.0597(3) 0.0758(18) Uani 1 1 d . . . H8 H 1.1463 0.5539 0.0604 0.098 Uiso 1 1 calc R . . C9 C 1.0519(3) 0.6779(5) 0.0576(2) 0.0524(12) Uani 1 1 d . . . H9 H 1.0065 0.6220 0.0552 0.068 Uiso 1 1 calc R . . C111 C 0.8487(3) 0.5748(3) 0.15239(17) 0.0345(9) Uani 1 1 d . . . C112 C 0.9478(3) 0.5590(4) 0.1733(2) 0.0494(11) Uani 1 1 d . . . H11A H 0.9722 0.6202 0.2032 0.064 Uiso 1 1 calc R . . H11B H 0.9730 0.5665 0.1384 0.064 Uiso 1 1 calc R . . H11C H 0.9611 0.4802 0.1915 0.064 Uiso 1 1 calc R . . C113 C 0.8124(4) 0.5562(4) 0.2077(2) 0.0544(12) Uani 1 1 d . . . H11D H 0.8243 0.4747 0.2225 0.071 Uiso 1 1 calc R . . H11E H 0.7497 0.5699 0.1965 0.071 Uiso 1 1 calc R . . H11F H 0.8401 0.6121 0.2396 0.071 Uiso 1 1 calc R . . C114 C 0.8115(3) 0.4792(4) 0.1053(2) 0.0507(12) Uani 1 1 d . . . H11G H 0.8207 0.4007 0.1243 0.066 Uiso 1 1 calc R . . H11H H 0.8407 0.4831 0.0722 0.066 Uiso 1 1 calc R . . H11I H 0.7492 0.4928 0.0891 0.066 Uiso 1 1 calc R . . C121 C 0.7179(3) 0.7878(4) 0.12197(18) 0.0356(9) Uani 1 1 d . . . C122 C 0.7067(3) 0.9050(5) 0.0870(3) 0.0596(14) Uani 1 1 d . . . H12A H 0.6485 0.9366 0.0841 0.077 Uiso 1 1 calc R . . H12B H 0.7145 0.8912 0.0462 0.077 Uiso 1 1 calc R . . H12C H 0.7501 0.9622 0.1082 0.077 Uiso 1 1 calc R . . C123 C 0.7117(3) 0.8157(5) 0.1863(2) 0.0516(12) Uani 1 1 d . . . H12D H 0.6555 0.8525 0.1850 0.067 Uiso 1 1 calc R . . H12E H 0.7584 0.8704 0.2053 0.067 Uiso 1 1 calc R . . H12F H 0.7174 0.7419 0.2098 0.067 Uiso 1 1 calc R . . C124 C 0.6438(3) 0.7037(5) 0.0918(2) 0.0560(13) Uani 1 1 d . . . H12G H 0.6484 0.6300 0.1153 0.073 Uiso 1 1 calc R . . H12H H 0.6479 0.6854 0.0506 0.073 Uiso 1 1 calc R . . H12I H 0.5880 0.7419 0.0903 0.073 Uiso 1 1 calc R . . C211 C 1.0179(3) 1.1384(3) 0.23212(19) 0.0354(9) Uani 1 1 d . . . C212 C 0.9454(3) 1.1874(4) 0.1804(2) 0.0537(12) Uani 1 1 d . . . H21C H 0.9254 1.2637 0.1926 0.070 Uiso 1 1 calc R . . H21D H 0.8969 1.1311 0.1713 0.070 Uiso 1 1 calc R . . H21E H 0.9675 1.1986 0.1444 0.070 Uiso 1 1 calc R . . C213 C 1.0919(3) 1.2289(4) 0.2456(2) 0.0459(11) Uani 1 1 d . . . H21F H 1.0709 1.3042 0.2583 0.060 Uiso 1 1 calc R . . H21G H 1.1127 1.2418 0.2092 0.060 Uiso 1 1 calc R . . H21H H 1.1395 1.1987 0.2782 0.060 Uiso 1 1 calc R . . C214 C 0.9825(3) 1.1206(4) 0.2883(2) 0.0495(12) Uani 1 1 d . . . H21I H 1.0293 1.0934 0.3222 0.064 Uiso 1 1 calc R . . H21L H 0.9362 1.0610 0.2796 0.064 Uiso 1 1 calc R . . H21M H 0.9593 1.1960 0.2990 0.064 Uiso 1 1 calc R . . C221 C 1.1516(2) 0.9270(3) 0.25023(18) 0.0330(8) Uani 1 1 d . . . C222 C 1.1537(3) 0.7984(4) 0.2279(2) 0.0479(11) Uani 1 1 d . . . H22A H 1.1536 0.7987 0.1849 0.062 Uiso 1 1 calc R . . H22B H 1.1026 0.7556 0.2333 0.062 Uiso 1 1 calc R . . H22C H 1.2063 0.7589 0.2512 0.062 Uiso 1 1 calc R . . C223 C 1.1516(3) 0.9244(5) 0.3169(2) 0.0542(13) Uani 1 1 d . . . H22D H 1.2049 0.8862 0.3401 0.070 Uiso 1 1 calc R . . H22E H 1.1012 0.8794 0.3221 0.070 Uiso 1 1 calc R . . H22F H 1.1488 1.0058 0.3315 0.070 Uiso 1 1 calc R . . C224 C 1.2321(3) 0.9919(5) 0.2414(3) 0.0625(15) Uani 1 1 d . . . H22G H 1.2843 0.9538 0.2661 0.081 Uiso 1 1 calc R . . H22H H 1.2303 1.0751 0.2538 0.081 Uiso 1 1 calc R . . H22I H 1.2331 0.9885 0.1987 0.081 Uiso 1 1 calc R . . C1S C 0.4125(6) 1.0614(12) 0.1562(4) 0.122(4) Uani 1 1 d . . . H1S1 H 0.435(7) 1.130(10) 0.182(5) 0.183 Uiso 1 1 calc . . . H1S2 H 0.373(7) 1.014(10) 0.175(5) 0.183 Uiso 1 1 calc . . . C2S C 0.400(2) 1.0160(15) 0.0607(4) 0.301(18) Uani 1 1 d . . . H2S1 H 0.352(18) 0.97(3) 0.037(13) 0.451 Uiso 1 1 calc . . . H2S2 H 0.43(2) 1.06(3) 0.031(13) 0.451 Uiso 1 1 calc . . . C3S C 0.4823(7) 0.9894(11) 0.1451(6) 0.132(4) Uani 1 1 d . . . H3S1 H 0.535(8) 1.039(11) 0.148(6) 0.199 Uiso 1 1 calc . . . H3S2 H 0.497(8) 0.925(11) 0.176(6) 0.199 Uiso 1 1 calc . . . C4S C 0.3671(8) 1.1009(11) 0.0900(9) 0.186(7) Uani 1 1 d . . . H4S1 H 0.303(11) 1.096(15) 0.082(8) 0.279 Uiso 1 1 calc . . . H4S2 H 0.385(10) 1.182(16) 0.081(7) 0.279 Uiso 1 1 calc . . . O1S O 0.4555(10) 0.9465(18) 0.0928(11) 0.359(13) Uani 1 1 d . . . HP1 H 1.0821 1.0528 0.1608 0.048(12) Uiso 1 1 d . . . 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 0.02677(7) 0.02155(7) 0.02186(7) 0.00280(5) 0.00785(5) -0.00036(5) Pt2 0.03674(8) 0.03030(8) 0.02116(7) 0.00044(5) 0.00952(6) -0.00211(6) Br1 0.0789(4) 0.0704(3) 0.0272(2) -0.0048(2) 0.0233(2) -0.0255(3) P2 0.0273(4) 0.0223(4) 0.0283(5) 0.0020(4) 0.0105(4) -0.0005(4) P1 0.0284(5) 0.0262(4) 0.0215(4) 0.0017(3) 0.0080(3) -0.0013(4) C1 0.046(2) 0.044(2) 0.0196(18) -0.0029(16) 0.0088(16) -0.0031(19) O1 0.0523(19) 0.061(2) 0.0378(17) -0.0111(15) 0.0063(14) -0.0141(17) C10 0.0294(18) 0.0310(19) 0.0262(18) 0.0015(15) 0.0057(14) -0.0047(15) C11 0.035(2) 0.033(2) 0.030(2) 0.0047(16) 0.0070(16) -0.0007(16) C12 0.040(2) 0.036(2) 0.0286(19) 0.0058(16) 0.0128(16) 0.0046(17) C13 0.046(3) 0.062(3) 0.031(2) 0.001(2) 0.0068(18) -0.002(2) C14 0.063(3) 0.077(4) 0.027(2) 0.000(2) 0.007(2) 0.012(3) C15 0.081(4) 0.062(3) 0.035(2) 0.014(2) 0.031(2) 0.025(3) C16 0.075(4) 0.047(3) 0.051(3) 0.007(2) 0.040(3) 0.001(2) C17 0.057(3) 0.043(2) 0.040(2) -0.0025(19) 0.025(2) -0.008(2) C2 0.043(2) 0.0309(19) 0.0268(19) 0.0075(15) 0.0081(16) -0.0013(17) C3 0.040(2) 0.034(2) 0.0223(17) 0.0041(15) 0.0126(15) -0.0041(16) C4 0.042(2) 0.046(2) 0.029(2) -0.0022(17) 0.0172(17) -0.0036(19) C5 0.050(3) 0.065(3) 0.041(2) -0.001(2) 0.025(2) -0.012(2) C6 0.051(3) 0.113(5) 0.069(4) -0.008(4) 0.035(3) -0.020(3) C7 0.058(4) 0.120(6) 0.103(5) 0.001(4) 0.050(4) 0.019(4) C8 0.069(4) 0.077(4) 0.097(5) -0.005(3) 0.049(4) 0.016(3) C9 0.054(3) 0.051(3) 0.061(3) -0.002(2) 0.031(2) 0.006(2) C111 0.047(2) 0.0255(19) 0.0293(19) 0.0081(15) 0.0063(17) -0.0051(17) C112 0.052(3) 0.033(2) 0.057(3) 0.012(2) 0.001(2) 0.006(2) C113 0.078(3) 0.048(3) 0.041(3) 0.010(2) 0.022(2) -0.015(2) C114 0.068(3) 0.027(2) 0.047(3) 0.0025(18) -0.004(2) -0.006(2) C121 0.0277(19) 0.048(2) 0.033(2) -0.0073(17) 0.0099(16) 0.0000(17) C122 0.048(3) 0.060(3) 0.074(4) 0.011(3) 0.021(3) 0.025(2) C123 0.037(2) 0.078(3) 0.043(3) -0.020(2) 0.0143(19) 0.000(2) C124 0.033(2) 0.084(4) 0.050(3) -0.027(3) 0.010(2) -0.008(2) C211 0.038(2) 0.0231(18) 0.047(2) -0.0016(16) 0.0147(18) 0.0000(16) C212 0.050(3) 0.032(2) 0.073(3) 0.001(2) 0.005(2) 0.013(2) C213 0.053(3) 0.032(2) 0.056(3) -0.010(2) 0.020(2) -0.011(2) C214 0.059(3) 0.037(2) 0.065(3) -0.009(2) 0.037(2) 0.001(2) C221 0.0285(19) 0.034(2) 0.036(2) 0.0029(16) 0.0067(16) 0.0001(16) C222 0.041(2) 0.036(2) 0.064(3) 0.001(2) 0.008(2) 0.0120(19) C223 0.046(3) 0.076(4) 0.036(2) 0.006(2) 0.001(2) 0.016(2) C224 0.028(2) 0.060(3) 0.098(4) 0.018(3) 0.013(2) -0.002(2) C1S 0.095(6) 0.196(12) 0.082(6) -0.034(6) 0.034(5) 0.025(7) C2S 0.68(5) 0.162(12) 0.039(5) 0.022(6) 0.057(12) 0.19(2) C3S 0.117(8) 0.120(9) 0.150(10) 0.013(7) 0.014(8) 0.047(7) C4S 0.103(7) 0.085(7) 0.33(2) 0.059(11) -0.019(10) 0.044(6) O1S 0.235(14) 0.37(2) 0.44(3) -0.29(2) 0.025(16) 0.054(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C10 1.970(4) . ? Pt1 C2 2.234(4) . ? Pt1 P2 2.3372(9) . ? Pt1 P1 2.3383(9) . ? Pt1 C3 2.402(4) . ? Pt2 C1 1.903(4) . ? Pt2 C3 2.066(4) . ? Pt2 P1 2.2943(9) . ? Pt2 Br1 2.5222(4) . ? P2 C211 1.872(4) . ? P2 C221 1.871(4) . ? P1 C121 1.891(4) . ? P1 C111 1.896(4) . ? C1 O1 1.138(5) . ? C10 C11 1.214(5) . ? C11 C12 1.439(5) . ? C12 C13 1.393(6) . ? C12 C17 1.398(6) . ? C13 C14 1.380(6) . ? C14 C15 1.364(8) . ? C15 C16 1.372(8) . ? C16 C17 1.380(6) . ? C2 C3 1.381(5) . ? C3 C4 1.494(6) . ? C4 C9 1.387(7) . ? C4 C5 1.406(6) . ? C5 C6 1.395(8) . ? C6 C7 1.383(10) . ? C7 C8 1.360(9) . ? C8 C9 1.391(7) . ? C111 C113 1.526(6) . ? C111 C114 1.532(6) . ? C111 C112 1.540(6) . ? C121 C123 1.526(6) . ? C121 C122 1.528(7) . ? C121 C124 1.535(6) . ? C211 C212 1.533(6) . ? C211 C214 1.537(6) . ? C211 C213 1.530(6) . ? C221 C223 1.521(6) . ? C221 C224 1.531(6) . ? C221 C222 1.538(6) . ? C1S C3S 1.447(14) . ? C1S C4S 1.567(18) . ? C2S O1S 1.27(2) . ? C2S C4S 1.35(2) . ? C2S C3S 2.06(2) . ? C3S O1S 1.260(18) . ? 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 C10 Pt1 C2 162.80(15) . . ? C10 Pt1 P2 88.66(11) . . ? C2 Pt1 P2 87.17(11) . . ? C10 Pt1 P1 93.23(11) . . ? C2 Pt1 P1 91.75(11) . . ? P2 Pt1 P1 176.82(3) . . ? C10 Pt1 C3 161.55(15) . . ? C2 Pt1 C3 34.41(13) . . ? P2 Pt1 C3 103.98(9) . . ? P1 Pt1 C3 73.59(9) . . ? C1 Pt2 C3 178.56(15) . . ? C1 Pt2 P1 100.16(11) . . ? C3 Pt2 P1 81.10(10) . . ? C1 Pt2 Br1 89.77(11) . . ? C3 Pt2 Br1 88.96(10) . . ? P1 Pt2 Br1 170.00(3) . . ? C211 P2 C221 114.64(19) . . ? C211 P2 Pt1 114.66(13) . . ? C221 P2 Pt1 115.72(13) . . ? C121 P1 C111 112.01(19) . . ? C121 P1 Pt2 109.95(13) . . ? C111 P1 Pt2 109.58(13) . . ? C121 P1 Pt1 111.06(13) . . ? C111 P1 Pt1 113.54(13) . . ? Pt2 P1 Pt1 100.05(3) . . ? O1 C1 Pt2 177.1(4) . . ? C11 C10 Pt1 174.1(4) . . ? C10 C11 C12 178.9(4) . . ? C13 C12 C17 117.7(4) . . ? C13 C12 C11 120.9(4) . . ? C17 C12 C11 121.4(4) . . ? C14 C13 C12 120.7(5) . . ? C15 C14 C13 120.6(5) . . ? C14 C15 C16 120.0(4) . . ? C15 C16 C17 120.2(5) . . ? C16 C17 C12 120.8(4) . . ? C3 C2 Pt1 79.5(2) . . ? C2 C3 C4 122.0(4) . . ? C2 C3 Pt2 118.3(3) . . ? C4 C3 Pt2 118.6(3) . . ? C2 C3 Pt1 66.1(2) . . ? C4 C3 Pt1 108.1(2) . . ? Pt2 C3 Pt1 104.97(15) . . ? C9 C4 C5 118.0(4) . . ? C9 C4 C3 120.1(4) . . ? C5 C4 C3 121.9(4) . . ? C6 C5 C4 119.4(5) . . ? C5 C6 C7 120.9(5) . . ? C8 C7 C6 120.1(6) . . ? C7 C8 C9 119.7(6) . . ? C4 C9 C8 121.9(5) . . ? C113 C111 C114 108.9(4) . . ? C113 C111 C112 107.3(4) . . ? C114 C111 C112 108.9(4) . . ? C113 C111 P1 113.1(3) . . ? C114 C111 P1 111.6(3) . . ? C112 C111 P1 106.9(3) . . ? C123 C121 C122 107.3(4) . . ? C123 C121 C124 109.4(4) . . ? C122 C121 C124 108.8(4) . . ? C123 C121 P1 112.6(3) . . ? C122 C121 P1 105.7(3) . . ? C124 C121 P1 112.8(3) . . ? C212 C211 C214 109.0(4) . . ? C212 C211 C213 108.1(4) . . ? C214 C211 C213 110.1(4) . . ? C212 C211 P2 104.6(3) . . ? C214 C211 P2 113.2(3) . . ? C213 C211 P2 111.6(3) . . ? C223 C221 C224 110.4(4) . . ? C223 C221 C222 108.6(4) . . ? C224 C221 C222 108.6(4) . . ? C223 C221 P2 112.8(3) . . ? C224 C221 P2 110.1(3) . . ? C222 C221 P2 106.4(3) . . ? C3S C1S C4S 100.4(9) . . ? O1S C2S C4S 116.9(13) . . ? O1S C2S C3S 35.2(8) . . ? C4S C2S C3S 82.8(9) . . ? O1S C3S C1S 106.7(11) . . ? O1S C3S C2S 35.4(9) . . ? C1S C3S C2S 75.3(8) . . ? C2S C4S C1S 97.7(8) . . ? C3S O1S C2S 109.5(12) . . ? 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 C10 Pt1 P2 C211 -72.44(18) . . . . ? C2 Pt1 P2 C211 90.87(18) . . . . ? P1 Pt1 P2 C211 161.1(6) . . . . ? C3 Pt1 P2 C211 121.15(18) . . . . ? C10 Pt1 P2 C221 64.47(18) . . . . ? C2 Pt1 P2 C221 -132.22(18) . . . . ? P1 Pt1 P2 C221 -62.0(6) . . . . ? C3 Pt1 P2 C221 -101.94(17) . . . . ? C1 Pt2 P1 C121 -58.07(19) . . . . ? C3 Pt2 P1 C121 121.23(18) . . . . ? Br1 Pt2 P1 C121 114.7(2) . . . . ? C1 Pt2 P1 C111 65.45(19) . . . . ? C3 Pt2 P1 C111 -115.25(18) . . . . ? Br1 Pt2 P1 C111 -121.8(2) . . . . ? C1 Pt2 P1 Pt1 -174.98(13) . . . . ? C3 Pt2 P1 Pt1 4.32(11) . . . . ? Br1 Pt2 P1 Pt1 -2.20(18) . . . . ? C10 Pt1 P1 C121 73.23(18) . . . . ? C2 Pt1 P1 C121 -90.30(18) . . . . ? P2 Pt1 P1 C121 -160.4(6) . . . . ? C3 Pt1 P1 C121 -119.90(17) . . . . ? C10 Pt1 P1 C111 -54.05(18) . . . . ? C2 Pt1 P1 C111 142.41(18) . . . . ? P2 Pt1 P1 C111 72.3(6) . . . . ? C3 Pt1 P1 C111 112.82(17) . . . . ? C10 Pt1 P1 Pt2 -170.69(11) . . . . ? C2 Pt1 P1 Pt2 25.78(11) . . . . ? P2 Pt1 P1 Pt2 -44.3(6) . . . . ? C3 Pt1 P1 Pt2 -3.82(10) . . . . ? C3 Pt2 C1 O1 57(12) . . . . ? P1 Pt2 C1 O1 -152(8) . . . . ? Br1 Pt2 C1 O1 29(8) . . . . ? C2 Pt1 C10 C11 14(4) . . . . ? P2 Pt1 C10 C11 90(3) . . . . ? P1 Pt1 C10 C11 -93(3) . . . . ? C3 Pt1 C10 C11 -136(3) . . . . ? Pt1 C10 C11 C12 -27(24) . . . . ? C10 C11 C12 C13 -65(22) . . . . ? C10 C11 C12 C17 115(22) . . . . ? C17 C12 C13 C14 1.3(7) . . . . ? C11 C12 C13 C14 -178.7(4) . . . . ? C12 C13 C14 C15 -1.3(8) . . . . ? C13 C14 C15 C16 0.8(8) . . . . ? C14 C15 C16 C17 -0.3(8) . . . . ? C15 C16 C17 C12 0.2(7) . . . . ? C13 C12 C17 C16 -0.7(7) . . . . ? C11 C12 C17 C16 179.2(4) . . . . ? C10 Pt1 C2 C3 -163.8(4) . . . . ? P2 Pt1 C2 C3 120.0(2) . . . . ? P1 Pt1 C2 C3 -57.0(2) . . . . ? Pt1 C2 C3 C4 -97.2(3) . . . . ? Pt1 C2 C3 Pt2 94.7(2) . . . . ? C1 Pt2 C3 C2 76(7) . . . . ? P1 Pt2 C3 C2 -74.9(3) . . . . ? Br1 Pt2 C3 C2 104.0(3) . . . . ? C1 Pt2 C3 C4 -92(7) . . . . ? P1 Pt2 C3 C4 116.6(3) . . . . ? Br1 Pt2 C3 C4 -64.5(3) . . . . ? C1 Pt2 C3 Pt1 147(7) . . . . ? P1 Pt2 C3 Pt1 -4.28(11) . . . . ? Br1 Pt2 C3 Pt1 174.59(13) . . . . ? C10 Pt1 C3 C2 164.9(4) . . . . ? P2 Pt1 C3 C2 -63.0(2) . . . . ? P1 Pt1 C3 C2 119.1(2) . . . . ? C10 Pt1 C3 C4 -77.4(5) . . . . ? C2 Pt1 C3 C4 117.7(4) . . . . ? P2 Pt1 C3 C4 54.6(3) . . . . ? P1 Pt1 C3 C4 -123.2(3) . . . . ? C10 Pt1 C3 Pt2 50.1(5) . . . . ? C2 Pt1 C3 Pt2 -114.8(3) . . . . ? P2 Pt1 C3 Pt2 -177.80(12) . . . . ? P1 Pt1 C3 Pt2 4.33(11) . . . . ? C2 C3 C4 C9 166.2(4) . . . . ? Pt2 C3 C4 C9 -25.8(5) . . . . ? Pt1 C3 C4 C9 93.5(4) . . . . ? C2 C3 C4 C5 -15.4(6) . . . . ? Pt2 C3 C4 C5 152.7(3) . . . . ? Pt1 C3 C4 C5 -88.1(4) . . . . ? C9 C4 C5 C6 -1.7(7) . . . . ? C3 C4 C5 C6 179.8(4) . . . . ? C4 C5 C6 C7 -1.3(8) . . . . ? C5 C6 C7 C8 2.5(10) . . . . ? C6 C7 C8 C9 -0.6(11) . . . . ? C5 C4 C9 C8 3.7(7) . . . . ? C3 C4 C9 C8 -177.8(5) . . . . ? C7 C8 C9 C4 -2.5(9) . . . . ? C121 P1 C111 C113 -38.0(4) . . . . ? Pt2 P1 C111 C113 -160.3(3) . . . . ? Pt1 P1 C111 C113 88.8(3) . . . . ? C121 P1 C111 C114 85.2(3) . . . . ? Pt2 P1 C111 C114 -37.1(3) . . . . ? Pt1 P1 C111 C114 -148.0(3) . . . . ? C121 P1 C111 C112 -155.8(3) . . . . ? Pt2 P1 C111 C112 81.9(3) . . . . ? Pt1 P1 C111 C112 -29.0(3) . . . . ? C111 P1 C121 C123 70.0(4) . . . . ? Pt2 P1 C121 C123 -167.9(3) . . . . ? Pt1 P1 C121 C123 -58.1(4) . . . . ? C111 P1 C121 C122 -173.2(3) . . . . ? Pt2 P1 C121 C122 -51.1(3) . . . . ? Pt1 P1 C121 C122 58.7(3) . . . . ? C111 P1 C121 C124 -54.4(4) . . . . ? Pt2 P1 C121 C124 67.6(3) . . . . ? Pt1 P1 C121 C124 177.4(3) . . . . ? C221 P2 C211 C212 170.6(3) . . . . ? Pt1 P2 C211 C212 -52.0(3) . . . . ? C221 P2 C211 C214 -70.9(4) . . . . ? Pt1 P2 C211 C214 66.5(3) . . . . ? C221 P2 C211 C213 54.0(4) . . . . ? Pt1 P2 C211 C213 -168.7(3) . . . . ? C211 P2 C221 C223 45.8(4) . . . . ? Pt1 P2 C221 C223 -91.1(3) . . . . ? C211 P2 C221 C224 -77.9(4) . . . . ? Pt1 P2 C221 C224 145.2(3) . . . . ? C211 P2 C221 C222 164.7(3) . . . . ? Pt1 P2 C221 C222 27.8(3) . . . . ? C4S C1S C3S O1S -29.2(19) . . . . ? C4S C1S C3S C2S -12.7(11) . . . . ? C4S C2S C3S O1S 167(4) . . . . ? O1S C2S C3S C1S -152(3) . . . . ? C4S C2S C3S C1S 14.7(14) . . . . ? O1S C2S C4S C1S -5(3) . . . . ? C3S C2S C4S C1S -13.2(12) . . . . ? C3S C1S C4S C2S 19.2(19) . . . . ? C1S C3S O1S C2S 28(3) . . . . ? C4S C2S O1S C3S -15(4) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.154 _refine_diff_density_min -0.951 _refine_diff_density_rms 0.108 #===END data_albi17 _database_code_depnum_ccdc_archive 'CCDC 254341' _audit_creation_method SHELXL-97 _chemical_formula_moiety 4[PF6].TME _chemical_name_common ;(Pt2(mu–kappaP:eta2- P(tBu)2–CC–Ph)(mu,eta2–C(Ph)CH2)(CO)(P(tBu)2H))(PF6) ; _chemical_formula_sum 'C37 H59 F6 O3 P3 Pt2' _chemical_formula_weight 1148.93 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 16.7547(1) _cell_length_b 20.0887(1) _cell_length_c 25.9733(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8742.1(1) _cell_formula_units_Z 8 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 9680 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 25.4 _exptl_crystal_description prismatic _exptl_crystal_colour 'ligth orange' _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.746 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4480 _exptl_absorpt_coefficient_mu 6.561 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.35 _exptl_absorpt_correction_T_max 0.46 _diffrn_special_details ; 2450 frames were collected on a Brucker SMART CCD diffractometer with a sample to detector distance of 50.0 mm. The counting time per frame was 20 sec and the scan width per frame 0.3 deg. ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 86396 _diffrn_reflns_av_R_equivalents 0.0518 _diffrn_reflns_av_sigmaI/netI 0.0261 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 27.45 _reflns_number_total 9947 _reflns_number_gt 7783 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'SAINT and SADABS' _computing_structure_solution 'SHELXS-97 (Sheldrick,1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP for Windows 1.074(Farrugia 1997)' _computing_publication_material 'WinGX 1.64.05 (L.J. Farruggia, 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^ > 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^)+(0.0259P)^2^+18.4667P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00016(1) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9947 _refine_ls_number_parameters 462 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0446 _refine_ls_R_factor_gt 0.0258 _refine_ls_wR_factor_ref 0.0632 _refine_ls_wR_factor_gt 0.0548 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0.045 _refine_ls_shift/su_mean 0.002 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 0.679525(10) 0.032654(7) 0.353548(6) 0.02506(5) Uani 1 1 d . . . Pt2 Pt 0.536190(9) 0.011945(8) 0.391411(6) 0.02609(5) Uani 1 1 d . . . P1 P 0.55103(6) 0.12494(5) 0.39693(4) 0.0275(2) Uani 1 1 d . . . P2 P 0.77908(7) 0.00993(6) 0.29598(5) 0.0315(2) Uani 1 1 d . . . HP2 H 0.8348 0.0598 0.2904 0.046(14) Uiso 1 1 d . . . C1 C 0.4297(3) -0.0021(2) 0.41368(17) 0.0317(10) Uani 1 1 d . . . O1 O 0.3666(2) -0.01002(18) 0.42791(14) 0.0471(8) Uani 1 1 d . . . C2 C 0.5677(3) -0.0847(2) 0.35464(18) 0.0340(10) Uani 1 1 d . . . H2A H 0.5469 -0.1253 0.3716 0.044 Uiso 1 1 calc R . . H2B H 0.5645 -0.0863 0.3166 0.044 Uiso 1 1 calc R . . C3 C 0.6372(3) -0.0573(2) 0.37547(16) 0.0283(9) Uani 1 1 d . . . C4 C 0.6756(3) -0.0933(2) 0.41972(17) 0.0317(9) Uani 1 1 d . . . C5 C 0.7088(3) -0.0595(3) 0.46138(19) 0.0423(11) Uani 1 1 d . . . H5 H 0.7080 -0.0123 0.4620 0.055 Uiso 1 1 calc R . . C6 C 0.7427(3) -0.0941(3) 0.5017(2) 0.0549(15) Uani 1 1 d . . . H6 H 0.7640 -0.0704 0.5302 0.071 Uiso 1 1 calc R . . C7 C 0.7460(4) -0.1623(3) 0.5013(2) 0.0596(16) Uani 1 1 d . . . H7 H 0.7699 -0.1856 0.5292 0.077 Uiso 1 1 calc R . . C8 C 0.7145(3) -0.1970(3) 0.4601(2) 0.0566(15) Uani 1 1 d . . . H8 H 0.7171 -0.2443 0.4594 0.074 Uiso 1 1 calc R . . C9 C 0.6791(3) -0.1628(2) 0.4195(2) 0.0426(11) Uani 1 1 d . . . H9 H 0.6570 -0.1869 0.3914 0.055 Uiso 1 1 calc R . . C10 C 0.6446(3) 0.1364(2) 0.36755(16) 0.0282(9) Uani 1 1 d . . . C11 C 0.7123(3) 0.1394(2) 0.34913(16) 0.0284(9) Uani 1 1 d . . . C12 C 0.7834(3) 0.1758(2) 0.33206(17) 0.0294(9) Uani 1 1 d . . . C13 C 0.7788(3) 0.2212(2) 0.29162(18) 0.0341(10) Uani 1 1 d . . . H13 H 0.7296 0.2285 0.2744 0.044 Uiso 1 1 calc R . . C14 C 0.8469(3) 0.2556(2) 0.27670(19) 0.0391(11) Uani 1 1 d . . . H14 H 0.8442 0.2861 0.2488 0.051 Uiso 1 1 calc R . . C15 C 0.9185(3) 0.2460(2) 0.3021(2) 0.0421(12) Uani 1 1 d . . . H15 H 0.9645 0.2704 0.2921 0.055 Uiso 1 1 calc R . . C16 C 0.9230(3) 0.2007(2) 0.3419(2) 0.0437(12) Uani 1 1 d . . . H16 H 0.9722 0.1945 0.3595 0.057 Uiso 1 1 calc R . . C17 C 0.8568(3) 0.1643(2) 0.35671(19) 0.0394(11) Uani 1 1 d . . . H17 H 0.8609 0.1319 0.3832 0.051 Uiso 1 1 calc R . . C111 C 0.5622(3) 0.1595(2) 0.46341(18) 0.0361(10) Uani 1 1 d . . . C112 C 0.6400(3) 0.1310(3) 0.48501(19) 0.0473(13) Uani 1 1 d . . . H11A H 0.6373 0.0822 0.4849 0.062 Uiso 1 1 calc R . . H11B H 0.6476 0.1468 0.5204 0.062 Uiso 1 1 calc R . . H11C H 0.6848 0.1456 0.4636 0.062 Uiso 1 1 calc R . . C113 C 0.4927(3) 0.1350(3) 0.4967(2) 0.0595(16) Uani 1 1 d . . . H11D H 0.4905 0.0862 0.4956 0.077 Uiso 1 1 calc R . . H11E H 0.4425 0.1533 0.4835 0.077 Uiso 1 1 calc R . . H11F H 0.5006 0.1496 0.5323 0.077 Uiso 1 1 calc R . . C114 C 0.5676(4) 0.2355(3) 0.4643(2) 0.0570(15) Uani 1 1 d . . . H11G H 0.6121 0.2500 0.4426 0.074 Uiso 1 1 calc R . . H11H H 0.5764 0.2506 0.4998 0.074 Uiso 1 1 calc R . . H11I H 0.5177 0.2545 0.4513 0.074 Uiso 1 1 calc R . . C121 C 0.4809(3) 0.1700(2) 0.3531(2) 0.0380(11) Uani 1 1 d . . . C122 C 0.4787(3) 0.1297(3) 0.3029(2) 0.0480(13) Uani 1 1 d . . . H12A H 0.4593 0.0846 0.3101 0.062 Uiso 1 1 calc R . . H12B H 0.5325 0.1273 0.2883 0.062 Uiso 1 1 calc R . . H12C H 0.4429 0.1515 0.2783 0.062 Uiso 1 1 calc R . . C123 C 0.3971(3) 0.1725(3) 0.3769(2) 0.0515(14) Uani 1 1 d . . . H12D H 0.3790 0.1271 0.3844 0.067 Uiso 1 1 calc R . . H12E H 0.3601 0.1936 0.3527 0.067 Uiso 1 1 calc R . . H12F H 0.3988 0.1983 0.4089 0.067 Uiso 1 1 calc R . . C124 C 0.5101(3) 0.2407(2) 0.3404(2) 0.0502(14) Uani 1 1 d . . . H12G H 0.5114 0.2674 0.3719 0.065 Uiso 1 1 calc R . . H12H H 0.4737 0.2613 0.3155 0.065 Uiso 1 1 calc R . . H12I H 0.5638 0.2384 0.3256 0.065 Uiso 1 1 calc R . . C211 C 0.7340(3) 0.0044(2) 0.23028(18) 0.0392(11) Uani 1 1 d . . . C212 C 0.7019(4) 0.0736(3) 0.2191(2) 0.073(2) Uani 1 1 d . . . H21C H 0.7459 0.1058 0.2200 0.095 Uiso 1 1 calc R . . H21D H 0.6620 0.0855 0.2451 0.095 Uiso 1 1 calc R . . H21E H 0.6772 0.0741 0.1849 0.095 Uiso 1 1 calc R . . C213 C 0.6664(4) -0.0463(3) 0.2287(2) 0.0623(17) Uani 1 1 d . . . H21F H 0.6877 -0.0907 0.2364 0.081 Uiso 1 1 calc R . . H21G H 0.6423 -0.0465 0.1943 0.081 Uiso 1 1 calc R . . H21H H 0.6259 -0.0345 0.2543 0.081 Uiso 1 1 calc R . . C214 C 0.7956(4) -0.0136(3) 0.1885(2) 0.0652(17) Uani 1 1 d . . . H21I H 0.8393 0.0187 0.1891 0.085 Uiso 1 1 calc R . . H21J H 0.7698 -0.0128 0.1546 0.085 Uiso 1 1 calc R . . H21K H 0.8167 -0.0583 0.1952 0.085 Uiso 1 1 calc R . . C221 C 0.8529(3) -0.0558(2) 0.3128(2) 0.0419(11) Uani 1 1 d . . . C222 C 0.8152(3) -0.1255(2) 0.3079(2) 0.0524(14) Uani 1 1 d . . . H22A H 0.7666 -0.1275 0.3289 0.068 Uiso 1 1 calc R . . H22B H 0.8532 -0.1591 0.3199 0.068 Uiso 1 1 calc R . . H22C H 0.8017 -0.1340 0.2718 0.068 Uiso 1 1 calc R . . C223 C 0.9291(3) -0.0509(3) 0.2804(3) 0.0647(17) Uani 1 1 d . . . H22D H 0.9522 -0.0063 0.2840 0.084 Uiso 1 1 calc R . . H22E H 0.9162 -0.0591 0.2441 0.084 Uiso 1 1 calc R . . H22F H 0.9678 -0.0842 0.2922 0.084 Uiso 1 1 calc R . . C224 C 0.8761(3) -0.0434(3) 0.3693(2) 0.0577(15) Uani 1 1 d . . . H22G H 0.8284 -0.0464 0.3910 0.075 Uiso 1 1 calc R . . H22H H 0.8996 0.0011 0.3727 0.075 Uiso 1 1 calc R . . H22I H 0.9150 -0.0770 0.3803 0.075 Uiso 1 1 calc R . . P3 P 0.34495(8) -0.21996(7) 0.35428(5) 0.0437(3) Uani 1 1 d . . . F1 F 0.4197(2) -0.2336(3) 0.39010(16) 0.1147(19) Uani 1 1 d . . . F2 F 0.3740(3) -0.2787(3) 0.3195(2) 0.134(2) Uani 1 1 d . . . F3 F 0.2717(2) -0.2039(2) 0.31857(15) 0.0894(13) Uani 1 1 d . . . F4 F 0.3253(4) -0.1549(3) 0.3839(2) 0.157(3) Uani 1 1 d . . . F5 F 0.3992(3) -0.1762(3) 0.3174(3) 0.141(2) Uani 1 1 d . . . F6 F 0.2935(3) -0.2592(5) 0.3898(3) 0.244(5) Uani 1 1 d . . . O1S O 0.9915(3) 0.0789(3) 0.43243(18) 0.0788(14) Uani 1 1 d . . . O2S O 0.9316(3) 0.1240(3) 0.5587(2) 0.0994(17) Uani 1 1 d . . . C1S C 1.0613(4) 0.0672(4) 0.4046(3) 0.085(2) Uani 1 1 d . . . H1S1 H 1.0476 0.0556 0.3690 0.110 Uiso 1 1 calc R . . H1S2 H 1.0909 0.0304 0.4204 0.110 Uiso 1 1 calc R . . H1S3 H 1.0944 0.1074 0.4047 0.110 Uiso 1 1 calc R . . C2S C 1.0042(4) 0.0965(3) 0.4835(3) 0.0711(19) Uani 1 1 d . . . H2S1 H 1.0386 0.1365 0.4856 0.092 Uiso 1 1 calc R . . H2S2 H 1.0307 0.0597 0.5022 0.092 Uiso 1 1 calc R . . C3S C 0.9236(4) 0.1106(4) 0.5067(3) 0.080(2) Uani 1 1 d . . . H3S1 H 0.8990 0.1493 0.4892 0.104 Uiso 1 1 calc R . . H3S2 H 0.8882 0.0717 0.5018 0.104 Uiso 1 1 calc R . . C4S C 0.8558(5) 0.1359(5) 0.5823(4) 0.111(3) Uani 1 1 d . . . H4S1 H 0.8634 0.1446 0.6191 0.145 Uiso 1 1 calc R . . H4S2 H 0.8217 0.0966 0.5779 0.145 Uiso 1 1 calc R . . H4S3 H 0.8304 0.1745 0.5661 0.145 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 0.02738(8) 0.02259(8) 0.02521(8) -0.00053(6) 0.00062(6) -0.00141(6) Pt2 0.02713(8) 0.02450(8) 0.02664(8) 0.00150(6) -0.00075(7) -0.00224(6) P1 0.0275(6) 0.0260(5) 0.0291(6) -0.0003(4) 0.0004(4) -0.0004(4) P2 0.0319(6) 0.0279(6) 0.0348(6) -0.0044(5) 0.0067(5) -0.0039(5) C1 0.032(2) 0.034(3) 0.029(2) 0.0029(18) -0.0046(19) -0.0023(18) O1 0.0339(18) 0.058(2) 0.049(2) 0.0072(17) 0.0053(16) -0.0085(16) C2 0.039(2) 0.028(2) 0.035(2) -0.0054(19) 0.006(2) -0.0044(19) C3 0.035(2) 0.026(2) 0.024(2) -0.0021(17) 0.0060(18) 0.0009(17) C4 0.035(2) 0.031(2) 0.029(2) 0.0039(17) 0.0040(19) 0.0025(19) C5 0.043(3) 0.043(3) 0.040(3) 0.001(2) -0.003(2) 0.011(2) C6 0.048(3) 0.077(4) 0.040(3) 0.002(3) -0.007(3) 0.017(3) C7 0.053(3) 0.072(4) 0.054(4) 0.027(3) 0.002(3) 0.026(3) C8 0.052(3) 0.043(3) 0.075(4) 0.019(3) 0.010(3) 0.014(3) C9 0.047(3) 0.035(3) 0.046(3) 0.006(2) 0.005(2) 0.002(2) C10 0.032(2) 0.024(2) 0.029(2) -0.0008(17) -0.0018(18) -0.0002(17) C11 0.035(2) 0.025(2) 0.026(2) -0.0012(16) -0.0046(18) -0.0026(17) C12 0.031(2) 0.023(2) 0.033(2) -0.0057(17) 0.0032(19) -0.0024(17) C13 0.034(2) 0.025(2) 0.043(3) -0.0021(19) 0.005(2) 0.0039(18) C14 0.046(3) 0.027(2) 0.045(3) 0.0016(19) 0.011(2) -0.002(2) C15 0.037(3) 0.037(3) 0.052(3) -0.012(2) 0.011(2) -0.015(2) C16 0.031(2) 0.042(3) 0.058(3) -0.011(2) -0.002(2) -0.009(2) C17 0.038(3) 0.034(3) 0.046(3) -0.001(2) -0.006(2) -0.004(2) C111 0.040(3) 0.035(2) 0.033(2) -0.0089(19) 0.003(2) -0.001(2) C112 0.060(3) 0.050(3) 0.032(3) -0.005(2) -0.007(2) 0.005(3) C113 0.057(4) 0.083(5) 0.039(3) -0.012(3) 0.016(3) -0.011(3) C114 0.078(4) 0.040(3) 0.052(3) -0.014(3) -0.015(3) 0.007(3) C121 0.032(2) 0.033(2) 0.049(3) 0.007(2) -0.007(2) 0.0005(18) C122 0.056(3) 0.043(3) 0.045(3) 0.007(2) -0.021(3) -0.001(2) C123 0.032(3) 0.051(3) 0.072(4) 0.010(3) -0.001(3) 0.009(2) C124 0.052(3) 0.034(3) 0.064(4) 0.015(2) -0.012(3) -0.001(2) C211 0.047(3) 0.041(3) 0.030(2) -0.003(2) 0.009(2) -0.002(2) C212 0.111(6) 0.068(4) 0.040(3) -0.003(3) -0.014(3) 0.020(4) C213 0.059(4) 0.087(5) 0.041(3) -0.002(3) -0.005(3) -0.026(3) C214 0.068(4) 0.084(5) 0.043(3) -0.012(3) 0.020(3) -0.013(3) C221 0.031(2) 0.042(3) 0.053(3) -0.004(2) 0.002(2) 0.003(2) C222 0.054(3) 0.036(3) 0.067(4) -0.004(3) 0.011(3) 0.008(2) C223 0.040(3) 0.069(4) 0.085(5) 0.000(3) 0.023(3) 0.009(3) C224 0.039(3) 0.062(4) 0.072(4) -0.006(3) -0.011(3) 0.008(3) P3 0.0408(7) 0.0525(8) 0.0380(7) -0.0007(6) -0.0039(6) 0.0067(6) F1 0.075(3) 0.199(5) 0.070(3) -0.027(3) -0.031(2) 0.067(3) F2 0.125(4) 0.120(4) 0.157(5) -0.079(4) -0.041(4) 0.037(3) F3 0.064(2) 0.128(4) 0.076(3) 0.004(2) -0.030(2) 0.012(2) F4 0.162(5) 0.184(6) 0.126(4) -0.095(4) -0.066(4) 0.098(5) F5 0.086(3) 0.146(5) 0.191(6) 0.078(4) 0.029(4) 0.012(3) F6 0.067(3) 0.364(11) 0.300(9) 0.282(9) 0.022(4) -0.009(5) O1S 0.054(3) 0.111(4) 0.071(3) -0.021(3) -0.001(2) 0.002(3) O2S 0.088(4) 0.112(4) 0.098(4) -0.017(3) 0.020(3) -0.008(3) C1S 0.064(4) 0.101(6) 0.089(5) -0.019(5) 0.007(4) 0.004(4) C2S 0.068(4) 0.062(4) 0.083(5) -0.017(4) -0.002(4) -0.007(3) C3S 0.073(5) 0.097(6) 0.070(5) -0.016(4) 0.007(4) 0.003(4) C4S 0.104(7) 0.107(7) 0.123(8) -0.015(6) 0.061(6) 0.000(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 Pt1 C3 2.023(4) . ? Pt1 C10 2.195(4) . ? Pt1 C11 2.216(4) . ? Pt1 P2 2.2861(11) . ? Pt1 Pt2 2.6282(2) . ? Pt2 C1 1.896(5) . ? Pt2 C2 2.227(4) . ? Pt2 C3 2.230(4) . ? Pt2 P1 2.2880(11) . ? P1 C10 1.759(4) . ? P1 C121 1.870(5) . ? P1 C111 1.870(5) . ? P2 C221 1.862(5) . ? P2 C211 1.870(5) . ? C1 O1 1.132(5) . ? C2 C3 1.398(6) . ? C3 C4 1.503(6) . ? C4 C5 1.393(7) . ? C4 C9 1.397(6) . ? C5 C6 1.379(7) . ? C6 C7 1.371(8) . ? C7 C8 1.383(9) . ? C8 C9 1.391(7) . ? C10 C11 1.232(6) . ? C11 C12 1.468(6) . ? C12 C13 1.392(6) . ? C12 C17 1.406(6) . ? C13 C14 1.390(6) . ? C14 C15 1.383(7) . ? C15 C16 1.380(7) . ? C16 C17 1.384(7) . ? C111 C112 1.531(7) . ? C111 C114 1.530(7) . ? C111 C113 1.531(7) . ? C121 C122 1.534(7) . ? C121 C123 1.534(7) . ? C121 C124 1.538(7) . ? C211 C212 1.517(8) . ? C211 C213 1.524(7) . ? C211 C214 1.541(7) . ? C221 C223 1.533(7) . ? C221 C224 1.538(8) . ? C221 C222 1.541(7) . ? P3 F6 1.488(5) . ? P3 F4 1.551(5) . ? P3 F2 1.564(5) . ? P3 F3 1.572(4) . ? P3 F1 1.584(4) . ? P3 F5 1.587(5) . ? O1S C2S 1.390(7) . ? O1S C1S 1.395(8) . ? O2S C3S 1.383(8) . ? O2S C4S 1.429(9) . ? C2S C3S 1.505(9) . ? 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 C3 Pt1 C10 135.09(16) . . ? C3 Pt1 C11 164.93(16) . . ? C10 Pt1 C11 32.43(16) . . ? C3 Pt1 P2 105.14(12) . . ? C10 Pt1 P2 119.51(12) . . ? C11 Pt1 P2 88.78(12) . . ? C3 Pt1 Pt2 55.47(12) . . ? C10 Pt1 Pt2 81.06(11) . . ? C11 Pt1 Pt2 113.49(12) . . ? P2 Pt1 Pt2 151.62(3) . . ? C1 Pt2 C2 102.95(18) . . ? C1 Pt2 C3 132.69(17) . . ? C2 Pt2 C3 36.55(16) . . ? C1 Pt2 P1 103.32(14) . . ? C2 Pt2 P1 150.00(12) . . ? C3 Pt2 P1 123.25(11) . . ? C1 Pt2 Pt1 175.71(13) . . ? C2 Pt2 Pt1 76.18(11) . . ? C3 Pt2 Pt1 48.37(11) . . ? P1 Pt2 Pt1 76.53(3) . . ? C10 P1 C121 103.5(2) . . ? C10 P1 C111 105.3(2) . . ? C121 P1 C111 116.5(2) . . ? C10 P1 Pt2 101.52(14) . . ? C121 P1 Pt2 111.93(15) . . ? C111 P1 Pt2 115.89(15) . . ? C221 P2 C211 116.2(2) . . ? C221 P2 Pt1 118.23(17) . . ? C211 P2 Pt1 108.28(16) . . ? O1 C1 Pt2 178.6(4) . . ? C3 C2 Pt2 71.9(2) . . ? C2 C3 C4 117.7(4) . . ? C2 C3 Pt1 122.3(3) . . ? C4 C3 Pt1 119.7(3) . . ? C2 C3 Pt2 71.6(2) . . ? C4 C3 Pt2 118.9(3) . . ? Pt1 C3 Pt2 76.16(14) . . ? C5 C4 C9 118.3(4) . . ? C5 C4 C3 122.0(4) . . ? C9 C4 C3 119.7(4) . . ? C6 C5 C4 120.6(5) . . ? C7 C6 C5 121.0(6) . . ? C6 C7 C8 119.6(5) . . ? C7 C8 C9 120.0(5) . . ? C8 C9 C4 120.6(5) . . ? C11 C10 P1 174.3(4) . . ? C11 C10 Pt1 74.7(3) . . ? P1 C10 Pt1 100.67(19) . . ? C10 C11 C12 152.8(4) . . ? C10 C11 Pt1 72.9(3) . . ? C12 C11 Pt1 134.4(3) . . ? C13 C12 C17 120.0(4) . . ? C13 C12 C11 120.6(4) . . ? C17 C12 C11 119.4(4) . . ? C14 C13 C12 119.4(4) . . ? C15 C14 C13 120.7(4) . . ? C16 C15 C14 119.8(4) . . ? C15 C16 C17 120.9(5) . . ? C16 C17 C12 119.2(5) . . ? C112 C111 C114 108.5(4) . . ? C112 C111 C113 108.7(4) . . ? C114 C111 C113 110.9(4) . . ? C112 C111 P1 106.5(3) . . ? C114 C111 P1 113.0(4) . . ? C113 C111 P1 109.0(3) . . ? C122 C121 C123 109.8(4) . . ? C122 C121 C124 108.2(4) . . ? C123 C121 C124 110.3(4) . . ? C122 C121 P1 106.1(3) . . ? C123 C121 P1 110.2(3) . . ? C124 C121 P1 112.2(3) . . ? C212 C211 C213 110.2(5) . . ? C212 C211 C214 108.5(5) . . ? C213 C211 C214 108.7(4) . . ? C212 C211 P2 105.3(3) . . ? C213 C211 P2 111.4(3) . . ? C214 C211 P2 112.7(4) . . ? C223 C221 C224 107.7(5) . . ? C223 C221 C222 110.8(4) . . ? C224 C221 C222 109.2(5) . . ? C223 C221 P2 112.3(4) . . ? C224 C221 P2 106.1(3) . . ? C222 C221 P2 110.6(3) . . ? F6 P3 F4 90.9(5) . . ? F6 P3 F2 98.0(5) . . ? F4 P3 F2 171.1(4) . . ? F6 P3 F3 91.3(3) . . ? F4 P3 F3 87.4(3) . . ? F2 P3 F3 93.2(3) . . ? F6 P3 F1 90.1(3) . . ? F4 P3 F1 91.3(3) . . ? F2 P3 F1 87.9(3) . . ? F3 P3 F1 178.1(3) . . ? F6 P3 F5 178.2(5) . . ? F4 P3 F5 87.3(4) . . ? F2 P3 F5 83.8(3) . . ? F3 P3 F5 88.7(3) . . ? F1 P3 F5 89.9(3) . . ? C2S O1S C1S 114.2(5) . . ? C3S O2S C4S 111.4(7) . . ? O1S C2S C3S 107.0(6) . . ? O2S C3S C2S 109.9(6) . . ? 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 C3 Pt1 Pt2 C1 -106.2(18) . . . . ? C10 Pt1 Pt2 C1 85.8(18) . . . . ? C11 Pt1 Pt2 C1 85.6(18) . . . . ? P2 Pt1 Pt2 C1 -53.5(18) . . . . ? C3 Pt1 Pt2 C2 -27.36(19) . . . . ? C10 Pt1 Pt2 C2 164.58(17) . . . . ? C11 Pt1 Pt2 C2 164.42(17) . . . . ? P2 Pt1 Pt2 C2 25.31(14) . . . . ? C10 Pt1 Pt2 C3 -168.06(18) . . . . ? C11 Pt1 Pt2 C3 -168.22(18) . . . . ? P2 Pt1 Pt2 C3 52.67(16) . . . . ? C3 Pt1 Pt2 P1 165.24(15) . . . . ? C10 Pt1 Pt2 P1 -2.82(11) . . . . ? C11 Pt1 Pt2 P1 -2.98(12) . . . . ? P2 Pt1 Pt2 P1 -142.09(7) . . . . ? C1 Pt2 P1 C10 -172.0(2) . . . . ? C2 Pt2 P1 C10 -21.5(3) . . . . ? C3 Pt2 P1 C10 16.7(2) . . . . ? Pt1 Pt2 P1 C10 3.55(14) . . . . ? C1 Pt2 P1 C121 -62.3(2) . . . . ? C2 Pt2 P1 C121 88.3(3) . . . . ? C3 Pt2 P1 C121 126.5(2) . . . . ? Pt1 Pt2 P1 C121 113.31(17) . . . . ? C1 Pt2 P1 C111 74.5(2) . . . . ? C2 Pt2 P1 C111 -134.9(3) . . . . ? C3 Pt2 P1 C111 -96.7(2) . . . . ? Pt1 Pt2 P1 C111 -109.87(17) . . . . ? C3 Pt1 P2 C221 -46.1(2) . . . . ? C10 Pt1 P2 C221 139.0(2) . . . . ? C11 Pt1 P2 C221 128.1(2) . . . . ? Pt2 Pt1 P2 C221 -88.79(19) . . . . ? C3 Pt1 P2 C211 88.8(2) . . . . ? C10 Pt1 P2 C211 -86.2(2) . . . . ? C11 Pt1 P2 C211 -97.0(2) . . . . ? Pt2 Pt1 P2 C211 46.05(19) . . . . ? C2 Pt2 C1 O1 129(19) . . . . ? C3 Pt2 C1 O1 104(19) . . . . ? P1 Pt2 C1 O1 -66(19) . . . . ? Pt1 Pt2 C1 O1 -154(17) . . . . ? C1 Pt2 C2 C3 -149.1(3) . . . . ? P1 Pt2 C2 C3 60.3(4) . . . . ? Pt1 Pt2 C2 C3 35.2(2) . . . . ? Pt2 C2 C3 C4 113.6(4) . . . . ? Pt2 C2 C3 Pt1 -59.4(3) . . . . ? C10 Pt1 C3 C2 74.1(4) . . . . ? C11 Pt1 C3 C2 103.3(7) . . . . ? P2 Pt1 C3 C2 -99.7(3) . . . . ? Pt2 Pt1 C3 C2 57.3(3) . . . . ? C10 Pt1 C3 C4 -98.8(4) . . . . ? C11 Pt1 C3 C4 -69.6(8) . . . . ? P2 Pt1 C3 C4 87.4(3) . . . . ? Pt2 Pt1 C3 C4 -115.6(3) . . . . ? C10 Pt1 C3 Pt2 16.8(3) . . . . ? C11 Pt1 C3 Pt2 46.1(7) . . . . ? P2 Pt1 C3 Pt2 -156.95(6) . . . . ? C1 Pt2 C3 C2 42.9(4) . . . . ? P1 Pt2 C3 C2 -148.7(2) . . . . ? Pt1 Pt2 C3 C2 -131.5(3) . . . . ? C1 Pt2 C3 C4 -69.1(4) . . . . ? C2 Pt2 C3 C4 -112.0(4) . . . . ? P1 Pt2 C3 C4 99.3(3) . . . . ? Pt1 Pt2 C3 C4 116.5(4) . . . . ? C1 Pt2 C3 Pt1 174.39(18) . . . . ? C2 Pt2 C3 Pt1 131.5(3) . . . . ? P1 Pt2 C3 Pt1 -17.24(17) . . . . ? C2 C3 C4 C5 -140.4(5) . . . . ? Pt1 C3 C4 C5 32.8(6) . . . . ? Pt2 C3 C4 C5 -57.2(5) . . . . ? C2 C3 C4 C9 39.9(6) . . . . ? Pt1 C3 C4 C9 -146.8(4) . . . . ? Pt2 C3 C4 C9 123.2(4) . . . . ? C9 C4 C5 C6 -1.2(7) . . . . ? C3 C4 C5 C6 179.2(5) . . . . ? C4 C5 C6 C7 1.3(8) . . . . ? C5 C6 C7 C8 -0.4(9) . . . . ? C6 C7 C8 C9 -0.5(9) . . . . ? C7 C8 C9 C4 0.6(8) . . . . ? C5 C4 C9 C8 0.2(7) . . . . ? C3 C4 C9 C8 179.9(4) . . . . ? C121 P1 C10 C11 -155(4) . . . . ? C111 P1 C10 C11 82(4) . . . . ? Pt2 P1 C10 C11 -39(4) . . . . ? C121 P1 C10 Pt1 -120.4(2) . . . . ? C111 P1 C10 Pt1 117.0(2) . . . . ? Pt2 P1 C10 Pt1 -4.21(17) . . . . ? C3 Pt1 C10 C11 166.3(3) . . . . ? P2 Pt1 C10 C11 -20.6(3) . . . . ? Pt2 Pt1 C10 C11 -179.7(3) . . . . ? C3 Pt1 C10 P1 -10.3(3) . . . . ? C11 Pt1 C10 P1 -176.6(4) . . . . ? P2 Pt1 C10 P1 162.76(11) . . . . ? Pt2 Pt1 C10 P1 3.63(15) . . . . ? P1 C10 C11 C12 -143(4) . . . . ? Pt1 C10 C11 C12 -178.2(9) . . . . ? P1 C10 C11 Pt1 36(4) . . . . ? C3 Pt1 C11 C10 -40.0(8) . . . . ? P2 Pt1 C11 C10 162.2(3) . . . . ? Pt2 Pt1 C11 C10 0.3(3) . . . . ? C3 Pt1 C11 C12 138.9(6) . . . . ? C10 Pt1 C11 C12 178.9(6) . . . . ? P2 Pt1 C11 C12 -19.0(4) . . . . ? Pt2 Pt1 C11 C12 179.2(4) . . . . ? C10 C11 C12 C13 -63.0(11) . . . . ? Pt1 C11 C12 C13 119.4(4) . . . . ? C10 C11 C12 C17 117.4(9) . . . . ? Pt1 C11 C12 C17 -60.2(6) . . . . ? C17 C12 C13 C14 -1.2(6) . . . . ? C11 C12 C13 C14 179.2(4) . . . . ? C12 C13 C14 C15 -1.0(7) . . . . ? C13 C14 C15 C16 1.3(7) . . . . ? C14 C15 C16 C17 0.5(7) . . . . ? C15 C16 C17 C12 -2.7(7) . . . . ? C13 C12 C17 C16 3.0(7) . . . . ? C11 C12 C17 C16 -177.4(4) . . . . ? C10 P1 C111 C112 -47.4(4) . . . . ? C121 P1 C111 C112 -161.3(3) . . . . ? Pt2 P1 C111 C112 63.9(4) . . . . ? C10 P1 C111 C114 71.7(4) . . . . ? C121 P1 C111 C114 -42.2(4) . . . . ? Pt2 P1 C111 C114 -177.1(3) . . . . ? C10 P1 C111 C113 -164.5(4) . . . . ? C121 P1 C111 C113 81.6(4) . . . . ? Pt2 P1 C111 C113 -53.3(4) . . . . ? C10 P1 C121 C122 68.5(4) . . . . ? C111 P1 C121 C122 -176.6(3) . . . . ? Pt2 P1 C121 C122 -40.1(4) . . . . ? C10 P1 C121 C123 -172.8(3) . . . . ? C111 P1 C121 C123 -57.8(4) . . . . ? Pt2 P1 C121 C123 78.7(4) . . . . ? C10 P1 C121 C124 -49.5(4) . . . . ? C111 P1 C121 C124 65.5(4) . . . . ? Pt2 P1 C121 C124 -158.0(3) . . . . ? C221 P2 C211 C212 -159.9(4) . . . . ? Pt1 P2 C211 C212 64.2(4) . . . . ? C221 P2 C211 C213 80.7(4) . . . . ? Pt1 P2 C211 C213 -55.2(4) . . . . ? C221 P2 C211 C214 -41.8(5) . . . . ? Pt1 P2 C211 C214 -177.7(3) . . . . ? C211 P2 C221 C223 66.7(5) . . . . ? Pt1 P2 C221 C223 -162.0(3) . . . . ? C211 P2 C221 C224 -175.9(3) . . . . ? Pt1 P2 C221 C224 -44.5(4) . . . . ? C211 P2 C221 C222 -57.6(4) . . . . ? Pt1 P2 C221 C222 73.8(4) . . . . ? C1S O1S C2S C3S 177.1(6) . . . . ? C4S O2S C3S C2S -178.4(6) . . . . ? O1S C2S C3S O2S 175.9(6) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.250 _refine_diff_density_min -0.826 _refine_diff_density_rms 0.118