# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'R Puddephatt' _publ_contact_author_email PUDD@UWO.CA _publ_section_title ; A Double Cubane Structure in Organoplatinum(IV) Chemistry ; loop_ _publ_author_name 'R Puddephatt' 'Michael C Jennings' 'Muhieddine S. Safa' # Attachment '5.cif' data_07255 _database_code_depnum_ccdc_archive 'CCDC 713894' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H36 O6 Pt4, 2(C15 H18 N2 O3 Pt)' _chemical_formula_sum 'C40 H72 N4 O12 Pt6' _chemical_formula_weight 1971.56 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 11.3138(4) _cell_length_b 13.9347(3) _cell_length_c 16.6656(5) _cell_angle_alpha 90.00 _cell_angle_beta 106.7800(10) _cell_angle_gamma 90.00 _cell_volume 2515.53(13) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 13502 _cell_measurement_theta_min 2.04 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.603 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1808 _exptl_absorpt_coefficient_mu 16.678 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1172 _exptl_absorpt_correction_T_max 0.6805 _exptl_absorpt_process_details 'DENZO-SMN (Otwinowski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD' _diffrn_measurement_method '\f scans, and \w scans with \k offsets' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26920 _diffrn_reflns_av_R_equivalents 0.0770 _diffrn_reflns_av_sigmaI/netI 0.0503 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 25.02 _reflns_number_total 4451 _reflns_number_gt 3807 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'COLLECT (Nonius, 1997-2001)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 2001)' _computing_publication_material SHELXTL/PC _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^)+(0.0540P)^2^] 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 4451 _refine_ls_number_parameters 296 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0460 _refine_ls_R_factor_gt 0.0364 _refine_ls_wR_factor_ref 0.0919 _refine_ls_wR_factor_gt 0.0880 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.002 _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 0.70790(3) -0.17039(2) 0.56670(2) 0.02109(12) Uani 1 1 d . . . C1 C 0.6237(10) -0.0821(6) 0.6311(6) 0.035(2) Uani 1 1 d . . . H1A H 0.6822 -0.0651 0.6851 0.053 Uiso 1 1 calc R . . H1B H 0.5525 -0.1151 0.6407 0.053 Uiso 1 1 calc R . . H1C H 0.5958 -0.0236 0.5984 0.053 Uiso 1 1 calc R . . C2 C 0.6485(10) -0.2910(6) 0.6145(7) 0.040(3) Uani 1 1 d . . . H2A H 0.7199 -0.3256 0.6502 0.060 Uiso 1 1 calc R . . H2B H 0.6038 -0.3327 0.5683 0.060 Uiso 1 1 calc R . . H2C H 0.5936 -0.2723 0.6477 0.060 Uiso 1 1 calc R . . O3 O 0.8718(6) -0.1868(4) 0.6533(3) 0.0280(15) Uani 1 1 d . . . O4 O 0.8461(5) -0.2608(4) 0.5339(3) 0.0224(13) Uani 1 1 d . . . C5 C 0.9224(9) -0.2428(6) 0.6073(5) 0.024(2) Uani 1 1 d . . . O6 O 1.0271(6) -0.2756(4) 0.6328(4) 0.0314(15) Uani 1 1 d . . . N11 N 0.5495(7) -0.1774(5) 0.4710(4) 0.0205(16) Uani 1 1 d . . . C12 C 0.4403(9) -0.1964(6) 0.4877(6) 0.031(2) Uani 1 1 d . . . H12A H 0.4370 -0.1925 0.5439 0.037 Uiso 1 1 calc R . . C13 C 0.3357(10) -0.2209(7) 0.4261(6) 0.038(2) Uani 1 1 d . . . H13A H 0.2622 -0.2372 0.4396 0.045 Uiso 1 1 calc R . . C14 C 0.3389(10) -0.2214(8) 0.3438(6) 0.047(3) Uani 1 1 d . . . H14A H 0.2670 -0.2359 0.2994 0.056 Uiso 1 1 calc R . . C15 C 0.4503(10) -0.2000(7) 0.3274(6) 0.036(2) Uani 1 1 d . . . H15A H 0.4542 -0.2019 0.2713 0.043 Uiso 1 1 calc R . . C16 C 0.5529(8) -0.1767(6) 0.3897(5) 0.023(2) Uani 1 1 d . . . C17 C 0.6680(9) -0.1512(6) 0.3695(6) 0.028(2) Uani 1 1 d . . . H17A H 0.6627 -0.1747 0.3125 0.034 Uiso 1 1 calc R . . H17B H 0.7384 -0.1841 0.4094 0.034 Uiso 1 1 calc R . . C18 C 0.6928(9) -0.0425(6) 0.3734(6) 0.030(2) Uani 1 1 d . . . H18A H 0.7254 -0.0257 0.3261 0.036 Uiso 1 1 calc R . . H18B H 0.6124 -0.0094 0.3636 0.036 Uiso 1 1 calc R . . C19 C 0.7803(8) -0.0013(6) 0.4527(5) 0.022(2) Uani 1 1 d . . . C20 C 0.8468(9) 0.0813(6) 0.4435(6) 0.029(2) Uani 1 1 d . . . H20A H 0.8361 0.1085 0.3896 0.035 Uiso 1 1 calc R . . C21 C 0.9272(10) 0.1223(6) 0.5129(6) 0.032(2) Uani 1 1 d . . . H21A H 0.9737 0.1773 0.5072 0.039 Uiso 1 1 calc R . . C22 C 0.9399(10) 0.0833(7) 0.5904(6) 0.036(3) Uani 1 1 d . . . H22A H 0.9952 0.1107 0.6391 0.044 Uiso 1 1 calc R . . C23 C 0.8708(9) 0.0037(6) 0.5962(5) 0.028(2) Uani 1 1 d . . . H23A H 0.8787 -0.0230 0.6499 0.033 Uiso 1 1 calc R . . N24 N 0.7923(7) -0.0376(4) 0.5285(4) 0.0208(16) Uani 1 1 d . . . Pt1 Pt 0.75279(3) 0.46766(2) 0.39608(2) 0.02253(12) Uani 1 1 d . . . Pt2 Pt 0.96736(3) 0.44670(2) 0.57980(2) 0.01993(12) Uani 1 1 d . . . C31 C 0.6538(9) 0.3672(7) 0.3186(6) 0.035(2) Uani 1 1 d . . . H31A H 0.5658 0.3827 0.3054 0.053 Uiso 1 1 calc R . . H31B H 0.6692 0.3043 0.3459 0.053 Uiso 1 1 calc R . . H31C H 0.6783 0.3658 0.2668 0.053 Uiso 1 1 calc R . . C32 C 0.6700(10) 0.5714(6) 0.3141(6) 0.039(3) Uani 1 1 d . . . H32A H 0.7156 0.5807 0.2728 0.058 Uiso 1 1 calc R . . H32B H 0.6693 0.6315 0.3444 0.058 Uiso 1 1 calc R . . H32C H 0.5850 0.5521 0.2853 0.058 Uiso 1 1 calc R . . C33 C 0.6131(9) 0.4766(7) 0.4497(6) 0.037(3) Uani 1 1 d . . . H33A H 0.5338 0.4748 0.4060 0.056 Uiso 1 1 calc R . . H33B H 0.6201 0.5369 0.4810 0.056 Uiso 1 1 calc R . . H33C H 0.6182 0.4224 0.4880 0.056 Uiso 1 1 calc R . . C34 C 0.8403(9) 0.4671(7) 0.6432(6) 0.033(2) Uani 1 1 d . . . H34A H 0.7861 0.4109 0.6359 0.050 Uiso 1 1 calc R . . H34B H 0.7909 0.5242 0.6214 0.050 Uiso 1 1 calc R . . H34C H 0.8826 0.4761 0.7029 0.050 Uiso 1 1 calc R . . C35 C 1.0326(9) 0.3346(6) 0.6568(5) 0.030(2) Uani 1 1 d . . . H35A H 1.0955 0.3006 0.6378 0.045 Uiso 1 1 calc R . . H35B H 0.9647 0.2906 0.6560 0.045 Uiso 1 1 calc R . . H35C H 1.0694 0.3581 0.7140 0.045 Uiso 1 1 calc R . . O36 O 0.8912(6) 0.5577(4) 0.4858(4) 0.0227(14) Uani 1 1 d D . . H36 H 0.872(8) 0.615(2) 0.493(5) 0.034 Uiso 1 1 d D . . O37 O 0.8489(6) 0.3633(4) 0.4922(4) 0.0255(15) Uani 1 1 d D . . H37 H 0.893(7) 0.326(5) 0.473(6) 0.038 Uiso 1 1 d D . . O38 O 1.0920(6) 0.5323(4) 0.6595(4) 0.0252(14) Uani 1 1 d D . . H38 H 1.067(9) 0.589(3) 0.648(6) 0.038 Uiso 1 1 d 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 Pt 0.0254(2) 0.02193(19) 0.0176(2) -0.00039(13) 0.00886(16) 0.00064(15) C1 0.049(7) 0.034(5) 0.031(5) -0.009(4) 0.024(5) -0.002(5) C2 0.049(7) 0.028(5) 0.052(7) 0.015(5) 0.030(6) 0.009(5) O3 0.039(4) 0.027(3) 0.020(3) 0.001(3) 0.012(3) 0.004(3) O4 0.024(4) 0.019(3) 0.022(3) -0.006(2) 0.003(3) 0.002(3) C5 0.034(6) 0.017(4) 0.020(5) 0.008(4) 0.002(4) -0.007(4) O6 0.032(4) 0.025(3) 0.033(4) 0.007(3) 0.003(3) 0.001(3) N11 0.022(4) 0.022(3) 0.013(3) 0.002(3) -0.001(3) 0.001(3) C12 0.024(6) 0.039(5) 0.036(6) 0.000(5) 0.016(5) 0.006(5) C13 0.025(6) 0.038(5) 0.050(7) 0.007(5) 0.011(5) 0.005(5) C14 0.035(7) 0.065(7) 0.032(6) 0.003(5) -0.003(5) -0.003(6) C15 0.043(7) 0.039(5) 0.024(5) 0.006(4) 0.007(5) 0.000(5) C16 0.025(5) 0.024(4) 0.017(4) -0.009(4) 0.000(4) -0.008(4) C17 0.032(6) 0.031(5) 0.026(5) 0.001(4) 0.016(5) 0.002(4) C18 0.034(6) 0.028(5) 0.027(5) 0.006(4) 0.006(5) 0.000(4) C19 0.021(5) 0.020(4) 0.026(5) -0.002(4) 0.008(4) -0.001(4) C20 0.033(6) 0.030(5) 0.029(5) 0.004(4) 0.016(5) 0.005(4) C21 0.044(7) 0.019(4) 0.038(6) 0.000(4) 0.018(5) -0.009(4) C22 0.051(7) 0.033(5) 0.030(5) -0.009(4) 0.018(5) 0.001(5) C23 0.036(6) 0.022(4) 0.024(5) 0.001(4) 0.004(5) 0.005(4) N24 0.023(4) 0.015(3) 0.023(4) 0.003(3) 0.006(3) 0.005(3) Pt1 0.0219(2) 0.02569(19) 0.0201(2) -0.00241(14) 0.00623(17) 0.00018(14) Pt2 0.0247(2) 0.02010(18) 0.01674(19) 0.00121(13) 0.00884(16) -0.00022(14) C31 0.030(6) 0.045(6) 0.033(5) -0.006(5) 0.011(5) -0.008(5) C32 0.040(7) 0.038(5) 0.035(6) -0.001(5) 0.006(5) 0.006(5) C33 0.026(6) 0.043(6) 0.042(6) -0.017(5) 0.007(5) 0.000(5) C34 0.025(6) 0.050(6) 0.031(5) 0.001(5) 0.020(5) -0.004(5) C35 0.040(6) 0.027(5) 0.025(5) 0.005(4) 0.010(5) -0.002(4) O36 0.027(4) 0.020(3) 0.024(3) 0.002(3) 0.011(3) 0.002(3) O37 0.030(4) 0.025(3) 0.028(3) -0.003(3) 0.018(3) 0.000(3) O38 0.026(4) 0.026(3) 0.027(3) 0.002(3) 0.013(3) 0.001(3) _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 O3 2.008(6) . ? Pt N11 2.028(7) . ? Pt C1 2.041(8) . ? Pt C2 2.054(9) . ? Pt O4 2.197(5) . ? Pt N24 2.256(6) . ? Pt C5 2.533(10) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? O3 C5 1.334(10) . ? O4 C5 1.302(10) . ? C5 O6 1.226(11) . ? N11 C16 1.368(11) . ? N11 C12 1.368(11) . ? C12 C13 1.367(13) . ? C12 H12A 0.9500 . ? C13 C14 1.382(14) . ? C13 H13A 0.9500 . ? C14 C15 1.396(14) . ? C14 H14A 0.9500 . ? C15 C16 1.354(13) . ? C15 H15A 0.9500 . ? C16 C17 1.479(12) . ? C17 C18 1.538(11) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.517(12) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 N24 1.331(10) . ? C19 C20 1.408(12) . ? C20 C21 1.372(13) . ? C20 H20A 0.9500 . ? C21 C22 1.369(13) . ? C21 H21A 0.9500 . ? C22 C23 1.377(13) . ? C22 H22A 0.9500 . ? C23 N24 1.347(11) . ? C23 H23A 0.9500 . ? Pt1 C31 2.011(9) . ? Pt1 C32 2.023(9) . ? Pt1 C33 2.031(9) . ? Pt1 O37 2.204(6) . ? Pt1 O38 2.209(6) 3_766 ? Pt1 O36 2.216(6) . ? Pt2 C35 2.022(8) . ? Pt2 O38 2.024(6) . ? Pt2 C34 2.035(8) . ? Pt2 O37 2.037(6) . ? Pt2 O36 2.184(6) 3_766 ? Pt2 O36 2.193(6) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? O36 Pt2 2.184(6) 3_766 ? O36 H36 0.842(10) . ? O37 H37 0.842(10) . ? O38 Pt1 2.209(6) 3_766 ? O38 H38 0.841(10) . ? 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 O3 Pt N11 169.5(3) . . ? O3 Pt C1 99.5(3) . . ? N11 Pt C1 90.1(3) . . ? O3 Pt C2 88.0(4) . . ? N11 Pt C2 87.2(4) . . ? C1 Pt C2 92.0(4) . . ? O3 Pt O4 62.5(2) . . ? N11 Pt O4 107.9(2) . . ? C1 Pt O4 162.0(3) . . ? C2 Pt O4 87.9(3) . . ? O3 Pt N24 85.3(3) . . ? N11 Pt N24 99.6(3) . . ? C1 Pt N24 87.3(3) . . ? C2 Pt N24 173.1(4) . . ? O4 Pt N24 90.6(2) . . ? O3 Pt C5 31.5(2) . . ? N11 Pt C5 138.7(3) . . ? C1 Pt C5 131.0(3) . . ? C2 Pt C5 88.0(3) . . ? O4 Pt C5 30.9(2) . . ? N24 Pt C5 87.2(3) . . ? Pt C1 H1A 109.5 . . ? Pt C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Pt C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Pt C2 H2A 109.5 . . ? Pt C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Pt C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C5 O3 Pt 96.5(5) . . ? C5 O4 Pt 88.9(5) . . ? O6 C5 O4 124.4(8) . . ? O6 C5 O3 123.4(8) . . ? O4 C5 O3 112.1(8) . . ? O6 C5 Pt 175.3(7) . . ? O4 C5 Pt 60.1(5) . . ? O3 C5 Pt 52.0(4) . . ? C16 N11 C12 119.2(8) . . ? C16 N11 Pt 120.5(6) . . ? C12 N11 Pt 119.7(6) . . ? C13 C12 N11 122.2(9) . . ? C13 C12 H12A 118.9 . . ? N11 C12 H12A 118.9 . . ? C12 C13 C14 118.8(10) . . ? C12 C13 H13A 120.6 . . ? C14 C13 H13A 120.6 . . ? C13 C14 C15 118.4(10) . . ? C13 C14 H14A 120.8 . . ? C15 C14 H14A 120.8 . . ? C16 C15 C14 121.6(9) . . ? C16 C15 H15A 119.2 . . ? C14 C15 H15A 119.2 . . ? C15 C16 N11 119.6(8) . . ? C15 C16 C17 120.0(8) . . ? N11 C16 C17 120.4(8) . . ? C16 C17 C18 112.8(7) . . ? C16 C17 H17A 109.0 . . ? C18 C17 H17A 109.0 . . ? C16 C17 H17B 109.0 . . ? C18 C17 H17B 109.0 . . ? H17A C17 H17B 107.8 . . ? C19 C18 C17 118.3(8) . . ? C19 C18 H18A 107.7 . . ? C17 C18 H18A 107.7 . . ? C19 C18 H18B 107.7 . . ? C17 C18 H18B 107.7 . . ? H18A C18 H18B 107.1 . . ? N24 C19 C20 120.2(8) . . ? N24 C19 C18 123.1(7) . . ? C20 C19 C18 116.7(8) . . ? C21 C20 C19 119.5(8) . . ? C21 C20 H20A 120.2 . . ? C19 C20 H20A 120.2 . . ? C22 C21 C20 119.6(8) . . ? C22 C21 H21A 120.2 . . ? C20 C21 H21A 120.2 . . ? C21 C22 C23 118.6(9) . . ? C21 C22 H22A 120.7 . . ? C23 C22 H22A 120.7 . . ? N24 C23 C22 122.4(8) . . ? N24 C23 H23A 118.8 . . ? C22 C23 H23A 118.8 . . ? C19 N24 C23 119.6(7) . . ? C19 N24 Pt 130.1(6) . . ? C23 N24 Pt 110.2(5) . . ? C31 Pt1 C32 90.0(4) . . ? C31 Pt1 C33 88.0(4) . . ? C32 Pt1 C33 89.2(4) . . ? C31 Pt1 O37 94.2(3) . . ? C32 Pt1 O37 175.7(3) . . ? C33 Pt1 O37 90.2(3) . . ? C31 Pt1 O38 95.3(3) . 3_766 ? C32 Pt1 O38 89.2(3) . 3_766 ? C33 Pt1 O38 176.3(3) . 3_766 ? O37 Pt1 O38 91.1(2) . 3_766 ? C31 Pt1 O36 168.9(3) . . ? C32 Pt1 O36 98.6(3) . . ? C33 Pt1 O36 99.0(3) . . ? O37 Pt1 O36 77.3(2) . . ? O38 Pt1 O36 77.9(2) 3_766 . ? C35 Pt2 O38 88.9(3) . . ? C35 Pt2 C34 87.8(4) . . ? O38 Pt2 C34 92.3(3) . . ? C35 Pt2 O37 93.3(3) . . ? O38 Pt2 O37 175.2(2) . . ? C34 Pt2 O37 92.0(3) . . ? C35 Pt2 O36 96.3(3) . 3_766 ? O38 Pt2 O36 82.7(2) . 3_766 ? C34 Pt2 O36 173.4(3) . 3_766 ? O37 Pt2 O36 92.9(2) . 3_766 ? C35 Pt2 O36 174.2(3) . . ? O38 Pt2 O36 96.2(2) . . ? C34 Pt2 O36 94.7(3) . . ? O37 Pt2 O36 81.3(2) . . ? O36 Pt2 O36 81.7(2) 3_766 . ? Pt1 C31 H31A 109.5 . . ? Pt1 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? Pt1 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? Pt1 C32 H32A 109.5 . . ? Pt1 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? Pt1 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? Pt1 C33 H33A 109.5 . . ? Pt1 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? Pt1 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? Pt2 C34 H34A 109.5 . . ? Pt2 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? Pt2 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? Pt2 C35 H35A 109.5 . . ? Pt2 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? Pt2 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? Pt2 O36 Pt2 98.3(2) 3_766 . ? Pt2 O36 Pt1 97.1(2) 3_766 . ? Pt2 O36 Pt1 97.9(2) . . ? Pt2 O36 H36 111(6) 3_766 . ? Pt2 O36 H36 129(6) . . ? Pt1 O36 H36 118(6) . . ? Pt2 O37 Pt1 103.2(2) . . ? Pt2 O37 H37 106(7) . . ? Pt1 O37 H37 111(7) . . ? Pt2 O38 Pt1 102.3(3) . 3_766 ? Pt2 O38 H38 106(7) . . ? Pt1 O38 H38 99(7) 3_766 . ? 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 N11 Pt O3 C5 26.0(16) . . . . ? C1 Pt O3 C5 -178.8(5) . . . . ? C2 Pt O3 C5 89.4(5) . . . . ? O4 Pt O3 C5 0.8(4) . . . . ? N24 Pt O3 C5 -92.3(5) . . . . ? O3 Pt O4 C5 -0.8(4) . . . . ? N11 Pt O4 C5 -176.1(4) . . . . ? C1 Pt O4 C5 0.4(12) . . . . ? C2 Pt O4 C5 -89.7(5) . . . . ? N24 Pt O4 C5 83.6(5) . . . . ? Pt O4 C5 O6 178.9(8) . . . . ? Pt O4 C5 O3 1.1(6) . . . . ? Pt O3 C5 O6 -179.1(7) . . . . ? Pt O3 C5 O4 -1.3(7) . . . . ? O3 Pt C5 O6 10(7) . . . . ? N11 Pt C5 O6 -163(7) . . . . ? C1 Pt C5 O6 11(8) . . . . ? C2 Pt C5 O6 -80(8) . . . . ? O4 Pt C5 O6 -169(8) . . . . ? N24 Pt C5 O6 95(8) . . . . ? O3 Pt C5 O4 178.6(7) . . . . ? N11 Pt C5 O4 5.6(6) . . . . ? C1 Pt C5 O4 -179.8(5) . . . . ? C2 Pt C5 O4 89.2(5) . . . . ? N24 Pt C5 O4 -95.8(4) . . . . ? N11 Pt C5 O3 -173.0(4) . . . . ? C1 Pt C5 O3 1.5(6) . . . . ? C2 Pt C5 O3 -89.5(5) . . . . ? O4 Pt C5 O3 -178.6(7) . . . . ? N24 Pt C5 O3 85.5(5) . . . . ? O3 Pt N11 C16 -63.7(16) . . . . ? C1 Pt N11 C16 140.8(6) . . . . ? C2 Pt N11 C16 -127.2(6) . . . . ? O4 Pt N11 C16 -40.3(6) . . . . ? N24 Pt N11 C16 53.5(6) . . . . ? C5 Pt N11 C16 -43.3(8) . . . . ? O3 Pt N11 C12 107.1(14) . . . . ? C1 Pt N11 C12 -48.4(7) . . . . ? C2 Pt N11 C12 43.6(7) . . . . ? O4 Pt N11 C12 130.5(6) . . . . ? N24 Pt N11 C12 -135.7(6) . . . . ? C5 Pt N11 C12 127.5(6) . . . . ? C16 N11 C12 C13 4.3(13) . . . . ? Pt N11 C12 C13 -166.6(7) . . . . ? N11 C12 C13 C14 -3.5(15) . . . . ? C12 C13 C14 C15 2.2(15) . . . . ? C13 C14 C15 C16 -1.8(16) . . . . ? C14 C15 C16 N11 2.5(14) . . . . ? C14 C15 C16 C17 -177.8(9) . . . . ? C12 N11 C16 C15 -3.7(12) . . . . ? Pt N11 C16 C15 167.2(7) . . . . ? C12 N11 C16 C17 176.7(8) . . . . ? Pt N11 C16 C17 -12.5(10) . . . . ? C15 C16 C17 C18 103.1(10) . . . . ? N11 C16 C17 C18 -77.3(11) . . . . ? C16 C17 C18 C19 97.4(10) . . . . ? C17 C18 C19 N24 -32.0(13) . . . . ? C17 C18 C19 C20 150.4(8) . . . . ? N24 C19 C20 C21 2.2(13) . . . . ? C18 C19 C20 C21 179.8(8) . . . . ? C19 C20 C21 C22 -1.3(14) . . . . ? C20 C21 C22 C23 -0.1(15) . . . . ? C21 C22 C23 N24 0.7(14) . . . . ? C20 C19 N24 C23 -1.6(12) . . . . ? C18 C19 N24 C23 -179.1(8) . . . . ? C20 C19 N24 Pt -177.2(6) . . . . ? C18 C19 N24 Pt 5.3(12) . . . . ? C22 C23 N24 C19 0.2(13) . . . . ? C22 C23 N24 Pt 176.6(7) . . . . ? O3 Pt N24 C19 141.7(8) . . . . ? N11 Pt N24 C19 -28.8(8) . . . . ? C1 Pt N24 C19 -118.5(8) . . . . ? C2 Pt N24 C19 157(2) . . . . ? O4 Pt N24 C19 79.4(7) . . . . ? C5 Pt N24 C19 110.2(8) . . . . ? O3 Pt N24 C23 -34.2(6) . . . . ? N11 Pt N24 C23 155.2(6) . . . . ? C1 Pt N24 C23 65.6(6) . . . . ? C2 Pt N24 C23 -19(3) . . . . ? O4 Pt N24 C23 -96.5(6) . . . . ? C5 Pt N24 C23 -65.7(6) . . . . ? C35 Pt2 O36 Pt2 -71(3) . . . 3_766 ? O38 Pt2 O36 Pt2 81.7(3) . . . 3_766 ? C34 Pt2 O36 Pt2 174.5(3) . . . 3_766 ? O37 Pt2 O36 Pt2 -94.2(2) . . . 3_766 ? O36 Pt2 O36 Pt2 0.0 3_766 . . 3_766 ? C35 Pt2 O36 Pt1 28(3) . . . . ? O38 Pt2 O36 Pt1 -179.9(2) . . . . ? C34 Pt2 O36 Pt1 -87.2(3) . . . . ? O37 Pt2 O36 Pt1 4.2(2) . . . . ? O36 Pt2 O36 Pt1 98.4(3) 3_766 . . . ? C31 Pt1 O36 Pt2 55.0(16) . . . 3_766 ? C32 Pt1 O36 Pt2 -85.7(4) . . . 3_766 ? C33 Pt1 O36 Pt2 -176.3(3) . . . 3_766 ? O37 Pt1 O36 Pt2 95.5(2) . . . 3_766 ? O38 Pt1 O36 Pt2 1.6(2) 3_766 . . 3_766 ? C31 Pt1 O36 Pt2 -44.4(16) . . . . ? C32 Pt1 O36 Pt2 174.9(3) . . . . ? C33 Pt1 O36 Pt2 84.3(4) . . . . ? O37 Pt1 O36 Pt2 -3.9(2) . . . . ? O38 Pt1 O36 Pt2 -97.9(2) 3_766 . . . ? C35 Pt2 O37 Pt1 178.1(3) . . . . ? O38 Pt2 O37 Pt1 -64(3) . . . . ? C34 Pt2 O37 Pt1 90.1(3) . . . . ? O36 Pt2 O37 Pt1 -85.4(2) 3_766 . . . ? O36 Pt2 O37 Pt1 -4.3(2) . . . . ? C31 Pt1 O37 Pt2 177.1(3) . . . . ? C32 Pt1 O37 Pt2 -12(5) . . . . ? C33 Pt1 O37 Pt2 -94.9(3) . . . . ? O38 Pt1 O37 Pt2 81.6(3) 3_766 . . . ? O36 Pt1 O37 Pt2 4.3(2) . . . . ? C35 Pt2 O38 Pt1 94.8(3) . . . 3_766 ? C34 Pt2 O38 Pt1 -177.5(3) . . . 3_766 ? O37 Pt2 O38 Pt1 -24(3) . . . 3_766 ? O36 Pt2 O38 Pt1 -1.7(2) 3_766 . . 3_766 ? O36 Pt2 O38 Pt1 -82.5(3) . . . 3_766 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O36 H36 O4 0.842(10) 1.91(2) 2.745(7) 168(9) 1_565 O37 H37 O6 0.842(10) 2.31(5) 3.079(8) 151(9) 3_756 O38 H38 O6 0.841(10) 1.941(19) 2.777(8) 172(10) 1_565 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.538 _refine_diff_density_min -1.867 _refine_diff_density_rms 0.255