# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Dr Marcel Mayor' _publ_contact_author_address ; Forschungszentrum Karlsruhe GmbH Institute for Nanotechnology P. O. Box 3640 Karslruhe D-76021 Karlsruhe GERMANY ; _publ_contact_author_email MARCEL.MAYOR@INT.FZK.DE _publ_section_title ; Intramolecular exchange interaction in twofold spin-labelled platinum complexes ; loop_ _publ_author_name 'Marcel Mayor' 'Christophe Stroh' 'Phillipe Turek' 'C.von Hanisch' data_test1 _database_code_depnum_ccdc_archive 'CCDC 238541' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C74 H78 N4 O6 P2 Pt' _chemical_formula_weight 1376.43 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.752(2) _cell_length_b 12.068(2) _cell_length_c 14.920(3) _cell_angle_alpha 76.54(3) _cell_angle_beta 89.08(3) _cell_angle_gamma 69.46(3) _cell_volume 1595.0(6) _cell_formula_units_Z 1 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plates _exptl_crystal_colour blue _exptl_crystal_size_max 2mm _exptl_crystal_size_mid 1mm _exptl_crystal_size_min 0.5mm _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.433 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 706 _exptl_absorpt_coefficient_mu 2.307 _exptl_absorpt_correction_type / _exptl_absorpt_correction_T_min / _exptl_absorpt_correction_T_max / _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(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 'Imaging plate' _diffrn_measurement_method 'Omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% / _diffrn_reflns_number 9542 _diffrn_reflns_av_R_equivalents 0.0625 _diffrn_reflns_av_sigmaI/netI 0.0507 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 26.18 _reflns_number_total 5825 _reflns_number_gt 5796 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0970P)^2^+0.1051P] 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 5825 _refine_ls_number_parameters 369 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0476 _refine_ls_R_factor_gt 0.0474 _refine_ls_wR_factor_ref 0.1217 _refine_ls_wR_factor_gt 0.1208 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _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 C1 C 0.0805(6) -0.1566(5) 0.0972(3) 0.0492(11) Uani 1 1 d . . . C2 C 0.1264(7) -0.2536(5) 0.1526(4) 0.0533(12) Uani 1 1 d . . . C3 C 0.1886(7) -0.3698(5) 0.2194(4) 0.0545(12) Uani 1 1 d . . . C4 C 0.2533(8) -0.4776(6) 0.1912(4) 0.0624(14) Uani 1 1 d . . . H4A H 0.2547 -0.4759 0.1273 0.075 Uiso 1 1 calc R . . C5 C 0.3165(8) -0.5887(6) 0.2570(5) 0.0674(15) Uani 1 1 d . . . H5A H 0.3602 -0.6620 0.2374 0.081 Uiso 1 1 calc R . . C6 C 0.3157(8) -0.5920(6) 0.3505(4) 0.0638(14) Uani 1 1 d . . . H6A H 0.3603 -0.6674 0.3946 0.077 Uiso 1 1 calc R . . C7 C 0.2496(7) -0.4855(6) 0.3799(4) 0.0596(13) Uani 1 1 d . . . C8 C 0.1856(7) -0.3745(5) 0.3144(4) 0.0566(12) Uani 1 1 d . . . H8A H 0.1397 -0.3018 0.3344 0.068 Uiso 1 1 calc R . . C9 C 0.2445(7) -0.4866(6) 0.4784(4) 0.0597(13) Uani 1 1 d . . . C10 C 0.1827(8) -0.4255(7) 0.6170(4) 0.0648(14) Uani 1 1 d . . . C11 C 0.2963(8) -0.5567(6) 0.6408(4) 0.0638(14) Uani 1 1 d . . . C12 C 0.2516(9) -0.3303(7) 0.6211(6) 0.0741(17) Uani 1 1 d . . . H12C H 0.1755 -0.2487 0.6056 0.089 Uiso 1 1 calc R . . H12B H 0.3274 -0.3345 0.5768 0.089 Uiso 1 1 calc R . . H12A H 0.2958 -0.3469 0.6836 0.089 Uiso 1 1 calc R . . C13 C 0.0468(9) -0.4076(8) 0.6720(5) 0.0771(18) Uani 1 1 d . . . H13C H -0.0193 -0.3222 0.6531 0.092 Uiso 1 1 calc R . . H13B H 0.0761 -0.4284 0.7380 0.092 Uiso 1 1 calc R . . H13A H -0.0038 -0.4605 0.6601 0.092 Uiso 1 1 calc R . . C14 C 0.4237(9) -0.5777(8) 0.7061(5) 0.0763(18) Uani 1 1 d . . . H14C H 0.4900 -0.6629 0.7174 0.092 Uiso 1 1 calc R . . H14B H 0.3873 -0.5598 0.7647 0.092 Uiso 1 1 calc R . . H14A H 0.4769 -0.5240 0.6789 0.092 Uiso 1 1 calc R . . C15 C 0.2288(10) -0.6552(8) 0.6721(5) 0.083(2) Uani 1 1 d . . . H15C H 0.3069 -0.7359 0.6858 0.099 Uiso 1 1 calc R . . H15B H 0.1599 -0.6498 0.6228 0.099 Uiso 1 1 calc R . . H15A H 0.1766 -0.6430 0.7277 0.099 Uiso 1 1 calc R . . C16 C 0.1246(6) 0.0427(5) 0.2079(3) 0.0494(11) Uani 1 1 d . . . C17 C 0.2427(7) -0.0649(6) 0.2366(4) 0.0588(13) Uani 1 1 d . . . H17A H 0.2960 -0.1039 0.1918 0.071 Uiso 1 1 calc R . . C18 C 0.2856(8) -0.1176(6) 0.3304(4) 0.0651(15) Uani 1 1 d . . . H18A H 0.3662 -0.1925 0.3488 0.078 Uiso 1 1 calc R . . C19 C 0.2130(10) -0.0626(7) 0.3946(5) 0.082(2) Uani 1 1 d . . . H19A H 0.2396 -0.1000 0.4584 0.098 Uiso 1 1 calc R . . C20 C 0.1022(12) 0.0457(9) 0.3682(5) 0.107(3) Uani 1 1 d . . . H20A H 0.0551 0.0864 0.4138 0.128 Uiso 1 1 calc R . . C21 C 0.0552(10) 0.0994(7) 0.2750(5) 0.080(2) Uani 1 1 d . . . H21A H -0.0246 0.1750 0.2579 0.096 Uiso 1 1 calc R . . C22 C -0.0668(6) 0.2589(5) 0.0809(3) 0.0465(10) Uani 1 1 d . . . C23 C -0.0325(7) 0.3615(5) 0.0803(4) 0.0558(12) Uani 1 1 d . . . H23A H 0.0670 0.3563 0.0816 0.067 Uiso 1 1 calc R . . C24 C -0.1458(9) 0.4725(5) 0.0779(4) 0.0674(17) Uani 1 1 d . . . H24A H -0.1230 0.5430 0.0771 0.081 Uiso 1 1 calc R . . C25 C -0.2892(8) 0.4803(6) 0.0765(4) 0.0672(16) Uani 1 1 d . . . H25A H -0.3654 0.5566 0.0732 0.081 Uiso 1 1 calc R . . C26 C -0.3235(7) 0.3779(7) 0.0799(5) 0.0678(15) Uani 1 1 d . . . H26A H -0.4228 0.3827 0.0822 0.081 Uiso 1 1 calc R . . C27 C -0.2128(6) 0.2680(5) 0.0800(4) 0.0564(12) Uani 1 1 d . . . H27A H -0.2369 0.1984 0.0793 0.068 Uiso 1 1 calc R . . C28 C 0.2372(6) 0.1387(5) 0.0428(3) 0.0469(10) Uani 1 1 d . . . C29 C 0.3353(7) 0.1551(6) 0.1012(4) 0.0573(13) Uani 1 1 d . . . H29A H 0.3159 0.1525 0.1641 0.069 Uiso 1 1 calc R . . C30 C 0.4603(7) 0.1750(6) 0.0686(4) 0.0636(14) Uani 1 1 d . . . H30A H 0.5250 0.1879 0.1086 0.076 Uiso 1 1 calc R . . C31 C 0.4910(7) 0.1762(5) -0.0230(4) 0.0598(13) Uani 1 1 d . . . H31A H 0.5777 0.1883 -0.0455 0.072 Uiso 1 1 calc R . . C32 C 0.3948(7) 0.1598(6) -0.0811(4) 0.0598(13) Uani 1 1 d . . . H32A H 0.4154 0.1613 -0.1438 0.072 Uiso 1 1 calc R . . C33 C 0.2691(7) 0.1412(5) -0.0493(4) 0.0541(12) Uani 1 1 d . . . H33A H 0.2040 0.1300 -0.0900 0.065 Uiso 1 1 calc R . . C34 C 0.439(3) -0.068(3) 0.6445(19) 0.248(12) Uiso 1 1 d . . . H34B H 0.4558 -0.1312 0.6095 0.298 Uiso 1 1 calc R . . H34A H 0.5369 -0.0669 0.6599 0.298 Uiso 1 1 calc R . . C35 C 0.396(2) -0.1011(17) 0.7112(12) 0.151(5) Uiso 1 1 d . . . H34A' H 0.4713 -0.1244 0.7629 0.181 Uiso 1 1 calc R . . H35B H 0.3709 -0.1731 0.7094 0.181 Uiso 1 1 calc R . . C36 C 0.262(3) 0.003(2) 0.7231(16) 0.214(9) Uiso 1 1 d . . . H36B H 0.2876 0.0589 0.7530 0.257 Uiso 1 1 calc R . . H36A H 0.1902 -0.0266 0.7588 0.257 Uiso 1 1 calc R . . C37 C 0.207(3) 0.061(2) 0.6230(16) 0.205(8) Uiso 1 1 d . . . H37B H 0.1361 0.1454 0.6157 0.247 Uiso 1 1 calc R . . H37A H 0.1605 0.0131 0.5982 0.247 Uiso 1 1 calc R . . N1 N 0.1413(6) -0.4102(5) 0.5184(4) 0.0669(13) Uani 1 1 d . . . N2 N 0.3458(7) -0.5670(5) 0.5456(4) 0.0662(13) Uani 1 1 d . . . O1 O 0.0232(6) -0.3234(6) 0.4772(4) 0.0890(15) Uani 1 1 d . . . O2 O 0.4649(7) -0.6510(5) 0.5347(3) 0.0879(16) Uani 1 1 d . . . O3 O 0.352(2) 0.062(2) 0.5728(14) 0.268(8) Uiso 1 1 d . . . Pt1 Pt 0.0000 0.0000 0.0000 0.04156(11) Uani 1 2 d S . . P1 P 0.07420(14) 0.10968(11) 0.08485(8) 0.0423(3) Uani 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 C1 0.054(3) 0.047(3) 0.045(2) -0.010(2) -0.004(2) -0.017(2) C2 0.062(3) 0.049(3) 0.046(3) -0.005(2) -0.007(2) -0.019(3) C3 0.059(3) 0.045(3) 0.052(3) 0.001(2) -0.011(2) -0.016(3) C4 0.074(4) 0.053(3) 0.053(3) -0.006(2) -0.004(3) -0.017(3) C5 0.077(4) 0.048(3) 0.070(4) -0.008(3) -0.003(3) -0.017(3) C6 0.067(4) 0.054(3) 0.057(3) 0.003(3) -0.005(3) -0.015(3) C7 0.059(3) 0.056(3) 0.056(3) -0.002(3) -0.004(2) -0.018(3) C8 0.060(3) 0.050(3) 0.052(3) -0.003(2) -0.005(2) -0.015(3) C9 0.057(3) 0.056(3) 0.054(3) -0.001(2) 0.000(2) -0.014(3) C10 0.065(4) 0.068(4) 0.057(3) -0.011(3) 0.001(3) -0.020(3) C11 0.070(4) 0.063(4) 0.054(3) -0.011(3) 0.005(3) -0.020(3) C12 0.069(4) 0.065(4) 0.084(5) -0.020(4) 0.009(3) -0.018(4) C13 0.072(5) 0.089(5) 0.069(4) -0.025(4) 0.009(3) -0.024(4) C14 0.082(5) 0.083(5) 0.059(3) -0.018(3) 0.002(3) -0.022(4) C15 0.103(6) 0.074(5) 0.070(4) -0.007(4) 0.000(4) -0.037(5) C16 0.057(3) 0.045(3) 0.043(2) -0.008(2) -0.004(2) -0.016(2) C17 0.058(3) 0.059(3) 0.051(3) -0.012(3) -0.011(2) -0.011(3) C18 0.070(4) 0.054(3) 0.063(3) -0.008(3) -0.013(3) -0.016(3) C19 0.104(6) 0.067(4) 0.050(3) -0.002(3) -0.011(3) -0.007(4) C20 0.125(8) 0.099(6) 0.049(4) -0.013(4) 0.007(4) 0.013(6) C21 0.088(5) 0.068(4) 0.052(3) -0.009(3) 0.000(3) 0.006(4) C22 0.054(3) 0.038(2) 0.041(2) -0.0055(19) -0.0012(19) -0.011(2) C23 0.069(4) 0.045(3) 0.050(3) -0.009(2) 0.009(2) -0.018(3) C24 0.100(5) 0.041(3) 0.057(3) -0.010(2) 0.012(3) -0.020(3) C25 0.073(4) 0.049(3) 0.056(3) -0.008(3) 0.006(3) 0.004(3) C26 0.048(3) 0.065(4) 0.076(4) -0.018(3) 0.004(3) -0.002(3) C27 0.049(3) 0.048(3) 0.065(3) -0.010(2) -0.003(2) -0.010(3) C28 0.051(3) 0.042(2) 0.048(2) -0.010(2) 0.000(2) -0.017(2) C29 0.058(3) 0.065(3) 0.056(3) -0.018(3) 0.003(2) -0.027(3) C30 0.062(4) 0.069(4) 0.067(3) -0.019(3) 0.000(3) -0.031(3) C31 0.055(3) 0.049(3) 0.072(4) -0.010(3) 0.010(3) -0.019(3) C32 0.066(4) 0.060(3) 0.054(3) -0.010(3) 0.010(2) -0.026(3) C33 0.059(3) 0.054(3) 0.046(3) -0.009(2) -0.001(2) -0.019(3) N1 0.060(3) 0.064(3) 0.062(3) -0.008(3) -0.004(2) -0.008(3) N2 0.070(4) 0.059(3) 0.056(3) -0.006(2) -0.002(2) -0.011(3) O1 0.077(4) 0.092(4) 0.074(3) -0.020(3) -0.004(2) -0.001(3) O2 0.088(4) 0.076(3) 0.065(3) -0.013(3) -0.005(2) 0.012(3) Pt1 0.04718(18) 0.03605(15) 0.03918(15) -0.00669(10) -0.00419(10) -0.01335(12) P1 0.0480(7) 0.0390(6) 0.0399(6) -0.0094(5) -0.0024(5) -0.0155(6) _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 C1 C2 1.203(8) . ? C1 Pt1 2.002(6) . ? C2 C3 1.449(8) . ? C3 C4 1.392(9) . ? C3 C8 1.405(8) . ? C4 C5 1.403(9) . ? C5 C6 1.386(9) . ? C6 C7 1.390(9) . ? C7 C8 1.401(8) . ? C7 C9 1.467(8) . ? C9 N1 1.344(9) . ? C9 N2 1.351(8) . ? C10 N1 1.484(8) . ? C10 C13 1.524(9) . ? C10 C12 1.532(10) . ? C10 C11 1.543(10) . ? C11 C14 1.504(10) . ? C11 N2 1.511(8) . ? C11 C15 1.532(9) . ? C16 C21 1.379(9) . ? C16 C17 1.379(8) . ? C16 P1 1.823(5) . ? C17 C18 1.399(8) . ? C18 C19 1.343(10) . ? C19 C20 1.347(12) . ? C20 C21 1.399(10) . ? C22 C23 1.389(7) . ? C22 C27 1.389(8) . ? C22 P1 1.832(5) . ? C23 C24 1.399(9) . ? C24 C25 1.368(11) . ? C25 C26 1.380(10) . ? C26 C27 1.385(9) . ? C28 C29 1.398(7) . ? C28 C33 1.400(7) . ? C28 P1 1.816(5) . ? C29 C30 1.382(8) . ? C30 C31 1.393(9) . ? C31 C32 1.382(9) . ? C32 C33 1.380(8) . ? C34 C35 1.11(3) . ? C34 O3 1.62(3) . ? C35 C36 1.50(3) . ? C36 C37 1.51(3) . ? C37 O3 1.59(3) . ? N1 O1 1.296(8) . ? N2 O2 1.283(8) . ? Pt1 C1 2.002(6) 2 ? Pt1 P1 2.3153(12) . ? Pt1 P1 2.3153(12) 2 ? 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 C1 Pt1 176.6(4) . . ? C1 C2 C3 177.2(6) . . ? C4 C3 C8 119.0(5) . . ? C4 C3 C2 121.1(5) . . ? C8 C3 C2 119.9(5) . . ? C3 C4 C5 120.2(6) . . ? C6 C5 C4 120.3(6) . . ? C5 C6 C7 120.2(6) . . ? C6 C7 C8 119.6(6) . . ? C6 C7 C9 121.4(6) . . ? C8 C7 C9 119.0(6) . . ? C7 C8 C3 120.7(6) . . ? N1 C9 N2 107.8(5) . . ? N1 C9 C7 127.3(6) . . ? N2 C9 C7 125.0(6) . . ? N1 C10 C13 109.6(6) . . ? N1 C10 C12 107.3(6) . . ? C13 C10 C12 111.2(6) . . ? N1 C10 C11 101.0(5) . . ? C13 C10 C11 114.5(6) . . ? C12 C10 C11 112.4(6) . . ? C14 C11 N2 111.1(6) . . ? C14 C11 C15 110.8(6) . . ? N2 C11 C15 105.3(5) . . ? C14 C11 C10 114.9(6) . . ? N2 C11 C10 99.9(5) . . ? C15 C11 C10 113.9(6) . . ? C21 C16 C17 117.4(5) . . ? C21 C16 P1 122.6(5) . . ? C17 C16 P1 119.9(4) . . ? C16 C17 C18 121.3(6) . . ? C19 C18 C17 120.1(7) . . ? C18 C19 C20 119.8(7) . . ? C19 C20 C21 121.3(7) . . ? C16 C21 C20 120.1(7) . . ? C23 C22 C27 119.5(5) . . ? C23 C22 P1 122.4(4) . . ? C27 C22 P1 118.1(4) . . ? C22 C23 C24 119.3(6) . . ? C25 C24 C23 120.6(6) . . ? C24 C25 C26 120.3(6) . . ? C25 C26 C27 119.8(6) . . ? C26 C27 C22 120.4(5) . . ? C29 C28 C33 118.6(5) . . ? C29 C28 P1 121.5(4) . . ? C33 C28 P1 119.9(4) . . ? C30 C29 C28 120.9(5) . . ? C29 C30 C31 119.8(5) . . ? C32 C31 C30 119.6(5) . . ? C33 C32 C31 120.8(5) . . ? C32 C33 C28 120.3(5) . . ? C35 C34 O3 123(3) . . ? C34 C35 C36 106(2) . . ? C35 C36 C37 99.8(19) . . ? C36 C37 O3 103.6(19) . . ? O1 N1 C9 126.2(6) . . ? O1 N1 C10 120.9(6) . . ? C9 N1 C10 112.6(5) . . ? O2 N2 C9 126.7(6) . . ? O2 N2 C11 121.3(5) . . ? C9 N2 C11 111.7(6) . . ? C37 O3 C34 87.7(18) . . ? C1 Pt1 C1 180.0(4) . 2 ? C1 Pt1 P1 93.57(14) . . ? C1 Pt1 P1 86.43(14) 2 . ? C1 Pt1 P1 86.43(14) . 2 ? C1 Pt1 P1 93.57(14) 2 2 ? P1 Pt1 P1 180.00(5) . 2 ? C28 P1 C16 102.8(2) . . ? C28 P1 C22 106.4(2) . . ? C16 P1 C22 103.9(2) . . ? C28 P1 Pt1 112.11(16) . . ? C16 P1 Pt1 118.16(16) . . ? C22 P1 Pt1 112.42(17) . . ? 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 Pt1 C1 C2 C3 126(10) . . . . ? C1 C2 C3 C4 -90(12) . . . . ? C1 C2 C3 C8 89(13) . . . . ? C8 C3 C4 C5 -1.1(9) . . . . ? C2 C3 C4 C5 178.2(6) . . . . ? C3 C4 C5 C6 -0.3(10) . . . . ? C4 C5 C6 C7 1.2(10) . . . . ? C5 C6 C7 C8 -0.8(9) . . . . ? C5 C6 C7 C9 178.8(6) . . . . ? C6 C7 C8 C3 -0.5(9) . . . . ? C9 C7 C8 C3 179.8(5) . . . . ? C4 C3 C8 C7 1.5(9) . . . . ? C2 C3 C8 C7 -177.8(5) . . . . ? C6 C7 C9 N1 -150.4(7) . . . . ? C8 C7 C9 N1 29.2(9) . . . . ? C6 C7 C9 N2 29.6(9) . . . . ? C8 C7 C9 N2 -150.8(6) . . . . ? N1 C10 C11 C14 143.4(6) . . . . ? C13 C10 C11 C14 -98.9(7) . . . . ? C12 C10 C11 C14 29.3(8) . . . . ? N1 C10 C11 N2 24.5(6) . . . . ? C13 C10 C11 N2 142.2(5) . . . . ? C12 C10 C11 N2 -89.6(6) . . . . ? N1 C10 C11 C15 -87.2(6) . . . . ? C13 C10 C11 C15 30.5(8) . . . . ? C12 C10 C11 C15 158.7(6) . . . . ? C21 C16 C17 C18 3.2(9) . . . . ? P1 C16 C17 C18 179.0(5) . . . . ? C16 C17 C18 C19 -1.1(10) . . . . ? C17 C18 C19 C20 -2.4(13) . . . . ? C18 C19 C20 C21 3.7(17) . . . . ? C17 C16 C21 C20 -2.0(12) . . . . ? P1 C16 C21 C20 -177.7(8) . . . . ? C19 C20 C21 C16 -1.4(17) . . . . ? C27 C22 C23 C24 -0.6(8) . . . . ? P1 C22 C23 C24 -179.6(4) . . . . ? C22 C23 C24 C25 0.3(9) . . . . ? C23 C24 C25 C26 1.6(9) . . . . ? C24 C25 C26 C27 -3.3(10) . . . . ? C25 C26 C27 C22 3.0(10) . . . . ? C23 C22 C27 C26 -1.0(8) . . . . ? P1 C22 C27 C26 178.0(5) . . . . ? C33 C28 C29 C30 0.9(9) . . . . ? P1 C28 C29 C30 178.9(5) . . . . ? C28 C29 C30 C31 -1.4(11) . . . . ? C29 C30 C31 C32 1.2(10) . . . . ? C30 C31 C32 C33 -0.5(10) . . . . ? C31 C32 C33 C28 0.0(10) . . . . ? C29 C28 C33 C32 -0.2(9) . . . . ? P1 C28 C33 C32 -178.2(5) . . . . ? O3 C34 C35 C36 -8(3) . . . . ? C34 C35 C36 C37 32(3) . . . . ? C35 C36 C37 O3 -44(2) . . . . ? N2 C9 N1 O1 -177.3(7) . . . . ? C7 C9 N1 O1 2.7(11) . . . . ? N2 C9 N1 C10 9.0(7) . . . . ? C7 C9 N1 C10 -171.0(6) . . . . ? C13 C10 N1 O1 42.3(9) . . . . ? C12 C10 N1 O1 -78.6(8) . . . . ? C11 C10 N1 O1 163.5(6) . . . . ? C13 C10 N1 C9 -143.6(6) . . . . ? C12 C10 N1 C9 95.5(7) . . . . ? C11 C10 N1 C9 -22.4(7) . . . . ? N1 C9 N2 O2 -176.7(7) . . . . ? C7 C9 N2 O2 3.4(11) . . . . ? N1 C9 N2 C11 9.3(7) . . . . ? C7 C9 N2 C11 -170.6(6) . . . . ? C14 C11 N2 O2 41.7(9) . . . . ? C15 C11 N2 O2 -78.3(8) . . . . ? C10 C11 N2 O2 163.4(6) . . . . ? C14 C11 N2 C9 -144.0(6) . . . . ? C15 C11 N2 C9 96.0(7) . . . . ? C10 C11 N2 C9 -22.2(7) . . . . ? C36 C37 O3 C34 35(2) . . . . ? C35 C34 O3 C37 -19(3) . . . . ? C2 C1 Pt1 C1 -69(24) . . . 2 ? C2 C1 Pt1 P1 -179(100) . . . . ? C2 C1 Pt1 P1 1(9) . . . 2 ? C29 C28 P1 C16 -24.8(5) . . . . ? C33 C28 P1 C16 153.2(5) . . . . ? C29 C28 P1 C22 84.0(5) . . . . ? C33 C28 P1 C22 -98.0(5) . . . . ? C29 C28 P1 Pt1 -152.7(4) . . . . ? C33 C28 P1 Pt1 25.2(5) . . . . ? C21 C16 P1 C28 114.5(6) . . . . ? C17 C16 P1 C28 -61.1(5) . . . . ? C21 C16 P1 C22 3.8(6) . . . . ? C17 C16 P1 C22 -171.8(4) . . . . ? C21 C16 P1 Pt1 -121.5(6) . . . . ? C17 C16 P1 Pt1 62.9(5) . . . . ? C23 C22 P1 C28 -21.7(5) . . . . ? C27 C22 P1 C28 159.3(4) . . . . ? C23 C22 P1 C16 86.4(4) . . . . ? C27 C22 P1 C16 -92.6(4) . . . . ? C23 C22 P1 Pt1 -144.8(4) . . . . ? C27 C22 P1 Pt1 36.2(4) . . . . ? C1 Pt1 P1 C28 103.3(2) . . . . ? C1 Pt1 P1 C28 -76.7(2) 2 . . . ? P1 Pt1 P1 C28 -38(100) 2 . . . ? C1 Pt1 P1 C16 -16.0(3) . . . . ? C1 Pt1 P1 C16 164.0(3) 2 . . . ? P1 Pt1 P1 C16 -158(100) 2 . . . ? C1 Pt1 P1 C22 -136.9(2) . . . . ? C1 Pt1 P1 C22 43.1(2) 2 . . . ? P1 Pt1 P1 C22 81(100) 2 . . . ? _diffrn_measured_fraction_theta_max 0.913 _diffrn_reflns_theta_full 26.18 _diffrn_measured_fraction_theta_full 0.913 _refine_diff_density_max 0.820 _refine_diff_density_min -2.752 _refine_diff_density_rms 0.126 data_testc2c _database_code_depnum_ccdc_archive 'CCDC 238542' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C66 H62 N4 O4 P2 Pt' _chemical_formula_weight 1232.23 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' 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 monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 34.963(7) _cell_length_b 9.4928(19) _cell_length_c 19.323(4) _cell_angle_alpha 90.00 _cell_angle_beta 119.33(3) _cell_angle_gamma 90.00 _cell_volume 5591.3(19) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plates _exptl_crystal_colour blue _exptl_crystal_size_max 2mm _exptl_crystal_size_mid 1mm _exptl_crystal_size_min 0.5mm _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.464 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2504 _exptl_absorpt_coefficient_mu 2.620 _exptl_absorpt_correction_type / _exptl_absorpt_correction_T_min / _exptl_absorpt_correction_T_max / _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _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 'Imaging plate' _diffrn_measurement_method 'Omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% / _diffrn_reflns_number 10025 _diffrn_reflns_av_R_equivalents 0.0401 _diffrn_reflns_av_sigmaI/netI 0.0345 _diffrn_reflns_limit_h_min -42 _diffrn_reflns_limit_h_max 43 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 26.10 _reflns_number_total 4567 _reflns_number_gt 3530 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0703P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4567 _refine_ls_number_parameters 349 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0452 _refine_ls_R_factor_gt 0.0362 _refine_ls_wR_factor_ref 0.1018 _refine_ls_wR_factor_gt 0.0984 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.073 _refine_ls_shift/su_mean 0.006 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 0.2500 0.7500 0.0000 0.02872(10) Uani 1 2 d S . . P1 P 0.29402(3) 0.61295(12) 0.11031(7) 0.0294(2) Uani 1 1 d . . . N1 N 0.00303(15) 0.7733(5) 0.1070(3) 0.0445(11) Uani 1 1 d . . . N2 N -0.02713(12) 0.6819(5) -0.0121(3) 0.0399(9) Uani 1 1 d . . . O1 O 0.03070(12) 0.8277(6) 0.1742(3) 0.0644(13) Uani 1 1 d . . . O2 O -0.03209(11) 0.6181(4) -0.0747(2) 0.0517(10) Uani 1 1 d . . . C1 C 0.20051(16) 0.7614(4) 0.0247(3) 0.0324(10) Uani 1 1 d . . . C2 C 0.17007(18) 0.7668(5) 0.0348(4) 0.0380(12) Uani 1 1 d . . . C3 C 0.12995(17) 0.7638(5) 0.0401(4) 0.0370(11) Uani 1 1 d . . . C4 C 0.08951(18) 0.7685(5) -0.0281(4) 0.0405(12) Uani 1 1 d . . . H4A H 0.0883 0.7792 -0.0781 0.049 Uiso 1 1 calc R . . C5 C 0.05080(19) 0.7578(5) -0.0254(4) 0.0419(12) Uani 1 1 d . . . H5A H 0.0234 0.7600 -0.0731 0.050 Uiso 1 1 calc R . . C6 C 0.05223(18) 0.7439(5) 0.0479(4) 0.0393(12) Uani 1 1 d . . . C7 C 0.09283(18) 0.7430(5) 0.1179(4) 0.0421(12) Uani 1 1 d . . . H7A H 0.0940 0.7354 0.1680 0.051 Uiso 1 1 calc R . . C8 C 0.13139(18) 0.7534(5) 0.1139(4) 0.0430(12) Uani 1 1 d . . . H8A H 0.1589 0.7534 0.1614 0.052 Uiso 1 1 calc R . . C9 C 0.01054(17) 0.7310(5) 0.0478(4) 0.0381(12) Uani 1 1 d . . . C10 C -0.04307(18) 0.7347(5) 0.0885(4) 0.0442(13) Uani 1 1 d . . . C11 C -0.0398(2) 0.5952(7) 0.1286(4) 0.0600(16) Uani 1 1 d . . . H11C H -0.0288 0.5232 0.1063 0.072 Uiso 1 1 calc R . . H11B H -0.0688 0.5677 0.1198 0.072 Uiso 1 1 calc R . . H11A H -0.0196 0.6042 0.1857 0.072 Uiso 1 1 calc R . . C12 C -0.06077(18) 0.8483(7) 0.1208(4) 0.0573(16) Uani 1 1 d . . . H12C H -0.0640 0.9366 0.0922 0.069 Uiso 1 1 calc R . . H12B H -0.0403 0.8622 0.1775 0.069 Uiso 1 1 calc R . . H12A H -0.0894 0.8190 0.1136 0.069 Uiso 1 1 calc R . . C13 C -0.06557(18) 0.7249(5) -0.0025(4) 0.0443(13) Uani 1 1 d . . . C14 C -0.08046(18) 0.8659(7) -0.0452(4) 0.0593(16) Uani 1 1 d . . . H14C H -0.0941 0.8510 -0.1027 0.071 Uiso 1 1 calc R . . H14B H -0.0551 0.9283 -0.0279 0.071 Uiso 1 1 calc R . . H14A H -0.1018 0.9092 -0.0326 0.071 Uiso 1 1 calc R . . C15 C -0.10179(15) 0.6146(7) -0.0405(4) 0.0508(14) Uani 1 1 d . . . H15C H -0.1138 0.6155 -0.0982 0.061 Uiso 1 1 calc R . . H15B H -0.1251 0.6361 -0.0280 0.061 Uiso 1 1 calc R . . H15A H -0.0897 0.5212 -0.0197 0.061 Uiso 1 1 calc R . . C16 C 0.27712(14) 0.5848(4) 0.1850(3) 0.0323(9) Uani 1 1 d . . . C17 C 0.30505(14) 0.6007(6) 0.2647(3) 0.0408(11) Uani 1 1 d . . . H17A H 0.3330 0.6421 0.2824 0.049 Uiso 1 1 calc R . . C18 C 0.29306(17) 0.5568(6) 0.3207(4) 0.0485(14) Uani 1 1 d . . . H18A H 0.3128 0.5674 0.3759 0.058 Uiso 1 1 calc R . . C19 C 0.25213(18) 0.4981(6) 0.2945(3) 0.0481(13) Uani 1 1 d . . . H19A H 0.2438 0.4677 0.3320 0.058 Uiso 1 1 calc R . . C20 C 0.22364(17) 0.4832(6) 0.2156(4) 0.0459(13) Uani 1 1 d . . . H20A H 0.1956 0.4427 0.1990 0.055 Uiso 1 1 calc R . . C21 C 0.23463(16) 0.5263(5) 0.1578(3) 0.0370(10) Uani 1 1 d . . . H21A H 0.2145 0.5167 0.1027 0.044 Uiso 1 1 calc R . . C22 C 0.30140(14) 0.4320(5) 0.0880(3) 0.0319(9) Uani 1 1 d . . . C23 C 0.31402(16) 0.3276(5) 0.1466(3) 0.0413(11) Uani 1 1 d . . . H23A H 0.3175 0.3503 0.1972 0.050 Uiso 1 1 calc R . . C24 C 0.32136(18) 0.1916(6) 0.1302(4) 0.0463(12) Uani 1 1 d . . . H24A H 0.3305 0.1217 0.1704 0.056 Uiso 1 1 calc R . . C25 C 0.31569(17) 0.1556(6) 0.0566(4) 0.0452(12) Uani 1 1 d . . . H25A H 0.3206 0.0616 0.0460 0.054 Uiso 1 1 calc R . . C26 C 0.3029(2) 0.2577(5) -0.0014(4) 0.0427(12) Uani 1 1 d . . . H26A H 0.2990 0.2332 -0.0521 0.051 Uiso 1 1 calc R . . C27 C 0.29548(14) 0.3955(5) 0.0130(3) 0.0352(10) Uani 1 1 d . . . H27A H 0.2865 0.4646 -0.0276 0.042 Uiso 1 1 calc R . . C28 C 0.34976(15) 0.6816(5) 0.1667(3) 0.0341(10) Uani 1 1 d . . . C29 C 0.38660(16) 0.5947(6) 0.2007(3) 0.0418(11) Uani 1 1 d . . . H29A H 0.3831 0.4955 0.1942 0.050 Uiso 1 1 calc R . . C30 C 0.42866(16) 0.6521(6) 0.2444(4) 0.0468(13) Uani 1 1 d . . . H30A H 0.4536 0.5921 0.2681 0.056 Uiso 1 1 calc R . . C31 C 0.43381(18) 0.7964(7) 0.2528(4) 0.0483(13) Uani 1 1 d . . . H31A H 0.4623 0.8362 0.2814 0.058 Uiso 1 1 calc R . . C32 C 0.39738(18) 0.8827(6) 0.2196(4) 0.0525(14) Uani 1 1 d . . . H32A H 0.4009 0.9819 0.2263 0.063 Uiso 1 1 calc R . . C33 C 0.35575(17) 0.8259(6) 0.1768(4) 0.0462(12) Uani 1 1 d . . . H33A H 0.3310 0.8866 0.1540 0.055 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 0.02968(14) 0.02930(15) 0.02963(16) 0.00235(10) 0.01642(12) 0.00182(9) P1 0.0330(5) 0.0281(6) 0.0279(6) 0.0015(5) 0.0156(5) 0.0021(4) N1 0.036(2) 0.054(3) 0.050(3) -0.009(2) 0.025(2) -0.0066(18) N2 0.0345(19) 0.048(3) 0.043(3) -0.002(2) 0.023(2) 0.0013(18) O1 0.048(2) 0.093(4) 0.056(3) -0.032(3) 0.029(2) -0.018(2) O2 0.0496(19) 0.068(3) 0.042(2) -0.015(2) 0.026(2) -0.0102(19) C1 0.031(2) 0.033(3) 0.023(3) 0.0036(19) 0.006(2) 0.0035(17) C2 0.037(3) 0.039(3) 0.047(4) 0.000(2) 0.027(3) -0.0020(18) C3 0.039(2) 0.035(3) 0.045(3) -0.003(2) 0.027(3) -0.0032(18) C4 0.043(3) 0.045(3) 0.041(3) 0.003(2) 0.026(3) 0.001(2) C5 0.041(3) 0.049(3) 0.033(3) -0.001(2) 0.016(3) 0.000(2) C6 0.039(3) 0.040(3) 0.046(4) -0.005(2) 0.027(3) -0.0040(19) C7 0.039(3) 0.055(3) 0.041(3) -0.002(2) 0.025(3) -0.002(2) C8 0.036(2) 0.052(3) 0.046(4) -0.002(2) 0.024(3) -0.003(2) C9 0.036(2) 0.042(3) 0.038(3) -0.005(2) 0.019(2) -0.0018(18) C10 0.033(2) 0.055(4) 0.050(4) -0.003(2) 0.025(3) 0.002(2) C11 0.063(3) 0.068(4) 0.058(4) 0.001(3) 0.036(3) -0.009(3) C12 0.051(3) 0.066(4) 0.062(4) -0.017(3) 0.033(3) 0.003(3) C13 0.038(3) 0.043(3) 0.059(4) 0.000(2) 0.030(3) 0.002(2) C14 0.048(3) 0.055(4) 0.063(5) 0.009(3) 0.019(3) 0.013(3) C15 0.035(2) 0.062(4) 0.054(4) -0.014(3) 0.021(3) -0.010(2) C16 0.036(2) 0.025(2) 0.039(3) -0.0001(19) 0.020(2) 0.0021(17) C17 0.034(2) 0.056(3) 0.033(3) -0.002(2) 0.016(2) 0.001(2) C18 0.043(3) 0.073(4) 0.032(3) -0.001(3) 0.020(3) 0.002(2) C19 0.051(3) 0.066(4) 0.033(3) 0.007(3) 0.025(3) 0.002(3) C20 0.040(3) 0.056(3) 0.045(3) 0.007(3) 0.023(3) -0.004(2) C21 0.042(2) 0.041(3) 0.027(3) 0.005(2) 0.016(2) -0.001(2) C22 0.0316(19) 0.032(2) 0.032(3) -0.0025(19) 0.016(2) -0.0023(17) C23 0.054(3) 0.032(3) 0.041(3) -0.001(2) 0.025(3) 0.003(2) C24 0.053(3) 0.038(3) 0.046(4) 0.006(3) 0.023(3) 0.005(2) C25 0.048(3) 0.036(3) 0.054(4) -0.009(2) 0.027(3) 0.001(2) C26 0.052(3) 0.039(3) 0.044(3) -0.002(2) 0.028(3) 0.001(2) C27 0.037(2) 0.036(2) 0.036(3) -0.001(2) 0.021(2) -0.0006(19) C28 0.038(2) 0.035(3) 0.035(3) -0.003(2) 0.022(2) -0.0047(19) C29 0.040(2) 0.038(3) 0.043(3) 0.001(2) 0.016(2) 0.006(2) C30 0.035(2) 0.049(3) 0.051(4) 0.000(3) 0.018(3) 0.005(2) C31 0.038(2) 0.061(3) 0.040(4) -0.003(3) 0.015(3) -0.010(2) C32 0.051(3) 0.037(3) 0.061(4) -0.004(3) 0.021(3) -0.006(2) C33 0.042(2) 0.042(3) 0.052(4) 0.001(3) 0.021(3) 0.003(2) _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 C1 2.010(5) . ? Pt1 C1 2.010(5) 7_565 ? Pt1 P1 2.3218(14) 7_565 ? Pt1 P1 2.3218(14) . ? P1 C22 1.820(4) . ? P1 C28 1.825(5) . ? P1 C16 1.827(4) . ? N1 O1 1.287(7) . ? N1 C9 1.354(7) . ? N1 C10 1.515(6) . ? N2 O2 1.285(6) . ? N2 C9 1.341(7) . ? N2 C13 1.501(5) . ? C1 C2 1.173(7) . ? C2 C3 1.457(6) . ? C3 C4 1.383(9) . ? C3 C8 1.405(8) . ? C4 C5 1.383(7) . ? C5 C6 1.400(8) . ? C6 C7 1.402(9) . ? C6 C9 1.461(7) . ? C7 C8 1.392(7) . ? C10 C11 1.510(8) . ? C10 C12 1.521(7) . ? C10 C13 1.538(10) . ? C13 C14 1.524(8) . ? C13 C15 1.526(7) . ? C16 C17 1.370(7) . ? C16 C21 1.424(6) . ? C17 C18 1.402(7) . ? C18 C19 1.380(8) . ? C19 C20 1.360(8) . ? C20 C21 1.408(6) . ? C22 C27 1.403(6) . ? C22 C23 1.403(7) . ? C23 C24 1.383(8) . ? C24 C25 1.380(8) . ? C25 C26 1.381(8) . ? C26 C27 1.388(6) . ? C28 C33 1.385(8) . ? C28 C29 1.394(7) . ? C29 C30 1.399(7) . ? C30 C31 1.381(9) . ? C31 C32 1.380(8) . ? C32 C33 1.384(8) . ? 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 C1 Pt1 C1 180.0(2) . 7_565 ? C1 Pt1 P1 85.81(14) . 7_565 ? C1 Pt1 P1 94.19(14) 7_565 7_565 ? C1 Pt1 P1 94.19(14) . . ? C1 Pt1 P1 85.81(14) 7_565 . ? P1 Pt1 P1 180.00(5) 7_565 . ? C22 P1 C28 104.2(2) . . ? C22 P1 C16 100.80(19) . . ? C28 P1 C16 104.2(2) . . ? C22 P1 Pt1 114.73(16) . . ? C28 P1 Pt1 112.43(17) . . ? C16 P1 Pt1 118.79(15) . . ? O1 N1 C9 127.6(4) . . ? O1 N1 C10 121.5(4) . . ? C9 N1 C10 110.7(5) . . ? O2 N2 C9 126.8(4) . . ? O2 N2 C13 121.9(4) . . ? C9 N2 C13 111.0(4) . . ? C2 C1 Pt1 176.3(5) . . ? C1 C2 C3 174.0(6) . . ? C4 C3 C8 118.8(5) . . ? C4 C3 C2 120.1(5) . . ? C8 C3 C2 121.1(5) . . ? C5 C4 C3 121.6(5) . . ? C4 C5 C6 119.6(6) . . ? C5 C6 C7 119.7(5) . . ? C5 C6 C9 117.7(5) . . ? C7 C6 C9 122.6(5) . . ? C8 C7 C6 119.8(5) . . ? C7 C8 C3 120.5(6) . . ? N2 C9 N1 108.5(4) . . ? N2 C9 C6 125.9(5) . . ? N1 C9 C6 125.5(5) . . ? C11 C10 N1 106.6(4) . . ? C11 C10 C12 110.7(5) . . ? N1 C10 C12 109.4(5) . . ? C11 C10 C13 113.7(5) . . ? N1 C10 C13 100.0(4) . . ? C12 C10 C13 115.4(5) . . ? N2 C13 C14 105.2(4) . . ? N2 C13 C15 109.6(4) . . ? C14 C13 C15 111.1(5) . . ? N2 C13 C10 99.8(4) . . ? C14 C13 C10 114.4(5) . . ? C15 C13 C10 115.5(5) . . ? C17 C16 C21 119.9(4) . . ? C17 C16 P1 123.0(3) . . ? C21 C16 P1 116.6(4) . . ? C16 C17 C18 121.2(4) . . ? C19 C18 C17 119.0(6) . . ? C20 C19 C18 120.9(4) . . ? C19 C20 C21 121.6(4) . . ? C20 C21 C16 117.5(5) . . ? C27 C22 C23 119.2(4) . . ? C27 C22 P1 120.7(4) . . ? C23 C22 P1 120.0(4) . . ? C24 C23 C22 119.7(5) . . ? C25 C24 C23 121.2(5) . . ? C24 C25 C26 119.3(5) . . ? C25 C26 C27 121.2(5) . . ? C26 C27 C22 119.4(5) . . ? C33 C28 C29 118.6(4) . . ? C33 C28 P1 118.8(3) . . ? C29 C28 P1 122.7(4) . . ? C28 C29 C30 120.6(5) . . ? C31 C30 C29 119.7(5) . . ? C32 C31 C30 119.8(5) . . ? C31 C32 C33 120.5(5) . . ? C32 C33 C28 120.8(5) . . ? 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 C1 Pt1 P1 C22 110.35(19) . . . . ? C1 Pt1 P1 C22 -69.65(19) 7_565 . . . ? P1 Pt1 P1 C22 -66(100) 7_565 . . . ? C1 Pt1 P1 C28 -130.8(2) . . . . ? C1 Pt1 P1 C28 49.2(2) 7_565 . . . ? P1 Pt1 P1 C28 53(100) 7_565 . . . ? C1 Pt1 P1 C16 -8.9(2) . . . . ? C1 Pt1 P1 C16 171.1(2) 7_565 . . . ? P1 Pt1 P1 C16 175(100) 7_565 . . . ? C1 Pt1 C1 C2 166(100) 7_565 . . . ? P1 Pt1 C1 C2 43(6) 7_565 . . . ? P1 Pt1 C1 C2 -137(6) . . . . ? Pt1 C1 C2 C3 28(10) . . . . ? C1 C2 C3 C4 -40(5) . . . . ? C1 C2 C3 C8 139(5) . . . . ? C8 C3 C4 C5 -2.5(7) . . . . ? C2 C3 C4 C5 176.3(4) . . . . ? C3 C4 C5 C6 0.9(7) . . . . ? C4 C5 C6 C7 1.0(7) . . . . ? C4 C5 C6 C9 -179.2(4) . . . . ? C5 C6 C7 C8 -1.2(7) . . . . ? C9 C6 C7 C8 179.0(4) . . . . ? C6 C7 C8 C3 -0.4(7) . . . . ? C4 C3 C8 C7 2.2(7) . . . . ? C2 C3 C8 C7 -176.6(4) . . . . ? O2 N2 C9 N1 -171.6(5) . . . . ? C13 N2 C9 N1 14.9(6) . . . . ? O2 N2 C9 C6 11.3(8) . . . . ? C13 N2 C9 C6 -162.2(5) . . . . ? O1 N1 C9 N2 -179.3(5) . . . . ? C10 N1 C9 N2 6.5(6) . . . . ? O1 N1 C9 C6 -2.2(9) . . . . ? C10 N1 C9 C6 -176.4(4) . . . . ? C5 C6 C9 N2 25.4(7) . . . . ? C7 C6 C9 N2 -154.8(5) . . . . ? C5 C6 C9 N1 -151.2(5) . . . . ? C7 C6 C9 N1 28.6(7) . . . . ? O1 N1 C10 C11 -79.7(6) . . . . ? C9 N1 C10 C11 94.8(6) . . . . ? O1 N1 C10 C12 40.1(7) . . . . ? C9 N1 C10 C12 -145.4(5) . . . . ? O1 N1 C10 C13 161.7(5) . . . . ? C9 N1 C10 C13 -23.8(5) . . . . ? O2 N2 C13 C14 -83.9(6) . . . . ? C9 N2 C13 C14 89.9(6) . . . . ? O2 N2 C13 C15 35.6(7) . . . . ? C9 N2 C13 C15 -150.6(5) . . . . ? O2 N2 C13 C10 157.3(5) . . . . ? C9 N2 C13 C10 -28.9(5) . . . . ? C11 C10 C13 N2 -84.2(5) . . . . ? N1 C10 C13 N2 29.1(4) . . . . ? C12 C10 C13 N2 146.2(4) . . . . ? C11 C10 C13 C14 164.1(4) . . . . ? N1 C10 C13 C14 -82.7(4) . . . . ? C12 C10 C13 C14 34.5(6) . . . . ? C11 C10 C13 C15 33.2(6) . . . . ? N1 C10 C13 C15 146.5(4) . . . . ? C12 C10 C13 C15 -96.4(6) . . . . ? C22 P1 C16 C17 101.4(4) . . . . ? C28 P1 C16 C17 -6.4(5) . . . . ? Pt1 P1 C16 C17 -132.4(4) . . . . ? C22 P1 C16 C21 -70.3(4) . . . . ? C28 P1 C16 C21 -178.1(4) . . . . ? Pt1 P1 C16 C21 55.9(4) . . . . ? C21 C16 C17 C18 1.7(7) . . . . ? P1 C16 C17 C18 -169.7(4) . . . . ? C16 C17 C18 C19 -0.7(8) . . . . ? C17 C18 C19 C20 -0.3(8) . . . . ? C18 C19 C20 C21 0.2(8) . . . . ? C19 C20 C21 C16 0.8(8) . . . . ? C17 C16 C21 C20 -1.7(7) . . . . ? P1 C16 C21 C20 170.2(4) . . . . ? C28 P1 C22 C27 -100.6(4) . . . . ? C16 P1 C22 C27 151.6(3) . . . . ? Pt1 P1 C22 C27 22.7(4) . . . . ? C28 P1 C22 C23 78.1(4) . . . . ? C16 P1 C22 C23 -29.7(4) . . . . ? Pt1 P1 C22 C23 -158.6(3) . . . . ? C27 C22 C23 C24 1.4(7) . . . . ? P1 C22 C23 C24 -177.3(4) . . . . ? C22 C23 C24 C25 -1.3(8) . . . . ? C23 C24 C25 C26 0.6(8) . . . . ? C24 C25 C26 C27 -0.2(8) . . . . ? C25 C26 C27 C22 0.4(8) . . . . ? C23 C22 C27 C26 -1.0(6) . . . . ? P1 C22 C27 C26 177.7(4) . . . . ? C22 P1 C28 C33 164.7(3) . . . . ? C16 P1 C28 C33 -90.0(4) . . . . ? Pt1 P1 C28 C33 39.9(4) . . . . ? C22 P1 C28 C29 -16.0(5) . . . . ? C16 P1 C28 C29 89.3(4) . . . . ? Pt1 P1 C28 C29 -140.8(4) . . . . ? C33 C28 C29 C30 0.3(7) . . . . ? P1 C28 C29 C30 -179.1(4) . . . . ? C28 C29 C30 C31 -1.0(8) . . . . ? C29 C30 C31 C32 1.4(8) . . . . ? C30 C31 C32 C33 -1.1(9) . . . . ? C31 C32 C33 C28 0.4(9) . . . . ? C29 C28 C33 C32 0.1(7) . . . . ? P1 C28 C33 C32 179.4(5) . . . . ? _diffrn_measured_fraction_theta_max 0.821 _diffrn_reflns_theta_full 26.10 _diffrn_measured_fraction_theta_full 0.821 _refine_diff_density_max 0.715 _refine_diff_density_min -1.577 _refine_diff_density_rms 0.101