Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Slawin, A.' 'Wainwright, Matthew' 'Woollins, Derek' _publ_contact_author_name 'Prof Derek Woollins' _publ_contact_author_address ; Chemistry U of St Andrews Dept of Chemistry University of St Andrews St Andrews KY16 9ST UNITED KINGDOM ; _publ_contact_author_email 'JDW3@ST-AND.AC.UK' _publ_section_title ; The Preparation and Coordination Chemistry of Phosphorus (III) Derivatives of Dialkyl Hydrazines ; data_15 _database_code_CSD 168562 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H34 Cl2 N2 O4 P2 Pt.0.5[C H2 Cl2]' _chemical_formula_sum 'C30.50 H35 Cl3 N2 O4 P2 Pt' _chemical_formula_weight 856.98 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' 'Cl' 'Cl' 0.1484 0.1585 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2861(2) _cell_length_b 11.91490(10) _cell_length_c 15.9825(2) _cell_angle_alpha 96.5460(10) _cell_angle_beta 99.1120(10) _cell_angle_gamma 106.8710(10) _cell_volume 1824.11(4) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 119 _cell_measurement_theta_min 12 _cell_measurement_theta_max 168 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max .31 _exptl_crystal_size_mid .14 _exptl_crystal_size_min .10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.560 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 846 _exptl_absorpt_coefficient_mu 4.188 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.656461 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 0.9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7820 _diffrn_reflns_av_R_equivalents 0.0160 _diffrn_reflns_av_sigmaI/netI 0.0364 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 23.23 _reflns_number_total 5135 _reflns_number_gt 4417 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART/SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _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^)+(0.0781P)^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 hand _refine_ls_extinction_coef ? _refine_ls_number_reflns 5135 _refine_ls_number_parameters 397 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0463 _refine_ls_R_factor_gt 0.0382 _refine_ls_wR_factor_ref 0.1076 _refine_ls_wR_factor_gt 0.1040 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.410 _refine_ls_shift/su_mean 0.009 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 0.05832(3) 0.48656(2) 0.252119(17) 0.04097(13) Uani 1 1 d . . . Cl1 Cl 0.03197(18) 0.67323(15) 0.22563(12) 0.0477(4) Uani 1 1 d . . . Cl2 Cl -0.18236(17) 0.41072(15) 0.25975(11) 0.0460(4) Uani 1 1 d . . . N1 N 0.2741(7) 0.3482(6) 0.2937(4) 0.0517(15) Uani 1 1 d . . . C29 C 0.3661(9) 0.3417(10) 0.3696(6) 0.075(3) Uani 1 1 d . . . H29A H 0.3167 0.2832 0.3996 0.112 Uiso 1 1 calc R . . H29B H 0.4006 0.4179 0.4064 0.112 Uiso 1 1 calc R . . H29C H 0.4425 0.3197 0.3534 0.112 Uiso 1 1 calc R . . N2 N 0.3381(6) 0.4312(5) 0.2449(4) 0.0514(15) Uani 1 1 d . . . C30 C 0.4143(11) 0.3865(9) 0.1872(7) 0.077(3) Uani 1 1 d . . . H30A H 0.4553 0.4477 0.1564 0.116 Uiso 1 1 calc R . . H30B H 0.3521 0.3189 0.1472 0.116 Uiso 1 1 calc R . . H30C H 0.4859 0.3633 0.2199 0.116 Uiso 1 1 calc R . . P1 P 0.1015(2) 0.32249(16) 0.28219(12) 0.0444(4) Uani 1 1 d . . . C1 C 0.0178(9) 0.1920(7) 0.2007(5) 0.0534(19) Uani 1 1 d . . . C2 C 0.0523(10) 0.0861(7) 0.2038(6) 0.066(2) Uani 1 1 d . . . O2 O 0.1531(7) 0.0897(5) 0.2696(4) 0.0729(17) Uani 1 1 d . . . C3 C -0.0179(13) -0.0142(8) 0.1398(7) 0.088(3) Uani 1 1 d . . . H3A H 0.0055 -0.0839 0.1408 0.105 Uiso 1 1 calc R . . C4 C -0.1194(14) -0.0089(10) 0.0767(8) 0.102(4) Uani 1 1 d . . . H4A H -0.1672 -0.0763 0.0357 0.123 Uiso 1 1 calc R . . C5 C -0.1532(12) 0.0928(10) 0.0719(7) 0.092(3) Uani 1 1 d . . . H5A H -0.2214 0.0947 0.0268 0.110 Uiso 1 1 calc R . . C6 C -0.0865(10) 0.1946(8) 0.1341(5) 0.067(2) Uani 1 1 d . . . H6A H -0.1113 0.2633 0.1312 0.081 Uiso 1 1 calc R . . C7 C 0.1810(15) -0.0231(10) 0.2779(10) 0.123(5) Uani 1 1 d . . . H7A H 0.2547 -0.0106 0.3265 0.185 Uiso 1 1 calc R . . H7B H 0.2076 -0.0515 0.2267 0.185 Uiso 1 1 calc R . . H7C H 0.0989 -0.0808 0.2860 0.185 Uiso 1 1 calc R . . C8 C 0.0510(8) 0.2780(7) 0.3797(5) 0.0493(18) Uani 1 1 d . . . C9 C 0.0986(8) 0.3612(7) 0.4582(5) 0.0528(19) Uani 1 1 d . . . O9 O 0.1901(7) 0.4681(5) 0.4552(3) 0.0682(16) Uani 1 1 d . . . C10 C 0.0537(9) 0.3307(9) 0.5315(5) 0.064(2) Uani 1 1 d . . . H10A H 0.0843 0.3860 0.5821 0.076 Uiso 1 1 calc R . . C11 C -0.0361(10) 0.2190(9) 0.5310(6) 0.075(3) Uani 1 1 d . . . H11A H -0.0626 0.1976 0.5814 0.090 Uiso 1 1 calc R . . C12 C -0.0857(10) 0.1401(10) 0.4551(7) 0.083(3) Uani 1 1 d . . . H12A H -0.1500 0.0661 0.4534 0.099 Uiso 1 1 calc R . . C13 C -0.0407(9) 0.1700(8) 0.3816(6) 0.068(2) Uani 1 1 d . . . H13A H -0.0741 0.1143 0.3312 0.081 Uiso 1 1 calc R . . C14 C 0.2529(15) 0.5480(10) 0.5336(6) 0.107(4) Uani 1 1 d . . . H14A H 0.3152 0.6195 0.5225 0.160 Uiso 1 1 calc R . . H14B H 0.3035 0.5116 0.5717 0.160 Uiso 1 1 calc R . . H14C H 0.1824 0.5671 0.5598 0.160 Uiso 1 1 calc R . . P2 P 0.2775(2) 0.54739(16) 0.23872(12) 0.0437(4) Uani 1 1 d . . . C15 C 0.3906(7) 0.6683(7) 0.3229(5) 0.0487(18) Uani 1 1 d . . . C16 C 0.5348(9) 0.7021(8) 0.3314(6) 0.060(2) Uani 1 1 d . . . O16 O 0.5792(6) 0.6447(6) 0.2696(5) 0.0790(19) Uani 1 1 d . . . C17 C 0.6210(10) 0.7885(9) 0.3987(7) 0.073(3) Uani 1 1 d . . . H17A H 0.7168 0.8072 0.4056 0.088 Uiso 1 1 calc R . . C18 C 0.5655(11) 0.8459(9) 0.4547(7) 0.080(3) Uani 1 1 d . . . H18A H 0.6239 0.9072 0.4976 0.096 Uiso 1 1 calc R . . C19 C 0.4204(10) 0.8140(8) 0.4488(6) 0.073(3) Uani 1 1 d . . . H19A H 0.3831 0.8512 0.4889 0.088 Uiso 1 1 calc R . . C20 C 0.3342(9) 0.7254(7) 0.3817(5) 0.059(2) Uani 1 1 d . . . H20A H 0.2385 0.7044 0.3763 0.071 Uiso 1 1 calc R . . C21 C 0.7185(11) 0.6969(13) 0.2568(8) 0.103(4) Uani 1 1 d . . . H21A H 0.7361 0.6469 0.2113 0.155 Uiso 1 1 calc R . . H21B H 0.7836 0.7042 0.3088 0.155 Uiso 1 1 calc R . . H21C H 0.7283 0.7742 0.2416 0.155 Uiso 1 1 calc R . . C22 C 0.3030(8) 0.5966(6) 0.1377(5) 0.0487(17) Uani 1 1 d . . . C23 C 0.2360(9) 0.5193(7) 0.0599(5) 0.059(2) Uani 1 1 d . . . O23 O 0.1586(7) 0.4068(5) 0.0671(4) 0.0788(19) Uani 1 1 d . . . C24 C 0.2521(11) 0.5558(9) -0.0182(6) 0.078(3) Uani 1 1 d . . . H24A H 0.2073 0.5047 -0.0697 0.093 Uiso 1 1 calc R . . C25 C 0.3362(12) 0.6698(9) -0.0177(6) 0.082(3) Uani 1 1 d . . . H25A H 0.3508 0.6936 -0.0698 0.098 Uiso 1 1 calc R . . C26 C 0.3982(12) 0.7480(9) 0.0561(6) 0.081(3) Uani 1 1 d . . . H26A H 0.4522 0.8251 0.0548 0.098 Uiso 1 1 calc R . . C27 C 0.3797(9) 0.7109(7) 0.1337(6) 0.060(2) Uani 1 1 d . . . H27A H 0.4202 0.7648 0.1845 0.072 Uiso 1 1 calc R . . C28 C 0.096(2) 0.3242(11) -0.0112(8) 0.159(8) Uani 1 1 d . . . H28A H 0.0444 0.2493 0.0016 0.239 Uiso 1 1 calc R . . H28B H 0.1672 0.3133 -0.0406 0.239 Uiso 1 1 calc R . . H28C H 0.0350 0.3547 -0.0471 0.239 Uiso 1 1 calc R . . C40 C 0.5868(15) 1.1150(13) 0.2186(8) 0.119(10) Uani 0.50 1 d PD . . H40A H 0.6733 1.1193 0.2001 0.143 Uiso 0.50 1 calc PR . . H40B H 0.5960 1.1939 0.2474 0.143 Uiso 0.50 1 calc PR . . Cl3 Cl 0.4590(6) 1.0802(4) 0.1293(3) 0.0808(14) Uani 0.50 1 d PD . . Cl4 Cl 0.5674(6) 1.0218(5) 0.2920(4) 0.109(2) Uani 0.50 1 d PD . . 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 0.04436(19) 0.03720(18) 0.03986(18) -0.00008(11) 0.00823(12) 0.01319(12) Cl1 0.0483(10) 0.0347(9) 0.0634(11) 0.0048(8) 0.0099(8) 0.0201(8) Cl2 0.0365(9) 0.0456(10) 0.0504(10) -0.0016(8) 0.0112(7) 0.0069(8) N1 0.055(4) 0.052(4) 0.051(4) 0.010(3) 0.004(3) 0.024(3) C29 0.059(5) 0.097(7) 0.077(6) 0.029(5) 0.012(5) 0.034(5) N2 0.052(4) 0.045(4) 0.064(4) 0.013(3) 0.019(3) 0.021(3) C30 0.098(7) 0.073(6) 0.088(7) 0.015(5) 0.048(6) 0.053(6) P1 0.0515(11) 0.0373(10) 0.0411(10) 0.0032(8) 0.0085(8) 0.0108(9) C1 0.070(5) 0.039(4) 0.048(4) -0.001(3) 0.012(4) 0.016(4) C2 0.078(6) 0.046(5) 0.071(6) -0.002(4) 0.017(5) 0.017(4) O2 0.100(5) 0.042(3) 0.076(4) 0.012(3) 0.005(4) 0.027(3) C3 0.114(9) 0.039(5) 0.090(7) -0.020(5) 0.005(7) 0.014(5) C4 0.117(9) 0.063(7) 0.099(9) -0.039(6) -0.012(7) 0.023(7) C5 0.094(8) 0.090(8) 0.065(6) -0.025(5) -0.010(5) 0.017(6) C6 0.080(6) 0.064(5) 0.051(5) -0.005(4) -0.001(4) 0.027(5) C7 0.135(11) 0.054(6) 0.167(13) 0.032(7) -0.019(9) 0.029(7) C8 0.052(4) 0.051(4) 0.043(4) 0.010(3) 0.010(3) 0.012(4) C9 0.059(5) 0.053(5) 0.044(4) 0.013(4) 0.007(4) 0.016(4) O9 0.090(4) 0.059(4) 0.039(3) 0.001(3) 0.003(3) 0.006(3) C10 0.067(5) 0.082(6) 0.045(5) 0.008(4) 0.013(4) 0.028(5) C11 0.086(7) 0.081(7) 0.062(6) 0.021(5) 0.026(5) 0.023(6) C12 0.073(6) 0.074(6) 0.092(8) 0.030(6) 0.028(5) -0.001(5) C13 0.073(6) 0.057(5) 0.060(5) 0.002(4) 0.012(4) 0.004(5) C14 0.156(11) 0.074(7) 0.050(6) -0.001(5) -0.016(6) -0.002(7) P2 0.0484(11) 0.0387(10) 0.0448(10) 0.0031(8) 0.0116(8) 0.0154(9) C15 0.045(4) 0.047(4) 0.052(4) 0.009(3) 0.007(3) 0.012(3) C16 0.062(5) 0.058(5) 0.063(5) 0.014(4) 0.011(4) 0.022(4) O16 0.052(3) 0.080(4) 0.101(5) -0.002(4) 0.023(3) 0.018(3) C17 0.066(6) 0.068(6) 0.078(7) 0.020(5) -0.001(5) 0.014(5) C18 0.087(7) 0.059(6) 0.067(6) 0.003(5) -0.010(5) -0.001(5) C19 0.080(7) 0.064(6) 0.063(6) -0.011(4) 0.013(5) 0.012(5) C20 0.062(5) 0.048(4) 0.060(5) -0.002(4) 0.014(4) 0.009(4) C21 0.064(7) 0.150(12) 0.102(9) 0.034(8) 0.036(6) 0.029(7) C22 0.058(5) 0.044(4) 0.047(4) 0.002(3) 0.013(3) 0.021(4) C23 0.071(5) 0.058(5) 0.050(5) 0.007(4) 0.021(4) 0.019(4) O23 0.113(5) 0.058(4) 0.050(3) -0.007(3) 0.024(3) 0.005(4) C24 0.107(8) 0.075(6) 0.048(5) 0.009(4) 0.021(5) 0.022(6) C25 0.113(8) 0.075(7) 0.064(6) 0.027(5) 0.029(6) 0.028(6) C26 0.109(8) 0.062(6) 0.069(6) 0.020(5) 0.021(6) 0.015(6) C27 0.072(5) 0.048(5) 0.060(5) 0.013(4) 0.014(4) 0.018(4) C28 0.26(2) 0.078(8) 0.072(8) -0.035(6) 0.054(10) -0.036(11) C40 0.19(3) 0.031(9) 0.100(18) 0.019(11) 0.045(18) -0.023(13) Cl3 0.119(4) 0.047(2) 0.069(3) 0.013(2) 0.004(3) 0.021(3) Cl4 0.098(4) 0.077(3) 0.109(4) 0.040(3) -0.035(3) -0.016(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 Pt1 P2 2.2119(19) . ? Pt1 P1 2.2137(19) . ? Pt1 Cl1 2.3933(16) . ? Pt1 Cl2 2.4047(17) . ? N1 N2 1.407(9) . ? N1 C29 1.440(10) . ? N1 P1 1.688(7) . ? N2 C30 1.452(10) . ? N2 P2 1.682(6) . ? P1 C8 1.807(7) . ? P1 C1 1.806(7) . ? C1 C6 1.395(12) . ? C1 C2 1.411(12) . ? C2 O2 1.342(11) . ? C2 C3 1.409(13) . ? O2 C7 1.469(12) . ? C3 C4 1.352(16) . ? C4 C5 1.362(16) . ? C5 C6 1.398(13) . ? C8 C13 1.364(11) . ? C8 C9 1.427(11) . ? C9 O9 1.358(10) . ? C9 C10 1.375(11) . ? O9 C14 1.417(10) . ? C10 C11 1.380(13) . ? C11 C12 1.371(14) . ? C12 C13 1.376(13) . ? P2 C22 1.812(8) . ? P2 C15 1.824(8) . ? C15 C20 1.393(11) . ? C15 C16 1.399(11) . ? C16 O16 1.350(11) . ? C16 C17 1.386(13) . ? O16 C21 1.444(11) . ? C17 C18 1.357(14) . ? C18 C19 1.414(14) . ? C19 C20 1.395(12) . ? C22 C27 1.375(11) . ? C22 C23 1.403(11) . ? C23 O23 1.374(10) . ? C23 C24 1.387(12) . ? O23 C28 1.429(12) . ? C24 C25 1.380(13) . ? C25 C26 1.354(13) . ? C26 C27 1.385(12) . ? C40 Cl4 1.7001(10) . ? C40 Cl3 1.6999(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 P2 Pt1 P1 85.05(7) . . ? P2 Pt1 Cl1 90.81(6) . . ? P1 Pt1 Cl1 175.03(7) . . ? P2 Pt1 Cl2 176.56(6) . . ? P1 Pt1 Cl2 93.29(7) . . ? Cl1 Pt1 Cl2 90.98(6) . . ? N2 N1 C29 113.6(6) . . ? N2 N1 P1 114.0(4) . . ? C29 N1 P1 126.0(6) . . ? N1 N2 C30 114.1(6) . . ? N1 N2 P2 115.5(5) . . ? C30 N2 P2 127.5(6) . . ? N1 P1 C8 108.0(3) . . ? N1 P1 C1 107.2(4) . . ? C8 P1 C1 104.6(4) . . ? N1 P1 Pt1 107.5(2) . . ? C8 P1 Pt1 114.1(3) . . ? C1 P1 Pt1 115.1(3) . . ? C6 C1 C2 119.0(8) . . ? C6 C1 P1 119.4(6) . . ? C2 C1 P1 121.7(6) . . ? O2 C2 C3 124.5(9) . . ? O2 C2 C1 115.9(7) . . ? C3 C2 C1 119.6(9) . . ? C2 O2 C7 116.2(7) . . ? C4 C3 C2 119.8(10) . . ? C3 C4 C5 121.5(9) . . ? C4 C5 C6 120.7(10) . . ? C5 C6 C1 119.4(9) . . ? C13 C8 C9 116.9(7) . . ? C13 C8 P1 123.1(6) . . ? C9 C8 P1 119.8(6) . . ? O9 C9 C10 123.6(8) . . ? O9 C9 C8 116.1(7) . . ? C10 C9 C8 120.2(8) . . ? C9 O9 C14 118.0(7) . . ? C11 C10 C9 120.8(8) . . ? C12 C11 C10 119.2(9) . . ? C11 C12 C13 120.2(9) . . ? C8 C13 C12 122.6(9) . . ? N2 P2 C22 107.5(3) . . ? N2 P2 C15 106.7(3) . . ? C22 P2 C15 106.0(3) . . ? N2 P2 Pt1 107.2(2) . . ? C22 P2 Pt1 114.4(3) . . ? C15 P2 Pt1 114.5(3) . . ? C20 C15 C16 119.0(7) . . ? C20 C15 P2 120.1(6) . . ? C16 C15 P2 120.8(6) . . ? O16 C16 C15 114.6(7) . . ? O16 C16 C17 124.6(8) . . ? C15 C16 C17 120.8(9) . . ? C16 O16 C21 118.4(8) . . ? C18 C17 C16 119.9(9) . . ? C17 C18 C19 121.0(9) . . ? C18 C19 C20 118.6(9) . . ? C15 C20 C19 120.5(8) . . ? C27 C22 C23 117.9(7) . . ? C27 C22 P2 122.3(6) . . ? C23 C22 P2 119.7(6) . . ? O23 C23 C24 123.4(8) . . ? O23 C23 C22 115.8(7) . . ? C24 C23 C22 120.7(8) . . ? C23 O23 C28 116.8(8) . . ? C25 C24 C23 118.5(9) . . ? C24 C25 C26 122.2(9) . . ? C27 C26 C25 118.7(9) . . ? C26 C27 C22 121.9(8) . . ? Cl4 C40 Cl3 117.3(4) . . ? 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 C29 N1 N2 C30 82.6(9) . . . . ? P1 N1 N2 C30 -123.8(7) . . . . ? C29 N1 N2 P2 -115.2(7) . . . . ? P1 N1 N2 P2 38.4(7) . . . . ? N2 N1 P1 C8 -152.6(5) . . . . ? C29 N1 P1 C8 -2.9(8) . . . . ? N2 N1 P1 C1 95.2(5) . . . . ? C29 N1 P1 C1 -115.1(8) . . . . ? N2 N1 P1 Pt1 -29.0(5) . . . . ? C29 N1 P1 Pt1 120.7(7) . . . . ? P2 Pt1 P1 N1 9.3(2) . . . . ? Cl1 Pt1 P1 N1 -24.3(8) . . . . ? Cl2 Pt1 P1 N1 -173.7(2) . . . . ? P2 Pt1 P1 C8 129.0(3) . . . . ? Cl1 Pt1 P1 C8 95.5(8) . . . . ? Cl2 Pt1 P1 C8 -54.0(3) . . . . ? P2 Pt1 P1 C1 -110.0(3) . . . . ? Cl1 Pt1 P1 C1 -143.6(8) . . . . ? Cl2 Pt1 P1 C1 67.0(3) . . . . ? N1 P1 C1 C6 -131.7(7) . . . . ? C8 P1 C1 C6 113.8(7) . . . . ? Pt1 P1 C1 C6 -12.2(8) . . . . ? N1 P1 C1 C2 50.1(8) . . . . ? C8 P1 C1 C2 -64.4(8) . . . . ? Pt1 P1 C1 C2 169.6(6) . . . . ? C6 C1 C2 O2 -179.8(8) . . . . ? P1 C1 C2 O2 -1.6(11) . . . . ? C6 C1 C2 C3 0.4(14) . . . . ? P1 C1 C2 C3 178.6(8) . . . . ? C3 C2 O2 C7 -5.7(15) . . . . ? C1 C2 O2 C7 174.6(9) . . . . ? O2 C2 C3 C4 179.1(11) . . . . ? C1 C2 C3 C4 -1.2(17) . . . . ? C2 C3 C4 C5 2(2) . . . . ? C3 C4 C5 C6 -2(2) . . . . ? C4 C5 C6 C1 1.3(17) . . . . ? C2 C1 C6 C5 -0.5(14) . . . . ? P1 C1 C6 C5 -178.8(8) . . . . ? N1 P1 C8 C13 -118.8(7) . . . . ? C1 P1 C8 C13 -4.9(8) . . . . ? Pt1 P1 C8 C13 121.7(7) . . . . ? N1 P1 C8 C9 66.6(7) . . . . ? C1 P1 C8 C9 -179.4(6) . . . . ? Pt1 P1 C8 C9 -52.8(7) . . . . ? C13 C8 C9 O9 179.8(7) . . . . ? P1 C8 C9 O9 -5.3(10) . . . . ? C13 C8 C9 C10 1.0(12) . . . . ? P1 C8 C9 C10 175.8(6) . . . . ? C10 C9 O9 C14 6.3(13) . . . . ? C8 C9 O9 C14 -172.5(9) . . . . ? O9 C9 C10 C11 -177.9(9) . . . . ? C8 C9 C10 C11 0.9(13) . . . . ? C9 C10 C11 C12 -3.1(15) . . . . ? C10 C11 C12 C13 3.4(16) . . . . ? C9 C8 C13 C12 -0.7(14) . . . . ? P1 C8 C13 C12 -175.4(8) . . . . ? C11 C12 C13 C8 -1.5(16) . . . . ? N1 N2 P2 C22 -151.6(5) . . . . ? C30 N2 P2 C22 7.7(9) . . . . ? N1 N2 P2 C15 95.0(6) . . . . ? C30 N2 P2 C15 -105.6(8) . . . . ? N1 N2 P2 Pt1 -28.2(6) . . . . ? C30 N2 P2 Pt1 131.2(7) . . . . ? P1 Pt1 P2 N2 7.6(3) . . . . ? Cl1 Pt1 P2 N2 -175.1(3) . . . . ? Cl2 Pt1 P2 N2 -53.6(11) . . . . ? P1 Pt1 P2 C22 126.7(3) . . . . ? Cl1 Pt1 P2 C22 -56.0(3) . . . . ? Cl2 Pt1 P2 C22 65.5(11) . . . . ? P1 Pt1 P2 C15 -110.6(3) . . . . ? Cl1 Pt1 P2 C15 66.7(3) . . . . ? Cl2 Pt1 P2 C15 -171.8(11) . . . . ? N2 P2 C15 C20 -127.1(7) . . . . ? C22 P2 C15 C20 118.5(7) . . . . ? Pt1 P2 C15 C20 -8.6(7) . . . . ? N2 P2 C15 C16 50.4(7) . . . . ? C22 P2 C15 C16 -63.9(7) . . . . ? Pt1 P2 C15 C16 168.9(5) . . . . ? C20 C15 C16 O16 -177.7(8) . . . . ? P2 C15 C16 O16 4.7(10) . . . . ? C20 C15 C16 C17 1.9(12) . . . . ? P2 C15 C16 C17 -175.7(7) . . . . ? C15 C16 O16 C21 161.1(8) . . . . ? C17 C16 O16 C21 -18.5(13) . . . . ? O16 C16 C17 C18 176.1(9) . . . . ? C15 C16 C17 C18 -3.5(13) . . . . ? C16 C17 C18 C19 4.0(15) . . . . ? C17 C18 C19 C20 -2.8(14) . . . . ? C16 C15 C20 C19 -0.8(12) . . . . ? P2 C15 C20 C19 176.8(7) . . . . ? C18 C19 C20 C15 1.2(14) . . . . ? N2 P2 C22 C27 -122.0(7) . . . . ? C15 P2 C22 C27 -8.2(8) . . . . ? Pt1 P2 C22 C27 119.0(6) . . . . ? N2 P2 C22 C23 62.2(7) . . . . ? C15 P2 C22 C23 176.1(6) . . . . ? Pt1 P2 C22 C23 -56.7(7) . . . . ? C27 C22 C23 O23 -178.9(7) . . . . ? P2 C22 C23 O23 -2.9(11) . . . . ? C27 C22 C23 C24 2.9(13) . . . . ? P2 C22 C23 C24 178.9(7) . . . . ? C24 C23 O23 C28 1.9(16) . . . . ? C22 C23 O23 C28 -176.3(11) . . . . ? O23 C23 C24 C25 -177.8(9) . . . . ? C22 C23 C24 C25 0.3(15) . . . . ? C23 C24 C25 C26 -2.9(17) . . . . ? C24 C25 C26 C27 2.0(18) . . . . ? C25 C26 C27 C22 1.5(16) . . . . ? C23 C22 C27 C26 -3.9(13) . . . . ? P2 C22 C27 C26 -179.7(8) . . . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 23.23 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.128 _refine_diff_density_min -1.082 _refine_diff_density_rms 0.129 data_14 _database_code_CSD 168563 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H38 Cl2 N2 O4 P2 Pt.1.5[C H2 Cl2].H2 O' _chemical_formula_sum 'C33.50 H43 Cl5 N2 O5 P2 Pt' _chemical_formula_weight 987.98 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' 'Cl' 'Cl' 0.1484 0.1585 '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 24.3478(7) _cell_length_b 14.2665(3) _cell_length_c 14.7842(4) _cell_angle_alpha 90.00 _cell_angle_beta 111.4580(10) _cell_angle_gamma 90.00 _cell_volume 4779.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 54 _cell_measurement_theta_min 12 _cell_measurement_theta_max 168 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.373 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1964 _exptl_absorpt_coefficient_mu 3.316 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.419079 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 0.9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13948 _diffrn_reflns_av_R_equivalents 0.1461 _diffrn_reflns_av_sigmaI/netI 0.2175 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 28.58 _reflns_number_total 5501 _reflns_number_gt 2555 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART/SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _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^)+(0.1193P)^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 SHELXL _refine_ls_extinction_coef 0.00000(16) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5501 _refine_ls_number_parameters 247 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1946 _refine_ls_R_factor_gt 0.0875 _refine_ls_wR_factor_ref 0.2447 _refine_ls_wR_factor_gt 0.1983 _refine_ls_goodness_of_fit_ref 0.953 _refine_ls_restrained_S_all 0.953 _refine_ls_shift/su_max 2.152 _refine_ls_shift/su_mean 0.036 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 0.5000 -0.44160(6) 0.2500 0.0418(3) Uani 1 2 d S . . Cl1 Cl 0.57465(14) -0.5591(3) 0.2780(2) 0.0495(8) Uani 1 1 d . . . P1 P 0.43487(14) -0.3267(3) 0.2285(2) 0.0408(8) Uani 1 1 d . . . C1 C 0.3879(5) -0.3412(9) 0.2982(8) 0.041(3) Uani 1 1 d . . . C2 C 0.4111(6) -0.3539(11) 0.4013(10) 0.055(4) Uani 1 1 d . . . C3 C 0.3751(7) -0.3731(13) 0.4507(11) 0.068(5) Uani 1 1 d . . . H3A H 0.3908 -0.3790 0.5180 0.082 Uiso 1 1 calc R . . C4 C 0.3142(7) -0.3840(13) 0.4004(12) 0.073(5) Uani 1 1 d . . . H4A H 0.2901 -0.3988 0.4346 0.088 Uiso 1 1 calc R . . C5 C 0.2901(6) -0.3731(13) 0.3023(13) 0.077(5) Uani 1 1 d . . . H5A H 0.2497 -0.3803 0.2695 0.092 Uiso 1 1 calc R . . C6 C 0.3264(6) -0.3512(11) 0.2521(10) 0.062(4) Uani 1 1 d . . . H6A H 0.3095 -0.3428 0.1852 0.074 Uiso 1 1 calc R . . C7 C 0.3841(5) -0.3142(9) 0.1005(9) 0.043(3) Uani 1 1 d . . . C8 C 0.3483(5) -0.2310(10) 0.0713(10) 0.048(3) Uani 1 1 d . . . C9 C 0.3154(7) -0.2165(13) -0.0258(12) 0.074(5) Uani 1 1 d . . . H9A H 0.2928 -0.1627 -0.0467 0.089 Uiso 1 1 calc R . . C10 C 0.3173(7) -0.2855(14) -0.0917(11) 0.075(5) Uani 1 1 d . . . H10A H 0.2948 -0.2761 -0.1570 0.090 Uiso 1 1 calc R . . C11 C 0.3489(7) -0.3633(12) -0.0678(10) 0.065(4) Uani 1 1 d . . . H11A H 0.3490 -0.4064 -0.1149 0.078 Uiso 1 1 calc R . . C12 C 0.3837(6) -0.3792(11) 0.0351(9) 0.051(4) Uani 1 1 d . . . H12A H 0.4054 -0.4341 0.0549 0.061 Uiso 1 1 calc R . . N1 N 0.4739(4) -0.2202(9) 0.2575(7) 0.054(3) Uani 1 1 d . . . C13 C 0.4679(8) -0.1580(16) 0.3244(15) 0.099(7) Uani 1 1 d . . . H13A H 0.4394 -0.1857 0.3485 0.119 Uiso 1 1 calc R . . H13B H 0.4491 -0.1026 0.2881 0.119 Uiso 1 1 calc R . . C14 C 0.5153(8) -0.1251(19) 0.4077(14) 0.119(8) Uani 1 1 d . . . H14A H 0.5004 -0.0824 0.4434 0.178 Uiso 1 1 calc R . . H14B H 0.5437 -0.0936 0.3875 0.178 Uiso 1 1 calc R . . H14C H 0.5338 -0.1773 0.4485 0.178 Uiso 1 1 calc R . . O2 O 0.4707(4) -0.3438(9) 0.4423(6) 0.073(3) Uani 1 1 d . . . C15 C 0.4948(7) -0.3633(19) 0.5449(11) 0.113(9) Uani 1 1 d . . . H15A H 0.5368 -0.3548 0.5688 0.170 Uiso 1 1 calc R . . H15B H 0.4859 -0.4269 0.5560 0.170 Uiso 1 1 calc R . . H15C H 0.4778 -0.3214 0.5782 0.170 Uiso 1 1 calc R . . O8 O 0.3506(4) -0.1697(7) 0.1438(7) 0.062(3) Uani 1 1 d . . . C16 C 0.3214(8) -0.0783(12) 0.1152(17) 0.095(6) Uani 1 1 d . . . H16A H 0.3261 -0.0421 0.1723 0.142 Uiso 1 1 calc R . . H16B H 0.2801 -0.0878 0.0787 0.142 Uiso 1 1 calc R . . H16C H 0.3388 -0.0453 0.0758 0.142 Uiso 1 1 calc R . . C20 C 0.1922(18) 0.377(3) 0.129(3) 0.110(15) Uani 0.50 1 d P . . H20A H 0.1773 0.3290 0.0800 0.131 Uiso 0.50 1 calc PR . . H20B H 0.1939 0.3505 0.1907 0.131 Uiso 0.50 1 calc PR . . Cl2 Cl 0.2619(5) 0.4068(10) 0.1385(9) 0.113(4) Uani 0.50 1 d P . . Cl3 Cl 0.1450(5) 0.4679(9) 0.1011(10) 0.123(5) Uani 0.50 1 d P . . C30 C 0.421(2) 0.199(4) 0.221(4) 0.046(14) Uiso 0.25 1 d P . . H30A H 0.4456 0.1686 0.1913 0.056 Uiso 0.25 1 calc PR . . H30B H 0.4349 0.2613 0.2427 0.056 Uiso 0.25 1 calc PR . . Cl4 Cl 0.3404(10) 0.1958(16) 0.142(2) 0.116(8) Uani 0.25 1 d P . . Cl5 Cl 0.4105(15) 0.1322(17) 0.3094(19) 0.140(10) Uani 0.25 1 d P . . O40 O 0.5000 -0.6785(18) 0.2500 0.151(9) Uiso 1 2 d S . . 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 0.0460(5) 0.0571(6) 0.0144(3) 0.000 0.0018(3) 0.000 Cl1 0.0566(18) 0.0487(19) 0.0383(17) 0.0027(17) 0.0117(14) 0.0102(17) P1 0.0447(18) 0.050(2) 0.0222(15) 0.0047(15) 0.0061(14) -0.0004(16) C1 0.044(7) 0.051(8) 0.023(6) 0.011(6) 0.006(5) 0.002(6) C2 0.063(9) 0.075(11) 0.030(7) -0.009(7) 0.023(7) -0.003(7) C3 0.061(10) 0.109(14) 0.038(8) 0.001(9) 0.023(8) 0.012(9) C4 0.072(11) 0.106(14) 0.050(10) 0.024(10) 0.031(9) 0.005(10) C5 0.044(8) 0.129(16) 0.061(11) 0.020(11) 0.025(8) -0.002(9) C6 0.061(9) 0.092(12) 0.028(7) 0.008(8) 0.011(7) 0.002(8) C7 0.047(7) 0.046(8) 0.035(7) 0.005(6) 0.016(6) -0.006(6) C8 0.043(7) 0.059(9) 0.038(7) 0.011(7) 0.011(6) 0.005(6) C9 0.065(9) 0.089(13) 0.043(9) 0.020(9) -0.010(8) 0.006(9) C10 0.078(11) 0.106(15) 0.027(8) 0.013(9) 0.005(8) 0.009(10) C11 0.082(11) 0.069(11) 0.029(7) -0.006(7) 0.001(7) 0.008(9) C12 0.059(8) 0.066(10) 0.020(6) 0.008(7) 0.004(6) 0.009(7) N1 0.022(5) 0.118(10) 0.022(5) -0.031(6) 0.006(4) 0.004(5) C13 0.089(13) 0.130(18) 0.085(14) -0.044(13) 0.039(12) -0.026(12) C14 0.085(13) 0.20(2) 0.061(13) -0.053(15) 0.013(10) -0.020(14) O2 0.053(6) 0.145(11) 0.014(4) 0.012(6) 0.003(4) 0.000(6) C15 0.066(11) 0.24(3) 0.020(8) 0.002(12) 0.003(7) 0.018(14) O8 0.068(6) 0.073(7) 0.038(5) 0.003(5) 0.012(5) 0.012(5) C16 0.087(13) 0.080(14) 0.113(17) 0.018(12) 0.032(12) 0.023(10) C20 0.14(4) 0.12(4) 0.09(3) -0.02(3) 0.06(3) -0.04(3) Cl2 0.092(7) 0.154(10) 0.094(8) -0.018(7) 0.036(6) -0.015(7) Cl3 0.108(8) 0.157(11) 0.137(10) 0.085(9) 0.084(8) 0.027(7) Cl4 0.123(17) 0.096(16) 0.14(2) 0.001(15) 0.058(15) -0.039(13) Cl5 0.23(3) 0.095(17) 0.090(17) -0.035(14) 0.059(19) 0.004(17) _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 P1 2.221(4) . ? Pt1 P1 2.221(4) 2_655 ? Pt1 Cl1 2.395(3) 2_655 ? Pt1 Cl1 2.395(3) . ? P1 N1 1.760(13) . ? P1 C1 1.811(13) . ? P1 C7 1.851(13) . ? C1 C6 1.408(17) . ? C1 C2 1.430(17) . ? C2 O2 1.360(16) . ? C2 C3 1.357(19) . ? C3 C4 1.40(2) . ? C4 C5 1.36(2) . ? C5 C6 1.38(2) . ? C7 C12 1.337(18) . ? C7 C8 1.443(18) . ? C8 O8 1.369(16) . ? C8 C9 1.379(19) . ? C9 C10 1.40(2) . ? C10 C11 1.32(2) . ? C11 C12 1.464(18) . ? N1 N1 1.366(18) 2_655 ? N1 C13 1.38(2) . ? C13 C14 1.43(2) . ? O2 C15 1.439(17) . ? O8 C16 1.472(18) . ? C20 Cl3 1.68(5) . ? C20 Cl2 1.70(4) . ? C30 Cl5 1.70(6) . ? C30 Cl4 1.87(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Pt1 P1 84.86(18) . 2_655 ? P1 Pt1 Cl1 92.02(12) . 2_655 ? P1 Pt1 Cl1 176.68(13) 2_655 2_655 ? P1 Pt1 Cl1 176.68(13) . . ? P1 Pt1 Cl1 92.02(12) 2_655 . ? Cl1 Pt1 Cl1 91.12(18) 2_655 . ? N1 P1 C1 110.9(5) . . ? N1 P1 C7 105.4(5) . . ? C1 P1 C7 105.5(5) . . ? N1 P1 Pt1 108.0(4) . . ? C1 P1 Pt1 113.6(4) . . ? C7 P1 Pt1 113.1(5) . . ? C6 C1 C2 116.0(12) . . ? C6 C1 P1 121.2(9) . . ? C2 C1 P1 122.4(9) . . ? O2 C2 C3 125.1(13) . . ? O2 C2 C1 113.7(11) . . ? C3 C2 C1 121.2(13) . . ? C2 C3 C4 120.1(14) . . ? C5 C4 C3 120.9(15) . . ? C4 C5 C6 119.1(14) . . ? C5 C6 C1 122.6(13) . . ? C12 C7 C8 120.6(12) . . ? C12 C7 P1 119.9(10) . . ? C8 C7 P1 119.3(10) . . ? O8 C8 C9 124.2(14) . . ? O8 C8 C7 116.3(11) . . ? C9 C8 C7 119.5(14) . . ? C8 C9 C10 117.7(15) . . ? C11 C10 C9 124.7(14) . . ? C10 C11 C12 117.8(14) . . ? C7 C12 C11 119.5(13) . . ? N1 N1 C13 117.8(11) 2_655 . ? N1 N1 P1 114.3(4) 2_655 . ? C13 N1 P1 122.7(11) . . ? N1 C13 C14 124.5(17) . . ? C2 O2 C15 114.0(11) . . ? C8 O8 C16 117.6(12) . . ? Cl3 C20 Cl2 113(3) . . ? Cl5 C30 Cl4 93(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P1 Pt1 P1 N1 -8.0(3) 2_655 . . . ? Cl1 Pt1 P1 N1 173.1(4) 2_655 . . . ? Cl1 Pt1 P1 N1 12(2) . . . . ? P1 Pt1 P1 C1 -131.5(5) 2_655 . . . ? Cl1 Pt1 P1 C1 49.6(4) 2_655 . . . ? Cl1 Pt1 P1 C1 -111(2) . . . . ? P1 Pt1 P1 C7 108.2(5) 2_655 . . . ? Cl1 Pt1 P1 C7 -70.7(4) 2_655 . . . ? Cl1 Pt1 P1 C7 128(2) . . . . ? N1 P1 C1 C6 120.5(11) . . . . ? C7 P1 C1 C6 6.8(13) . . . . ? Pt1 P1 C1 C6 -117.7(10) . . . . ? N1 P1 C1 C2 -66.9(13) . . . . ? C7 P1 C1 C2 179.4(11) . . . . ? Pt1 P1 C1 C2 54.9(12) . . . . ? C6 C1 C2 O2 179.8(12) . . . . ? P1 C1 C2 O2 6.9(18) . . . . ? C6 C1 C2 C3 -1(2) . . . . ? P1 C1 C2 C3 -174.0(12) . . . . ? O2 C2 C3 C4 -178.7(16) . . . . ? C1 C2 C3 C4 2(3) . . . . ? C2 C3 C4 C5 -2(3) . . . . ? C3 C4 C5 C6 0(3) . . . . ? C4 C5 C6 C1 1(3) . . . . ? C2 C1 C6 C5 -1(2) . . . . ? P1 C1 C6 C5 172.4(13) . . . . ? N1 P1 C7 C12 127.0(11) . . . . ? C1 P1 C7 C12 -115.6(11) . . . . ? Pt1 P1 C7 C12 9.2(12) . . . . ? N1 P1 C7 C8 -48.7(11) . . . . ? C1 P1 C7 C8 68.8(11) . . . . ? Pt1 P1 C7 C8 -166.4(8) . . . . ? C12 C7 C8 O8 178.5(12) . . . . ? P1 C7 C8 O8 -5.9(16) . . . . ? C12 C7 C8 C9 -3(2) . . . . ? P1 C7 C8 C9 172.8(11) . . . . ? O8 C8 C9 C10 -179.9(14) . . . . ? C7 C8 C9 C10 2(2) . . . . ? C8 C9 C10 C11 -1(3) . . . . ? C9 C10 C11 C12 1(3) . . . . ? C8 C7 C12 C11 3(2) . . . . ? P1 C7 C12 C11 -172.5(11) . . . . ? C10 C11 C12 C7 -2(2) . . . . ? C1 P1 N1 N1 153.7(9) . . . 2_655 ? C7 P1 N1 N1 -92.5(10) . . . 2_655 ? Pt1 P1 N1 N1 28.6(11) . . . 2_655 ? C1 P1 N1 C13 -0.4(15) . . . . ? C7 P1 N1 C13 113.4(14) . . . . ? Pt1 P1 N1 C13 -125.5(13) . . . . ? N1 N1 C13 C14 -30(3) 2_655 . . . ? P1 N1 C13 C14 124(2) . . . . ? C3 C2 O2 C15 5(2) . . . . ? C1 C2 O2 C15 -175.6(16) . . . . ? C9 C8 O8 C16 -7(2) . . . . ? C7 C8 O8 C16 171.7(12) . . . . ? _diffrn_measured_fraction_theta_max 0.902 _diffrn_reflns_theta_full 28.58 _diffrn_measured_fraction_theta_full 0.902 _refine_diff_density_max 3.134 _refine_diff_density_min -4.765 _refine_diff_density_rms 0.240 data_8 _database_code_CSD 168564 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H30 Cl2 N2 O4 P2 Pt' _chemical_formula_sum 'C28 H30 Cl2 N2 O4 P2 Pt' _chemical_formula_weight 786.47 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' 'Cl' 'Cl' 0.1484 0.1585 '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 Orthorhombic _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 8.7379(3) _cell_length_b 17.2627(5) _cell_length_c 40.8907(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6167.9(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 169 _cell_measurement_theta_min 12 _cell_measurement_theta_max 168 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max .21 _exptl_crystal_size_mid .11 _exptl_crystal_size_min .08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.694 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3088 _exptl_absorpt_coefficient_mu 4.862 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.648006 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 0.9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25273 _diffrn_reflns_av_R_equivalents 0.0566 _diffrn_reflns_av_sigmaI/netI 0.0382 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 23.27 _reflns_number_total 4399 _reflns_number_gt 3186 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART/SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _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^)+(0.0342P)^2^+4.6247P] 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 SHELXL _refine_ls_extinction_coef 0.00123(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4399 _refine_ls_number_parameters 353 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0586 _refine_ls_R_factor_gt 0.0339 _refine_ls_wR_factor_ref 0.0696 _refine_ls_wR_factor_gt 0.0631 _refine_ls_goodness_of_fit_ref 0.982 _refine_ls_restrained_S_all 0.982 _refine_ls_shift/su_max 0.060 _refine_ls_shift/su_mean 0.004 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 0.27245(2) -0.451402(15) 0.368062(6) 0.04731(11) Uani 1 1 d . . . Cl1 Cl 0.4250(2) -0.53352(11) 0.40003(4) 0.0754(5) Uani 1 1 d . . . Cl2 Cl 0.26449(19) -0.54223(9) 0.32545(4) 0.0631(4) Uani 1 1 d . . . P1 P 0.13098(18) -0.37024(9) 0.34051(4) 0.0475(4) Uani 1 1 d . . . N1 N 0.1174(6) -0.2895(3) 0.36168(12) 0.0583(15) Uani 1 1 d . . . C13 C 0.0037(9) -0.2279(4) 0.3558(2) 0.081(2) Uani 1 1 d . . . H13A H -0.0391 -0.2341 0.3341 0.097 Uiso 1 1 calc R . . H13B H 0.0542 -0.1779 0.3567 0.097 Uiso 1 1 calc R . . C14 C -0.1245(11) -0.2296(5) 0.3807(2) 0.118(3) Uani 1 1 d . . . H14A H -0.1970 -0.1895 0.3758 0.177 Uiso 1 1 calc R . . H14B H -0.0831 -0.2213 0.4022 0.177 Uiso 1 1 calc R . . H14C H -0.1746 -0.2790 0.3800 0.177 Uiso 1 1 calc R . . P2 P 0.26002(19) -0.36097(11) 0.40508(4) 0.0542(4) Uani 1 1 d . . . N2 N 0.2244(6) -0.2746(3) 0.38773(14) 0.0618(15) Uani 1 1 d . . . C27 C 0.3626(15) -0.2288(6) 0.3748(2) 0.132(5) Uani 1 1 d . . . H27A H 0.4407 -0.2657 0.3684 0.159 Uiso 1 1 calc R . . H27B H 0.3308 -0.2015 0.3553 0.159 Uiso 1 1 calc R . . C28 C 0.4267(13) -0.1776(7) 0.3950(3) 0.151(4) Uani 1 1 d . . . H28A H 0.5114 -0.1531 0.3842 0.227 Uiso 1 1 calc R . . H28B H 0.4624 -0.2037 0.4143 0.227 Uiso 1 1 calc R . . H28C H 0.3525 -0.1392 0.4010 0.227 Uiso 1 1 calc R . . O1 O 0.1721(5) -0.3507(2) 0.30330(10) 0.0574(11) Uani 1 1 d . . . C1 C 0.3133(7) -0.3145(4) 0.29576(14) 0.0495(16) Uani 1 1 d . . . C2 C 0.3156(8) -0.2360(4) 0.29130(16) 0.0615(18) Uani 1 1 d . . . H2A H 0.2260 -0.2073 0.2930 0.074 Uiso 1 1 calc R . . C3 C 0.4517(10) -0.2003(4) 0.28432(18) 0.076(2) Uani 1 1 d . . . H3A H 0.4544 -0.1468 0.2816 0.091 Uiso 1 1 calc R . . C4 C 0.5834(9) -0.2422(5) 0.28128(19) 0.084(2) Uani 1 1 d . . . H4A H 0.6755 -0.2175 0.2767 0.100 Uiso 1 1 calc R . . C5 C 0.5788(9) -0.3223(5) 0.28503(19) 0.084(2) Uani 1 1 d . . . H5A H 0.6676 -0.3513 0.2823 0.101 Uiso 1 1 calc R . . C6 C 0.4428(9) -0.3590(4) 0.29277(16) 0.068(2) Uani 1 1 d . . . H6A H 0.4391 -0.4123 0.2959 0.082 Uiso 1 1 calc R . . O7 O -0.0447(4) -0.3898(2) 0.33640(10) 0.0577(12) Uani 1 1 d . . . C7 C -0.1178(6) -0.4486(4) 0.31838(16) 0.0536(16) Uani 1 1 d . . . C8 C -0.0868(8) -0.4621(4) 0.28623(16) 0.0650(19) Uani 1 1 d . . . H8A H -0.0073 -0.4363 0.2757 0.078 Uiso 1 1 calc R . . C9 C -0.1773(9) -0.5156(5) 0.2694(2) 0.076(2) Uani 1 1 d . . . H9A H -0.1593 -0.5255 0.2474 0.091 Uiso 1 1 calc R . . C10 C -0.2926(9) -0.5534(5) 0.2854(3) 0.089(3) Uani 1 1 d . . . H10A H -0.3524 -0.5895 0.2744 0.107 Uiso 1 1 calc R . . C11 C -0.3197(9) -0.5385(5) 0.3173(2) 0.087(2) Uani 1 1 d . . . H11A H -0.3995 -0.5641 0.3278 0.104 Uiso 1 1 calc R . . C12 C -0.2318(8) -0.4862(5) 0.3346(2) 0.072(2) Uani 1 1 d . . . H12A H -0.2498 -0.4769 0.3567 0.086 Uiso 1 1 calc R . . O15 O 0.1232(5) -0.3685(3) 0.43044(10) 0.0650(12) Uani 1 1 d . . . C15 C 0.0477(8) -0.4377(5) 0.43774(18) 0.067(2) Uani 1 1 d . . . C16 C -0.0933(10) -0.4504(7) 0.4262(2) 0.113(3) Uani 1 1 d . . . H16A H -0.1389 -0.4142 0.4125 0.136 Uiso 1 1 calc R . . C17 C -0.1738(14) -0.5192(9) 0.4348(3) 0.140(5) Uani 1 1 d . . . H17A H -0.2717 -0.5297 0.4271 0.168 Uiso 1 1 calc R . . C18 C -0.0989(17) -0.5681(8) 0.4549(4) 0.144(5) Uani 1 1 d . . . H18A H -0.1479 -0.6140 0.4607 0.173 Uiso 1 1 calc R . . C19 C 0.0416(15) -0.5553(7) 0.4673(3) 0.136(4) Uani 1 1 d . . . H19A H 0.0878 -0.5901 0.4815 0.163 Uiso 1 1 calc R . . C20 C 0.1127(10) -0.4888(5) 0.4578(2) 0.099(3) Uani 1 1 d . . . H20A H 0.2106 -0.4787 0.4656 0.119 Uiso 1 1 calc R . . O21 O 0.4079(5) -0.3448(3) 0.42564(12) 0.0814(15) Uani 1 1 d . . . C21 C 0.4239(8) -0.3385(4) 0.45983(18) 0.0628(19) Uani 1 1 d . . . C22 C 0.5132(10) -0.3897(5) 0.4750(3) 0.109(3) Uani 1 1 d . . . H22A H 0.5589 -0.4299 0.4634 0.131 Uiso 1 1 calc R . . C23 C 0.5373(14) -0.3822(9) 0.5087(4) 0.135(5) Uani 1 1 d . . . H23A H 0.5957 -0.4186 0.5199 0.162 Uiso 1 1 calc R . . C24 C 0.4774(17) -0.3238(10) 0.5242(3) 0.139(6) Uani 1 1 d . . . H24A H 0.4982 -0.3182 0.5464 0.167 Uiso 1 1 calc R . . C25 C 0.3863(15) -0.2708(7) 0.5096(3) 0.120(4) Uani 1 1 d . . . H25A H 0.3424 -0.2303 0.5213 0.144 Uiso 1 1 calc R . . C26 C 0.3617(10) -0.2799(5) 0.4764(2) 0.085(2) Uani 1 1 d . . . H26A H 0.3006 -0.2443 0.4654 0.101 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 0.05019(16) 0.04561(16) 0.04615(16) -0.00203(13) -0.00058(12) -0.00278(12) Cl1 0.0855(13) 0.0720(13) 0.0687(12) 0.0028(10) -0.0176(10) 0.0182(10) Cl2 0.0832(12) 0.0444(9) 0.0618(11) -0.0103(8) -0.0042(8) 0.0009(9) P1 0.0522(10) 0.0446(10) 0.0458(11) -0.0029(8) -0.0022(8) -0.0051(8) N1 0.065(4) 0.056(4) 0.054(4) -0.011(3) -0.014(3) 0.003(3) C13 0.082(6) 0.053(5) 0.109(7) -0.011(4) -0.024(5) 0.017(4) C14 0.105(7) 0.117(8) 0.132(9) -0.021(7) 0.019(6) 0.040(6) P2 0.0551(10) 0.0579(10) 0.0497(11) -0.0115(8) -0.0065(8) -0.0017(9) N2 0.071(4) 0.042(3) 0.072(4) -0.018(3) -0.012(3) -0.007(3) C27 0.202(12) 0.089(7) 0.106(8) 0.020(6) -0.059(8) -0.071(8) C28 0.151(10) 0.140(10) 0.162(11) 0.022(9) -0.025(9) -0.037(8) O1 0.059(3) 0.062(3) 0.051(3) 0.001(2) -0.006(2) -0.014(2) C1 0.060(4) 0.049(4) 0.039(4) 0.000(3) -0.005(3) -0.007(3) C2 0.082(5) 0.051(4) 0.052(5) 0.013(3) 0.002(4) -0.001(4) C3 0.089(6) 0.056(5) 0.082(6) 0.015(4) 0.010(4) -0.016(4) C4 0.073(6) 0.087(7) 0.090(7) 0.008(5) 0.019(4) -0.014(5) C5 0.075(6) 0.077(6) 0.102(7) 0.007(5) 0.022(5) 0.013(5) C6 0.084(5) 0.051(4) 0.070(5) 0.004(4) 0.016(4) 0.005(4) O7 0.048(3) 0.064(3) 0.061(3) -0.012(2) -0.004(2) -0.006(2) C7 0.042(4) 0.056(4) 0.062(5) 0.000(4) -0.012(3) 0.001(3) C8 0.062(4) 0.078(5) 0.055(5) -0.009(4) 0.000(3) -0.006(4) C9 0.075(5) 0.082(6) 0.072(6) -0.023(4) -0.016(4) 0.002(4) C10 0.075(6) 0.064(5) 0.127(8) -0.025(6) -0.031(5) -0.004(5) C11 0.071(5) 0.080(6) 0.109(7) -0.002(6) -0.007(5) -0.021(4) C12 0.068(5) 0.080(5) 0.068(5) 0.003(4) -0.002(4) -0.021(4) O15 0.069(3) 0.067(3) 0.059(3) -0.010(3) 0.003(2) 0.003(3) C15 0.057(5) 0.088(6) 0.056(5) -0.008(4) 0.008(4) -0.001(4) C16 0.082(7) 0.176(11) 0.082(6) -0.020(7) -0.006(5) -0.025(7) C17 0.078(8) 0.193(16) 0.150(13) -0.048(10) 0.013(7) -0.053(9) C18 0.119(12) 0.149(13) 0.165(14) -0.040(10) 0.062(10) -0.046(10) C19 0.133(10) 0.116(10) 0.158(11) 0.024(8) 0.040(8) -0.009(8) C20 0.085(6) 0.088(7) 0.124(8) 0.021(6) 0.018(6) -0.003(5) O21 0.060(3) 0.122(5) 0.062(3) -0.032(3) -0.018(2) 0.006(3) C21 0.063(5) 0.063(5) 0.062(5) -0.005(4) -0.019(4) 0.002(4) C22 0.101(7) 0.086(7) 0.140(10) 0.001(7) -0.052(7) 0.011(5) C23 0.119(9) 0.146(13) 0.140(14) 0.061(10) -0.062(9) -0.020(9) C24 0.155(13) 0.189(17) 0.073(9) 0.027(10) -0.036(8) -0.081(12) C25 0.174(11) 0.119(10) 0.067(8) -0.030(6) 0.034(7) -0.028(8) C26 0.114(7) 0.077(6) 0.063(6) -0.002(5) -0.009(5) 0.005(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 P2 2.1773(17) . ? Pt1 P1 2.1819(16) . ? Pt1 Cl2 2.3451(16) . ? Pt1 Cl1 2.3443(17) . ? P1 O7 1.580(4) . ? P1 O1 1.599(4) . ? P1 N1 1.645(5) . ? N1 N2 1.440(7) . ? N1 C13 1.475(8) . ? C13 C14 1.514(11) . ? P2 O21 1.567(4) . ? P2 O15 1.588(5) . ? P2 N2 1.680(6) . ? N2 C27 1.536(12) . ? C27 C28 1.332(11) . ? O1 C1 1.416(7) . ? C1 C2 1.367(8) . ? C1 C6 1.373(8) . ? C2 C3 1.370(9) . ? C3 C4 1.365(10) . ? C4 C5 1.391(10) . ? C5 C6 1.384(9) . ? O7 C7 1.409(7) . ? C7 C8 1.362(8) . ? C7 C12 1.361(9) . ? C8 C9 1.398(9) . ? C9 C10 1.368(11) . ? C10 C11 1.348(11) . ? C11 C12 1.382(10) . ? O15 C15 1.397(8) . ? C15 C20 1.332(10) . ? C15 C16 1.337(10) . ? C16 C17 1.425(15) . ? C17 C18 1.348(16) . ? C18 C19 1.346(15) . ? C19 C20 1.361(12) . ? O21 C21 1.409(8) . ? C21 C26 1.333(10) . ? C21 C22 1.332(10) . ? C22 C23 1.400(14) . ? C23 C24 1.302(16) . ? C24 C25 1.351(16) . ? C25 C26 1.385(11) . ? 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 P2 Pt1 P1 82.55(6) . . ? P2 Pt1 Cl2 174.00(6) . . ? P1 Pt1 Cl2 91.65(6) . . ? P2 Pt1 Cl1 94.25(7) . . ? P1 Pt1 Cl1 176.81(6) . . ? Cl2 Pt1 Cl1 91.55(6) . . ? O7 P1 O1 99.3(2) . . ? O7 P1 N1 99.6(3) . . ? O1 P1 N1 109.7(3) . . ? O7 P1 Pt1 117.92(18) . . ? O1 P1 Pt1 119.98(17) . . ? N1 P1 Pt1 108.25(19) . . ? N2 N1 C13 115.4(5) . . ? N2 N1 P1 119.6(4) . . ? C13 N1 P1 125.1(5) . . ? N1 C13 C14 112.1(7) . . ? O21 P2 O15 106.6(3) . . ? O21 P2 N2 102.8(3) . . ? O15 P2 N2 102.1(3) . . ? O21 P2 Pt1 117.4(2) . . ? O15 P2 Pt1 115.65(19) . . ? N2 P2 Pt1 110.6(2) . . ? N1 N2 C27 110.4(6) . . ? N1 N2 P2 105.9(4) . . ? C27 N2 P2 117.1(6) . . ? C28 C27 N2 117.4(10) . . ? C1 O1 P1 119.7(3) . . ? C2 C1 C6 122.0(6) . . ? C2 C1 O1 118.6(6) . . ? C6 C1 O1 119.4(6) . . ? C1 C2 C3 119.2(7) . . ? C4 C3 C2 120.8(7) . . ? C3 C4 C5 119.5(7) . . ? C6 C5 C4 120.3(7) . . ? C1 C6 C5 118.2(7) . . ? C7 O7 P1 130.5(4) . . ? C8 C7 C12 122.4(7) . . ? C8 C7 O7 122.5(6) . . ? C12 C7 O7 114.8(6) . . ? C7 C8 C9 118.4(7) . . ? C10 C9 C8 119.7(8) . . ? C11 C10 C9 120.2(8) . . ? C10 C11 C12 121.5(8) . . ? C7 C12 C11 117.9(8) . . ? C15 O15 P2 124.4(4) . . ? C20 C15 C16 120.2(9) . . ? C20 C15 O15 119.7(7) . . ? C16 C15 O15 120.0(8) . . ? C15 C16 C17 120.2(11) . . ? C18 C17 C16 115.7(12) . . ? C17 C18 C19 124.6(14) . . ? C18 C19 C20 116.7(12) . . ? C15 C20 C19 122.6(10) . . ? C21 O21 P2 128.9(4) . . ? C26 C21 C22 120.4(8) . . ? C26 C21 O21 121.4(7) . . ? C22 C21 O21 118.0(8) . . ? C21 C22 C23 118.9(10) . . ? C24 C23 C22 119.5(13) . . ? C23 C24 C25 123.1(14) . . ? C24 C25 C26 116.6(11) . . ? C21 C26 C25 121.4(9) . . ? 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 P2 Pt1 P1 O7 -105.83(19) . . . . ? Cl2 Pt1 P1 O7 72.62(19) . . . . ? Cl1 Pt1 P1 O7 -107.8(12) . . . . ? P2 Pt1 P1 O1 133.00(19) . . . . ? Cl2 Pt1 P1 O1 -48.55(19) . . . . ? Cl1 Pt1 P1 O1 131.0(12) . . . . ? P2 Pt1 P1 N1 6.1(2) . . . . ? Cl2 Pt1 P1 N1 -175.5(2) . . . . ? Cl1 Pt1 P1 N1 4.1(13) . . . . ? O7 P1 N1 N2 140.8(5) . . . . ? O1 P1 N1 N2 -115.6(5) . . . . ? Pt1 P1 N1 N2 17.0(5) . . . . ? O7 P1 N1 C13 -40.5(6) . . . . ? O1 P1 N1 C13 63.1(6) . . . . ? Pt1 P1 N1 C13 -164.3(5) . . . . ? N2 N1 C13 C14 -78.0(8) . . . . ? P1 N1 C13 C14 103.3(7) . . . . ? P1 Pt1 P2 O21 -141.5(3) . . . . ? Cl2 Pt1 P2 O21 -156.5(6) . . . . ? Cl1 Pt1 P2 O21 38.4(3) . . . . ? P1 Pt1 P2 O15 91.3(2) . . . . ? Cl2 Pt1 P2 O15 76.3(7) . . . . ? Cl1 Pt1 P2 O15 -88.9(2) . . . . ? P1 Pt1 P2 N2 -24.1(2) . . . . ? Cl2 Pt1 P2 N2 -39.1(7) . . . . ? Cl1 Pt1 P2 N2 155.8(2) . . . . ? C13 N1 N2 C27 -86.9(8) . . . . ? P1 N1 N2 C27 91.9(7) . . . . ? C13 N1 N2 P2 145.4(5) . . . . ? P1 N1 N2 P2 -35.8(6) . . . . ? O21 P2 N2 N1 164.4(4) . . . . ? O15 P2 N2 N1 -85.3(4) . . . . ? Pt1 P2 N2 N1 38.3(4) . . . . ? O21 P2 N2 C27 40.8(6) . . . . ? O15 P2 N2 C27 151.2(5) . . . . ? Pt1 P2 N2 C27 -85.2(5) . . . . ? N1 N2 C27 C28 145.8(10) . . . . ? P2 N2 C27 C28 -92.9(11) . . . . ? O7 P1 O1 C1 167.4(4) . . . . ? N1 P1 O1 C1 63.6(5) . . . . ? Pt1 P1 O1 C1 -62.6(5) . . . . ? P1 O1 C1 C2 -97.7(6) . . . . ? P1 O1 C1 C6 83.0(7) . . . . ? C6 C1 C2 C3 -1.5(10) . . . . ? O1 C1 C2 C3 179.3(6) . . . . ? C1 C2 C3 C4 1.1(11) . . . . ? C2 C3 C4 C5 0.6(12) . . . . ? C3 C4 C5 C6 -1.9(12) . . . . ? C2 C1 C6 C5 0.1(10) . . . . ? O1 C1 C6 C5 179.3(6) . . . . ? C4 C5 C6 C1 1.6(11) . . . . ? O1 P1 O7 C7 62.3(6) . . . . ? N1 P1 O7 C7 174.3(5) . . . . ? Pt1 P1 O7 C7 -69.0(6) . . . . ? P1 O7 C7 C8 -51.0(8) . . . . ? P1 O7 C7 C12 134.9(5) . . . . ? C12 C7 C8 C9 1.0(11) . . . . ? O7 C7 C8 C9 -172.7(6) . . . . ? C7 C8 C9 C10 -0.7(11) . . . . ? C8 C9 C10 C11 0.7(13) . . . . ? C9 C10 C11 C12 -1.0(13) . . . . ? C8 C7 C12 C11 -1.3(11) . . . . ? O7 C7 C12 C11 172.9(6) . . . . ? C10 C11 C12 C7 1.2(12) . . . . ? O21 P2 O15 C15 -109.7(6) . . . . ? N2 P2 O15 C15 142.9(5) . . . . ? Pt1 P2 O15 C15 22.8(6) . . . . ? P2 O15 C15 C20 78.3(8) . . . . ? P2 O15 C15 C16 -105.7(7) . . . . ? C20 C15 C16 C17 -1.0(14) . . . . ? O15 C15 C16 C17 -177.0(8) . . . . ? C15 C16 C17 C18 0.3(17) . . . . ? C16 C17 C18 C19 1(2) . . . . ? C17 C18 C19 C20 -2(2) . . . . ? C16 C15 C20 C19 0.4(14) . . . . ? O15 C15 C20 C19 176.4(8) . . . . ? C18 C19 C20 C15 0.9(16) . . . . ? O15 P2 O21 C21 0.8(7) . . . . ? N2 P2 O21 C21 107.7(6) . . . . ? Pt1 P2 O21 C21 -130.7(5) . . . . ? P2 O21 C21 C26 -67.4(9) . . . . ? P2 O21 C21 C22 117.8(7) . . . . ? C26 C21 C22 C23 1.7(14) . . . . ? O21 C21 C22 C23 176.6(8) . . . . ? C21 C22 C23 C24 -2.8(18) . . . . ? C22 C23 C24 C25 3(2) . . . . ? C23 C24 C25 C26 -2(2) . . . . ? C22 C21 C26 C25 -0.7(13) . . . . ? O21 C21 C26 C25 -175.4(8) . . . . ? C24 C25 C26 C21 0.7(15) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 23.27 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.564 _refine_diff_density_min -0.817 _refine_diff_density_rms 0.081 data_9 _database_code_CSD 168964 _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Slawin, A.' 'Wainwright, Matthew' 'Woollins, Derek' _publ_contact_author_name 'Prof Derek Woollins' _publ_contact_author_address ; Chemistry U of St Andrews Dept of Chemistry University of St Andrews St Andrews KY16 9ST UNITED KINGDOM ; _publ_contact_author_email 'JDW3@ST-AND.AC.UK' _publ_section_title ; The Preparation and Coordination Chemistry of Phosphorus (III) Derivatives of Dialkyl Hydrazines ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H30 Cl2 N2 O4 P2 Pd' _chemical_formula_sum 'C28 H30 Cl2 N2 O4 P2 Pd' _chemical_formula_weight 697.78 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 22.2887(4) _cell_length_b 8.8062(2) _cell_length_c 32.0433(5) _cell_angle_alpha 90.00 _cell_angle_beta 105.61 _cell_angle_gamma 90.00 _cell_volume 6057.3(2) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 56 _cell_measurement_theta_min 23 _cell_measurement_theta_max 337 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max .15 _exptl_crystal_size_mid .2 _exptl_crystal_size_min .2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.530 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2832 _exptl_absorpt_coefficient_mu 0.931 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.774110 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 0.9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25083 _diffrn_reflns_av_R_equivalents 0.0637 _diffrn_reflns_av_sigmaI/netI 0.0761 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 23.26 _reflns_number_total 8637 _reflns_number_gt 5675 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART/SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _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^)+(0.0195P)^2^+3.6920P] 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 SHELXL _refine_ls_extinction_coef 0.00105(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 8637 _refine_ls_number_parameters 704 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0909 _refine_ls_R_factor_gt 0.0449 _refine_ls_wR_factor_ref 0.0872 _refine_ls_wR_factor_gt 0.0728 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.000 _refine_ls_shift/su_max 0.015 _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 Pd1 Pd 0.961416(19) 0.62972(5) 0.720890(13) 0.03974(14) Uani 1 1 d . . . Cl1 Cl 0.97168(7) 0.4595(2) 0.66705(5) 0.0650(5) Uani 1 1 d . . . Cl2 Cl 0.85289(6) 0.64174(19) 0.69419(5) 0.0596(4) Uani 1 1 d . . . P1 P 0.95771(7) 0.78278(18) 0.77437(4) 0.0408(4) Uani 1 1 d . . . O1 O 0.91236(16) 0.7397(4) 0.80393(11) 0.0485(10) Uani 1 1 d . . . C1 C 0.9228(2) 0.5995(7) 0.82666(18) 0.0447(15) Uani 1 1 d . . . C2 C 0.9521(3) 0.6048(8) 0.87054(18) 0.0562(17) Uani 1 1 d . . . H2A H 0.9623 0.6968 0.8850 0.067 Uiso 1 1 calc R . . C3 C 0.9657(3) 0.4669(8) 0.89228(19) 0.0608(18) Uani 1 1 d . . . H3A H 0.9859 0.4663 0.9217 0.073 Uiso 1 1 calc R . . C4 C 0.9499(3) 0.3332(8) 0.8710(2) 0.0664(19) Uani 1 1 d . . . H4A H 0.9593 0.2421 0.8860 0.080 Uiso 1 1 calc R . . C5 C 0.9201(3) 0.3315(8) 0.8271(2) 0.072(2) Uani 1 1 d . . . H5A H 0.9095 0.2395 0.8128 0.086 Uiso 1 1 calc R . . C6 C 0.9062(3) 0.4658(8) 0.80484(19) 0.0532(16) Uani 1 1 d . . . H6A H 0.8858 0.4659 0.7754 0.064 Uiso 1 1 calc R . . O7 O 0.93812(16) 0.9538(4) 0.76372(11) 0.0494(10) Uani 1 1 d . . . C7 C 0.8809(3) 1.0196(7) 0.74154(18) 0.0474(15) Uani 1 1 d . . . C8 C 0.8247(3) 0.9630(8) 0.7439(2) 0.0653(18) Uani 1 1 d . . . H8A H 0.8226 0.8743 0.7592 0.078 Uiso 1 1 calc R . . C9 C 0.7707(3) 1.0413(10) 0.7227(2) 0.084(2) Uani 1 1 d . . . H9A H 0.7319 1.0044 0.7236 0.101 Uiso 1 1 calc R . . C10 C 0.7748(4) 1.1727(10) 0.7007(2) 0.092(3) Uani 1 1 d . . . H10A H 0.7389 1.2265 0.6874 0.111 Uiso 1 1 calc R . . C11 C 0.8310(4) 1.2245(9) 0.6983(2) 0.090(3) Uani 1 1 d . . . H11A H 0.8332 1.3115 0.6824 0.107 Uiso 1 1 calc R . . C12 C 0.8845(3) 1.1496(7) 0.71919(18) 0.0607(18) Uani 1 1 d . . . H12A H 0.9230 1.1872 0.7181 0.073 Uiso 1 1 calc R . . N1 N 1.02965(19) 0.8063(5) 0.80518(13) 0.0438(12) Uani 1 1 d . . . C13 C 1.0492(3) 0.9267(7) 0.83788(18) 0.0620(18) Uani 1 1 d . . . H13A H 1.0748 0.8823 0.8644 0.074 Uiso 1 1 calc R . . H13B H 1.0125 0.9698 0.8442 0.074 Uiso 1 1 calc R . . C14 C 1.0848(3) 1.0502(8) 0.8238(2) 0.095(2) Uani 1 1 d . . . H14A H 1.0965 1.1249 0.8464 0.142 Uiso 1 1 calc R . . H14B H 1.0593 1.0968 0.7980 0.142 Uiso 1 1 calc R . . H14C H 1.1215 1.0087 0.8180 0.142 Uiso 1 1 calc R . . N2 N 1.07673(19) 0.6978(5) 0.80314(13) 0.0445(12) Uani 1 1 d . . . C27 C 1.0812(3) 0.5702(8) 0.83641(18) 0.071(2) Uani 1 1 d . . . H27A H 1.0707 0.6114 0.8616 0.085 Uiso 1 1 calc R . . H27B H 1.0505 0.4931 0.8240 0.085 Uiso 1 1 calc R . . C28 C 1.1423(3) 0.4985(8) 0.8504(2) 0.085(2) Uani 1 1 d . . . H28A H 1.1416 0.4205 0.8712 0.127 Uiso 1 1 calc R . . H28B H 1.1730 0.5733 0.8634 0.127 Uiso 1 1 calc R . . H28C H 1.1527 0.4545 0.8258 0.127 Uiso 1 1 calc R . . P2 P 1.06198(7) 0.64803(18) 0.75060(5) 0.0413(4) Uani 1 1 d . . . O15 O 1.09557(16) 0.7801(4) 0.73211(11) 0.0505(10) Uani 1 1 d . . . C15 C 1.0703(3) 0.8456(7) 0.69068(18) 0.0463(15) Uani 1 1 d . . . C16 C 1.0462(3) 0.9858(8) 0.6878(2) 0.071(2) Uani 1 1 d . . . H16A H 1.0442 1.0381 0.7127 0.085 Uiso 1 1 calc R . . C17 C 1.0242(3) 1.0522(8) 0.6470(3) 0.081(2) Uani 1 1 d . . . H17A H 1.0075 1.1495 0.6443 0.098 Uiso 1 1 calc R . . C18 C 1.0273(3) 0.9740(9) 0.6113(2) 0.081(2) Uani 1 1 d . . . H18A H 1.0129 1.0183 0.5841 0.097 Uiso 1 1 calc R . . C19 C 1.0512(3) 0.8326(9) 0.6149(2) 0.082(2) Uani 1 1 d . . . H19A H 1.0527 0.7795 0.5901 0.098 Uiso 1 1 calc R . . C20 C 1.0736(3) 0.7655(7) 0.6552(2) 0.0623(18) Uani 1 1 d . . . H20A H 1.0903 0.6681 0.6579 0.075 Uiso 1 1 calc R . . O21 O 1.10252(17) 0.5012(4) 0.75281(12) 0.0573(11) Uani 1 1 d . . . C21 C 1.1519(3) 0.4774(7) 0.73331(18) 0.0488(16) Uani 1 1 d . . . C22 C 1.1416(3) 0.3832(8) 0.6990(2) 0.076(2) Uani 1 1 d . . . H22A H 1.1027 0.3392 0.6877 0.091 Uiso 1 1 calc R . . C23 C 1.1907(4) 0.3529(10) 0.6808(2) 0.097(3) Uani 1 1 d . . . H23A H 1.1849 0.2872 0.6573 0.116 Uiso 1 1 calc R . . C24 C 1.2454(5) 0.4180(11) 0.6971(3) 0.099(3) Uani 1 1 d . . . H24A H 1.2776 0.3984 0.6844 0.119 Uiso 1 1 calc R . . C25 C 1.2562(3) 0.5129(10) 0.7319(3) 0.093(3) Uani 1 1 d . . . H25A H 1.2954 0.5553 0.7433 0.112 Uiso 1 1 calc R . . C26 C 1.2077(3) 0.5451(8) 0.7498(2) 0.074(2) Uani 1 1 d . . . H26A H 1.2134 0.6123 0.7730 0.089 Uiso 1 1 calc R . . Pd2 Pd 0.710702(19) 0.78292(5) 0.472177(13) 0.03796(14) Uani 1 1 d . . . Cl3 Cl 0.71567(7) 0.65089(19) 0.40975(5) 0.0637(5) Uani 1 1 d . . . Cl4 Cl 0.60116(6) 0.78979(18) 0.45289(4) 0.0525(4) Uani 1 1 d . . . P3 P 0.71612(7) 0.90616(16) 0.53304(4) 0.0388(4) Uani 1 1 d . . . O31 O 0.70586(15) 1.0843(4) 0.52779(11) 0.0447(10) Uani 1 1 d . . . C31 C 0.6513(3) 1.1654(6) 0.50744(17) 0.0423(14) Uani 1 1 d . . . C32 C 0.5948(3) 1.1344(7) 0.51588(18) 0.0537(16) Uani 1 1 d . . . H32A H 0.5906 1.0541 0.5338 0.064 Uiso 1 1 calc R . . C33 C 0.5447(3) 1.2267(8) 0.4969(2) 0.0659(19) Uani 1 1 d . . . H33A H 0.5064 1.2077 0.5024 0.079 Uiso 1 1 calc R . . C34 C 0.5495(3) 1.3431(8) 0.4708(2) 0.067(2) Uani 1 1 d . . . H34A H 0.5152 1.4038 0.4584 0.081 Uiso 1 1 calc R . . C35 C 0.6061(4) 1.3705(8) 0.4628(2) 0.073(2) Uani 1 1 d . . . H35A H 0.6102 1.4510 0.4450 0.087 Uiso 1 1 calc R . . C36 C 0.6569(3) 1.2799(7) 0.4810(2) 0.0616(18) Uani 1 1 d . . . H36A H 0.6948 1.2979 0.4749 0.074 Uiso 1 1 calc R . . O37 O 0.67059(15) 0.8731(4) 0.56272(11) 0.0448(9) Uani 1 1 d . . . C37 C 0.6683(2) 0.7329(6) 0.58331(17) 0.0409(14) Uani 1 1 d . . . C38 C 0.7003(3) 0.7204(7) 0.62597(18) 0.0567(17) Uani 1 1 d . . . H38A H 0.7251 0.7996 0.6402 0.068 Uiso 1 1 calc R . . C39 C 0.6948(3) 0.5867(9) 0.6477(2) 0.074(2) Uani 1 1 d . . . H39A H 0.7166 0.5745 0.6766 0.089 Uiso 1 1 calc R . . C40 C 0.6571(3) 0.4729(8) 0.6261(2) 0.074(2) Uani 1 1 d . . . H40A H 0.6526 0.3843 0.6408 0.089 Uiso 1 1 calc R . . C41 C 0.6259(3) 0.4879(7) 0.5831(2) 0.0655(18) Uani 1 1 d . . . H41A H 0.6012 0.4088 0.5687 0.079 Uiso 1 1 calc R . . C42 C 0.6310(3) 0.6202(7) 0.56141(18) 0.0526(16) Uani 1 1 d . . . H42A H 0.6096 0.6322 0.5324 0.063 Uiso 1 1 calc R . . N3 N 0.7886(2) 0.8936(5) 0.56441(13) 0.0440(12) Uani 1 1 d . . . C43 C 0.8148(3) 0.9965(7) 0.60094(17) 0.0565(17) Uani 1 1 d . . . H43A H 0.8389 0.9375 0.6253 0.068 Uiso 1 1 calc R . . H43B H 0.7810 1.0445 0.6097 0.068 Uiso 1 1 calc R . . C44 C 0.8559(3) 1.1177(7) 0.5901(2) 0.076(2) Uani 1 1 d . . . H44A H 0.8720 1.1810 0.6150 0.115 Uiso 1 1 calc R . . H44B H 0.8321 1.1785 0.5666 0.115 Uiso 1 1 calc R . . H44C H 0.8899 1.0710 0.5818 0.115 Uiso 1 1 calc R . . N4 N 0.83345(19) 0.8060(5) 0.55005(13) 0.0420(11) Uani 1 1 d . . . C57 C 0.8546(3) 0.6662(7) 0.57644(19) 0.0644(19) Uani 1 1 d . . . H57A H 0.8655 0.6941 0.6068 0.077 Uiso 1 1 calc R . . H57B H 0.8923 0.6295 0.5701 0.077 Uiso 1 1 calc R . . C58 C 0.8085(3) 0.5381(7) 0.5695(2) 0.082(2) Uani 1 1 d . . . H58A H 0.8262 0.4542 0.5878 0.123 Uiso 1 1 calc R . . H58B H 0.7983 0.5066 0.5397 0.123 Uiso 1 1 calc R . . H58C H 0.7713 0.5716 0.5765 0.123 Uiso 1 1 calc R . . P4 P 0.81242(6) 0.79977(17) 0.49618(4) 0.0396(4) Uani 1 1 d . . . O45 O 0.84179(16) 0.9528(4) 0.48488(11) 0.0472(10) Uani 1 1 d . . . C45 C 0.8193(3) 1.0392(7) 0.4469(2) 0.0522(16) Uani 1 1 d . . . C46 C 0.8049(3) 1.1863(8) 0.4515(3) 0.083(2) Uani 1 1 d . . . H46A H 0.8083 1.2263 0.4789 0.099 Uiso 1 1 calc R . . C47 C 0.7851(5) 1.2763(12) 0.4153(4) 0.131(5) Uani 1 1 d . . . H47A H 0.7734 1.3767 0.4178 0.158 Uiso 1 1 calc R . . C48 C 0.7829(4) 1.2159(15) 0.3764(4) 0.135(5) Uani 1 1 d . . . H48A H 0.7705 1.2770 0.3519 0.162 Uiso 1 1 calc R . . C49 C 0.7984(4) 1.0683(12) 0.3715(3) 0.110(3) Uani 1 1 d . . . H49A H 0.7961 1.0295 0.3442 0.132 Uiso 1 1 calc R . . C50 C 0.8174(3) 0.9775(8) 0.4077(2) 0.075(2) Uani 1 1 d . . . H50A H 0.8287 0.8768 0.4053 0.090 Uiso 1 1 calc R . . O51 O 0.85216(16) 0.6660(4) 0.48533(12) 0.0509(10) Uani 1 1 d . . . C51 C 0.9097(3) 0.6732(6) 0.47473(17) 0.0425(15) Uani 1 1 d . . . C52 C 0.9140(3) 0.5923(7) 0.4396(2) 0.0670(19) Uani 1 1 d . . . H52A H 0.8800 0.5392 0.4228 0.080 Uiso 1 1 calc R . . C53 C 0.9708(5) 0.5914(8) 0.4296(3) 0.089(3) Uani 1 1 d . . . H53A H 0.9753 0.5359 0.4060 0.107 Uiso 1 1 calc R . . C54 C 1.0193(4) 0.6706(10) 0.4540(3) 0.090(3) Uani 1 1 d . . . H54A H 1.0568 0.6717 0.4466 0.108 Uiso 1 1 calc R . . C55 C 1.0142(3) 0.7489(9) 0.4894(2) 0.081(2) Uani 1 1 d . . . H55A H 1.0482 0.8016 0.5064 0.097 Uiso 1 1 calc R . . C56 C 0.9584(3) 0.7498(8) 0.5000(2) 0.070(2) Uani 1 1 d . . . H56A H 0.9544 0.8024 0.5243 0.084 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 Pd1 0.0408(3) 0.0454(3) 0.0317(2) -0.0023(2) 0.00738(19) -0.0012(2) Cl1 0.0628(11) 0.0783(12) 0.0554(10) -0.0271(9) 0.0186(8) -0.0060(9) Cl2 0.0406(9) 0.0810(12) 0.0504(9) -0.0062(9) 0.0003(7) 0.0010(8) P1 0.0385(9) 0.0440(10) 0.0374(9) 0.0017(7) 0.0061(7) 0.0071(8) O1 0.049(3) 0.057(3) 0.043(2) 0.0030(19) 0.0174(19) 0.0135(19) C1 0.033(3) 0.066(5) 0.040(4) 0.003(3) 0.018(3) 0.006(3) C2 0.061(4) 0.069(5) 0.042(4) 0.002(3) 0.020(3) 0.005(4) C3 0.063(4) 0.078(6) 0.041(4) 0.003(4) 0.015(3) 0.000(4) C4 0.073(5) 0.063(5) 0.067(5) 0.013(4) 0.025(4) -0.001(4) C5 0.096(6) 0.058(5) 0.062(5) -0.002(4) 0.024(4) -0.026(4) C6 0.054(4) 0.062(5) 0.043(4) -0.003(4) 0.013(3) -0.008(3) O7 0.043(2) 0.040(2) 0.058(2) 0.003(2) 0.0005(19) 0.0096(19) C7 0.051(4) 0.043(4) 0.044(4) -0.006(3) 0.006(3) 0.020(3) C8 0.055(4) 0.067(5) 0.074(5) 0.013(4) 0.018(4) 0.018(4) C9 0.053(5) 0.110(7) 0.083(5) -0.003(5) 0.007(4) 0.027(5) C10 0.106(7) 0.093(7) 0.063(5) 0.009(5) -0.003(5) 0.066(6) C11 0.127(8) 0.068(6) 0.064(5) 0.005(4) 0.009(6) 0.041(6) C12 0.078(5) 0.045(4) 0.053(4) -0.001(3) 0.006(4) 0.011(4) N1 0.041(3) 0.047(3) 0.038(3) -0.012(2) 0.002(2) 0.007(2) C13 0.058(4) 0.067(5) 0.053(4) -0.020(4) 0.000(3) 0.008(4) C14 0.095(6) 0.079(6) 0.107(6) -0.029(5) 0.020(5) -0.023(5) N2 0.044(3) 0.049(3) 0.039(3) 0.001(2) 0.008(2) 0.015(2) C27 0.067(5) 0.106(6) 0.037(4) 0.011(4) 0.007(3) 0.030(4) C28 0.084(5) 0.093(6) 0.070(5) 0.005(4) 0.007(4) 0.029(5) P2 0.0401(9) 0.0459(10) 0.0374(9) -0.0002(7) 0.0094(7) 0.0041(7) O15 0.042(2) 0.056(3) 0.051(2) 0.005(2) 0.0072(19) -0.006(2) C15 0.048(4) 0.047(4) 0.043(4) 0.002(3) 0.010(3) -0.006(3) C16 0.080(5) 0.061(5) 0.067(5) -0.010(4) 0.011(4) 0.013(4) C17 0.086(6) 0.056(5) 0.091(6) 0.013(5) 0.004(5) 0.012(4) C18 0.096(6) 0.067(6) 0.067(5) 0.018(5) 0.001(4) -0.001(5) C19 0.117(7) 0.073(6) 0.056(5) 0.003(4) 0.023(4) 0.003(5) C20 0.082(5) 0.047(4) 0.059(4) 0.009(4) 0.022(4) 0.011(3) O21 0.058(3) 0.053(3) 0.065(3) 0.003(2) 0.024(2) 0.017(2) C21 0.054(4) 0.055(4) 0.037(4) 0.001(3) 0.012(3) 0.019(3) C22 0.069(5) 0.077(5) 0.072(5) -0.020(4) 0.002(4) 0.031(4) C23 0.116(7) 0.111(8) 0.060(5) -0.032(5) 0.018(5) 0.042(6) C24 0.119(8) 0.114(9) 0.085(7) 0.027(6) 0.063(6) 0.053(7) C25 0.056(5) 0.101(7) 0.129(8) 0.023(6) 0.036(5) 0.014(5) C26 0.057(5) 0.087(6) 0.073(5) -0.017(4) 0.008(4) 0.013(4) Pd2 0.0404(3) 0.0382(3) 0.0338(2) 0.0008(2) 0.0076(2) 0.0038(2) Cl3 0.0680(11) 0.0721(12) 0.0492(9) -0.0188(8) 0.0126(8) 0.0105(9) Cl4 0.0406(9) 0.0659(11) 0.0460(9) 0.0013(8) 0.0033(7) 0.0046(8) P3 0.0422(9) 0.0362(10) 0.0389(9) 0.0009(7) 0.0128(7) 0.0036(7) O31 0.038(2) 0.036(2) 0.060(2) -0.0020(19) 0.0131(19) 0.0035(18) C31 0.047(4) 0.032(4) 0.048(4) 0.000(3) 0.012(3) 0.009(3) C32 0.051(4) 0.043(4) 0.069(4) 0.010(3) 0.020(3) 0.010(3) C33 0.048(4) 0.058(5) 0.091(5) -0.004(4) 0.018(4) 0.005(4) C34 0.064(5) 0.045(5) 0.078(5) -0.010(4) -0.008(4) 0.016(4) C35 0.088(6) 0.055(5) 0.069(5) 0.019(4) 0.011(4) 0.011(4) C36 0.059(4) 0.052(4) 0.075(5) 0.013(4) 0.020(4) 0.012(4) O37 0.049(2) 0.041(2) 0.050(2) 0.002(2) 0.0232(19) 0.0024(19) C37 0.040(4) 0.042(4) 0.042(4) 0.008(3) 0.013(3) 0.003(3) C38 0.048(4) 0.078(5) 0.041(4) 0.009(3) 0.007(3) -0.019(3) C39 0.049(4) 0.112(7) 0.051(4) 0.040(4) -0.004(3) -0.003(4) C40 0.060(5) 0.072(5) 0.086(6) 0.039(4) 0.012(4) 0.000(4) C41 0.073(5) 0.048(5) 0.071(5) 0.000(4) 0.011(4) -0.007(4) C42 0.053(4) 0.055(4) 0.046(4) 0.003(3) 0.006(3) 0.002(3) N3 0.048(3) 0.045(3) 0.039(3) -0.005(2) 0.011(2) 0.006(2) C43 0.059(4) 0.057(4) 0.047(4) -0.019(3) 0.003(3) 0.000(3) C44 0.078(5) 0.074(5) 0.075(5) -0.029(4) 0.018(4) -0.016(4) N4 0.043(3) 0.041(3) 0.042(3) 0.002(2) 0.010(2) 0.011(2) C57 0.074(5) 0.065(5) 0.052(4) 0.021(4) 0.013(3) 0.032(4) C58 0.110(6) 0.047(5) 0.102(6) 0.025(4) 0.051(5) 0.021(4) P4 0.0388(9) 0.0394(9) 0.0404(9) -0.0006(7) 0.0103(7) 0.0036(7) O45 0.049(2) 0.044(2) 0.049(2) 0.003(2) 0.0141(19) -0.004(2) C45 0.045(4) 0.045(4) 0.067(5) 0.019(4) 0.017(3) -0.006(3) C46 0.079(5) 0.047(5) 0.130(7) 0.018(5) 0.042(5) 0.014(4) C47 0.089(7) 0.079(8) 0.239(14) 0.066(10) 0.065(10) 0.032(6) C48 0.076(7) 0.133(12) 0.184(12) 0.116(11) 0.013(8) 0.001(7) C49 0.112(7) 0.116(8) 0.087(6) 0.041(6) 0.001(5) -0.032(6) C50 0.092(6) 0.066(5) 0.061(5) 0.019(4) 0.009(4) -0.014(4) O51 0.045(2) 0.044(3) 0.070(3) -0.008(2) 0.025(2) 0.0066(19) C51 0.046(4) 0.050(4) 0.034(3) 0.007(3) 0.015(3) 0.013(3) C52 0.079(5) 0.065(5) 0.064(5) -0.013(4) 0.031(4) -0.007(4) C53 0.142(8) 0.053(5) 0.102(7) 0.007(4) 0.082(6) 0.009(5) C54 0.076(6) 0.072(7) 0.145(9) 0.041(6) 0.069(6) 0.025(5) C55 0.052(5) 0.106(7) 0.079(6) 0.016(5) 0.006(4) 0.003(4) C56 0.044(4) 0.114(7) 0.052(4) -0.002(4) 0.010(4) 0.005(4) _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 Pd1 P2 2.1926(15) . ? Pd1 P1 2.1992(15) . ? Pd1 Cl1 2.3425(15) . ? Pd1 Cl2 2.3409(15) . ? P1 O7 1.579(4) . ? P1 O1 1.606(4) . ? P1 N1 1.654(4) . ? O1 C1 1.420(6) . ? C1 C6 1.369(7) . ? C1 C2 1.383(7) . ? C2 C3 1.392(8) . ? C3 C4 1.360(8) . ? C4 C5 1.383(8) . ? C5 C6 1.373(8) . ? O7 C7 1.408(6) . ? C7 C12 1.365(8) . ? C7 C8 1.368(8) . ? C8 C9 1.395(8) . ? C9 C10 1.371(10) . ? C10 C11 1.354(10) . ? C11 C12 1.369(8) . ? N1 N2 1.434(5) . ? N1 C13 1.472(6) . ? C13 C14 1.485(8) . ? N2 C27 1.533(7) . ? N2 P2 1.684(4) . ? C27 C28 1.459(7) . ? P2 O21 1.568(4) . ? P2 O15 1.582(4) . ? O15 C15 1.417(6) . ? C15 C16 1.340(8) . ? C15 C20 1.355(7) . ? C16 C17 1.396(8) . ? C17 C18 1.351(9) . ? C18 C19 1.348(9) . ? C19 C20 1.387(8) . ? O21 C21 1.419(6) . ? C21 C22 1.347(8) . ? C21 C26 1.353(8) . ? C22 C23 1.397(9) . ? C23 C24 1.322(10) . ? C24 C25 1.361(10) . ? C25 C26 1.384(8) . ? Pd2 P4 2.1943(15) . ? Pd2 P3 2.2065(15) . ? Pd2 Cl3 2.3420(15) . ? Pd2 Cl4 2.3526(14) . ? P3 O31 1.587(4) . ? P3 O37 1.593(3) . ? P3 N3 1.662(4) . ? O31 C31 1.410(6) . ? C31 C36 1.345(7) . ? C31 C32 1.385(7) . ? C32 C33 1.382(8) . ? C33 C34 1.346(8) . ? C34 C35 1.374(8) . ? C35 C36 1.378(8) . ? O37 C37 1.407(6) . ? C37 C42 1.362(7) . ? C37 C38 1.365(7) . ? C38 C39 1.390(8) . ? C39 C40 1.370(9) . ? C40 C41 1.372(8) . ? C41 C42 1.378(8) . ? N3 N4 1.432(5) . ? N3 C43 1.471(6) . ? C43 C44 1.507(8) . ? N4 C57 1.496(6) . ? N4 P4 1.663(4) . ? C57 C58 1.503(8) . ? P4 O51 1.568(4) . ? P4 O45 1.582(4) . ? O45 C45 1.409(6) . ? C45 C50 1.360(8) . ? C45 C46 1.352(8) . ? C46 C47 1.374(11) . ? C47 C48 1.347(13) . ? C48 C49 1.364(13) . ? C49 C50 1.377(9) . ? O51 C51 1.414(6) . ? C51 C52 1.356(7) . ? C51 C56 1.348(8) . ? C52 C53 1.386(9) . ? C53 C54 1.346(10) . ? C54 C55 1.358(9) . ? C55 C56 1.373(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 P2 Pd1 P1 82.24(5) . . ? P2 Pd1 Cl1 94.35(6) . . ? P1 Pd1 Cl1 176.04(6) . . ? P2 Pd1 Cl2 172.02(6) . . ? P1 Pd1 Cl2 90.30(5) . . ? Cl1 Pd1 Cl2 93.20(6) . . ? O7 P1 O1 99.9(2) . . ? O7 P1 N1 100.2(2) . . ? O1 P1 N1 109.9(2) . . ? O7 P1 Pd1 118.83(15) . . ? O1 P1 Pd1 118.47(16) . . ? N1 P1 Pd1 107.95(16) . . ? C1 O1 P1 117.7(3) . . ? C6 C1 C2 122.5(6) . . ? C6 C1 O1 120.1(5) . . ? C2 C1 O1 117.4(6) . . ? C1 C2 C3 117.4(6) . . ? C4 C3 C2 120.8(6) . . ? C3 C4 C5 120.6(6) . . ? C4 C5 C6 119.9(6) . . ? C1 C6 C5 118.9(6) . . ? C7 O7 P1 131.4(4) . . ? C12 C7 C8 121.2(6) . . ? C12 C7 O7 115.9(6) . . ? C8 C7 O7 122.7(6) . . ? C7 C8 C9 118.5(7) . . ? C10 C9 C8 119.9(7) . . ? C11 C10 C9 120.3(8) . . ? C10 C11 C12 120.5(8) . . ? C7 C12 C11 119.6(7) . . ? N2 N1 C13 115.6(4) . . ? N2 N1 P1 119.5(3) . . ? C13 N1 P1 124.7(4) . . ? N1 C13 C14 113.1(5) . . ? N1 N2 C27 111.6(4) . . ? N1 N2 P2 105.7(3) . . ? C27 N2 P2 117.6(4) . . ? C28 C27 N2 114.3(5) . . ? O21 P2 O15 107.3(2) . . ? O21 P2 N2 102.4(2) . . ? O15 P2 N2 101.5(2) . . ? O21 P2 Pd1 117.91(17) . . ? O15 P2 Pd1 115.02(15) . . ? N2 P2 Pd1 110.79(16) . . ? C15 O15 P2 122.8(3) . . ? C16 C15 C20 122.3(6) . . ? C16 C15 O15 119.3(6) . . ? C20 C15 O15 118.4(6) . . ? C15 C16 C17 118.8(6) . . ? C18 C17 C16 119.6(7) . . ? C19 C18 C17 120.6(7) . . ? C18 C19 C20 120.5(7) . . ? C15 C20 C19 118.2(6) . . ? C21 O21 P2 127.4(4) . . ? C22 C21 C26 121.8(6) . . ? C22 C21 O21 117.9(6) . . ? C26 C21 O21 120.2(5) . . ? C21 C22 C23 118.6(7) . . ? C24 C23 C22 119.7(7) . . ? C23 C24 C25 122.0(8) . . ? C24 C25 C26 118.8(8) . . ? C21 C26 C25 119.1(7) . . ? P4 Pd2 P3 81.46(5) . . ? P4 Pd2 Cl3 92.92(6) . . ? P3 Pd2 Cl3 174.36(6) . . ? P4 Pd2 Cl4 172.60(6) . . ? P3 Pd2 Cl4 91.46(5) . . ? Cl3 Pd2 Cl4 94.17(5) . . ? O31 P3 O37 98.44(19) . . ? O31 P3 N3 102.6(2) . . ? O37 P3 N3 107.4(2) . . ? O31 P3 Pd2 114.85(14) . . ? O37 P3 Pd2 123.07(15) . . ? N3 P3 Pd2 108.34(16) . . ? C31 O31 P3 129.2(3) . . ? C36 C31 C32 120.9(6) . . ? C36 C31 O31 117.2(5) . . ? C32 C31 O31 121.8(5) . . ? C33 C32 C31 117.9(6) . . ? C34 C33 C32 122.0(6) . . ? C33 C34 C35 118.8(6) . . ? C36 C35 C34 120.6(6) . . ? C31 C36 C35 119.7(6) . . ? C37 O37 P3 123.3(3) . . ? C42 C37 C38 122.6(6) . . ? C42 C37 O37 119.5(5) . . ? C38 C37 O37 117.7(5) . . ? C37 C38 C39 118.5(6) . . ? C40 C39 C38 119.5(6) . . ? C41 C40 C39 120.8(6) . . ? C40 C41 C42 120.0(6) . . ? C37 C42 C41 118.6(6) . . ? N4 N3 C43 115.2(4) . . ? N4 N3 P3 119.4(3) . . ? C43 N3 P3 123.6(4) . . ? N3 C43 C44 112.9(5) . . ? N3 N4 C57 113.8(4) . . ? N3 N4 P4 109.0(3) . . ? C57 N4 P4 121.2(4) . . ? N4 C57 C58 115.8(5) . . ? O51 P4 O45 107.2(2) . . ? O51 P4 N4 103.7(2) . . ? O45 P4 N4 101.0(2) . . ? O51 P4 Pd2 117.61(16) . . ? O45 P4 Pd2 115.44(15) . . ? N4 P4 Pd2 109.99(16) . . ? C45 O45 P4 125.8(3) . . ? C50 C45 C46 122.3(7) . . ? C50 C45 O45 119.9(6) . . ? C46 C45 O45 117.6(7) . . ? C45 C46 C47 119.6(9) . . ? C48 C47 C46 118.4(11) . . ? C47 C48 C49 122.3(11) . . ? C48 C49 C50 119.3(10) . . ? C45 C50 C49 118.1(8) . . ? C51 O51 P4 128.5(3) . . ? C52 C51 C56 122.4(6) . . ? C52 C51 O51 116.5(6) . . ? C56 C51 O51 120.9(5) . . ? C51 C52 C53 117.9(7) . . ? C54 C53 C52 120.2(7) . . ? C53 C54 C55 120.9(7) . . ? C54 C55 C56 119.6(7) . . ? C51 C56 C55 119.0(7) . . ? 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 P2 Pd1 P1 O7 108.79(17) . . . . ? Cl1 Pd1 P1 O7 139.4(9) . . . . ? Cl2 Pd1 P1 O7 -68.37(17) . . . . ? P2 Pd1 P1 O1 -129.81(17) . . . . ? Cl1 Pd1 P1 O1 -99.2(9) . . . . ? Cl2 Pd1 P1 O1 53.02(17) . . . . ? P2 Pd1 P1 N1 -4.17(18) . . . . ? Cl1 Pd1 P1 N1 26.5(10) . . . . ? Cl2 Pd1 P1 N1 178.67(18) . . . . ? O7 P1 O1 C1 -169.5(4) . . . . ? N1 P1 O1 C1 -64.8(4) . . . . ? Pd1 P1 O1 C1 59.9(4) . . . . ? P1 O1 C1 C6 -74.5(6) . . . . ? P1 O1 C1 C2 103.1(5) . . . . ? C6 C1 C2 C3 1.4(9) . . . . ? O1 C1 C2 C3 -176.2(5) . . . . ? C1 C2 C3 C4 -0.8(9) . . . . ? C2 C3 C4 C5 0.1(10) . . . . ? C3 C4 C5 C6 0.0(10) . . . . ? C2 C1 C6 C5 -1.3(9) . . . . ? O1 C1 C6 C5 176.2(5) . . . . ? C4 C5 C6 C1 0.6(9) . . . . ? O1 P1 O7 C7 -61.9(5) . . . . ? N1 P1 O7 C7 -174.4(4) . . . . ? Pd1 P1 O7 C7 68.4(5) . . . . ? P1 O7 C7 C12 -148.1(4) . . . . ? P1 O7 C7 C8 35.5(8) . . . . ? C12 C7 C8 C9 0.1(9) . . . . ? O7 C7 C8 C9 176.3(5) . . . . ? C7 C8 C9 C10 -0.7(10) . . . . ? C8 C9 C10 C11 1.9(12) . . . . ? C9 C10 C11 C12 -2.5(12) . . . . ? C8 C7 C12 C11 -0.6(9) . . . . ? O7 C7 C12 C11 -177.1(5) . . . . ? C10 C11 C12 C7 1.8(11) . . . . ? O7 P1 N1 N2 -145.0(4) . . . . ? O1 P1 N1 N2 110.5(4) . . . . ? Pd1 P1 N1 N2 -20.1(4) . . . . ? O7 P1 N1 C13 39.8(5) . . . . ? O1 P1 N1 C13 -64.7(5) . . . . ? Pd1 P1 N1 C13 164.8(4) . . . . ? N2 N1 C13 C14 79.5(6) . . . . ? P1 N1 C13 C14 -105.2(6) . . . . ? C13 N1 N2 C27 84.7(6) . . . . ? P1 N1 N2 C27 -90.9(5) . . . . ? C13 N1 N2 P2 -146.4(4) . . . . ? P1 N1 N2 P2 38.1(5) . . . . ? N1 N2 C27 C28 -153.4(5) . . . . ? P2 N2 C27 C28 84.3(6) . . . . ? N1 N2 P2 O21 -165.3(3) . . . . ? C27 N2 P2 O21 -40.0(4) . . . . ? N1 N2 P2 O15 83.9(3) . . . . ? C27 N2 P2 O15 -150.8(4) . . . . ? N1 N2 P2 Pd1 -38.7(4) . . . . ? C27 N2 P2 Pd1 86.6(4) . . . . ? P1 Pd1 P2 O21 140.49(18) . . . . ? Cl1 Pd1 P2 O21 -37.48(18) . . . . ? Cl2 Pd1 P2 O21 161.4(4) . . . . ? P1 Pd1 P2 O15 -91.23(17) . . . . ? Cl1 Pd1 P2 O15 90.80(17) . . . . ? Cl2 Pd1 P2 O15 -70.3(5) . . . . ? P1 Pd1 P2 N2 23.07(19) . . . . ? Cl1 Pd1 P2 N2 -154.90(19) . . . . ? Cl2 Pd1 P2 N2 44.0(5) . . . . ? O21 P2 O15 C15 111.5(4) . . . . ? N2 P2 O15 C15 -141.5(4) . . . . ? Pd1 P2 O15 C15 -21.8(5) . . . . ? P2 O15 C15 C16 107.2(6) . . . . ? P2 O15 C15 C20 -75.2(6) . . . . ? C20 C15 C16 C17 -0.6(10) . . . . ? O15 C15 C16 C17 177.0(5) . . . . ? C15 C16 C17 C18 0.3(11) . . . . ? C16 C17 C18 C19 0.4(12) . . . . ? C17 C18 C19 C20 -0.7(12) . . . . ? C16 C15 C20 C19 0.2(10) . . . . ? O15 C15 C20 C19 -177.3(5) . . . . ? C18 C19 C20 C15 0.4(11) . . . . ? O15 P2 O21 C21 -13.2(5) . . . . ? N2 P2 O21 C21 -119.5(5) . . . . ? Pd1 P2 O21 C21 118.7(4) . . . . ? P2 O21 C21 C22 -108.0(6) . . . . ? P2 O21 C21 C26 73.7(7) . . . . ? C26 C21 C22 C23 1.3(10) . . . . ? O21 C21 C22 C23 -176.9(6) . . . . ? C21 C22 C23 C24 -0.8(12) . . . . ? C22 C23 C24 C25 1.1(14) . . . . ? C23 C24 C25 C26 -1.8(13) . . . . ? C22 C21 C26 C25 -2.1(10) . . . . ? O21 C21 C26 C25 176.2(6) . . . . ? C24 C25 C26 C21 2.2(11) . . . . ? P4 Pd2 P3 O31 98.88(16) . . . . ? Cl3 Pd2 P3 O31 103.2(6) . . . . ? Cl4 Pd2 P3 O31 -78.96(16) . . . . ? P4 Pd2 P3 O37 -141.46(18) . . . . ? Cl3 Pd2 P3 O37 -137.1(6) . . . . ? Cl4 Pd2 P3 O37 40.69(18) . . . . ? P4 Pd2 P3 N3 -15.18(17) . . . . ? Cl3 Pd2 P3 N3 -10.9(7) . . . . ? Cl4 Pd2 P3 N3 166.98(17) . . . . ? O37 P3 O31 C31 -64.3(4) . . . . ? N3 P3 O31 C31 -174.3(4) . . . . ? Pd2 P3 O31 C31 68.3(4) . . . . ? P3 O31 C31 C36 -134.6(5) . . . . ? P3 O31 C31 C32 48.7(7) . . . . ? C36 C31 C32 C33 -1.2(9) . . . . ? O31 C31 C32 C33 175.4(5) . . . . ? C31 C32 C33 C34 0.3(9) . . . . ? C32 C33 C34 C35 0.1(10) . . . . ? C33 C34 C35 C36 0.4(10) . . . . ? C32 C31 C36 C35 1.7(9) . . . . ? O31 C31 C36 C35 -175.0(5) . . . . ? C34 C35 C36 C31 -1.4(10) . . . . ? O31 P3 O37 C37 -169.8(4) . . . . ? N3 P3 O37 C37 -63.6(4) . . . . ? Pd2 P3 O37 C37 63.1(4) . . . . ? P3 O37 C37 C42 -86.3(6) . . . . ? P3 O37 C37 C38 98.7(5) . . . . ? C42 C37 C38 C39 0.5(9) . . . . ? O37 C37 C38 C39 175.3(5) . . . . ? C37 C38 C39 C40 -1.0(10) . . . . ? C38 C39 C40 C41 1.5(11) . . . . ? C39 C40 C41 C42 -1.5(11) . . . . ? C38 C37 C42 C41 -0.5(9) . . . . ? O37 C37 C42 C41 -175.2(5) . . . . ? C40 C41 C42 C37 1.0(9) . . . . ? O31 P3 N3 N4 -124.7(4) . . . . ? O37 P3 N3 N4 132.1(4) . . . . ? Pd2 P3 N3 N4 -2.8(4) . . . . ? O31 P3 N3 C43 39.1(5) . . . . ? O37 P3 N3 C43 -64.0(5) . . . . ? Pd2 P3 N3 C43 161.0(4) . . . . ? N4 N3 C43 C44 63.1(6) . . . . ? P3 N3 C43 C44 -101.3(5) . . . . ? C43 N3 N4 C57 82.2(6) . . . . ? P3 N3 N4 C57 -112.6(4) . . . . ? C43 N3 N4 P4 -139.3(4) . . . . ? P3 N3 N4 P4 25.9(5) . . . . ? N3 N4 C57 C58 73.7(6) . . . . ? P4 N4 C57 C58 -59.3(6) . . . . ? N3 N4 P4 O51 -164.0(3) . . . . ? C57 N4 P4 O51 -29.1(5) . . . . ? N3 N4 P4 O45 85.1(3) . . . . ? C57 N4 P4 O45 -140.1(4) . . . . ? N3 N4 P4 Pd2 -37.4(4) . . . . ? C57 N4 P4 Pd2 97.5(4) . . . . ? P3 Pd2 P4 O51 146.95(18) . . . . ? Cl3 Pd2 P4 O51 -32.62(18) . . . . ? Cl4 Pd2 P4 O51 163.9(4) . . . . ? P3 Pd2 P4 O45 -84.83(16) . . . . ? Cl3 Pd2 P4 O45 95.59(16) . . . . ? Cl4 Pd2 P4 O45 -67.8(5) . . . . ? P3 Pd2 P4 N4 28.64(18) . . . . ? Cl3 Pd2 P4 N4 -150.94(18) . . . . ? Cl4 Pd2 P4 N4 45.6(5) . . . . ? O51 P4 O45 C45 99.8(5) . . . . ? N4 P4 O45 C45 -151.9(4) . . . . ? Pd2 P4 O45 C45 -33.4(5) . . . . ? P4 O45 C45 C50 -61.8(7) . . . . ? P4 O45 C45 C46 123.3(5) . . . . ? C50 C45 C46 C47 2.8(11) . . . . ? O45 C45 C46 C47 177.5(6) . . . . ? C45 C46 C47 C48 -2.5(14) . . . . ? C46 C47 C48 C49 1.5(17) . . . . ? C47 C48 C49 C50 -0.6(16) . . . . ? C46 C45 C50 C49 -1.8(10) . . . . ? O45 C45 C50 C49 -176.5(6) . . . . ? C48 C49 C50 C45 0.7(12) . . . . ? O45 P4 O51 C51 10.3(5) . . . . ? N4 P4 O51 C51 -96.0(5) . . . . ? Pd2 P4 O51 C51 142.3(4) . . . . ? P4 O51 C51 C52 -132.2(5) . . . . ? P4 O51 C51 C56 51.5(7) . . . . ? C56 C51 C52 C53 -0.8(10) . . . . ? O51 C51 C52 C53 -177.1(5) . . . . ? C51 C52 C53 C54 -0.9(11) . . . . ? C52 C53 C54 C55 1.9(12) . . . . ? C53 C54 C55 C56 -1.3(12) . . . . ? C52 C51 C56 C55 1.4(10) . . . . ? O51 C51 C56 C55 177.5(5) . . . . ? C54 C55 C56 C51 -0.4(11) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.338 _refine_diff_density_min -0.331 _refine_diff_density_rms 0.075