Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 188 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Alexandra Slawin' 'Matthew Wainwright' 'J. Derek Woollins' _publ_contact_author_name 'J. Derek Woollins' _publ_contact_author_address ; Department of Chemistry University of St Andrews St Andrews Fife KY16 9ST UNITED KINGDOM ; _publ_contact_author_email 'J.D.WOOLINS@ST-ANDREWS.AC.UK' data_3 _database_code_CSD 168899 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C27 H26 Cl2 N2 O P2 Pt' _chemical_formula_structural 'C27 H26 Cl2 N2 O P2 Pt' _chemical_formula_analytical 'C27 H26 Cl2 N2 O P2 Pt' _chemical_formula_sum 'C27 H26 Cl2 N2 O P2 Pt' _chemical_formula_weight 722.43 _chemical_melting_point ? _chemical_compound_source ? 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 P2(1)cn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y, -z' 'x, -y+1/2, z+1/2' 'x+1/2, y+1/2, -z+1/2' _cell_length_a 10.0447(5) _cell_length_b 14.4768(7) _cell_length_c 18.5427(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2696.4(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 58 _cell_measurement_theta_min 23 _cell_measurement_theta_max 337 _exptl_crystal_description prism _exptl_crystal_colour clear _exptl_crystal_size_max .16 _exptl_crystal_size_mid .16 _exptl_crystal_size_min .28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.780 _exptl_crystal_density_method ? _exptl_crystal_F_000 1408 _exptl_absorpt_coefficient_mu 5.544 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.670491 _exptl_absorpt_correction_T_max 1.00000 _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 SMART _diffrn_measurement_method CCD _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11318 _diffrn_reflns_av_R_equivalents 0.0421 _diffrn_reflns_av_sigmaI/netI 0.0461 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 23.26 _reflns_number_total 3199 _reflns_number_observed 2605 _reflns_observed_criterion >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART/SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement on F^2^ for ALL reflections except for 50 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0164P)^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 riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00155(8) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.007(7) _refine_ls_number_reflns 3149 _refine_ls_number_parameters 317 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0309 _refine_ls_R_factor_obs 0.0209 _refine_ls_wR_factor_all 0.0457 _refine_ls_wR_factor_obs 0.0389 _refine_ls_goodness_of_fit_all 0.828 _refine_ls_goodness_of_fit_obs 0.885 _refine_ls_restrained_S_all 0.953 _refine_ls_restrained_S_obs 0.884 _refine_ls_shift/esd_max -0.012 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pt1 Pt 0.23906(9) 0.278598(12) 0.145838(9) 0.02651(8) Uani 1 d . . Cl1 Cl 0.2497(5) 0.28332(10) 0.27275(7) 0.0428(6) Uani 1 d . . Cl2 Cl 0.0065(4) 0.2567(2) 0.1534(2) 0.0543(8) Uani 1 d . . P1 P 0.4586(3) 0.28431(13) 0.14674(13) 0.0274(6) Uani 1 d . . N1 N 0.5314(5) 0.2920(3) 0.0633(3) 0.0348(14) Uani 1 d . . C1 C 0.5373(7) 0.3759(4) 0.1978(3) 0.030(2) Uani 1 d . . C2 C 0.4716(9) 0.4591(5) 0.2046(3) 0.047(2) Uani 1 d . . H2A H 0.3840(9) 0.4655(5) 0.1891(3) 0.056 Uiso 1 calc R . C3 C 0.5406(11) 0.5348(5) 0.2359(4) 0.065(3) Uani 1 d . . H3A H 0.4980(11) 0.5916(5) 0.2404(4) 0.078 Uiso 1 calc R . C4 C 0.6689(10) 0.5253(6) 0.2597(4) 0.070(3) Uani 1 d . . H4A H 0.7130(10) 0.5759(6) 0.2793(4) 0.084 Uiso 1 calc R . C5 C 0.7320(18) 0.4431(6) 0.2548(4) 0.080(3) Uani 1 d . . H5A H 0.8181(18) 0.4364(6) 0.2726(4) 0.096 Uiso 1 calc R . C6 C 0.6660(9) 0.3675(6) 0.2224(4) 0.064(2) Uani 1 d . . H6A H 0.7101(9) 0.3113(6) 0.2177(4) 0.077 Uiso 1 calc R . C7 C 0.5209(7) 0.1751(4) 0.1805(3) 0.027(2) Uani 1 d . . C8 C 0.5386(7) 0.1617(5) 0.2547(3) 0.039(2) Uani 1 d . . H8A H 0.5267(7) 0.2110(5) 0.2862(3) 0.047 Uiso 1 calc R . C9 C 0.5735(8) 0.0764(5) 0.2814(4) 0.050(2) Uani 1 d . . H9A H 0.5824(8) 0.0678(5) 0.3309(4) 0.060 Uiso 1 calc R . C10 C 0.5952(9) 0.0037(5) 0.2349(5) 0.060(2) Uani 1 d . . H10A H 0.6195(9) -0.0538(5) 0.2531(5) 0.072 Uiso 1 calc R . C11 C 0.5812(9) 0.0156(5) 0.1619(4) 0.055(2) Uani 1 d . . H11A H 0.5968(9) -0.0338(5) 0.1310(4) 0.066 Uiso 1 calc R . C12 C 0.5437(8) 0.1011(4) 0.1332(4) 0.041(2) Uani 1 d . . H12A H 0.5341(8) 0.1088(4) 0.0837(4) 0.050 Uiso 1 calc R . C13 C 0.4839(10) 0.3465(7) 0.0056(5) 0.037(2) Uani 1 d . . O13 O 0.5641(9) 0.3890(5) -0.0312(4) 0.059(2) Uani 1 d . . N2 N 0.3528(8) 0.3434(4) -0.0126(3) 0.036(2) Uani 1 d . . P2 P 0.2385(6) 0.26785(9) 0.02720(7) 0.0292(3) Uani 1 d . . C14 C 0.0891(8) 0.2930(5) -0.0200(4) 0.029(2) Uani 1 d . . C15 C 0.0144(11) 0.3714(7) -0.0054(6) 0.050(3) Uani 1 d . . H15A H 0.0380(11) 0.4094(7) 0.0329(6) 0.060 Uiso 1 calc R . C16 C -0.0930(12) 0.3929(8) -0.0468(6) 0.049(3) Uani 1 d . . H16A H -0.1388(12) 0.4476(8) -0.0379(6) 0.059 Uiso 1 calc R . C17 C -0.1347(8) 0.3372(6) -0.1003(4) 0.052(2) Uani 1 d . . H17A H -0.2102(8) 0.3525(6) -0.1268(4) 0.063 Uiso 1 calc R . C18 C -0.0669(9) 0.2590(6) -0.1156(4) 0.057(2) Uani 1 d . . H18A H -0.0961(9) 0.2204(6) -0.1525(4) 0.069 Uiso 1 calc R . C19 C 0.0472(8) 0.2362(5) -0.0762(4) 0.048(2) Uani 1 d . . H19A H 0.0950(8) 0.1831(5) -0.0874(4) 0.057 Uiso 1 calc R . C20 C 0.2915(6) 0.1524(4) -0.0012(3) 0.030(2) Uani 1 d . . C21 C 0.3799(7) 0.1401(5) -0.0599(4) 0.043(2) Uani 1 d . . H21A H 0.4135(7) 0.1905(5) -0.0851(4) 0.052 Uiso 1 calc R . C22 C 0.4151(9) 0.0503(6) -0.0788(4) 0.058(2) Uani 1 d . . H22A H 0.4716(9) 0.0406(6) -0.1179(4) 0.070 Uiso 1 calc R . C23 C 0.3683(10) -0.0234(5) -0.0411(5) 0.066(3) Uani 1 d . . H23A H 0.3933(10) -0.0827(5) -0.0549(5) 0.080 Uiso 1 calc R . C24 C 0.2861(8) -0.0120(5) 0.0159(5) 0.061(3) Uani 1 d . . H24A H 0.2566(8) -0.0633(5) 0.0415(5) 0.073 Uiso 1 calc R . C25 C 0.2446(15) 0.0779(4) 0.0370(3) 0.046(2) Uani 1 d . . H25A H 0.1870(15) 0.0860(4) 0.0758(3) 0.055 Uiso 1 calc R . C26 C 0.6799(7) 0.2823(5) 0.0612(4) 0.057(2) Uani 1 d . . H26A H 0.7088(7) 0.2450(5) 0.1011(4) 0.086 Uiso 1 calc R . H26B H 0.7202(7) 0.3422(5) 0.0643(4) 0.086 Uiso 1 calc R . H26C H 0.7059(7) 0.2533(5) 0.0168(4) 0.086 Uiso 1 calc R . C27 C 0.3128(7) 0.4000(5) -0.0758(3) 0.054(2) Uani 1 d . . H27A H 0.2191(7) 0.3928(5) -0.0842(3) 0.081 Uiso 1 calc R . H27B H 0.3613(7) 0.3800(5) -0.1176(3) 0.081 Uiso 1 calc R . H27C H 0.3321(7) 0.4638(5) -0.0664(3) 0.081 Uiso 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 0.03165(13) 0.02506(11) 0.02282(11) -0.00064(10) 0.0036(4) 0.0024(3) Cl1 0.054(2) 0.0502(8) 0.0246(6) 0.0022(7) 0.0054(14) 0.011(2) Cl2 0.036(2) 0.082(2) 0.0445(14) 0.0111(12) 0.0061(13) -0.007(2) P1 0.0280(15) 0.0261(10) 0.0282(12) 0.0001(10) -0.0007(11) 0.0014(10) N1 0.032(3) 0.044(3) 0.028(3) 0.007(3) -0.003(3) -0.001(3) C1 0.036(5) 0.028(4) 0.027(4) 0.002(3) 0.004(3) 0.001(4) C2 0.068(6) 0.036(4) 0.036(4) -0.003(3) -0.006(4) -0.002(4) C3 0.122(10) 0.026(4) 0.048(5) -0.002(4) -0.009(6) -0.008(6) C4 0.109(9) 0.049(5) 0.053(5) 0.004(4) -0.018(5) -0.033(6) C5 0.073(6) 0.074(5) 0.092(6) 0.000(5) -0.034(11) -0.032(11) C6 0.069(6) 0.050(5) 0.072(6) -0.004(4) -0.010(5) -0.009(5) C7 0.030(4) 0.025(3) 0.026(3) 0.001(3) 0.005(3) -0.001(4) C8 0.039(5) 0.037(4) 0.041(4) -0.005(3) -0.003(4) 0.006(4) C9 0.048(5) 0.059(5) 0.043(5) 0.025(4) 0.001(4) 0.009(5) C10 0.060(6) 0.036(5) 0.084(7) 0.016(5) -0.001(5) 0.009(5) C11 0.065(6) 0.028(4) 0.073(6) -0.010(4) 0.005(5) 0.010(4) C12 0.050(5) 0.034(4) 0.041(4) -0.002(3) 0.001(4) 0.012(4) C13 0.033(5) 0.048(5) 0.030(5) 0.001(4) -0.001(4) -0.008(5) O13 0.047(5) 0.078(5) 0.051(4) 0.032(4) 0.003(4) -0.016(4) N2 0.054(5) 0.024(3) 0.030(3) 0.006(3) -0.009(3) -0.010(4) P2 0.0337(8) 0.0277(7) 0.0262(6) 0.0009(6) 0.002(2) 0.001(2) C14 0.031(4) 0.027(4) 0.030(4) 0.007(4) 0.004(3) 0.002(4) C15 0.066(9) 0.058(6) 0.027(5) 0.006(4) 0.013(5) 0.023(6) C16 0.039(7) 0.066(7) 0.042(6) 0.008(5) -0.004(5) 0.011(6) C17 0.023(5) 0.079(6) 0.055(5) 0.018(5) -0.005(4) 0.004(5) C18 0.047(5) 0.086(6) 0.038(4) -0.010(4) -0.020(4) -0.005(5) C19 0.056(6) 0.046(4) 0.042(4) -0.003(4) -0.003(4) 0.002(4) C20 0.032(4) 0.031(3) 0.027(3) -0.006(3) -0.003(3) 0.002(3) C21 0.043(5) 0.052(5) 0.034(4) -0.004(3) 0.001(4) 0.011(4) C22 0.059(6) 0.071(6) 0.045(5) -0.022(4) 0.004(4) 0.022(5) C23 0.082(8) 0.045(5) 0.072(6) -0.029(5) -0.021(6) 0.022(5) C24 0.073(8) 0.030(4) 0.080(5) -0.007(4) -0.015(5) -0.001(4) C25 0.058(5) 0.036(3) 0.045(3) -0.008(3) 0.011(8) -0.002(8) C26 0.040(4) 0.076(5) 0.056(4) 0.023(4) 0.002(4) 0.002(5) C27 0.058(6) 0.064(5) 0.040(4) 0.023(4) -0.009(4) -0.011(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 Pt1 P2 2.2054(13) . ? Pt1 P1 2.207(4) . ? Pt1 Cl1 2.3567(13) . ? Pt1 Cl2 2.362(4) . ? P1 N1 1.716(6) . ? P1 C1 1.810(7) . ? P1 C7 1.812(7) . ? N1 C13 1.413(10) . ? N1 C26 1.499(8) . ? C1 C2 1.380(9) . ? C1 C6 1.376(10) . ? C2 C3 1.421(10) . ? C3 C4 1.369(11) . ? C4 C5 1.352(14) . ? C5 C6 1.414(12) . ? C7 C12 1.402(8) . ? C7 C8 1.402(8) . ? C8 C9 1.375(9) . ? C9 C10 1.379(10) . ? C10 C11 1.373(10) . ? C11 C12 1.398(9) . ? C13 O13 1.222(11) . ? C13 N2 1.360(12) . ? N2 C27 1.485(8) . ? N2 P2 1.749(8) . ? P2 C14 1.776(9) . ? P2 C20 1.832(6) . ? C14 C15 1.386(11) . ? C14 C19 1.392(9) . ? C15 C16 1.361(15) . ? C16 C17 1.346(12) . ? C17 C18 1.350(10) . ? C18 C19 1.400(11) . ? C20 C25 1.374(9) . ? C20 C21 1.417(9) . ? C21 C22 1.391(9) . ? C22 C23 1.359(10) . ? C23 C24 1.352(10) . ? C24 C25 1.422(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P2 Pt1 P1 90.7(2) . . ? P2 Pt1 Cl1 176.6(2) . . ? P1 Pt1 Cl1 86.91(14) . . ? P2 Pt1 Cl2 92.7(2) . . ? P1 Pt1 Cl2 173.22(8) . . ? Cl1 Pt1 Cl2 89.38(14) . . ? N1 P1 C1 103.8(3) . . ? N1 P1 C7 102.7(3) . . ? C1 P1 C7 107.9(3) . . ? N1 P1 Pt1 114.9(2) . . ? C1 P1 Pt1 117.9(3) . . ? C7 P1 Pt1 108.3(3) . . ? C13 N1 C26 111.7(6) . . ? C13 N1 P1 125.1(6) . . ? C26 N1 P1 116.2(4) . . ? C2 C1 C6 119.7(7) . . ? C2 C1 P1 118.6(6) . . ? C6 C1 P1 121.3(6) . . ? C1 C2 C3 118.5(8) . . ? C4 C3 C2 120.9(8) . . ? C5 C4 C3 120.6(10) . . ? C4 C5 C6 119.3(14) . . ? C1 C6 C5 120.9(9) . . ? C12 C7 C8 119.1(6) . . ? C12 C7 P1 120.5(5) . . ? C8 C7 P1 120.2(5) . . ? C9 C8 C7 120.7(7) . . ? C8 C9 C10 120.0(7) . . ? C9 C10 C11 120.3(7) . . ? C10 C11 C12 120.9(7) . . ? C11 C12 C7 118.9(6) . . ? O13 C13 N2 121.1(9) . . ? O13 C13 N1 118.8(9) . . ? N2 C13 N1 119.8(8) . . ? C13 N2 C27 116.1(7) . . ? C13 N2 P2 123.5(6) . . ? C27 N2 P2 120.0(6) . . ? N2 P2 C14 102.6(3) . . ? N2 P2 C20 105.0(4) . . ? C14 P2 C20 106.9(3) . . ? N2 P2 Pt1 112.0(3) . . ? C14 P2 Pt1 118.7(3) . . ? C20 P2 Pt1 110.5(2) . . ? C15 C14 C19 117.8(8) . . ? C15 C14 P2 121.9(7) . . ? C19 C14 P2 120.2(6) . . ? C16 C15 C14 120.4(10) . . ? C17 C16 C15 121.7(11) . . ? C16 C17 C18 120.0(8) . . ? C17 C18 C19 120.1(7) . . ? C14 C19 C18 119.9(7) . . ? C25 C20 C21 120.8(6) . . ? C25 C20 P2 118.0(5) . . ? C21 C20 P2 121.2(5) . . ? C22 C21 C20 118.1(7) . . ? C23 C22 C21 121.0(8) . . ? C22 C23 C24 121.2(7) . . ? C23 C24 C25 120.4(8) . . ? C20 C25 C24 118.4(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 N1 7.1(2) . . . . ? Cl1 Pt1 P1 N1 -175.4(2) . . . . ? Cl2 Pt1 P1 N1 127.7(5) . . . . ? P2 Pt1 P1 C1 130.0(2) . . . . ? Cl1 Pt1 P1 C1 -52.5(2) . . . . ? Cl2 Pt1 P1 C1 -109.4(5) . . . . ? P2 Pt1 P1 C7 -107.1(2) . . . . ? Cl1 Pt1 P1 C7 70.4(2) . . . . ? Cl2 Pt1 P1 C7 13.5(6) . . . . ? C1 P1 N1 C13 -89.8(7) . . . . ? C7 P1 N1 C13 157.8(6) . . . . ? Pt1 P1 N1 C13 40.4(7) . . . . ? C1 P1 N1 C26 58.3(6) . . . . ? C7 P1 N1 C26 -54.0(6) . . . . ? Pt1 P1 N1 C26 -171.5(4) . . . . ? N1 P1 C1 C2 97.9(6) . . . . ? C7 P1 C1 C2 -153.6(5) . . . . ? Pt1 P1 C1 C2 -30.5(6) . . . . ? N1 P1 C1 C6 -74.7(6) . . . . ? C7 P1 C1 C6 33.9(7) . . . . ? Pt1 P1 C1 C6 156.9(5) . . . . ? C6 C1 C2 C3 1.3(10) . . . . ? P1 C1 C2 C3 -171.4(5) . . . . ? C1 C2 C3 C4 -0.8(11) . . . . ? C2 C3 C4 C5 -1.0(13) . . . . ? C3 C4 C5 C6 2.4(14) . . . . ? C2 C1 C6 C5 0.1(12) . . . . ? P1 C1 C6 C5 172.6(7) . . . . ? C4 C5 C6 C1 -1.9(14) . . . . ? N1 P1 C7 C12 -34.1(7) . . . . ? C1 P1 C7 C12 -143.4(6) . . . . ? Pt1 P1 C7 C12 87.9(6) . . . . ? N1 P1 C7 C8 150.0(5) . . . . ? C1 P1 C7 C8 40.7(7) . . . . ? Pt1 P1 C7 C8 -88.0(6) . . . . ? C12 C7 C8 C9 -2.3(10) . . . . ? P1 C7 C8 C9 173.7(6) . . . . ? C7 C8 C9 C10 1.9(12) . . . . ? C8 C9 C10 C11 -0.5(13) . . . . ? C9 C10 C11 C12 -0.5(13) . . . . ? C10 C11 C12 C7 0.2(12) . . . . ? C8 C7 C12 C11 1.2(11) . . . . ? P1 C7 C12 C11 -174.8(6) . . . . ? C26 N1 C13 O13 -10.4(12) . . . . ? P1 N1 C13 O13 138.9(8) . . . . ? C26 N1 C13 N2 162.9(8) . . . . ? P1 N1 C13 N2 -47.8(11) . . . . ? O13 C13 N2 C27 -4.4(13) . . . . ? N1 C13 N2 C27 -177.6(7) . . . . ? O13 C13 N2 P2 167.9(7) . . . . ? N1 C13 N2 P2 -5.2(12) . . . . ? C13 N2 P2 C14 -178.0(7) . . . . ? C27 N2 P2 C14 -5.9(6) . . . . ? C13 N2 P2 C20 -66.4(7) . . . . ? C27 N2 P2 C20 105.7(6) . . . . ? C13 N2 P2 Pt1 53.6(8) . . . . ? C27 N2 P2 Pt1 -134.3(5) . . . . ? P1 Pt1 P2 N2 -42.7(3) . . . . ? Cl1 Pt1 P2 N2 -89.1(25) . . . . ? Cl2 Pt1 P2 N2 143.1(3) . . . . ? P1 Pt1 P2 C14 -162.0(3) . . . . ? Cl1 Pt1 P2 C14 151.6(25) . . . . ? Cl2 Pt1 P2 C14 23.8(3) . . . . ? P1 Pt1 P2 C20 74.0(3) . . . . ? Cl1 Pt1 P2 C20 27.6(28) . . . . ? Cl2 Pt1 P2 C20 -100.2(3) . . . . ? N2 P2 C14 C15 -76.8(7) . . . . ? C20 P2 C14 C15 173.0(7) . . . . ? Pt1 P2 C14 C15 47.3(8) . . . . ? N2 P2 C14 C19 99.7(7) . . . . ? C20 P2 C14 C19 -10.5(7) . . . . ? Pt1 P2 C14 C19 -136.2(5) . . . . ? C19 C14 C15 C16 -2.4(13) . . . . ? P2 C14 C15 C16 174.2(8) . . . . ? C14 C15 C16 C17 3.6(16) . . . . ? C15 C16 C17 C18 -2.1(15) . . . . ? C16 C17 C18 C19 -0.4(12) . . . . ? C15 C14 C19 C18 0.0(12) . . . . ? P2 C14 C19 C18 -176.7(6) . . . . ? C17 C18 C19 C14 1.4(12) . . . . ? N2 P2 C20 C25 162.2(7) . . . . ? C14 P2 C20 C25 -89.2(8) . . . . ? Pt1 P2 C20 C25 41.3(8) . . . . ? N2 P2 C20 C21 -16.8(6) . . . . ? C14 P2 C20 C21 91.8(6) . . . . ? Pt1 P2 C20 C21 -137.7(5) . . . . ? C25 C20 C21 C22 1.6(11) . . . . ? P2 C20 C21 C22 -179.5(6) . . . . ? C20 C21 C22 C23 -1.3(12) . . . . ? C21 C22 C23 C24 0.0(13) . . . . ? C22 C23 C24 C25 1.2(14) . . . . ? C21 C20 C25 C24 -0.4(14) . . . . ? P2 C20 C25 C24 -179.4(7) . . . . ? C23 C24 C25 C20 -1.0(15) . . . . ? _refine_diff_density_max 0.525 _refine_diff_density_min -0.600 _refine_diff_density_rms 0.070 data_4 _database_code_CSD 168900 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C29 H30 Cl2 N2 O P2 Pt' _chemical_formula_structural 'C29 H30 Cl2 N2 O P2 Pt' _chemical_formula_analytical 'C29 H30 Cl2 N2 O P2 Pt' _chemical_formula_sum 'C29 H30 Cl2 N2 O P2 Pt' _chemical_formula_weight 750.48 _chemical_melting_point ? _chemical_compound_source ? 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 9.8640(4) _cell_length_b 10.8209(4) _cell_length_c 15.1644(6) _cell_angle_alpha 78.4300(10) _cell_angle_beta 80.0560(10) _cell_angle_gamma 66.6640(10) _cell_volume 1448.16(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 23 _cell_measurement_theta_min 23 _cell_measurement_theta_max 337 _exptl_crystal_description plate _exptl_crystal_colour clear _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.721 _exptl_crystal_density_method ? _exptl_crystal_F_000 736 _exptl_absorpt_coefficient_mu 5.165 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.700399 _exptl_absorpt_correction_T_max 1.00000 _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 SMART _diffrn_measurement_method CCD _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8990 _diffrn_reflns_av_R_equivalents 0.0183 _diffrn_reflns_av_sigmaI/netI 0.0408 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 28.59 _reflns_number_total 6504 _reflns_number_observed 5727 _reflns_observed_criterion >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART/SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement on F^2^ for ALL reflections except for 50 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0309P)^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 riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0012(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6454 _refine_ls_number_parameters 335 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0312 _refine_ls_R_factor_obs 0.0257 _refine_ls_wR_factor_all 0.0724 _refine_ls_wR_factor_obs 0.0590 _refine_ls_goodness_of_fit_all 0.978 _refine_ls_goodness_of_fit_obs 1.024 _refine_ls_restrained_S_all 1.182 _refine_ls_restrained_S_obs 1.024 _refine_ls_shift/esd_max 0.004 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pt1 Pt 0.142593(14) 0.438084(12) 0.232692(8) 0.02583(5) Uani 1 d . . Cl1 Cl 0.00360(12) 0.67193(9) 0.22441(8) 0.0476(2) Uani 1 d . . P1 P -0.05027(9) 0.37554(9) 0.27277(6) 0.0268(2) Uani 1 d . . C1 C -0.2222(4) 0.4924(4) 0.3231(2) 0.0333(7) Uani 1 d . . N1 N -0.0092(3) 0.2320(3) 0.3532(2) 0.0334(6) Uani 1 d . . Cl2 Cl 0.35710(10) 0.49098(10) 0.18893(7) 0.0438(2) Uani 1 d . . C2 C -0.2204(4) 0.5797(4) 0.3779(3) 0.0418(9) Uani 1 d . . H2A H -0.1304(4) 0.5806(4) 0.3880(3) 0.050 Uiso 1 calc R . N2 N 0.2001(3) 0.1096(3) 0.2565(2) 0.0333(6) Uani 1 d . . P2 P 0.28436(10) 0.22435(8) 0.21669(6) 0.0281(2) Uani 1 d . . C3 C -0.3527(5) 0.6660(5) 0.4180(3) 0.0556(11) Uani 1 d . . H3A H -0.3516(5) 0.7256(5) 0.4541(3) 0.067 Uiso 1 calc R . C4 C -0.4862(5) 0.6626(6) 0.4037(3) 0.0632(13) Uani 1 d . . H4A H -0.5748(5) 0.7193(6) 0.4311(3) 0.076 Uiso 1 calc R . C5 C -0.4888(5) 0.5763(6) 0.3494(3) 0.0599(13) Uani 1 d . . H5A H -0.5790(5) 0.5752(6) 0.3399(3) 0.072 Uiso 1 calc R . C6 C -0.3579(4) 0.4913(5) 0.3090(3) 0.0453(9) Uani 1 d . . H6A H -0.3600(4) 0.4330(5) 0.2723(3) 0.054 Uiso 1 calc R . C7 C -0.1030(4) 0.3343(4) 0.1772(2) 0.0320(7) Uani 1 d . . C8 C -0.1158(4) 0.4278(4) 0.0982(2) 0.0409(8) Uani 1 d . . H8A H -0.0988(4) 0.5068(4) 0.0970(2) 0.049 Uiso 1 calc R . C9 C -0.1538(5) 0.4034(5) 0.0215(3) 0.0556(11) Uani 1 d . . H9A H -0.1642(5) 0.4667(5) -0.0309(3) 0.067 Uiso 1 calc R . C10 C -0.1760(5) 0.2852(6) 0.0229(3) 0.0573(12) Uani 1 d . . H10A H -0.1985(5) 0.2679(6) -0.0293(3) 0.069 Uiso 1 calc R . C11 C -0.1652(5) 0.1927(5) 0.1005(3) 0.0564(12) Uani 1 d . . H11A H -0.1814(5) 0.1136(5) 0.1007(3) 0.068 Uiso 1 calc R . C12 C -0.1298(5) 0.2170(4) 0.1794(3) 0.0438(9) Uani 1 d . . H12A H -0.1243(5) 0.1555(4) 0.2325(3) 0.053 Uiso 1 calc R . C13 C 0.1140(4) 0.1145(4) 0.3412(3) 0.0388(8) Uani 1 d . . O13 O 0.1418(4) 0.0159(3) 0.4001(2) 0.0654(9) Uani 1 d . . C14 C 0.4565(4) 0.1513(4) 0.2702(2) 0.0352(8) Uani 1 d . . C15 C 0.4592(5) 0.1961(5) 0.3493(3) 0.0535(11) Uani 1 d . . H15A H 0.3790(5) 0.2690(5) 0.3698(3) 0.064 Uiso 1 calc R . C16 C 0.5817(6) 0.1317(6) 0.3975(4) 0.073(2) Uani 1 d . . H16A H 0.5827(6) 0.1606(6) 0.4511(4) 0.087 Uiso 1 calc R . C17 C 0.7018(5) 0.0256(5) 0.3669(4) 0.0629(13) Uani 1 d . . H17A H 0.7840(5) -0.0165(5) 0.3995(4) 0.075 Uiso 1 calc R . C18 C 0.7010(5) -0.0178(4) 0.2895(4) 0.0567(12) Uani 1 d . . H18A H 0.7826(5) -0.0902(4) 0.2695(4) 0.068 Uiso 1 calc R . C19 C 0.5794(4) 0.0443(4) 0.2391(3) 0.0453(10) Uani 1 d . . H19A H 0.5804(4) 0.0147(4) 0.1854(3) 0.054 Uiso 1 calc R . C20 C 0.3302(4) 0.2121(4) 0.0968(2) 0.0341(7) Uani 1 d . . C21 C 0.2389(4) 0.1835(4) 0.0495(3) 0.0418(9) Uani 1 d . . H21A H 0.1612(4) 0.1592(4) 0.0807(3) 0.050 Uiso 1 calc R . C22 C 0.2641(5) 0.1912(5) -0.0436(3) 0.0528(11) Uani 1 d . . H22A H 0.2043(5) 0.1705(5) -0.0748(3) 0.063 Uiso 1 calc R . C23 C 0.3779(6) 0.2296(5) -0.0907(3) 0.0572(12) Uani 1 d . . H23A H 0.3931(6) 0.2366(5) -0.1535(3) 0.069 Uiso 1 calc R . C24 C 0.4687(5) 0.2576(5) -0.0445(3) 0.0562(12) Uani 1 d . . H24A H 0.5458(5) 0.2824(5) -0.0763(3) 0.067 Uiso 1 calc R . C25 C 0.4459(5) 0.2491(4) 0.0494(3) 0.0446(9) Uani 1 d . . H25A H 0.5076(5) 0.2679(4) 0.0802(3) 0.054 Uiso 1 calc R . C26 C -0.0863(5) 0.2360(5) 0.4466(3) 0.0529(11) Uani 1 d . . H26A H -0.0870(5) 0.1464(5) 0.4716(3) 0.063 Uiso 1 calc R . H26B H -0.1886(5) 0.2988(5) 0.4440(3) 0.063 Uiso 1 calc R . C27 C 0.2892(5) -0.0332(4) 0.2383(3) 0.0470(10) Uani 1 d . . H27A H 0.3459(5) -0.0841(4) 0.2890(3) 0.056 Uiso 1 calc R . H27B H 0.3588(5) -0.0316(4) 0.1848(3) 0.056 Uiso 1 calc R . C28 C -0.0144(8) 0.2790(7) 0.5084(3) 0.090(2) Uani 1 d . . H28A H -0.0682(8) 0.2797(7) 0.5675(3) 0.134 Uiso 1 calc R . H28B H -0.0154(8) 0.3685(7) 0.4847(3) 0.134 Uiso 1 calc R . H28C H 0.0863(8) 0.2162(7) 0.5123(3) 0.134 Uiso 1 calc R . C29 C 0.1914(6) -0.1045(5) 0.2242(4) 0.072(2) Uani 1 d . . H29A H 0.2522(6) -0.1953(5) 0.2128(4) 0.108 Uiso 1 calc R . H29B H 0.1365(6) -0.0553(5) 0.1734(4) 0.108 Uiso 1 calc R . H29C H 0.1237(6) -0.1078(5) 0.2775(4) 0.108 Uiso 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 0.02674(7) 0.02219(7) 0.02940(8) -0.00446(4) -0.00097(5) -0.01050(5) Cl1 0.0474(5) 0.0237(4) 0.0643(6) -0.0088(4) 0.0057(5) -0.0091(4) P1 0.0258(4) 0.0267(4) 0.0269(4) -0.0035(3) 0.0003(3) -0.0103(3) C1 0.030(2) 0.035(2) 0.031(2) -0.0047(14) -0.0006(14) -0.0099(15) N1 0.037(2) 0.032(2) 0.0283(15) -0.0006(12) 0.0015(12) -0.0134(13) Cl2 0.0371(5) 0.0438(5) 0.0578(6) -0.0064(4) -0.0022(4) -0.0244(4) C2 0.039(2) 0.049(2) 0.038(2) -0.014(2) 0.003(2) -0.016(2) N2 0.033(2) 0.0235(14) 0.042(2) -0.0061(12) 0.0022(13) -0.0110(12) P2 0.0277(4) 0.0238(4) 0.0319(4) -0.0064(3) 0.0016(3) -0.0095(3) C3 0.053(3) 0.059(3) 0.055(3) -0.033(2) 0.011(2) -0.016(2) C4 0.042(2) 0.074(3) 0.060(3) -0.028(3) 0.013(2) -0.006(2) C5 0.032(2) 0.085(4) 0.054(3) -0.028(3) 0.003(2) -0.009(2) C6 0.033(2) 0.059(3) 0.046(2) -0.021(2) 0.001(2) -0.016(2) C7 0.027(2) 0.040(2) 0.031(2) -0.0066(14) -0.0006(13) -0.0143(15) C8 0.044(2) 0.041(2) 0.037(2) -0.002(2) -0.005(2) -0.018(2) C9 0.057(3) 0.071(3) 0.038(2) 0.002(2) -0.012(2) -0.025(2) C10 0.056(3) 0.090(4) 0.042(2) -0.021(2) -0.006(2) -0.039(3) C11 0.059(3) 0.070(3) 0.060(3) -0.025(2) 0.000(2) -0.040(3) C12 0.047(2) 0.053(2) 0.042(2) -0.010(2) 0.000(2) -0.030(2) C13 0.041(2) 0.032(2) 0.040(2) 0.001(2) 0.000(2) -0.015(2) O13 0.075(2) 0.038(2) 0.058(2) 0.0140(14) 0.008(2) -0.010(2) C14 0.031(2) 0.032(2) 0.039(2) -0.0027(15) -0.0026(15) -0.0106(15) C15 0.042(2) 0.056(3) 0.050(2) -0.019(2) -0.009(2) 0.001(2) C16 0.057(3) 0.093(4) 0.057(3) -0.017(3) -0.023(2) -0.006(3) C17 0.047(3) 0.059(3) 0.070(3) 0.008(2) -0.021(2) -0.008(2) C18 0.035(2) 0.033(2) 0.087(4) -0.003(2) -0.006(2) 0.000(2) C19 0.035(2) 0.033(2) 0.064(3) -0.013(2) 0.001(2) -0.008(2) C20 0.036(2) 0.029(2) 0.032(2) -0.0073(14) 0.0042(14) -0.0087(15) C21 0.038(2) 0.045(2) 0.044(2) -0.016(2) 0.002(2) -0.015(2) C22 0.051(3) 0.056(3) 0.046(2) -0.020(2) -0.006(2) -0.008(2) C23 0.067(3) 0.050(3) 0.038(2) -0.014(2) 0.005(2) -0.005(2) C24 0.060(3) 0.057(3) 0.046(2) -0.013(2) 0.020(2) -0.025(2) C25 0.049(2) 0.047(2) 0.041(2) -0.013(2) 0.007(2) -0.023(2) C26 0.057(3) 0.052(3) 0.032(2) 0.004(2) 0.012(2) -0.014(2) C27 0.048(2) 0.022(2) 0.067(3) -0.009(2) 0.001(2) -0.010(2) C28 0.131(6) 0.081(4) 0.038(3) -0.005(3) -0.026(3) -0.015(4) C29 0.075(3) 0.040(2) 0.111(5) -0.027(3) 0.005(3) -0.031(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 P1 2.2141(8) . ? Pt1 P2 2.2157(8) . ? Pt1 Cl1 2.3414(9) . ? Pt1 Cl2 2.3595(9) . ? P1 N1 1.725(3) . ? P1 C7 1.809(3) . ? P1 C1 1.817(4) . ? C1 C2 1.384(5) . ? C1 C6 1.397(5) . ? N1 C13 1.385(5) . ? N1 C26 1.488(5) . ? C2 C3 1.390(6) . ? N2 C13 1.411(5) . ? N2 C27 1.500(5) . ? N2 P2 1.714(3) . ? P2 C20 1.815(4) . ? P2 C14 1.822(4) . ? C3 C4 1.387(7) . ? C4 C5 1.373(7) . ? C5 C6 1.379(6) . ? C7 C12 1.388(5) . ? C7 C8 1.393(5) . ? C8 C9 1.385(6) . ? C9 C10 1.375(7) . ? C10 C11 1.374(7) . ? C11 C12 1.403(6) . ? C13 O13 1.217(5) . ? C14 C15 1.389(6) . ? C14 C19 1.393(5) . ? C15 C16 1.384(6) . ? C16 C17 1.372(7) . ? C17 C18 1.352(7) . ? C18 C19 1.395(6) . ? C20 C25 1.394(5) . ? C20 C21 1.399(5) . ? C21 C22 1.383(6) . ? C22 C23 1.385(7) . ? C23 C24 1.379(7) . ? C24 C25 1.393(6) . ? C26 C28 1.504(7) . ? C27 C29 1.515(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 P2 88.80(3) . . ? P1 Pt1 Cl1 95.50(3) . . ? P2 Pt1 Cl1 170.68(3) . . ? P1 Pt1 Cl2 176.54(3) . . ? P2 Pt1 Cl2 87.74(3) . . ? Cl1 Pt1 Cl2 87.92(4) . . ? N1 P1 C7 106.9(2) . . ? N1 P1 C1 103.0(2) . . ? C7 P1 C1 104.6(2) . . ? N1 P1 Pt1 111.02(11) . . ? C7 P1 Pt1 111.24(11) . . ? C1 P1 Pt1 119.12(12) . . ? C2 C1 C6 119.4(4) . . ? C2 C1 P1 120.8(3) . . ? C6 C1 P1 119.7(3) . . ? C13 N1 C26 115.1(3) . . ? C13 N1 P1 122.5(2) . . ? C26 N1 P1 121.4(3) . . ? C1 C2 C3 120.2(4) . . ? C13 N2 C27 112.5(3) . . ? C13 N2 P2 120.6(2) . . ? C27 N2 P2 115.6(2) . . ? N2 P2 C20 103.8(2) . . ? N2 P2 C14 103.9(2) . . ? C20 P2 C14 108.2(2) . . ? N2 P2 Pt1 114.86(11) . . ? C20 P2 Pt1 108.62(12) . . ? C14 P2 Pt1 116.48(12) . . ? C4 C3 C2 119.5(4) . . ? C5 C4 C3 120.6(4) . . ? C4 C5 C6 120.0(4) . . ? C5 C6 C1 120.2(4) . . ? C12 C7 C8 120.1(3) . . ? C12 C7 P1 123.7(3) . . ? C8 C7 P1 116.3(3) . . ? C9 C8 C7 120.1(4) . . ? C10 C9 C8 119.9(4) . . ? C11 C10 C9 120.7(4) . . ? C10 C11 C12 120.2(4) . . ? C7 C12 C11 119.0(4) . . ? O13 C13 N1 121.0(4) . . ? O13 C13 N2 121.1(4) . . ? N1 C13 N2 117.8(3) . . ? C15 C14 C19 119.3(4) . . ? C15 C14 P2 118.2(3) . . ? C19 C14 P2 122.2(3) . . ? C16 C15 C14 119.8(4) . . ? C17 C16 C15 120.6(5) . . ? C18 C17 C16 120.1(4) . . ? C17 C18 C19 121.0(4) . . ? C14 C19 C18 119.2(4) . . ? C25 C20 C21 119.6(3) . . ? C25 C20 P2 119.4(3) . . ? C21 C20 P2 120.5(3) . . ? C22 C21 C20 120.0(4) . . ? C21 C22 C23 120.3(4) . . ? C24 C23 C22 120.0(4) . . ? C23 C24 C25 120.5(4) . . ? C24 C25 C20 119.6(4) . . ? N1 C26 C28 112.9(4) . . ? N2 C27 C29 111.9(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 P2 Pt1 P1 N1 47.93(11) . . . . ? Cl1 Pt1 P1 N1 -140.35(11) . . . . ? Cl2 Pt1 P1 N1 48.3(6) . . . . ? P2 Pt1 P1 C7 -70.92(13) . . . . ? Cl1 Pt1 P1 C7 100.79(13) . . . . ? Cl2 Pt1 P1 C7 -70.6(6) . . . . ? P2 Pt1 P1 C1 167.30(13) . . . . ? Cl1 Pt1 P1 C1 -20.98(14) . . . . ? Cl2 Pt1 P1 C1 167.6(5) . . . . ? N1 P1 C1 C2 89.9(3) . . . . ? C7 P1 C1 C2 -158.5(3) . . . . ? Pt1 P1 C1 C2 -33.5(3) . . . . ? N1 P1 C1 C6 -87.9(3) . . . . ? C7 P1 C1 C6 23.7(4) . . . . ? Pt1 P1 C1 C6 148.7(3) . . . . ? C7 P1 N1 C13 68.7(3) . . . . ? C1 P1 N1 C13 178.7(3) . . . . ? Pt1 P1 N1 C13 -52.7(3) . . . . ? C7 P1 N1 C26 -123.7(3) . . . . ? C1 P1 N1 C26 -13.8(3) . . . . ? Pt1 P1 N1 C26 114.8(3) . . . . ? C6 C1 C2 C3 -0.4(6) . . . . ? P1 C1 C2 C3 -178.3(3) . . . . ? C13 N2 P2 C20 -163.2(3) . . . . ? C27 N2 P2 C20 55.9(3) . . . . ? C13 N2 P2 C14 83.7(3) . . . . ? C27 N2 P2 C14 -57.2(3) . . . . ? C13 N2 P2 Pt1 -44.7(3) . . . . ? C27 N2 P2 Pt1 174.4(2) . . . . ? P1 Pt1 P2 N2 -9.72(12) . . . . ? Cl1 Pt1 P2 N2 -127.4(2) . . . . ? Cl2 Pt1 P2 N2 170.30(12) . . . . ? P1 Pt1 P2 C20 106.00(13) . . . . ? Cl1 Pt1 P2 C20 -11.7(3) . . . . ? Cl2 Pt1 P2 C20 -73.98(13) . . . . ? P1 Pt1 P2 C14 -131.52(13) . . . . ? Cl1 Pt1 P2 C14 110.8(2) . . . . ? Cl2 Pt1 P2 C14 48.50(13) . . . . ? C1 C2 C3 C4 0.9(7) . . . . ? C2 C3 C4 C5 -0.9(8) . . . . ? C3 C4 C5 C6 0.4(8) . . . . ? C4 C5 C6 C1 0.0(8) . . . . ? C2 C1 C6 C5 -0.1(6) . . . . ? P1 C1 C6 C5 177.8(4) . . . . ? N1 P1 C7 C12 10.6(4) . . . . ? C1 P1 C7 C12 -98.2(3) . . . . ? Pt1 P1 C7 C12 131.9(3) . . . . ? N1 P1 C7 C8 -169.1(3) . . . . ? C1 P1 C7 C8 82.0(3) . . . . ? Pt1 P1 C7 C8 -47.8(3) . . . . ? C12 C7 C8 C9 -0.6(6) . . . . ? P1 C7 C8 C9 179.1(3) . . . . ? C7 C8 C9 C10 -1.3(7) . . . . ? C8 C9 C10 C11 1.9(7) . . . . ? C9 C10 C11 C12 -0.6(8) . . . . ? C8 C7 C12 C11 1.9(6) . . . . ? P1 C7 C12 C11 -177.9(3) . . . . ? C10 C11 C12 C7 -1.3(7) . . . . ? C26 N1 C13 O13 10.1(6) . . . . ? P1 N1 C13 O13 178.3(3) . . . . ? C26 N1 C13 N2 -174.2(3) . . . . ? P1 N1 C13 N2 -5.9(5) . . . . ? C27 N2 C13 O13 18.3(5) . . . . ? P2 N2 C13 O13 -123.6(4) . . . . ? C27 N2 C13 N1 -157.4(3) . . . . ? P2 N2 C13 N1 60.6(4) . . . . ? N2 P2 C14 C15 -96.0(3) . . . . ? C20 P2 C14 C15 154.1(3) . . . . ? Pt1 P2 C14 C15 31.4(4) . . . . ? N2 P2 C14 C19 78.0(3) . . . . ? C20 P2 C14 C19 -31.9(4) . . . . ? Pt1 P2 C14 C19 -154.6(3) . . . . ? C19 C14 C15 C16 -1.8(7) . . . . ? P2 C14 C15 C16 172.4(4) . . . . ? C14 C15 C16 C17 1.2(9) . . . . ? C15 C16 C17 C18 -0.5(9) . . . . ? C16 C17 C18 C19 0.4(8) . . . . ? C15 C14 C19 C18 1.7(6) . . . . ? P2 C14 C19 C18 -172.2(3) . . . . ? C17 C18 C19 C14 -1.0(7) . . . . ? N2 P2 C20 C25 -155.7(3) . . . . ? C14 P2 C20 C25 -45.7(3) . . . . ? Pt1 P2 C20 C25 81.7(3) . . . . ? N2 P2 C20 C21 32.8(3) . . . . ? C14 P2 C20 C21 142.8(3) . . . . ? Pt1 P2 C20 C21 -89.9(3) . . . . ? C25 C20 C21 C22 0.3(6) . . . . ? P2 C20 C21 C22 171.9(3) . . . . ? C20 C21 C22 C23 -1.2(6) . . . . ? C21 C22 C23 C24 1.4(7) . . . . ? C22 C23 C24 C25 -0.7(7) . . . . ? C23 C24 C25 C20 -0.1(7) . . . . ? C21 C20 C25 C24 0.3(6) . . . . ? P2 C20 C25 C24 -171.3(3) . . . . ? C13 N1 C26 C28 82.4(5) . . . . ? P1 N1 C26 C28 -86.0(4) . . . . ? C13 N2 C27 C29 68.8(5) . . . . ? P2 N2 C27 C29 -147.3(3) . . . . ? _refine_diff_density_max 1.971 _refine_diff_density_min -1.570 _refine_diff_density_rms 0.105 data_10 _database_code_CSD 168901 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C37 H42 Cl4 N2 O P2 Pd2' _chemical_formula_structural 'C37 H42 Cl4 N2 O P2 Pd2' _chemical_formula_analytical 'C37 H42 Cl4 N2 O P2 Pd2' _chemical_formula_sum 'C37 H42 Cl4 N2 O P2 Pd2' _chemical_formula_weight 947.27 _chemical_melting_point ? _chemical_compound_source ? 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)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.2866(3) _cell_length_b 27.6453(5) _cell_length_c 9.7662(2) _cell_angle_alpha 90.00 _cell_angle_beta 92.6320(10) _cell_angle_gamma 90.00 _cell_volume 3853.16(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 22 _cell_measurement_theta_min 23 _cell_measurement_theta_max 337 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max .06 _exptl_crystal_size_mid .2 _exptl_crystal_size_min .2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.633 _exptl_crystal_density_method ? _exptl_crystal_F_000 1904 _exptl_absorpt_coefficient_mu 1.326 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.812523 _exptl_absorpt_correction_T_max 1.0000 _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 SMART _diffrn_measurement_method CCD _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23436 _diffrn_reflns_av_R_equivalents 0.0489 _diffrn_reflns_av_sigmaI/netI 0.0768 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 28.77 _reflns_number_total 9018 _reflns_number_observed 4874 _reflns_observed_criterion >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART/SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement on F^2^ for ALL reflections except for 49 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0682P)^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 riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00107(13) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 8969 _refine_ls_number_parameters 434 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1178 _refine_ls_R_factor_obs 0.0470 _refine_ls_wR_factor_all 0.1472 _refine_ls_wR_factor_obs 0.1041 _refine_ls_goodness_of_fit_all 0.969 _refine_ls_goodness_of_fit_obs 0.983 _refine_ls_restrained_S_all 1.006 _refine_ls_restrained_S_obs 0.983 _refine_ls_shift/esd_max 0.010 _refine_ls_shift/esd_mean 0.001 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pd1 Pd 0.74193(2) 0.544623(13) -0.24495(4) 0.03197(13) Uani 1 d . . Cl1 Cl 0.84579(9) 0.48493(5) -0.3188(2) 0.0524(4) Uani 1 d . . Cl2 Cl 0.64112(9) 0.48410(5) -0.16672(15) 0.0507(4) Uani 1 d . . P1 P 0.84236(8) 0.60103(5) -0.30514(13) 0.0323(3) Uani 1 d . . C1 C 0.9557(3) 0.5848(2) -0.2283(5) 0.0398(12) Uani 1 d . . C2 C 0.9600(4) 0.5708(2) -0.0917(5) 0.0484(14) Uani 1 d . . H2A H 0.9059(4) 0.5708(2) -0.0423(5) 0.058 Uiso 1 calc R . C3 C 1.0441(4) 0.5568(2) -0.0290(6) 0.056(2) Uani 1 d . . H3A H 1.0471(4) 0.5489(2) 0.0636(6) 0.068 Uiso 1 calc R . C4 C 1.1219(4) 0.5547(2) -0.1015(7) 0.073(2) Uani 1 d . . H4A H 1.1783(4) 0.5446(2) -0.0598(7) 0.088 Uiso 1 calc R . C5 C 1.1172(4) 0.5676(3) -0.2369(9) 0.115(3) Uani 1 d . . H5A H 1.1713(4) 0.5663(3) -0.2863(9) 0.138 Uiso 1 calc R . C6 C 1.0341(4) 0.5825(3) -0.3024(7) 0.083(2) Uani 1 d . . H6A H 1.0319(4) 0.5908(3) -0.3948(7) 0.099 Uiso 1 calc R . C7 C 0.8552(3) 0.6093(2) -0.4875(5) 0.0394(12) Uani 1 d . . C8 C 0.8458(4) 0.6548(2) -0.5460(5) 0.0508(14) Uani 1 d . . H8A H 0.8327(4) 0.6814(2) -0.4917(5) 0.061 Uiso 1 calc R . C9 C 0.8557(4) 0.6607(2) -0.6845(6) 0.066(2) Uani 1 d . . H9A H 0.8489(4) 0.6913(2) -0.7235(6) 0.079 Uiso 1 calc R . C10 C 0.8751(5) 0.6226(3) -0.7636(7) 0.076(2) Uani 1 d . . H10A H 0.8816(5) 0.6270(3) -0.8571(7) 0.091 Uiso 1 calc R . C11 C 0.8853(6) 0.5777(3) -0.7086(7) 0.092(3) Uani 1 d . . H11A H 0.8996(6) 0.5517(3) -0.7642(7) 0.111 Uiso 1 calc R . C12 C 0.8745(5) 0.5706(2) -0.5699(6) 0.071(2) Uani 1 d . . H12A H 0.8803(5) 0.5397(2) -0.5326(6) 0.085 Uiso 1 calc R . N1 N 0.8232(3) 0.65780(14) -0.2436(4) 0.0369(10) Uani 1 d . . C26 C 0.9066(3) 0.6910(2) -0.2284(6) 0.0487(14) Uani 1 d . . H26A H 0.9613(3) 0.6746(2) -0.2612(6) 0.058 Uiso 1 calc R . H26B H 0.8953(3) 0.7195(2) -0.2847(6) 0.058 Uiso 1 calc R . C28 C 0.9263(5) 0.7065(2) -0.0815(6) 0.079(2) Uani 1 d . . H28A H 0.9799(5) 0.7274(2) -0.0763(6) 0.119 Uiso 1 calc R . H28B H 0.9385(5) 0.6784(2) -0.0255(6) 0.119 Uiso 1 calc R . H28C H 0.8729(5) 0.7234(2) -0.0493(6) 0.119 Uiso 1 calc R . C13 C 0.7388(3) 0.6823(2) -0.2491(5) 0.0402(12) Uani 1 d . . O13 O 0.7367(2) 0.72627(13) -0.2490(4) 0.0652(12) Uani 1 d . . N2 N 0.6544(3) 0.65668(14) -0.2535(4) 0.0358(10) Uani 1 d . . C27 C 0.5696(3) 0.6888(2) -0.2670(5) 0.0440(13) Uani 1 d . . H27A H 0.5799(3) 0.7173(2) -0.2101(5) 0.053 Uiso 1 calc R . H27B H 0.5159(3) 0.6717(2) -0.2338(5) 0.053 Uiso 1 calc R . C29 C 0.5483(4) 0.7045(2) -0.4127(6) 0.071(2) Uani 1 d . . H29A H 0.4939(4) 0.7249(2) -0.4165(6) 0.106 Uiso 1 calc R . H29B H 0.5368(4) 0.6765(2) -0.4692(6) 0.106 Uiso 1 calc R . H29C H 0.6008(4) 0.7221(2) -0.4454(6) 0.106 Uiso 1 calc R . P2 P 0.63911(8) 0.60006(5) -0.18730(13) 0.0315(3) Uani 1 d . . C14 C 0.6282(3) 0.6098(2) -0.0060(5) 0.0376(12) Uani 1 d . . C15 C 0.6390(4) 0.6556(2) 0.0504(5) 0.0474(14) Uani 1 d . . H15A H 0.6511(4) 0.6818(2) -0.0057(5) 0.057 Uiso 1 calc R . C16 C 0.6318(4) 0.6623(2) 0.1894(6) 0.058(2) Uani 1 d . . H16A H 0.6386(4) 0.6933(2) 0.2261(6) 0.070 Uiso 1 calc R . C17 C 0.6151(4) 0.6248(2) 0.2732(6) 0.065(2) Uani 1 d . . H17A H 0.6122(4) 0.6297(2) 0.3671(6) 0.077 Uiso 1 calc R . C18 C 0.6025(5) 0.5794(2) 0.2188(6) 0.064(2) Uani 1 d . . H18A H 0.5893(5) 0.5536(2) 0.2761(6) 0.077 Uiso 1 calc R . C19 C 0.6092(4) 0.5715(2) 0.0808(6) 0.056(2) Uani 1 d . . H19A H 0.6011(4) 0.5404(2) 0.0453(6) 0.067 Uiso 1 calc R . C20 C 0.5266(3) 0.5812(2) -0.2619(5) 0.0380(12) Uani 1 d . . C21 C 0.5211(4) 0.5703(2) -0.4009(5) 0.0501(14) Uani 1 d . . H21A H 0.5737(4) 0.5740(2) -0.4526(5) 0.060 Uiso 1 calc R . C22 C 0.4383(4) 0.5540(2) -0.4628(6) 0.056(2) Uani 1 d . . H22A H 0.4348(4) 0.5475(2) -0.5563(6) 0.067 Uiso 1 calc R . C23 C 0.3621(4) 0.5474(2) -0.3874(7) 0.069(2) Uani 1 d . . H23A H 0.3062(4) 0.5365(2) -0.4289(7) 0.083 Uiso 1 calc R . C24 C 0.3680(4) 0.5570(3) -0.2485(8) 0.082(2) Uani 1 d . . H24A H 0.3160(4) 0.5517(3) -0.1965(8) 0.099 Uiso 1 calc R . C25 C 0.4496(4) 0.5745(2) -0.1853(6) 0.064(2) Uani 1 d . . H25A H 0.4522(4) 0.5817(2) -0.0921(6) 0.077 Uiso 1 calc R . Pd2 Pd 0.23755(3) 0.73101(2) 0.24281(5) 0.0588(2) Uani 1 d . . Cl3 Cl 0.1301(2) 0.78347(8) 0.1426(3) 0.1321(10) Uani 1 d . . Cl4 Cl 0.3292(2) 0.79338(8) 0.3232(3) 0.1442(12) Uani 1 d . . C31 C 0.1885(4) 0.6699(2) 0.1126(6) 0.061(2) Uani 1 d . . H31A H 0.1801(4) 0.6916(2) 0.0403(6) 0.073 Uiso 1 calc R . C32 C 0.1301(4) 0.6749(2) 0.2183(7) 0.061(2) Uani 1 d . . H32A H 0.0843(4) 0.6988(2) 0.2102(7) 0.074 Uiso 1 calc R . C33 C 0.1336(4) 0.6452(2) 0.3453(7) 0.072(2) Uani 1 d . . H33A H 0.1035(4) 0.6144(2) 0.3254(7) 0.086 Uiso 1 calc R . H33B H 0.0979(4) 0.6615(2) 0.4137(7) 0.086 Uiso 1 calc R . C34 C 0.2319(5) 0.6358(2) 0.4052(7) 0.075(2) Uani 1 d . . H34A H 0.2284(5) 0.6293(2) 0.5024(7) 0.089 Uiso 1 calc R . H34B H 0.2562(5) 0.6069(2) 0.3628(7) 0.089 Uiso 1 calc R . C35 C 0.2996(4) 0.6763(3) 0.3868(7) 0.075(2) Uani 1 d . . H35A H 0.3033(4) 0.6998(3) 0.4550(7) 0.090 Uiso 1 calc R . C36 C 0.3572(4) 0.6822(2) 0.2782(7) 0.067(2) Uani 1 d . . H36A H 0.3974(4) 0.7087(2) 0.2814(7) 0.080 Uiso 1 calc R . C37 C 0.3606(4) 0.6500(2) 0.1563(7) 0.071(2) Uani 1 d . . H37A H 0.3982(4) 0.6218(2) 0.1807(7) 0.085 Uiso 1 calc R . H37B H 0.3915(4) 0.6670(2) 0.0842(7) 0.085 Uiso 1 calc R . C38 C 0.2647(4) 0.6332(2) 0.1010(7) 0.069(2) Uani 1 d . . H38A H 0.2691(4) 0.6245(2) 0.0052(7) 0.083 Uiso 1 calc R . H38B H 0.2475(4) 0.6043(2) 0.1501(7) 0.083 Uiso 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 0.0326(2) 0.0255(2) 0.0377(2) 0.0008(2) 0.00074(15) 0.0002(2) Cl1 0.0529(8) 0.0338(8) 0.0710(10) -0.0022(7) 0.0078(7) 0.0099(6) Cl2 0.0525(8) 0.0335(8) 0.0669(10) 0.0045(7) 0.0104(7) -0.0078(6) P1 0.0316(7) 0.0310(7) 0.0345(7) 0.0017(6) 0.0022(5) 0.0001(5) C1 0.035(3) 0.035(3) 0.049(3) 0.003(3) -0.004(2) 0.001(2) C2 0.047(3) 0.053(4) 0.045(3) -0.001(3) -0.003(3) -0.001(3) C3 0.061(4) 0.055(4) 0.051(4) 0.005(3) -0.022(3) -0.004(3) C4 0.038(3) 0.090(6) 0.089(5) 0.023(4) -0.018(3) 0.000(3) C5 0.032(4) 0.200(10) 0.114(7) 0.073(7) 0.009(4) 0.023(5) C6 0.035(3) 0.142(7) 0.073(5) 0.042(5) 0.011(3) 0.007(4) C7 0.041(3) 0.041(3) 0.036(3) 0.001(3) 0.003(2) 0.002(2) C8 0.067(4) 0.046(4) 0.040(3) 0.001(3) 0.003(3) 0.009(3) C9 0.098(5) 0.054(4) 0.045(4) 0.016(3) 0.010(3) 0.001(3) C10 0.115(6) 0.079(6) 0.036(4) 0.003(4) 0.016(4) 0.001(4) C11 0.158(8) 0.075(6) 0.046(4) -0.004(4) 0.024(5) 0.023(5) C12 0.119(6) 0.042(4) 0.052(4) 0.003(3) 0.022(4) 0.011(4) N1 0.034(2) 0.029(2) 0.048(3) -0.003(2) 0.004(2) -0.002(2) C26 0.044(3) 0.034(3) 0.067(4) 0.004(3) 0.000(3) -0.011(2) C28 0.099(5) 0.061(5) 0.074(5) -0.004(4) -0.025(4) -0.031(4) C13 0.046(3) 0.033(3) 0.042(3) 0.000(3) 0.004(2) -0.004(2) O13 0.064(3) 0.024(2) 0.107(4) 0.005(2) 0.003(2) -0.001(2) N2 0.036(2) 0.030(2) 0.041(2) 0.004(2) 0.004(2) 0.006(2) C27 0.044(3) 0.034(3) 0.054(4) 0.000(3) 0.002(2) 0.012(2) C29 0.080(5) 0.060(4) 0.071(5) 0.001(4) -0.019(4) 0.026(3) P2 0.0323(7) 0.0293(7) 0.0328(7) 0.0005(6) 0.0026(5) -0.0004(5) C14 0.034(3) 0.039(3) 0.040(3) -0.004(3) 0.004(2) -0.002(2) C15 0.061(4) 0.041(3) 0.041(3) 0.001(3) 0.001(3) -0.004(3) C16 0.082(4) 0.052(4) 0.041(4) -0.016(3) 0.006(3) -0.011(3) C17 0.088(5) 0.067(5) 0.040(4) -0.006(3) 0.009(3) -0.004(4) C18 0.105(5) 0.054(4) 0.035(3) 0.009(3) 0.011(3) -0.007(4) C19 0.082(4) 0.042(4) 0.045(4) 0.003(3) 0.011(3) -0.008(3) C20 0.032(3) 0.037(3) 0.045(3) -0.005(2) -0.001(2) 0.003(2) C21 0.053(3) 0.058(4) 0.039(3) -0.004(3) 0.000(3) -0.005(3) C22 0.060(4) 0.064(4) 0.042(3) -0.008(3) -0.016(3) 0.003(3) C23 0.047(4) 0.077(5) 0.080(5) -0.013(4) -0.021(3) -0.001(3) C24 0.036(4) 0.120(7) 0.092(6) -0.018(5) 0.008(3) -0.001(4) C25 0.035(3) 0.098(5) 0.061(4) -0.021(4) 0.007(3) -0.001(3) Pd2 0.0537(3) 0.0364(3) 0.0882(4) -0.0029(3) 0.0214(3) -0.0007(2) Cl3 0.118(2) 0.088(2) 0.196(3) 0.070(2) 0.071(2) 0.0589(13) Cl4 0.135(2) 0.092(2) 0.212(3) -0.083(2) 0.088(2) -0.0685(15) C31 0.059(4) 0.058(4) 0.064(4) 0.004(3) -0.011(3) 0.000(3) C32 0.052(4) 0.047(4) 0.084(5) 0.003(4) 0.000(3) -0.008(3) C33 0.075(5) 0.054(4) 0.087(5) -0.002(4) 0.011(4) -0.013(3) C34 0.092(5) 0.059(5) 0.072(5) 0.010(4) 0.006(4) 0.004(4) C35 0.062(4) 0.086(6) 0.075(5) -0.011(4) -0.017(4) 0.005(4) C36 0.047(4) 0.071(5) 0.080(5) -0.007(4) -0.014(3) 0.007(3) C37 0.066(4) 0.062(5) 0.084(5) -0.011(4) 0.000(4) 0.016(3) C38 0.089(5) 0.054(4) 0.064(4) -0.008(3) 0.000(4) 0.000(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 2.2135(13) . ? Pd1 P1 2.2165(13) . ? Pd1 Cl1 2.3545(13) . ? Pd1 Cl2 2.3577(13) . ? P1 N1 1.707(4) . ? P1 C7 1.813(5) . ? P1 C1 1.810(5) . ? C1 C6 1.362(7) . ? C1 C2 1.388(7) . ? C2 C3 1.378(7) . ? C3 C4 1.346(8) . ? C4 C5 1.368(9) . ? C5 C6 1.385(8) . ? C7 C12 1.375(7) . ? C7 C8 1.385(7) . ? C8 C9 1.376(7) . ? C9 C10 1.344(8) . ? C10 C11 1.357(9) . ? C11 C12 1.384(8) . ? N1 C13 1.382(6) . ? N1 C26 1.506(6) . ? C26 C28 1.511(7) . ? C13 O13 1.215(6) . ? C13 N2 1.397(6) . ? N2 C27 1.504(6) . ? N2 P2 1.712(4) . ? C27 C29 1.505(7) . ? P2 C14 1.805(5) . ? P2 C20 1.810(5) . ? C14 C15 1.385(7) . ? C14 C19 1.392(7) . ? C15 C16 1.379(7) . ? C16 C17 1.350(8) . ? C17 C18 1.371(8) . ? C18 C19 1.373(7) . ? C20 C25 1.371(7) . ? C20 C21 1.390(7) . ? C21 C22 1.379(7) . ? C22 C23 1.353(8) . ? C23 C24 1.382(9) . ? C24 C25 1.381(8) . ? Pd2 C36 2.192(6) . ? Pd2 C32 2.189(5) . ? Pd2 C31 2.209(6) . ? Pd2 C35 2.221(7) . ? Pd2 Cl4 2.282(2) . ? Pd2 Cl3 2.297(2) . ? C31 C32 1.364(8) . ? C31 C38 1.497(8) . ? C32 C33 1.486(8) . ? C33 C34 1.519(8) . ? C34 C35 1.496(9) . ? C35 C36 1.381(8) . ? C36 C37 1.490(8) . ? C37 C38 1.522(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 91.47(5) . . ? P2 Pd1 Cl1 176.50(5) . . ? P1 Pd1 Cl1 89.26(5) . . ? P2 Pd1 Cl2 89.22(5) . . ? P1 Pd1 Cl2 176.10(5) . . ? Cl1 Pd1 Cl2 90.28(5) . . ? N1 P1 C7 104.7(2) . . ? N1 P1 C1 103.7(2) . . ? C7 P1 C1 108.0(2) . . ? N1 P1 Pd1 115.93(14) . . ? C7 P1 Pd1 116.5(2) . . ? C1 P1 Pd1 107.1(2) . . ? C6 C1 C2 119.8(5) . . ? C6 C1 P1 122.2(4) . . ? C2 C1 P1 117.8(4) . . ? C3 C2 C1 120.2(5) . . ? C4 C3 C2 120.2(6) . . ? C3 C4 C5 119.5(6) . . ? C4 C5 C6 121.8(6) . . ? C1 C6 C5 118.5(6) . . ? C12 C7 C8 118.9(5) . . ? C12 C7 P1 120.6(4) . . ? C8 C7 P1 120.5(4) . . ? C9 C8 C7 120.1(5) . . ? C10 C9 C8 120.3(6) . . ? C9 C10 C11 120.7(6) . . ? C10 C11 C12 120.1(7) . . ? C11 C12 C7 119.8(6) . . ? C13 N1 C26 112.9(4) . . ? C13 N1 P1 126.2(3) . . ? C26 N1 P1 117.2(3) . . ? C28 C26 N1 112.2(4) . . ? O13 C13 N1 120.7(4) . . ? O13 C13 N2 119.1(4) . . ? N1 C13 N2 120.2(4) . . ? C13 N2 C27 113.2(4) . . ? C13 N2 P2 125.3(3) . . ? C27 N2 P2 117.2(3) . . ? N2 C27 C29 112.3(4) . . ? N2 P2 C14 104.6(2) . . ? N2 P2 C20 103.8(2) . . ? C14 P2 C20 108.8(2) . . ? N2 P2 Pd1 116.05(14) . . ? C14 P2 Pd1 116.2(2) . . ? C20 P2 Pd1 106.6(2) . . ? C15 C14 C19 118.4(5) . . ? C15 C14 P2 120.9(4) . . ? C19 C14 P2 120.8(4) . . ? C16 C15 C14 120.2(5) . . ? C17 C16 C15 121.0(6) . . ? C16 C17 C18 119.5(6) . . ? C19 C18 C17 120.8(6) . . ? C18 C19 C14 120.0(5) . . ? C25 C20 C21 119.5(5) . . ? C25 C20 P2 122.6(4) . . ? C21 C20 P2 117.7(4) . . ? C22 C21 C20 120.5(5) . . ? C23 C22 C21 120.0(5) . . ? C22 C23 C24 119.6(5) . . ? C23 C24 C25 121.2(6) . . ? C20 C25 C24 119.1(6) . . ? C36 Pd2 C32 96.8(3) . . ? C36 Pd2 C31 81.1(2) . . ? C32 Pd2 C31 36.1(2) . . ? C36 Pd2 C35 36.5(2) . . ? C32 Pd2 C35 81.1(2) . . ? C31 Pd2 C35 87.2(3) . . ? C36 Pd2 Cl4 88.8(2) . . ? C32 Pd2 Cl4 164.1(2) . . ? C31 Pd2 Cl4 159.6(2) . . ? C35 Pd2 Cl4 95.2(2) . . ? C36 Pd2 Cl3 163.0(2) . . ? C32 Pd2 Cl3 87.1(2) . . ? C31 Pd2 Cl3 92.8(2) . . ? C35 Pd2 Cl3 159.8(2) . . ? Cl4 Pd2 Cl3 91.79(12) . . ? C32 C31 C38 126.7(6) . . ? C32 C31 Pd2 71.1(4) . . ? C38 C31 Pd2 110.4(4) . . ? C31 C32 C33 125.3(6) . . ? C31 C32 Pd2 72.7(4) . . ? C33 C32 Pd2 107.7(4) . . ? C32 C33 C34 114.3(5) . . ? C35 C34 C33 114.6(5) . . ? C36 C35 C34 126.2(7) . . ? C36 C35 Pd2 70.6(4) . . ? C34 C35 Pd2 110.1(4) . . ? C35 C36 C37 125.8(7) . . ? C35 C36 Pd2 72.9(4) . . ? C37 C36 Pd2 107.3(4) . . ? C36 C37 C38 113.8(5) . . ? C31 C38 C37 114.4(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 P2 Pd1 P1 N1 17.7(2) . . . . ? Cl1 Pd1 P1 N1 -165.7(2) . . . . ? Cl2 Pd1 P1 N1 -82.4(8) . . . . ? P2 Pd1 P1 C7 -106.2(2) . . . . ? Cl1 Pd1 P1 C7 70.4(2) . . . . ? Cl2 Pd1 P1 C7 153.7(7) . . . . ? P2 Pd1 P1 C1 132.9(2) . . . . ? Cl1 Pd1 P1 C1 -50.5(2) . . . . ? Cl2 Pd1 P1 C1 32.7(8) . . . . ? N1 P1 C1 C6 -107.8(5) . . . . ? C7 P1 C1 C6 2.9(6) . . . . ? Pd1 P1 C1 C6 129.1(5) . . . . ? N1 P1 C1 C2 77.1(4) . . . . ? C7 P1 C1 C2 -172.1(4) . . . . ? Pd1 P1 C1 C2 -46.0(4) . . . . ? C6 C1 C2 C3 3.2(9) . . . . ? P1 C1 C2 C3 178.4(4) . . . . ? C1 C2 C3 C4 -2.9(9) . . . . ? C2 C3 C4 C5 1.5(11) . . . . ? C3 C4 C5 C6 -0.5(14) . . . . ? C2 C1 C6 C5 -2.1(11) . . . . ? P1 C1 C6 C5 -177.1(6) . . . . ? C4 C5 C6 C1 0.8(14) . . . . ? N1 P1 C7 C12 178.0(5) . . . . ? C1 P1 C7 C12 67.9(5) . . . . ? Pd1 P1 C7 C12 -52.5(5) . . . . ? N1 P1 C7 C8 -2.0(5) . . . . ? C1 P1 C7 C8 -112.1(4) . . . . ? Pd1 P1 C7 C8 127.5(4) . . . . ? C12 C7 C8 C9 0.0(8) . . . . ? P1 C7 C8 C9 -180.0(4) . . . . ? C7 C8 C9 C10 -0.4(9) . . . . ? C8 C9 C10 C11 -0.1(11) . . . . ? C9 C10 C11 C12 0.9(12) . . . . ? C10 C11 C12 C7 -1.3(12) . . . . ? C8 C7 C12 C11 0.8(10) . . . . ? P1 C7 C12 C11 -179.2(6) . . . . ? C7 P1 N1 C13 81.0(4) . . . . ? C1 P1 N1 C13 -165.9(4) . . . . ? Pd1 P1 N1 C13 -48.8(5) . . . . ? C7 P1 N1 C26 -75.8(4) . . . . ? C1 P1 N1 C26 37.4(4) . . . . ? Pd1 P1 N1 C26 154.4(3) . . . . ? C13 N1 C26 C28 81.5(6) . . . . ? P1 N1 C26 C28 -118.7(5) . . . . ? C26 N1 C13 O13 3.9(7) . . . . ? P1 N1 C13 O13 -153.7(4) . . . . ? C26 N1 C13 N2 -175.5(4) . . . . ? P1 N1 C13 N2 26.9(7) . . . . ? O13 C13 N2 C27 3.7(7) . . . . ? N1 C13 N2 C27 -176.8(4) . . . . ? O13 C13 N2 P2 -152.0(4) . . . . ? N1 C13 N2 P2 27.5(7) . . . . ? C13 N2 C27 C29 81.2(6) . . . . ? P2 N2 C27 C29 -120.9(4) . . . . ? C13 N2 P2 C14 79.9(4) . . . . ? C27 N2 P2 C14 -75.0(4) . . . . ? C13 N2 P2 C20 -166.1(4) . . . . ? C27 N2 P2 C20 39.1(4) . . . . ? C13 N2 P2 Pd1 -49.5(4) . . . . ? C27 N2 P2 Pd1 155.6(3) . . . . ? P1 Pd1 P2 N2 18.7(2) . . . . ? Cl1 Pd1 P2 N2 -83.3(8) . . . . ? Cl2 Pd1 P2 N2 -165.1(2) . . . . ? P1 Pd1 P2 C14 -104.9(2) . . . . ? Cl1 Pd1 P2 C14 153.1(8) . . . . ? Cl2 Pd1 P2 C14 71.3(2) . . . . ? P1 Pd1 P2 C20 133.7(2) . . . . ? Cl1 Pd1 P2 C20 31.7(9) . . . . ? Cl2 Pd1 P2 C20 -50.1(2) . . . . ? N2 P2 C14 C15 -4.2(5) . . . . ? C20 P2 C14 C15 -114.5(4) . . . . ? Pd1 P2 C14 C15 125.2(4) . . . . ? N2 P2 C14 C19 176.2(4) . . . . ? C20 P2 C14 C19 65.8(5) . . . . ? Pd1 P2 C14 C19 -54.4(5) . . . . ? C19 C14 C15 C16 0.6(8) . . . . ? P2 C14 C15 C16 -179.0(4) . . . . ? C14 C15 C16 C17 0.6(9) . . . . ? C15 C16 C17 C18 -1.8(10) . . . . ? C16 C17 C18 C19 1.8(10) . . . . ? C17 C18 C19 C14 -0.6(10) . . . . ? C15 C14 C19 C18 -0.6(8) . . . . ? P2 C14 C19 C18 179.0(5) . . . . ? N2 P2 C20 C25 -113.1(5) . . . . ? C14 P2 C20 C25 -2.1(6) . . . . ? Pd1 P2 C20 C25 123.9(5) . . . . ? N2 P2 C20 C21 71.1(5) . . . . ? C14 P2 C20 C21 -177.9(4) . . . . ? Pd1 P2 C20 C21 -51.9(4) . . . . ? C25 C20 C21 C22 1.7(9) . . . . ? P2 C20 C21 C22 177.6(4) . . . . ? C20 C21 C22 C23 -1.6(9) . . . . ? C21 C22 C23 C24 -0.1(10) . . . . ? C22 C23 C24 C25 1.7(11) . . . . ? C21 C20 C25 C24 -0.1(9) . . . . ? P2 C20 C25 C24 -175.7(5) . . . . ? C23 C24 C25 C20 -1.6(11) . . . . ? C36 Pd2 C31 C32 114.8(4) . . . . ? C32 Pd2 C31 C32 0.000(2) . . . . ? C35 Pd2 C31 C32 78.6(4) . . . . ? Cl4 Pd2 C31 C32 176.0(4) . . . . ? Cl3 Pd2 C31 C32 -81.2(4) . . . . ? C36 Pd2 C31 C38 -8.4(5) . . . . ? C32 Pd2 C31 C38 -123.2(6) . . . . ? C35 Pd2 C31 C38 -44.5(5) . . . . ? Cl4 Pd2 C31 C38 52.8(8) . . . . ? Cl3 Pd2 C31 C38 155.7(4) . . . . ? C38 C31 C32 C33 2.1(10) . . . . ? Pd2 C31 C32 C33 -99.8(6) . . . . ? C38 C31 C32 Pd2 101.9(6) . . . . ? Pd2 C31 C32 Pd2 0.000(1) . . . . ? C36 Pd2 C32 C31 -64.6(4) . . . . ? C31 Pd2 C32 C31 0.000(2) . . . . ? C35 Pd2 C32 C31 -97.6(4) . . . . ? Cl4 Pd2 C32 C31 -174.9(5) . . . . ? Cl3 Pd2 C32 C31 98.8(4) . . . . ? C36 Pd2 C32 C33 57.8(5) . . . . ? C31 Pd2 C32 C33 122.4(6) . . . . ? C35 Pd2 C32 C33 24.8(4) . . . . ? Cl4 Pd2 C32 C33 -52.5(9) . . . . ? Cl3 Pd2 C32 C33 -138.8(4) . . . . ? C31 C32 C33 C34 42.3(9) . . . . ? Pd2 C32 C33 C34 -38.8(7) . . . . ? C32 C33 C34 C35 33.9(8) . . . . ? C33 C34 C35 C36 -90.8(8) . . . . ? C33 C34 C35 Pd2 -10.6(7) . . . . ? C36 Pd2 C35 C36 0.000(2) . . . . ? C32 Pd2 C35 C36 114.6(4) . . . . ? C31 Pd2 C35 C36 78.7(4) . . . . ? Cl4 Pd2 C35 C36 -81.0(4) . . . . ? Cl3 Pd2 C35 C36 169.3(4) . . . . ? C36 Pd2 C35 C34 -122.6(7) . . . . ? C32 Pd2 C35 C34 -8.0(5) . . . . ? C31 Pd2 C35 C34 -43.8(5) . . . . ? Cl4 Pd2 C35 C34 156.4(5) . . . . ? Cl3 Pd2 C35 C34 46.7(9) . . . . ? C34 C35 C36 C37 2.0(11) . . . . ? Pd2 C35 C36 C37 -99.3(6) . . . . ? C34 C35 C36 Pd2 101.2(6) . . . . ? Pd2 C35 C36 Pd2 0.000(1) . . . . ? C32 Pd2 C36 C35 -64.8(4) . . . . ? C31 Pd2 C36 C35 -97.4(4) . . . . ? C35 Pd2 C36 C35 0.000(2) . . . . ? Cl4 Pd2 C36 C35 100.3(4) . . . . ? Cl3 Pd2 C36 C35 -167.3(5) . . . . ? C32 Pd2 C36 C37 58.3(5) . . . . ? C31 Pd2 C36 C37 25.7(5) . . . . ? C35 Pd2 C36 C37 123.1(7) . . . . ? Cl4 Pd2 C36 C37 -136.6(5) . . . . ? Cl3 Pd2 C36 C37 -44.2(9) . . . . ? C35 C36 C37 C38 41.2(9) . . . . ? Pd2 C36 C37 C38 -39.9(7) . . . . ? C32 C31 C38 C37 -92.1(8) . . . . ? Pd2 C31 C38 C37 -10.8(7) . . . . ? C36 C37 C38 C31 34.9(8) . . . . ? _refine_diff_density_max 0.893 _refine_diff_density_min -1.100 _refine_diff_density_rms 0.099 data_12 _database_code_CSD 168902 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C58 H60 N4 O4 P4 Pd2.C H2 Cl2' _chemical_formula_structural 'C59 H62 Cl2 N4 O4 P4 Pd2' _chemical_formula_analytical 'C59 H62 Cl2 N4 O4 P4 Pd2' _chemical_formula_sum 'C59 H62 Cl2 N4 O4 P4 Pd2' _chemical_formula_weight 1298.71 _chemical_melting_point ? _chemical_compound_source ? 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 10.4350(2) _cell_length_b 18.7436(3) _cell_length_c 15.69190(10) _cell_angle_alpha 90.00 _cell_angle_beta 94.3620(10) _cell_angle_gamma 90.00 _cell_volume 3060.28(8) _cell_formula_units_Z 2 _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 yellow _exptl_crystal_size_max .1 _exptl_crystal_size_mid .15 _exptl_crystal_size_min .15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.409 _exptl_crystal_density_method ? _exptl_crystal_F_000 1324 _exptl_absorpt_coefficient_mu 0.826 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.174335 _exptl_absorpt_correction_T_max 1.000000 _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 SMART _diffrn_measurement_method CCD _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6700 _diffrn_reflns_av_R_equivalents 0.0821 _diffrn_reflns_av_sigmaI/netI 0.2357 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 23.92 _reflns_number_total 4475 _reflns_number_observed 1785 _reflns_observed_criterion >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART/SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement on F^2^ for ALL reflections except for 55 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.1687P)^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 riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4420 _refine_ls_number_parameters 348 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2169 _refine_ls_R_factor_obs 0.1033 _refine_ls_wR_factor_all 0.3540 _refine_ls_wR_factor_obs 0.2379 _refine_ls_goodness_of_fit_all 0.891 _refine_ls_goodness_of_fit_obs 1.153 _refine_ls_restrained_S_all 1.048 _refine_ls_restrained_S_obs 1.153 _refine_ls_shift/esd_max -2.110 _refine_ls_shift/esd_mean 0.013 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pd1 Pd 0.01173(12) 0.93530(6) 0.38812(7) 0.0477(5) Uani 1 d . . O1 O -0.0865(8) 0.9699(5) 0.5657(5) 0.038(2) Uani 1 d . . P1 P -0.0168(4) 0.9120(2) 0.5241(2) 0.0463(12) Uani 1 d . . C1 C -0.0951(16) 0.8331(9) 0.5565(9) 0.052(5) Uani 1 d . . C2 C -0.2274(16) 0.8339(10) 0.5556(11) 0.065(5) Uani 1 d . . H2A H -0.2715(16) 0.8761(10) 0.5429(11) 0.078 Uiso 1 calc R . C3 C -0.2947(22) 0.7743(11) 0.5727(15) 0.102(8) Uani 1 d . . H3A H -0.3840(22) 0.7740(11) 0.5673(15) 0.122 Uiso 1 calc R . C4 C -0.2250(22) 0.7130(11) 0.5990(11) 0.078(6) Uani 1 d . . H4A H -0.2683(22) 0.6718(11) 0.6131(11) 0.093 Uiso 1 calc R . C5 C -0.0948(22) 0.7139(10) 0.6038(11) 0.073(6) Uani 1 d . . H5A H -0.0485(22) 0.6736(10) 0.6224(11) 0.088 Uiso 1 calc R . C6 C -0.0314(18) 0.7748(10) 0.5811(11) 0.063(5) Uani 1 d . . H6A H 0.0579(18) 0.7748(10) 0.5832(11) 0.075 Uiso 1 calc R . C7 C 0.1444(13) 0.9015(8) 0.5766(10) 0.043(4) Uani 1 d . . C8 C 0.1716(19) 0.9132(11) 0.6655(13) 0.077(6) Uani 1 d . . H8A H 0.1038(19) 0.9240(11) 0.6984(13) 0.092 Uiso 1 calc R . C9 C 0.2878(24) 0.9096(11) 0.7033(15) 0.084(6) Uani 1 d . . H9A H 0.3009(24) 0.9208(11) 0.7611(15) 0.101 Uiso 1 calc R . C10 C 0.3862(25) 0.8904(15) 0.6608(19) 0.113(9) Uani 1 d . . H10A H 0.4666(25) 0.8838(15) 0.6896(19) 0.135 Uiso 1 calc R . C11 C 0.3708(18) 0.8802(13) 0.5769(17) 0.095(7) Uani 1 d . . H11A H 0.4416(18) 0.8698(13) 0.5465(17) 0.114 Uiso 1 calc R . C12 C 0.2428(19) 0.8855(12) 0.5317(13) 0.092(7) Uani 1 d . . H12A H 0.2311(19) 0.8777(12) 0.4731(13) 0.111 Uiso 1 calc R . N21 N 0.0460(10) 0.9589(8) 0.2683(7) 0.043(4) Uani 1 d . . C21 C 0.0212(20) 0.9198(10) 0.2079(12) 0.073(7) Uani 1 d . . O21 O 0.0333(14) 0.9260(6) 0.1273(7) 0.086(4) Uani 1 d . . N22 N -0.0625(12) 0.8612(7) 0.2226(7) 0.048(3) Uani 1 d . . P2 P -0.0747(4) 0.8432(2) 0.3240(2) 0.0499(12) Uani 1 d . . C23 C -0.2462(18) 0.8303(10) 0.3317(10) 0.063(5) Uani 1 d . . C24 C -0.3122(18) 0.8904(9) 0.3535(11) 0.068(5) Uani 1 d . . H24A H -0.2696(18) 0.9331(9) 0.3660(11) 0.081 Uiso 1 calc R . C25 C -0.4460(19) 0.8851(13) 0.3562(14) 0.088(7) Uani 1 d . . H25A H -0.4925(19) 0.9250(13) 0.3708(14) 0.106 Uiso 1 calc R . C26 C -0.5078(20) 0.8243(17) 0.3382(14) 0.099(8) Uani 1 d . . H26A H -0.5962(20) 0.8213(17) 0.3419(14) 0.119 Uiso 1 calc R . C27 C -0.4424(20) 0.7680(14) 0.3151(14) 0.089(7) Uani 1 d . . H27A H -0.4862(20) 0.7259(14) 0.3009(14) 0.107 Uiso 1 calc R . C28 C -0.3129(19) 0.7701(11) 0.3118(12) 0.072(6) Uani 1 d . . H28A H -0.2695(19) 0.7295(11) 0.2956(12) 0.086 Uiso 1 calc R . C29 C 0.0045(16) 0.7623(9) 0.3401(10) 0.058(5) Uani 1 d . . C30 C -0.0324(19) 0.7081(11) 0.3888(12) 0.076(6) Uani 1 d . . H30A H -0.1092(19) 0.7123(11) 0.4148(12) 0.091 Uiso 1 calc R . C31 C 0.0384(20) 0.6471(11) 0.4017(13) 0.080(6) Uani 1 d . . H31A H 0.0084(20) 0.6101(11) 0.4342(13) 0.097 Uiso 1 calc R . C32 C 0.1519(21) 0.6413(11) 0.3669(13) 0.088(7) Uani 1 d . . H32A H 0.2023(21) 0.6008(11) 0.3765(13) 0.106 Uiso 1 calc R . C33 C 0.1920(20) 0.6950(12) 0.3177(14) 0.092(8) Uani 1 d . . H33A H 0.2701(20) 0.6910(12) 0.2931(14) 0.110 Uiso 1 calc R . C34 C 0.1227(17) 0.7519(11) 0.3045(11) 0.072(6) Uani 1 d . . H34A H 0.1525(17) 0.7875(11) 0.2698(11) 0.087 Uiso 1 calc R . C35 C 0.1447(15) 1.0127(9) 0.2558(11) 0.058(5) Uani 1 d . . H35A H 0.1360(15) 1.0268(9) 0.1961(11) 0.069 Uiso 1 calc R . H35B H 0.1251(15) 1.0543(9) 0.2891(11) 0.069 Uiso 1 calc R . C36 C 0.2729(19) 0.9955(12) 0.2761(13) 0.097(7) Uani 1 d . . H36A H 0.3260(19) 1.0357(12) 0.2647(13) 0.146 Uiso 1 calc R . H36B H 0.2962(19) 0.9556(12) 0.2420(13) 0.146 Uiso 1 calc R . H36C H 0.2852(19) 0.9832(12) 0.3355(13) 0.146 Uiso 1 calc R . C37 C -0.1112(26) 0.8152(12) 0.1568(13) 0.093(8) Uani 1 d . . H37A H -0.1328(26) 0.7696(12) 0.1813(13) 0.112 Uiso 1 calc R . H37B H -0.0452(26) 0.8069(12) 0.1176(13) 0.112 Uiso 1 calc R . C38 C -0.2290(29) 0.8455(17) 0.1080(15) 0.142(11) Uani 1 d . . H38A H -0.2590(29) 0.8127(17) 0.0639(15) 0.213 Uiso 1 calc R . H38B H -0.2077(29) 0.8901(17) 0.0826(15) 0.213 Uiso 1 calc R . H38C H -0.2951(29) 0.8529(17) 0.1463(15) 0.213 Uiso 1 calc R . C40 C -0.3368(28) 0.5335(16) 0.4697(18) 0.045(7) Uiso 0.50 d P . H40A H -0.3804(28) 0.5354(16) 0.5221(18) 0.054 Uiso 0.50 calc PR . H40B H -0.3683(28) 0.4918(16) 0.4381(18) 0.054 Uiso 0.50 calc PR . Cl1 Cl -0.3788(15) 0.6092(7) 0.4092(7) 0.116(5) Uani 0.50 d P . Cl2 Cl -0.1787(11) 0.5229(6) 0.4954(11) 0.133(6) Uani 0.50 d P . 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 0.0476(9) 0.0570(9) 0.0408(7) 0.0006(7) 0.0196(6) -0.0024(7) O1 0.034(6) 0.037(6) 0.044(5) -0.017(5) 0.004(5) -0.021(5) P1 0.038(3) 0.061(3) 0.041(2) -0.002(2) 0.013(2) -0.003(2) C1 0.058(12) 0.065(12) 0.036(8) 0.001(9) 0.020(8) 0.007(10) C2 0.043(11) 0.072(13) 0.080(12) -0.004(11) 0.012(10) -0.006(10) C3 0.093(17) 0.061(14) 0.160(22) 0.022(14) 0.072(17) -0.019(14) C4 0.103(17) 0.066(14) 0.071(12) -0.008(11) 0.052(12) -0.017(13) C5 0.100(17) 0.059(13) 0.063(11) 0.025(10) 0.021(12) 0.005(12) C6 0.055(12) 0.061(13) 0.074(12) 0.005(10) 0.016(10) 0.009(10) C7 0.024(8) 0.051(10) 0.053(10) 0.006(8) -0.008(8) 0.000(8) C8 0.044(13) 0.107(17) 0.080(14) -0.012(13) 0.004(11) 0.003(12) C9 0.072(17) 0.087(16) 0.093(16) 0.011(13) 0.000(15) 0.008(13) C10 0.073(18) 0.138(24) 0.120(22) 0.059(20) -0.044(18) -0.012(17) C11 0.031(12) 0.132(21) 0.123(20) 0.019(18) 0.003(13) 0.005(13) C12 0.064(15) 0.131(19) 0.085(14) 0.018(14) 0.027(12) 0.037(14) N21 0.009(6) 0.093(11) 0.024(6) -0.004(7) -0.015(5) 0.011(7) C21 0.092(16) 0.073(14) 0.059(12) 0.035(11) 0.045(12) 0.032(12) O21 0.123(12) 0.092(10) 0.049(7) -0.002(7) 0.044(8) -0.022(8) N22 0.042(8) 0.076(10) 0.026(6) -0.014(7) -0.007(6) -0.010(7) P2 0.048(3) 0.063(3) 0.041(2) -0.001(2) 0.015(2) -0.005(2) C23 0.078(13) 0.066(13) 0.049(10) 0.003(10) 0.028(10) -0.009(12) C24 0.074(14) 0.041(11) 0.091(14) -0.004(10) 0.021(11) 0.009(10) C25 0.044(12) 0.092(17) 0.131(19) -0.026(15) 0.023(13) 0.007(13) C26 0.042(13) 0.144(24) 0.112(18) -0.026(18) 0.009(12) -0.019(16) C27 0.045(13) 0.115(19) 0.107(17) -0.011(15) 0.005(12) -0.030(13) C28 0.065(14) 0.071(14) 0.081(13) -0.011(11) 0.017(11) -0.019(11) C29 0.063(12) 0.061(12) 0.054(10) 0.007(9) 0.023(9) 0.012(10) C30 0.074(14) 0.082(15) 0.076(13) 0.003(12) 0.033(11) 0.004(12) C31 0.087(16) 0.060(13) 0.096(15) 0.042(11) 0.016(13) 0.018(12) C32 0.095(17) 0.074(14) 0.101(15) 0.020(12) 0.039(14) 0.047(13) C33 0.081(15) 0.078(15) 0.124(18) 0.006(14) 0.059(14) 0.038(13) C34 0.054(12) 0.092(15) 0.073(12) 0.001(12) 0.021(10) 0.011(12) C35 0.043(11) 0.055(11) 0.078(12) 0.007(9) 0.023(10) -0.006(9) C36 0.058(15) 0.125(20) 0.110(16) 0.030(15) 0.015(13) 0.000(13) C37 0.134(21) 0.090(16) 0.059(12) -0.016(13) 0.032(14) -0.041(16) C38 0.158(29) 0.179(32) 0.086(17) 0.004(20) -0.006(19) -0.054(25) Cl1 0.184(14) 0.087(9) 0.074(7) 0.024(7) -0.014(8) -0.033(9) Cl2 0.073(8) 0.069(8) 0.265(18) 0.023(10) 0.061(10) -0.018(7) _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 N21 1.990(11) . ? Pd1 O1 2.051(9) 3_576 ? Pd1 P2 2.160(5) . ? Pd1 P1 2.221(4) . ? O1 P1 1.484(9) . ? O1 Pd1 2.051(9) 3_576 ? P1 C1 1.78(2) . ? P1 C7 1.827(15) . ? C1 C6 1.32(2) . ? C1 C2 1.38(2) . ? C2 C3 1.36(2) . ? C3 C4 1.40(3) . ? C4 C5 1.36(3) . ? C5 C6 1.38(2) . ? C7 C12 1.32(2) . ? C7 C8 1.42(2) . ? C8 C9 1.31(3) . ? C9 C10 1.32(3) . ? C10 C11 1.33(3) . ? C11 C12 1.47(3) . ? N21 C21 1.21(2) . ? N21 C35 1.47(2) . ? C21 O21 1.28(2) . ? C21 N22 1.43(2) . ? N22 C37 1.41(2) . ? N22 P2 1.639(12) . ? P2 C29 1.74(2) . ? P2 C23 1.82(2) . ? C23 C28 1.35(2) . ? C23 C24 1.38(2) . ? C24 C25 1.40(2) . ? C25 C26 1.33(3) . ? C26 C27 1.32(3) . ? C27 C28 1.36(3) . ? C29 C30 1.35(2) . ? C29 C34 1.41(2) . ? C30 C31 1.37(2) . ? C31 C32 1.35(2) . ? C32 C33 1.35(2) . ? C33 C34 1.30(2) . ? C35 C36 1.39(2) . ? C37 C38 1.51(3) . ? C40 Cl2 1.68(3) . ? C40 Cl1 1.74(3) . ? 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 N21 Pd1 O1 92.9(5) . 3_576 ? N21 Pd1 P2 80.6(4) . . ? O1 Pd1 P2 172.3(3) 3_576 . ? N21 Pd1 P1 176.9(4) . . ? O1 Pd1 P1 84.6(3) 3_576 . ? P2 Pd1 P1 102.1(2) . . ? P1 O1 Pd1 127.0(5) . 3_576 ? O1 P1 C1 103.3(6) . . ? O1 P1 C7 110.2(7) . . ? C1 P1 C7 102.0(8) . . ? O1 P1 Pd1 112.7(4) . . ? C1 P1 Pd1 122.3(5) . . ? C7 P1 Pd1 105.6(5) . . ? C6 C1 C2 119.4(16) . . ? C6 C1 P1 122.6(13) . . ? C2 C1 P1 118.0(14) . . ? C3 C2 C1 121.5(19) . . ? C2 C3 C4 117.9(21) . . ? C5 C4 C3 120.1(18) . . ? C4 C5 C6 119.6(19) . . ? C1 C6 C5 121.3(18) . . ? C12 C7 C8 117.0(17) . . ? C12 C7 P1 120.6(14) . . ? C8 C7 P1 122.4(12) . . ? C9 C8 C7 123.1(18) . . ? C8 C9 C10 121.0(23) . . ? C9 C10 C11 120.1(24) . . ? C10 C11 C12 120.5(20) . . ? C7 C12 C11 118.2(19) . . ? C21 N21 C35 114.9(14) . . ? C21 N21 Pd1 124.3(12) . . ? C35 N21 Pd1 117.3(10) . . ? N21 C21 O21 133.2(18) . . ? N21 C21 N22 115.7(13) . . ? O21 C21 N22 109.6(19) . . ? C37 N22 C21 122.7(14) . . ? C37 N22 P2 122.4(12) . . ? C21 N22 P2 114.0(12) . . ? N22 P2 C29 104.4(7) . . ? N22 P2 C23 103.9(7) . . ? C29 P2 C23 109.5(8) . . ? N22 P2 Pd1 103.2(5) . . ? C29 P2 Pd1 116.9(7) . . ? C23 P2 Pd1 116.9(6) . . ? C28 C23 C24 118.8(18) . . ? C28 C23 P2 126.0(14) . . ? C24 C23 P2 114.9(15) . . ? C23 C24 C25 117.9(18) . . ? C26 C25 C24 121.5(18) . . ? C27 C26 C25 119.3(20) . . ? C26 C27 C28 121.6(22) . . ? C23 C28 C27 120.8(19) . . ? C30 C29 C34 114.7(17) . . ? C30 C29 P2 126.1(13) . . ? C34 C29 P2 119.1(13) . . ? C29 C30 C31 122.8(16) . . ? C32 C31 C30 119.3(17) . . ? C31 C32 C33 119.4(18) . . ? C34 C33 C32 120.6(17) . . ? C33 C34 C29 123.2(18) . . ? C36 C35 N21 118.9(15) . . ? N22 C37 C38 112.1(20) . . ? Cl2 C40 Cl1 115.4(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 Pd1 O1 P1 C1 146.8(8) 3_576 . . . ? Pd1 O1 P1 C7 38.4(9) 3_576 . . . ? Pd1 O1 P1 Pd1 -79.2(7) 3_576 . . . ? N21 Pd1 P1 O1 87.3(71) . . . . ? O1 Pd1 P1 O1 52.0(6) 3_576 . . . ? P2 Pd1 P1 O1 -124.2(4) . . . . ? N21 Pd1 P1 C1 -148.6(71) . . . . ? O1 Pd1 P1 C1 176.0(8) 3_576 . . . ? P2 Pd1 P1 C1 -0.1(7) . . . . ? N21 Pd1 P1 C7 -33.0(72) . . . . ? O1 Pd1 P1 C7 -68.4(6) 3_576 . . . ? P2 Pd1 P1 C7 115.5(6) . . . . ? O1 P1 C1 C6 -137.5(14) . . . . ? C7 P1 C1 C6 -23.0(15) . . . . ? Pd1 P1 C1 C6 94.3(15) . . . . ? O1 P1 C1 C2 42.5(14) . . . . ? C7 P1 C1 C2 157.0(13) . . . . ? Pd1 P1 C1 C2 -85.7(12) . . . . ? C6 C1 C2 C3 -5.3(27) . . . . ? P1 C1 C2 C3 174.7(16) . . . . ? C1 C2 C3 C4 5.5(31) . . . . ? C2 C3 C4 C5 -2.2(31) . . . . ? C3 C4 C5 C6 -1.3(29) . . . . ? C2 C1 C6 C5 1.6(26) . . . . ? P1 C1 C6 C5 -178.4(13) . . . . ? C4 C5 C6 C1 1.6(28) . . . . ? O1 P1 C7 C12 -143.6(15) . . . . ? C1 P1 C7 C12 107.1(16) . . . . ? Pd1 P1 C7 C12 -21.7(16) . . . . ? O1 P1 C7 C8 33.3(16) . . . . ? C1 P1 C7 C8 -75.9(16) . . . . ? Pd1 P1 C7 C8 155.3(14) . . . . ? C12 C7 C8 C9 0.8(31) . . . . ? P1 C7 C8 C9 -176.3(17) . . . . ? C7 C8 C9 C10 -4.2(35) . . . . ? C8 C9 C10 C11 5.9(38) . . . . ? C9 C10 C11 C12 -4.3(40) . . . . ? C8 C7 C12 C11 0.7(28) . . . . ? P1 C7 C12 C11 177.8(16) . . . . ? C10 C11 C12 C7 1.0(36) . . . . ? O1 Pd1 N21 C21 179.4(14) 3_576 . . . ? P2 Pd1 N21 C21 -4.6(14) . . . . ? P1 Pd1 N21 C21 144.2(65) . . . . ? O1 Pd1 N21 C35 21.7(11) 3_576 . . . ? P2 Pd1 N21 C35 -162.3(11) . . . . ? P1 Pd1 N21 C35 -13.5(78) . . . . ? C35 N21 C21 O21 -23.5(30) . . . . ? Pd1 N21 C21 O21 178.3(17) . . . . ? C35 N21 C21 N22 172.2(14) . . . . ? Pd1 N21 C21 N22 14.1(22) . . . . ? N21 C21 N22 C37 173.3(18) . . . . ? O21 C21 N22 C37 5.4(25) . . . . ? N21 C21 N22 P2 -17.6(20) . . . . ? O21 C21 N22 P2 174.5(12) . . . . ? C37 N22 P2 C29 59.2(18) . . . . ? C21 N22 P2 C29 -110.0(12) . . . . ? C37 N22 P2 C23 -55.6(18) . . . . ? C21 N22 P2 C23 135.2(12) . . . . ? C37 N22 P2 Pd1 -178.1(15) . . . . ? C21 N22 P2 Pd1 12.7(12) . . . . ? N21 Pd1 P2 N22 -4.8(6) . . . . ? O1 Pd1 P2 N22 26.9(20) 3_576 . . . ? P1 Pd1 P2 N22 176.8(5) . . . . ? N21 Pd1 P2 C29 109.1(6) . . . . ? O1 Pd1 P2 C29 140.8(19) 3_576 . . . ? P1 Pd1 P2 C29 -69.2(6) . . . . ? N21 Pd1 P2 C23 -118.2(7) . . . . ? O1 Pd1 P2 C23 -86.4(20) 3_576 . . . ? P1 Pd1 P2 C23 63.5(6) . . . . ? N22 P2 C23 C28 81.4(17) . . . . ? C29 P2 C23 C28 -29.7(18) . . . . ? Pd1 P2 C23 C28 -165.7(14) . . . . ? N22 P2 C23 C24 -93.2(14) . . . . ? C29 P2 C23 C24 155.7(13) . . . . ? Pd1 P2 C23 C24 19.7(15) . . . . ? C28 C23 C24 C25 1.8(27) . . . . ? P2 C23 C24 C25 176.8(15) . . . . ? C23 C24 C25 C26 -0.1(32) . . . . ? C24 C25 C26 C27 -1.8(38) . . . . ? C25 C26 C27 C28 2.1(39) . . . . ? C24 C23 C28 C27 -1.6(29) . . . . ? P2 C23 C28 C27 -176.0(16) . . . . ? C26 C27 C28 C23 -0.3(35) . . . . ? N22 P2 C29 C30 -140.7(17) . . . . ? C23 P2 C29 C30 -30.0(20) . . . . ? Pd1 P2 C29 C30 106.0(18) . . . . ? N22 P2 C29 C34 43.6(16) . . . . ? C23 P2 C29 C34 154.4(15) . . . . ? Pd1 P2 C29 C34 -69.6(15) . . . . ? C34 C29 C30 C31 -1.0(30) . . . . ? P2 C29 C30 C31 -176.8(17) . . . . ? C29 C30 C31 C32 2.2(35) . . . . ? C30 C31 C32 C33 -2.0(36) . . . . ? C31 C32 C33 C34 0.5(37) . . . . ? C32 C33 C34 C29 0.8(36) . . . . ? C30 C29 C34 C33 -0.6(30) . . . . ? P2 C29 C34 C33 175.6(19) . . . . ? C21 N21 C35 C36 -88.6(21) . . . . ? Pd1 N21 C35 C36 71.2(19) . . . . ? C21 N22 C37 C38 -83.3(22) . . . . ? P2 N22 C37 C38 108.5(18) . . . . ? _refine_diff_density_max 1.707 _refine_diff_density_min -3.409 _refine_diff_density_rms 0.201 data_13 _database_code_CSD 168903 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C31 H26 Mo N2 O5 P2' _chemical_formula_structural 'C31 H26 Mo N2 O5 P2' _chemical_formula_analytical 'C31 H26 Mo N2 O5 P2' _chemical_formula_sum 'C31 H26 Mo N2 O5 P2' _chemical_formula_weight 664.42 _chemical_melting_point ? _chemical_compound_source ? 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' 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.05470(10) _cell_length_b 17.0186(2) _cell_length_c 14.662 _cell_angle_alpha 90.00 _cell_angle_beta 94.4850(10) _cell_angle_gamma 90.00 _cell_volume 2998.72(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 51 _cell_measurement_theta_min 23 _cell_measurement_theta_max 337 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max .04 _exptl_crystal_size_mid .15 _exptl_crystal_size_min .2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.472 _exptl_crystal_density_method ? _exptl_crystal_F_000 1352 _exptl_absorpt_coefficient_mu 0.586 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.853453 _exptl_absorpt_correction_T_max 1.0000 _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 SMART _diffrn_measurement_method CCD _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12800 _diffrn_reflns_av_R_equivalents 0.0232 _diffrn_reflns_av_sigmaI/netI 0.0278 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 23.25 _reflns_number_total 4303 _reflns_number_observed 3487 _reflns_observed_criterion >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART/SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement on F^2^ for ALL reflections except for 50 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0456P)^2^+0.0098P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0041(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4253 _refine_ls_number_parameters 371 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0386 _refine_ls_R_factor_obs 0.0251 _refine_ls_wR_factor_all 0.0790 _refine_ls_wR_factor_obs 0.0609 _refine_ls_goodness_of_fit_all 0.950 _refine_ls_goodness_of_fit_obs 0.978 _refine_ls_restrained_S_all 1.136 _refine_ls_restrained_S_obs 0.978 _refine_ls_shift/esd_max -0.003 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mo1 Mo 0.39254(2) 0.030220(13) 0.800381(14) 0.03737(10) Uani 1 d . . C31 C 0.3553(2) -0.0372(2) 0.9058(2) 0.0535(7) Uani 1 d . . O31 O 0.3314(2) -0.0752(2) 0.9661(2) 0.0885(8) Uani 1 d . . C32 C 0.4232(2) 0.1207(2) 0.8884(2) 0.0559(8) Uani 1 d . . O32 O 0.4438(2) 0.1703(2) 0.9396(2) 0.0945(8) Uani 1 d . . C33 C 0.3747(2) -0.0664(2) 0.7185(2) 0.0466(7) Uani 1 d . . O33 O 0.3700(2) -0.12321(13) 0.67588(15) 0.0730(6) Uani 1 d . . C34 C 0.5536(3) 0.0013(2) 0.8198(2) 0.0542(7) Uani 1 d . . O34 O 0.6458(2) -0.01545(15) 0.8312(2) 0.0835(7) Uani 1 d . . P1 P 0.40985(5) 0.12659(4) 0.67496(4) 0.0371(2) Uani 1 d . . C1 C 0.5483(2) 0.16516(15) 0.6543(2) 0.0443(6) Uani 1 d . . C2 C 0.6287(2) 0.1705(2) 0.7276(2) 0.0606(8) Uani 1 d . . H2A H 0.6124(2) 0.1542(2) 0.7856(2) 0.073 Uiso 1 calc R . C3 C 0.7330(2) 0.2002(2) 0.7138(3) 0.0760(10) Uani 1 d . . H3A H 0.7864(2) 0.2045(2) 0.7629(3) 0.091 Uiso 1 calc R . C4 C 0.7583(2) 0.2232(2) 0.6284(3) 0.0790(11) Uani 1 d . . H4A H 0.8286(2) 0.2430(2) 0.6198(3) 0.095 Uiso 1 calc R . C5 C 0.6807(3) 0.2173(2) 0.5561(3) 0.0775(10) Uani 1 d . . H5A H 0.6985(3) 0.2322(2) 0.4979(3) 0.093 Uiso 1 calc R . C6 C 0.5745(2) 0.1890(2) 0.5691(2) 0.0585(8) Uani 1 d . . H6A H 0.5211(2) 0.1862(2) 0.5199(2) 0.070 Uiso 1 calc R . C7 C 0.3503(2) 0.10871(15) 0.5574(2) 0.0378(6) Uani 1 d . . C8 C 0.2890(2) 0.1659(2) 0.5074(2) 0.0473(7) Uani 1 d . . H8A H 0.2786(2) 0.2151(2) 0.5331(2) 0.057 Uiso 1 calc R . C9 C 0.2440(2) 0.1500(2) 0.4204(2) 0.0585(8) Uani 1 d . . H9A H 0.2025(2) 0.1883(2) 0.3879(2) 0.070 Uiso 1 calc R . C10 C 0.2596(2) 0.0782(2) 0.3811(2) 0.0626(9) Uani 1 d . . H10A H 0.2279(2) 0.0677(2) 0.3225(2) 0.075 Uiso 1 calc R . C11 C 0.3219(2) 0.0217(2) 0.4283(2) 0.0585(8) Uani 1 d . . H11A H 0.3344(2) -0.0265(2) 0.4012(2) 0.070 Uiso 1 calc R . C12 C 0.3662(2) 0.0371(2) 0.5171(2) 0.0458(7) Uani 1 d . . H12A H 0.4070(2) -0.0016(2) 0.5495(2) 0.055 Uiso 1 calc R . N1 N 0.3398(2) 0.21177(12) 0.70304(14) 0.0407(5) Uani 1 d . . C26 C 0.3969(2) 0.2886(2) 0.7135(3) 0.0714(10) Uani 1 d . . H26A H 0.4756(2) 0.2811(2) 0.7112(3) 0.107 Uiso 1 calc R . H26B H 0.3824(2) 0.3114(2) 0.7712(3) 0.107 Uiso 1 calc R . H26C H 0.3699(2) 0.3229(2) 0.6648(3) 0.107 Uiso 1 calc R . C13 C 0.2257(2) 0.2153(2) 0.7053(2) 0.0375(6) Uani 1 d . . O13 O 0.17682(14) 0.27802(11) 0.70763(13) 0.0534(5) Uani 1 d . . N2 N 0.1645(2) 0.14462(12) 0.69825(13) 0.0364(5) Uani 1 d . . C27 C 0.0459(2) 0.1600(2) 0.6686(2) 0.0493(7) Uani 1 d . . H27A H 0.0059(2) 0.1112(2) 0.6643(2) 0.074 Uiso 1 calc R . H27B H 0.0409(2) 0.1853(2) 0.6099(2) 0.074 Uiso 1 calc R . H27C H 0.0142(2) 0.1934(2) 0.7124(2) 0.074 Uiso 1 calc R . P2 P 0.19303(5) 0.06273(4) 0.76605(4) 0.0355(2) Uani 1 d . . C14 C 0.0994(2) 0.0775(2) 0.8580(2) 0.0447(7) Uani 1 d . . C15 C 0.1421(3) 0.1096(2) 0.9398(2) 0.0578(8) Uani 1 d . . H15A H 0.2182(3) 0.1186(2) 0.9498(2) 0.069 Uiso 1 calc R . C16 C 0.0715(3) 0.1286(2) 1.0078(2) 0.0720(10) Uani 1 d . . H16A H 0.1007(3) 0.1504(2) 1.0627(2) 0.086 Uiso 1 calc R . C17 C -0.0399(3) 0.1152(2) 0.9937(2) 0.0728(10) Uani 1 d . . H17A H -0.0867(3) 0.1290(2) 1.0387(2) 0.087 Uiso 1 calc R . C18 C -0.0835(3) 0.0818(2) 0.9143(2) 0.0714(10) Uani 1 d . . H18A H -0.1594(3) 0.0714(2) 0.9059(2) 0.086 Uiso 1 calc R . C19 C -0.0150(2) 0.0634(2) 0.8468(2) 0.0624(8) Uani 1 d . . H19A H -0.0454(2) 0.0412(2) 0.7925(2) 0.075 Uiso 1 calc R . C20 C 0.1256(2) -0.01556(15) 0.6969(2) 0.0381(6) Uani 1 d . . C21 C 0.1260(2) -0.0154(2) 0.6024(2) 0.0424(6) Uani 1 d . . H21A H 0.1486(2) 0.0294(2) 0.5725(2) 0.051 Uiso 1 calc R . C22 C 0.0930(2) -0.0816(2) 0.5521(2) 0.0575(8) Uani 1 d . . H22A H 0.0957(2) -0.0814(2) 0.4889(2) 0.069 Uiso 1 calc R . C23 C 0.0566(3) -0.1470(2) 0.5950(2) 0.0673(9) Uani 1 d . . H23A H 0.0344(3) -0.1912(2) 0.5610(2) 0.081 Uiso 1 calc R . C24 C 0.0531(3) -0.1471(2) 0.6878(2) 0.0679(9) Uani 1 d . . H24A H 0.0268(3) -0.1912(2) 0.7168(2) 0.081 Uiso 1 calc R . C25 C 0.0882(2) -0.0825(2) 0.7392(2) 0.0581(8) Uani 1 d . . H25A H 0.0868(2) -0.0838(2) 0.8025(2) 0.070 Uiso 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 Mo1 0.03608(14) 0.0365(2) 0.03855(15) -0.00191(10) -0.00360(9) 0.00167(10) C31 0.058(2) 0.054(2) 0.047(2) 0.0050(15) -0.0037(14) 0.0045(15) O31 0.111(2) 0.090(2) 0.066(2) 0.0264(14) 0.0117(14) 0.005(2) C32 0.049(2) 0.057(2) 0.060(2) -0.008(2) -0.0056(14) 0.0039(15) O32 0.090(2) 0.087(2) 0.104(2) -0.052(2) -0.0130(14) -0.0021(15) C33 0.046(2) 0.043(2) 0.049(2) 0.0043(14) -0.0033(13) 0.0068(13) O33 0.089(2) 0.0440(14) 0.083(2) -0.0176(12) -0.0085(12) 0.0083(12) C34 0.051(2) 0.047(2) 0.062(2) -0.0103(15) -0.0085(14) 0.0046(14) O34 0.0455(13) 0.087(2) 0.115(2) -0.0222(15) -0.0170(12) 0.0185(12) P1 0.0325(3) 0.0333(4) 0.0457(4) -0.0027(3) 0.0037(3) -0.0001(3) C1 0.0347(14) 0.0311(15) 0.067(2) -0.0005(13) 0.0070(13) -0.0007(11) C2 0.042(2) 0.063(2) 0.076(2) 0.001(2) 0.0009(15) -0.0061(15) C3 0.039(2) 0.080(3) 0.107(3) 0.004(2) -0.009(2) -0.015(2) C4 0.037(2) 0.073(2) 0.127(3) 0.023(2) 0.010(2) -0.011(2) C5 0.049(2) 0.082(3) 0.103(3) 0.030(2) 0.017(2) -0.006(2) C6 0.044(2) 0.055(2) 0.077(2) 0.015(2) 0.0069(15) -0.0004(14) C7 0.0316(13) 0.040(2) 0.0426(14) 0.0029(12) 0.0105(11) 0.0008(11) C8 0.051(2) 0.046(2) 0.046(2) 0.0028(13) 0.0099(13) 0.0058(13) C9 0.059(2) 0.071(2) 0.045(2) 0.013(2) 0.0045(14) 0.016(2) C10 0.061(2) 0.087(3) 0.039(2) -0.004(2) 0.0024(14) 0.000(2) C11 0.064(2) 0.059(2) 0.054(2) -0.016(2) 0.014(2) 0.002(2) C12 0.045(2) 0.046(2) 0.047(2) -0.0026(13) 0.0067(12) 0.0032(13) N1 0.0403(12) 0.0303(12) 0.0518(13) -0.0056(10) 0.0042(10) -0.0008(9) C26 0.060(2) 0.037(2) 0.119(3) -0.021(2) 0.020(2) -0.0085(14) C13 0.0428(15) 0.036(2) 0.0336(13) -0.0049(11) 0.0035(11) 0.0013(13) O13 0.0509(11) 0.0379(12) 0.0713(13) -0.0065(10) 0.0035(9) 0.0120(9) N2 0.0325(11) 0.0381(13) 0.0383(11) 0.0002(9) 0.0011(9) 0.0049(9) C27 0.0369(14) 0.054(2) 0.056(2) -0.0010(14) -0.0051(12) 0.0033(13) P2 0.0353(3) 0.0393(4) 0.0318(3) -0.0009(3) 0.0026(3) -0.0007(3) C14 0.051(2) 0.048(2) 0.0359(15) 0.0026(13) 0.0082(12) 0.0006(13) C15 0.067(2) 0.062(2) 0.046(2) -0.0070(15) 0.0095(14) -0.002(2) C16 0.105(3) 0.068(2) 0.045(2) -0.010(2) 0.019(2) 0.002(2) C17 0.081(2) 0.082(3) 0.060(2) 0.010(2) 0.033(2) 0.015(2) C18 0.057(2) 0.095(3) 0.064(2) 0.014(2) 0.023(2) 0.007(2) C19 0.049(2) 0.092(2) 0.047(2) 0.000(2) 0.0101(14) -0.001(2) C20 0.0321(13) 0.039(2) 0.0431(15) 0.0004(12) 0.0002(11) 0.0005(11) C21 0.0398(14) 0.044(2) 0.043(2) -0.0030(12) 0.0019(11) -0.0059(12) C22 0.058(2) 0.062(2) 0.051(2) -0.012(2) -0.0048(14) -0.008(2) C23 0.065(2) 0.052(2) 0.082(3) -0.016(2) -0.012(2) -0.010(2) C24 0.072(2) 0.043(2) 0.087(3) 0.012(2) -0.005(2) -0.020(2) C25 0.065(2) 0.057(2) 0.052(2) 0.012(2) -0.0025(14) -0.011(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 Mo1 C34 2.001(3) . ? Mo1 C31 2.003(3) . ? Mo1 C32 2.024(3) . ? Mo1 C33 2.037(3) . ? Mo1 P2 2.4808(6) . ? Mo1 P1 2.4849(7) . ? C31 O31 1.150(3) . ? C32 O32 1.144(3) . ? C33 O33 1.151(3) . ? C34 O34 1.148(3) . ? P1 N1 1.743(2) . ? P1 C7 1.840(3) . ? P1 C1 1.841(2) . ? C1 C6 1.373(4) . ? C1 C2 1.394(4) . ? C2 C3 1.384(4) . ? C3 C4 1.369(5) . ? C4 C5 1.362(4) . ? C5 C6 1.396(4) . ? C7 C12 1.375(3) . ? C7 C8 1.396(3) . ? C8 C9 1.372(4) . ? C9 C10 1.371(4) . ? C10 C11 1.373(4) . ? C11 C12 1.392(4) . ? N1 C13 1.379(3) . ? N1 C26 1.480(3) . ? C13 O13 1.221(3) . ? C13 N2 1.411(3) . ? N2 C27 1.485(3) . ? N2 P2 1.731(2) . ? P2 C20 1.827(2) . ? P2 C14 1.842(2) . ? C14 C15 1.381(4) . ? C14 C19 1.397(4) . ? C15 C16 1.398(4) . ? C16 C17 1.363(5) . ? C17 C18 1.364(5) . ? C18 C19 1.374(4) . ? C20 C21 1.385(3) . ? C20 C25 1.389(4) . ? C21 C22 1.388(4) . ? C22 C23 1.368(4) . ? C23 C24 1.365(4) . ? C24 C25 1.381(4) . ? 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 C34 Mo1 C31 91.28(12) . . ? C34 Mo1 C32 88.28(11) . . ? C31 Mo1 C32 89.13(12) . . ? C34 Mo1 C33 86.67(11) . . ? C31 Mo1 C33 88.45(11) . . ? C32 Mo1 C33 174.35(11) . . ? C34 Mo1 P2 176.29(8) . . ? C31 Mo1 P2 90.70(8) . . ? C32 Mo1 P2 94.90(8) . . ? C33 Mo1 P2 90.24(7) . . ? C34 Mo1 P1 97.54(9) . . ? C31 Mo1 P1 170.25(8) . . ? C32 Mo1 P1 87.00(9) . . ? C33 Mo1 P1 96.16(8) . . ? P2 Mo1 P1 80.72(2) . . ? O31 C31 Mo1 178.4(3) . . ? O32 C32 Mo1 177.5(3) . . ? O33 C33 Mo1 175.5(2) . . ? O34 C34 Mo1 179.8(2) . . ? N1 P1 C7 101.42(10) . . ? N1 P1 C1 101.82(11) . . ? C7 P1 C1 101.35(12) . . ? N1 P1 Mo1 107.69(7) . . ? C7 P1 Mo1 122.35(8) . . ? C1 P1 Mo1 119.14(9) . . ? C6 C1 C2 119.2(2) . . ? C6 C1 P1 122.1(2) . . ? C2 C1 P1 118.8(2) . . ? C3 C2 C1 119.7(3) . . ? C4 C3 C2 120.5(3) . . ? C5 C4 C3 120.3(3) . . ? C4 C5 C6 120.0(3) . . ? C1 C6 C5 120.4(3) . . ? C12 C7 C8 118.6(2) . . ? C12 C7 P1 119.5(2) . . ? C8 C7 P1 121.9(2) . . ? C9 C8 C7 120.3(3) . . ? C10 C9 C8 120.6(3) . . ? C9 C10 C11 120.0(3) . . ? C10 C11 C12 119.7(3) . . ? C7 C12 C11 120.8(3) . . ? C13 N1 C26 114.6(2) . . ? C13 N1 P1 123.0(2) . . ? C26 N1 P1 121.9(2) . . ? O13 C13 N1 121.5(2) . . ? O13 C13 N2 119.7(2) . . ? N1 C13 N2 118.6(2) . . ? C13 N2 C27 110.9(2) . . ? C13 N2 P2 124.4(2) . . ? C27 N2 P2 117.0(2) . . ? N2 P2 C20 102.04(10) . . ? N2 P2 C14 101.83(11) . . ? C20 P2 C14 103.55(12) . . ? N2 P2 Mo1 116.23(7) . . ? C20 P2 Mo1 109.42(8) . . ? C14 P2 Mo1 121.45(9) . . ? C15 C14 C19 117.9(3) . . ? C15 C14 P2 118.8(2) . . ? C19 C14 P2 123.1(2) . . ? C14 C15 C16 120.3(3) . . ? C17 C16 C15 120.1(3) . . ? C18 C17 C16 120.6(3) . . ? C17 C18 C19 119.8(3) . . ? C18 C19 C14 121.3(3) . . ? C21 C20 C25 118.4(2) . . ? C21 C20 P2 121.1(2) . . ? C25 C20 P2 119.7(2) . . ? C22 C21 C20 120.4(3) . . ? C23 C22 C21 120.4(3) . . ? C24 C23 C22 119.7(3) . . ? C23 C24 C25 120.7(3) . . ? C24 C25 C20 120.4(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 C34 Mo1 C31 O31 172.8(1000) . . . . ? C32 Mo1 C31 O31 84.5(97) . . . . ? C33 Mo1 C31 O31 -100.6(97) . . . . ? P2 Mo1 C31 O31 -10.4(97) . . . . ? P1 Mo1 C31 O31 17.9(101) . . . . ? C34 Mo1 C32 O32 -26.1(66) . . . . ? C31 Mo1 C32 O32 65.2(66) . . . . ? C33 Mo1 C32 O32 0.5(74) . . . . ? P2 Mo1 C32 O32 155.9(66) . . . . ? P1 Mo1 C32 O32 -123.7(66) . . . . ? C34 Mo1 C33 O33 32.7(33) . . . . ? C31 Mo1 C33 O33 -58.6(33) . . . . ? C32 Mo1 C33 O33 6.1(41) . . . . ? P2 Mo1 C33 O33 -149.3(33) . . . . ? P1 Mo1 C33 O33 130.0(33) . . . . ? C31 Mo1 C34 O34 -6.3(964) . . . . ? C32 Mo1 C34 O34 82.8(1000) . . . . ? C33 Mo1 C34 O34 -94.7(964) . . . . ? P2 Mo1 C34 O34 -128.5(1000) . . . . ? P1 Mo1 C34 O34 169.5(1000) . . . . ? C34 Mo1 P1 N1 -130.52(11) . . . . ? C31 Mo1 P1 N1 24.1(5) . . . . ? C32 Mo1 P1 N1 -42.66(10) . . . . ? C33 Mo1 P1 N1 142.03(10) . . . . ? P2 Mo1 P1 N1 52.80(7) . . . . ? C34 Mo1 P1 C7 112.86(12) . . . . ? C31 Mo1 P1 C7 -92.5(5) . . . . ? C32 Mo1 P1 C7 -159.28(12) . . . . ? C33 Mo1 P1 C7 25.41(12) . . . . ? P2 Mo1 P1 C7 -63.82(9) . . . . ? C34 Mo1 P1 C1 -15.44(13) . . . . ? C31 Mo1 P1 C1 139.2(5) . . . . ? C32 Mo1 P1 C1 72.42(13) . . . . ? C33 Mo1 P1 C1 -102.89(12) . . . . ? P2 Mo1 P1 C1 167.88(10) . . . . ? N1 P1 C1 C6 -90.7(2) . . . . ? C7 P1 C1 C6 13.7(3) . . . . ? Mo1 P1 C1 C6 151.1(2) . . . . ? N1 P1 C1 C2 89.0(2) . . . . ? C7 P1 C1 C2 -166.6(2) . . . . ? Mo1 P1 C1 C2 -29.1(2) . . . . ? C6 C1 C2 C3 0.5(4) . . . . ? P1 C1 C2 C3 -179.3(2) . . . . ? C1 C2 C3 C4 -0.9(5) . . . . ? C2 C3 C4 C5 0.1(6) . . . . ? C3 C4 C5 C6 1.1(6) . . . . ? C2 C1 C6 C5 0.8(4) . . . . ? P1 C1 C6 C5 -179.5(2) . . . . ? C4 C5 C6 C1 -1.6(5) . . . . ? N1 P1 C7 C12 -165.9(2) . . . . ? C1 P1 C7 C12 89.4(2) . . . . ? Mo1 P1 C7 C12 -46.3(2) . . . . ? N1 P1 C7 C8 14.0(2) . . . . ? C1 P1 C7 C8 -90.7(2) . . . . ? Mo1 P1 C7 C8 133.6(2) . . . . ? C12 C7 C8 C9 1.2(4) . . . . ? P1 C7 C8 C9 -178.7(2) . . . . ? C7 C8 C9 C10 -0.7(4) . . . . ? C8 C9 C10 C11 -0.8(5) . . . . ? C9 C10 C11 C12 1.9(5) . . . . ? C8 C7 C12 C11 -0.1(4) . . . . ? P1 C7 C12 C11 179.8(2) . . . . ? C10 C11 C12 C7 -1.4(4) . . . . ? C7 P1 N1 C13 61.3(2) . . . . ? C1 P1 N1 C13 165.7(2) . . . . ? Mo1 P1 N1 C13 -68.3(2) . . . . ? C7 P1 N1 C26 -109.8(2) . . . . ? C1 P1 N1 C26 -5.5(2) . . . . ? Mo1 P1 N1 C26 120.6(2) . . . . ? C26 N1 C13 O13 6.1(4) . . . . ? P1 N1 C13 O13 -165.7(2) . . . . ? C26 N1 C13 N2 -178.4(2) . . . . ? P1 N1 C13 N2 9.8(3) . . . . ? O13 C13 N2 C27 16.0(3) . . . . ? N1 C13 N2 C27 -159.6(2) . . . . ? O13 C13 N2 P2 -132.3(2) . . . . ? N1 C13 N2 P2 52.1(3) . . . . ? C13 N2 P2 C20 -158.8(2) . . . . ? C27 N2 P2 C20 54.6(2) . . . . ? C13 N2 P2 C14 94.3(2) . . . . ? C27 N2 P2 C14 -52.3(2) . . . . ? C13 N2 P2 Mo1 -39.9(2) . . . . ? C27 N2 P2 Mo1 173.52(15) . . . . ? C34 Mo1 P2 N2 -75.9(14) . . . . ? C31 Mo1 P2 N2 161.86(11) . . . . ? C32 Mo1 P2 N2 72.67(12) . . . . ? C33 Mo1 P2 N2 -109.69(11) . . . . ? P1 Mo1 P2 N2 -13.48(8) . . . . ? C34 Mo1 P2 C20 38.9(14) . . . . ? C31 Mo1 P2 C20 -83.29(12) . . . . ? C32 Mo1 P2 C20 -172.48(12) . . . . ? C33 Mo1 P2 C20 5.17(11) . . . . ? P1 Mo1 P2 C20 101.37(9) . . . . ? C34 Mo1 P2 C14 159.4(14) . . . . ? C31 Mo1 P2 C14 37.16(13) . . . . ? C32 Mo1 P2 C14 -52.03(14) . . . . ? C33 Mo1 P2 C14 125.62(13) . . . . ? P1 Mo1 P2 C14 -138.18(11) . . . . ? N2 P2 C14 C15 -98.4(2) . . . . ? C20 P2 C14 C15 155.9(2) . . . . ? Mo1 P2 C14 C15 32.7(3) . . . . ? N2 P2 C14 C19 76.5(3) . . . . ? C20 P2 C14 C19 -29.1(3) . . . . ? Mo1 P2 C14 C19 -152.4(2) . . . . ? C19 C14 C15 C16 -1.3(5) . . . . ? P2 C14 C15 C16 173.8(2) . . . . ? C14 C15 C16 C17 0.3(5) . . . . ? C15 C16 C17 C18 1.3(5) . . . . ? C16 C17 C18 C19 -1.8(6) . . . . ? C17 C18 C19 C14 0.7(5) . . . . ? C15 C14 C19 C18 0.9(5) . . . . ? P2 C14 C19 C18 -174.1(3) . . . . ? N2 P2 C20 C21 37.1(2) . . . . ? C14 P2 C20 C21 142.6(2) . . . . ? Mo1 P2 C20 C21 -86.6(2) . . . . ? N2 P2 C20 C25 -153.0(2) . . . . ? C14 P2 C20 C25 -47.5(2) . . . . ? Mo1 P2 C20 C25 83.3(2) . . . . ? C25 C20 C21 C22 -1.9(4) . . . . ? P2 C20 C21 C22 168.1(2) . . . . ? C20 C21 C22 C23 1.9(4) . . . . ? C21 C22 C23 C24 -0.2(5) . . . . ? C22 C23 C24 C25 -1.4(5) . . . . ? C23 C24 C25 C20 1.3(5) . . . . ? C21 C20 C25 C24 0.3(4) . . . . ? P2 C20 C25 C24 -169.8(2) . . . . ? _refine_diff_density_max 0.227 _refine_diff_density_min -0.264 _refine_diff_density_rms 0.042 data_15 _database_code_CSD 168904 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C29 H30 Au2 Cl2 N2 O P2.C H Cl3 ' _chemical_formula_structural 'C30 H31 Au2 Cl5 N2 O P2' _chemical_formula_analytical 'C30 H31 Au2 Cl5 N2 O P2' _chemical_formula_sum 'C30 H31 Au2 Cl5 N2 O P2' _chemical_formula_weight 1068.69 _chemical_melting_point ? _chemical_compound_source ? 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' 'Au' 'Au' -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.5596(5) _cell_length_b 15.4267(5) _cell_length_c 16.1541(5) _cell_angle_alpha 90.00 _cell_angle_beta 98.36 _cell_angle_gamma 90.00 _cell_volume 3589.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 37 _cell_measurement_theta_min 23 _cell_measurement_theta_max 337 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max .1 _exptl_crystal_size_mid .1 _exptl_crystal_size_min .3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.977 _exptl_crystal_density_method ? _exptl_crystal_F_000 2024 _exptl_absorpt_coefficient_mu 8.652 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.549824 _exptl_absorpt_correction_T_max 1.000000 _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 SMART _diffrn_measurement_method CCD _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21674 _diffrn_reflns_av_R_equivalents 0.0428 _diffrn_reflns_av_sigmaI/netI 0.0647 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 28.69 _reflns_number_total 8391 _reflns_number_observed 5380 _reflns_observed_criterion >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART/SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement on F^2^ for ALL reflections except for 50 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0508P)^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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8341 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0747 _refine_ls_R_factor_obs 0.0354 _refine_ls_wR_factor_all 0.1052 _refine_ls_wR_factor_obs 0.0752 _refine_ls_goodness_of_fit_all 0.849 _refine_ls_goodness_of_fit_obs 0.905 _refine_ls_restrained_S_all 1.008 _refine_ls_restrained_S_obs 0.905 _refine_ls_shift/esd_max -0.122 _refine_ls_shift/esd_mean 0.007 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Au1 Au 0.73636(2) 0.90347(2) 0.101736(15) 0.04376(8) Uani 1 d . . Cl1 Cl 0.79076(13) 0.89256(11) -0.02563(10) 0.0556(4) Uani 1 d . . P1 P 0.67722(12) 0.93446(11) 0.21869(10) 0.0426(4) Uani 1 d . . Au2 Au 0.85655(2) 0.76540(2) 0.617084(15) 0.04293(8) Uani 1 d . . Cl2 Cl 0.95411(14) 0.67433(15) 0.70129(13) 0.0775(6) Uani 1 d . . C1 C 0.7233(6) 1.0384(4) 0.2593(4) 0.059(2) Uani 1 d . . C2 C 0.8196(7) 1.0456(6) 0.2777(5) 0.079(3) Uani 1 d . . H2A H 0.8581(7) 0.9994(6) 0.2692(5) 0.095 Uiso 1 calc R . C3 C 0.8568(9) 1.1262(9) 0.3097(6) 0.114(4) Uani 1 d . . H3A H 0.9208(9) 1.1330(9) 0.3216(6) 0.137 Uiso 1 calc R . C4 C 0.8012(17) 1.1926(9) 0.3231(8) 0.156(8) Uani 1 d . . H4A H 0.8273(17) 1.2436(9) 0.3464(8) 0.187 Uiso 1 calc R . C5 C 0.7050(14) 1.1862(7) 0.3027(9) 0.146(7) Uani 1 d . . H5A H 0.6670(14) 1.2333(7) 0.3099(9) 0.175 Uiso 1 calc R . C6 C 0.6665(8) 1.1072(5) 0.2711(6) 0.095(3) Uani 1 d . . H6A H 0.6025(8) 1.1015(5) 0.2582(6) 0.114 Uiso 1 calc R . C7 C 0.5523(5) 0.9449(4) 0.2006(4) 0.051(2) Uani 1 d . . C8 C 0.5117(6) 0.9753(8) 0.1234(5) 0.115(4) Uani 1 d . . H8A H 0.5485(6) 0.9881(8) 0.0825(5) 0.137 Uiso 1 calc R . C9 C 0.4177(8) 0.9865(11) 0.1070(7) 0.162(7) Uani 1 d . . H9A H 0.3917(8) 1.0114(11) 0.0566(7) 0.194 Uiso 1 calc R . C10 C 0.3616(6) 0.9620(7) 0.1628(6) 0.101(3) Uani 1 d . . H10A H 0.2975(6) 0.9668(7) 0.1490(6) 0.122 Uiso 1 calc R . C11 C 0.3987(6) 0.9306(6) 0.2390(6) 0.077(2) Uani 1 d . . H11A H 0.3604(6) 0.9148(6) 0.2778(6) 0.092 Uiso 1 calc R . C12 C 0.4962(5) 0.9221(5) 0.2584(5) 0.063(2) Uani 1 d . . H12A H 0.5224(5) 0.9010(5) 0.3105(5) 0.076 Uiso 1 calc R . N1 N 0.7100(3) 0.8641(3) 0.2993(3) 0.0382(11) Uani 1 d . . C26 C 0.7138(5) 0.7700(4) 0.2838(4) 0.052(2) Uani 1 d . . H26A H 0.7462(5) 0.7425(4) 0.3336(4) 0.062 Uiso 1 calc R . H26B H 0.7503(5) 0.7604(4) 0.2389(4) 0.062 Uiso 1 calc R . C28 C 0.6228(7) 0.7268(5) 0.2613(6) 0.083(3) Uani 1 d . . H28A H 0.6323(7) 0.6661(5) 0.2523(6) 0.125 Uiso 1 calc R . H28B H 0.5906(7) 0.7522(5) 0.2111(6) 0.125 Uiso 1 calc R . H28C H 0.5866(7) 0.7339(5) 0.3060(6) 0.125 Uiso 1 calc R . C13 C 0.7141(4) 0.8967(4) 0.3816(4) 0.0352(13) Uani 1 d . . O13 O 0.6604(3) 0.9518(3) 0.3987(2) 0.0427(10) Uani 1 d . . N2 N 0.7827(3) 0.8622(3) 0.4412(3) 0.0360(11) Uani 1 d . . C27 C 0.8745(4) 0.8336(4) 0.4204(4) 0.046(2) Uani 1 d . . H27A H 0.8714(4) 0.8299(4) 0.3601(4) 0.056 Uiso 1 calc R . H27B H 0.8889(4) 0.7764(4) 0.4435(4) 0.056 Uiso 1 calc R . C29 C 0.9502(5) 0.8957(6) 0.4546(6) 0.081(3) Uani 1 d . . H29A H 1.0083(5) 0.8760(6) 0.4401(6) 0.122 Uiso 1 calc R . H29B H 0.9543(5) 0.8985(6) 0.5144(6) 0.122 Uiso 1 calc R . H29C H 0.9364(5) 0.9522(6) 0.4312(6) 0.122 Uiso 1 calc R . P2 P 0.76606(10) 0.86457(10) 0.54358(9) 0.0351(3) Uani 1 d . . C14 C 0.7908(4) 0.9724(4) 0.5879(4) 0.0419(15) Uani 1 d . . C15 C 0.7764(5) 1.0478(5) 0.5423(5) 0.065(2) Uani 1 d . . H15A H 0.7511(5) 1.0456(5) 0.4861(5) 0.078 Uiso 1 calc R . C16 C 0.7997(5) 1.1278(5) 0.5804(6) 0.075(2) Uani 1 d . . H16A H 0.7930(5) 1.1786(5) 0.5491(6) 0.090 Uiso 1 calc R . C17 C 0.8328(5) 1.1307(6) 0.6651(6) 0.076(3) Uani 1 d . . H17A H 0.8445(5) 1.1841(6) 0.6913(6) 0.092 Uiso 1 calc R . C18 C 0.8484(6) 1.0575(6) 0.7101(6) 0.080(3) Uani 1 d . . H18A H 0.8744(6) 1.0604(6) 0.7661(6) 0.096 Uiso 1 calc R . C19 C 0.8257(5) 0.9772(5) 0.6730(5) 0.062(2) Uani 1 d . . H19A H 0.8339(5) 0.9269(5) 0.7050(5) 0.074 Uiso 1 calc R . C20 C 0.6414(4) 0.8460(4) 0.5390(4) 0.0361(13) Uani 1 d . . C21 C 0.6047(5) 0.7694(4) 0.5043(4) 0.053(2) Uani 1 d . . H21A H 0.6434(5) 0.7287(4) 0.4846(4) 0.064 Uiso 1 calc R . C22 C 0.5109(5) 0.7530(5) 0.4986(6) 0.074(2) Uani 1 d . . H22A H 0.4860(5) 0.7014(5) 0.4754(6) 0.089 Uiso 1 calc R . C23 C 0.4554(6) 0.8136(6) 0.5276(6) 0.084(3) Uani 1 d . . H23A H 0.3918(6) 0.8035(6) 0.5225(6) 0.101 Uiso 1 calc R . C24 C 0.4906(5) 0.8889(5) 0.5639(6) 0.072(2) Uani 1 d . . H24A H 0.4518(5) 0.9285(5) 0.5849(6) 0.086 Uiso 1 calc R . C25 C 0.5840(5) 0.9053(4) 0.5690(5) 0.053(2) Uani 1 d . . H25A H 0.6084(5) 0.9567(4) 0.5929(5) 0.064 Uiso 1 calc R . C30 C 1.1021(18) 0.6008(13) 0.4558(16) 0.351(20) Uani 1 d . . H30A H 1.1031(18) 0.5374(13) 0.4527(16) 0.421 Uiso 1 calc R . Cl3 Cl 1.2107(4) 0.6322(3) 0.4468(4) 0.211(2) Uani 1 d . . Cl4 Cl 1.0619(4) 0.6216(4) 0.5362(3) 0.218(2) Uani 1 d . . Cl5 Cl 1.0178(3) 0.6358(4) 0.3639(3) 0.204(2) Uani 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 Au1 0.0488(2) 0.0477(2) 0.03443(13) 0.00053(11) 0.00463(11) 0.00122(12) Cl1 0.0680(12) 0.0593(11) 0.0417(9) 0.0029(8) 0.0158(8) 0.0031(9) P1 0.0498(10) 0.0435(9) 0.0343(8) 0.0015(7) 0.0050(7) 0.0024(8) Au2 0.03239(14) 0.0524(2) 0.04099(14) 0.00397(11) -0.00480(10) 0.00467(11) Cl2 0.0550(12) 0.096(2) 0.0749(13) 0.0275(11) -0.0130(10) 0.0220(11) C1 0.101(7) 0.039(4) 0.042(4) -0.002(3) 0.023(4) -0.005(4) C2 0.097(7) 0.078(6) 0.060(5) -0.001(4) 0.002(5) -0.031(5) C3 0.141(11) 0.124(10) 0.073(7) 0.000(7) 0.006(7) -0.085(9) C4 0.335(27) 0.069(8) 0.076(8) -0.007(7) 0.070(13) -0.067(14) C5 0.269(20) 0.048(7) 0.144(13) -0.012(7) 0.112(14) -0.021(10) C6 0.148(10) 0.046(5) 0.103(7) 0.010(5) 0.059(7) 0.000(5) C7 0.054(4) 0.061(4) 0.039(4) 0.001(3) 0.009(3) 0.015(3) C8 0.065(6) 0.221(12) 0.057(5) 0.047(7) 0.005(4) 0.067(7) C9 0.081(8) 0.330(20) 0.073(7) 0.066(10) 0.009(6) 0.101(10) C10 0.056(6) 0.165(10) 0.078(7) 0.004(7) -0.006(5) 0.036(6) C11 0.057(5) 0.097(7) 0.076(6) -0.002(5) 0.013(4) -0.007(5) C12 0.051(5) 0.078(5) 0.055(5) 0.006(4) -0.010(4) -0.007(4) N1 0.044(3) 0.038(3) 0.033(3) -0.002(2) 0.006(2) 0.003(2) C26 0.078(5) 0.039(4) 0.041(4) -0.001(3) 0.017(3) 0.002(3) C28 0.108(8) 0.050(5) 0.087(6) -0.012(4) -0.004(5) -0.018(5) C13 0.035(3) 0.035(3) 0.035(3) 0.000(3) 0.006(3) -0.004(3) O13 0.045(3) 0.044(2) 0.038(2) 0.000(2) 0.002(2) 0.012(2) N2 0.034(3) 0.043(3) 0.031(3) -0.002(2) 0.004(2) 0.007(2) C27 0.031(3) 0.060(4) 0.049(4) -0.002(3) 0.009(3) 0.004(3) C29 0.033(4) 0.122(8) 0.092(7) -0.012(5) 0.017(4) -0.014(4) P2 0.0310(8) 0.0395(8) 0.0333(8) -0.0029(7) -0.0010(6) 0.0030(7) C14 0.039(4) 0.039(4) 0.046(4) -0.017(3) 0.000(3) 0.004(3) C15 0.059(5) 0.053(5) 0.074(5) -0.013(4) -0.018(4) 0.003(4) C16 0.062(5) 0.045(4) 0.114(8) -0.016(5) -0.005(5) -0.005(4) C17 0.051(5) 0.066(6) 0.111(8) -0.050(5) 0.009(5) -0.011(4) C18 0.069(6) 0.096(7) 0.072(6) -0.052(5) 0.004(4) -0.022(5) C19 0.065(5) 0.062(5) 0.056(4) -0.013(4) 0.002(4) -0.013(4) C20 0.027(3) 0.041(3) 0.038(3) 0.003(3) 0.001(2) 0.008(3) C21 0.042(4) 0.055(4) 0.061(4) -0.003(3) 0.003(3) -0.001(3) C22 0.040(4) 0.065(5) 0.115(7) -0.015(5) 0.003(4) -0.008(4) C23 0.038(5) 0.082(6) 0.131(8) 0.002(6) 0.013(5) -0.004(5) C24 0.048(5) 0.078(6) 0.095(6) 0.009(5) 0.027(4) 0.020(4) C25 0.044(4) 0.050(4) 0.068(5) 0.002(3) 0.014(3) 0.011(3) C30 0.411(31) 0.301(22) 0.440(32) 0.299(23) 0.394(30) 0.279(23) Cl3 0.250(6) 0.100(3) 0.290(7) 0.008(3) 0.057(5) 0.005(3) Cl4 0.249(6) 0.238(5) 0.165(4) -0.035(4) 0.021(4) 0.046(4) Cl5 0.190(4) 0.290(6) 0.139(3) 0.018(4) 0.051(3) 0.097(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 Au1 P1 2.239(2) . ? Au1 Cl1 2.316(2) . ? Au1 Au2 3.1279(4) 4_575 ? P1 N1 1.709(5) . ? P1 C7 1.807(7) . ? P1 C1 1.823(7) . ? Au2 P2 2.243(2) . ? Au2 Cl2 2.298(2) . ? Au2 Au1 3.1280(4) 4_576 ? C1 C6 1.376(11) . ? C1 C2 1.394(11) . ? C2 C3 1.423(13) . ? C3 C4 1.34(2) . ? C4 C5 1.40(2) . ? C5 C6 1.40(2) . ? C7 C8 1.381(10) . ? C7 C12 1.374(10) . ? C8 C9 1.368(12) . ? C9 C10 1.355(14) . ? C10 C11 1.359(12) . ? C11 C12 1.415(11) . ? N1 C13 1.415(7) . ? N1 C26 1.475(7) . ? C26 C28 1.480(10) . ? C13 O13 1.213(6) . ? C13 N2 1.389(7) . ? N2 C27 1.492(7) . ? N2 P2 1.706(5) . ? C27 C29 1.504(9) . ? P2 C14 1.827(6) . ? P2 C20 1.828(6) . ? C14 C15 1.376(9) . ? C14 C19 1.397(9) . ? C15 C16 1.397(10) . ? C16 C17 1.384(12) . ? C17 C18 1.345(12) . ? C18 C19 1.394(10) . ? C20 C25 1.374(8) . ? C20 C21 1.383(8) . ? C21 C22 1.378(9) . ? C22 C23 1.364(11) . ? C23 C24 1.366(11) . ? C24 C25 1.373(10) . ? C30 Cl4 1.53(2) . ? C30 Cl3 1.68(2) . ? C30 Cl5 1.86(3) . ? 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 Au1 Cl1 171.29(6) . . ? P1 Au1 Au2 112.97(4) . 4_575 ? Cl1 Au1 Au2 75.53(4) . 4_575 ? N1 P1 C7 110.1(3) . . ? N1 P1 C1 103.7(3) . . ? C7 P1 C1 106.8(4) . . ? N1 P1 Au1 114.1(2) . . ? C7 P1 Au1 112.6(2) . . ? C1 P1 Au1 108.9(2) . . ? P2 Au2 Cl2 174.48(7) . . ? P2 Au2 Au1 104.32(4) . 4_576 ? Cl2 Au2 Au1 80.11(6) . 4_576 ? C6 C1 C2 121.0(8) . . ? C6 C1 P1 122.1(8) . . ? C2 C1 P1 116.9(6) . . ? C1 C2 C3 117.7(10) . . ? C4 C3 C2 121.2(13) . . ? C5 C4 C3 121.1(14) . . ? C4 C5 C6 118.7(14) . . ? C1 C6 C5 120.2(12) . . ? C8 C7 C12 118.9(7) . . ? C8 C7 P1 117.7(6) . . ? C12 C7 P1 123.4(5) . . ? C7 C8 C9 120.1(9) . . ? C10 C9 C8 121.3(9) . . ? C9 C10 C11 120.2(8) . . ? C10 C11 C12 119.2(8) . . ? C7 C12 C11 120.1(7) . . ? C13 N1 C26 120.8(5) . . ? C13 N1 P1 117.3(4) . . ? C26 N1 P1 120.6(4) . . ? N1 C26 C28 115.5(6) . . ? O13 C13 N2 122.2(5) . . ? O13 C13 N1 121.5(5) . . ? N2 C13 N1 116.3(5) . . ? C13 N2 C27 122.3(5) . . ? C13 N2 P2 118.3(4) . . ? C27 N2 P2 118.9(4) . . ? N2 C27 C29 111.2(5) . . ? N2 P2 C14 110.6(3) . . ? N2 P2 C20 103.7(3) . . ? C14 P2 C20 107.3(3) . . ? N2 P2 Au2 110.1(2) . . ? C14 P2 Au2 110.3(2) . . ? C20 P2 Au2 114.7(2) . . ? C15 C14 C19 119.1(6) . . ? C15 C14 P2 123.7(5) . . ? C19 C14 P2 117.2(5) . . ? C14 C15 C16 120.2(7) . . ? C17 C16 C15 119.4(8) . . ? C16 C17 C18 120.9(7) . . ? C17 C18 C19 120.3(8) . . ? C14 C19 C18 119.9(8) . . ? C25 C20 C21 119.5(6) . . ? C25 C20 P2 122.3(5) . . ? C21 C20 P2 118.3(5) . . ? C20 C21 C22 120.4(7) . . ? C23 C22 C21 118.8(8) . . ? C24 C23 C22 121.7(7) . . ? C23 C24 C25 119.2(7) . . ? C24 C25 C20 120.3(7) . . ? Cl4 C30 Cl3 119.5(22) . . ? Cl4 C30 Cl5 109.0(10) . . ? Cl3 C30 Cl5 111.5(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 Cl1 Au1 P1 N1 -164.9(4) . . . . ? Au2 Au1 P1 N1 2.3(2) 4_575 . . . ? Cl1 Au1 P1 C7 68.8(5) . . . . ? Au2 Au1 P1 C7 -124.0(3) 4_575 . . . ? Cl1 Au1 P1 C1 -49.5(5) . . . . ? Au2 Au1 P1 C1 117.7(3) 4_575 . . . ? N1 P1 C1 C6 -116.3(6) . . . . ? C7 P1 C1 C6 0.0(7) . . . . ? Au1 P1 C1 C6 121.8(6) . . . . ? N1 P1 C1 C2 64.0(6) . . . . ? C7 P1 C1 C2 -179.7(5) . . . . ? Au1 P1 C1 C2 -57.9(6) . . . . ? C6 C1 C2 C3 0.6(11) . . . . ? P1 C1 C2 C3 -179.8(6) . . . . ? C1 C2 C3 C4 1.1(14) . . . . ? C2 C3 C4 C5 -2.8(19) . . . . ? C3 C4 C5 C6 2.8(21) . . . . ? C2 C1 C6 C5 -0.5(13) . . . . ? P1 C1 C6 C5 179.9(8) . . . . ? C4 C5 C6 C1 -1.2(17) . . . . ? N1 P1 C7 C8 -159.4(7) . . . . ? C1 P1 C7 C8 88.6(8) . . . . ? Au1 P1 C7 C8 -30.9(8) . . . . ? N1 P1 C7 C12 18.7(7) . . . . ? C1 P1 C7 C12 -93.3(7) . . . . ? Au1 P1 C7 C12 147.2(6) . . . . ? C12 C7 C8 C9 3.4(17) . . . . ? P1 C7 C8 C9 -178.4(11) . . . . ? C7 C8 C9 C10 -5.3(23) . . . . ? C8 C9 C10 C11 4.1(22) . . . . ? C9 C10 C11 C12 -1.3(17) . . . . ? C8 C7 C12 C11 -0.6(13) . . . . ? P1 C7 C12 C11 -178.7(6) . . . . ? C10 C11 C12 C7 -0.5(13) . . . . ? C7 P1 N1 C13 -80.9(5) . . . . ? C1 P1 N1 C13 33.1(5) . . . . ? Au1 P1 N1 C13 151.5(4) . . . . ? C7 P1 N1 C26 86.3(5) . . . . ? C1 P1 N1 C26 -159.7(5) . . . . ? Au1 P1 N1 C26 -41.3(5) . . . . ? C13 N1 C26 C28 96.3(7) . . . . ? P1 N1 C26 C28 -70.5(7) . . . . ? C26 N1 C13 O13 -133.2(6) . . . . ? P1 N1 C13 O13 34.0(7) . . . . ? C26 N1 C13 N2 46.6(8) . . . . ? P1 N1 C13 N2 -146.2(4) . . . . ? O13 C13 N2 C27 -147.3(6) . . . . ? N1 C13 N2 C27 32.9(8) . . . . ? O13 C13 N2 P2 24.8(7) . . . . ? N1 C13 N2 P2 -155.1(4) . . . . ? C13 N2 C27 C29 107.1(7) . . . . ? P2 N2 C27 C29 -64.9(7) . . . . ? C13 N2 P2 C14 -78.5(5) . . . . ? C27 N2 P2 C14 93.8(5) . . . . ? C13 N2 P2 C20 36.2(5) . . . . ? C27 N2 P2 C20 -151.5(4) . . . . ? C13 N2 P2 Au2 159.4(4) . . . . ? C27 N2 P2 Au2 -28.3(5) . . . . ? Cl2 Au2 P2 N2 128.6(7) . . . . ? Au1 Au2 P2 N2 -88.5(2) 4_576 . . . ? Cl2 Au2 P2 C14 6.3(8) . . . . ? Au1 Au2 P2 C14 149.2(2) 4_576 . . . ? Cl2 Au2 P2 C20 -114.9(7) . . . . ? Au1 Au2 P2 C20 28.0(2) 4_576 . . . ? N2 P2 C14 C15 31.7(7) . . . . ? C20 P2 C14 C15 -80.8(6) . . . . ? Au2 P2 C14 C15 153.6(5) . . . . ? N2 P2 C14 C19 -148.7(5) . . . . ? C20 P2 C14 C19 98.8(5) . . . . ? Au2 P2 C14 C19 -26.8(6) . . . . ? C19 C14 C15 C16 2.3(11) . . . . ? P2 C14 C15 C16 -178.1(6) . . . . ? C14 C15 C16 C17 -3.3(12) . . . . ? C15 C16 C17 C18 4.2(12) . . . . ? C16 C17 C18 C19 -4.1(13) . . . . ? C15 C14 C19 C18 -2.1(11) . . . . ? P2 C14 C19 C18 178.3(6) . . . . ? C17 C18 C19 C14 3.0(12) . . . . ? N2 P2 C20 C25 -119.9(5) . . . . ? C14 P2 C20 C25 -2.8(6) . . . . ? Au2 P2 C20 C25 120.0(5) . . . . ? N2 P2 C20 C21 60.4(5) . . . . ? C14 P2 C20 C21 177.4(5) . . . . ? Au2 P2 C20 C21 -59.7(5) . . . . ? C25 C20 C21 C22 1.0(10) . . . . ? P2 C20 C21 C22 -179.3(6) . . . . ? C20 C21 C22 C23 0.1(13) . . . . ? C21 C22 C23 C24 -1.7(15) . . . . ? C22 C23 C24 C25 2.1(14) . . . . ? C23 C24 C25 C20 -0.9(12) . . . . ? C21 C20 C25 C24 -0.6(10) . . . . ? P2 C20 C25 C24 179.7(6) . . . . ? _refine_diff_density_max 1.245 _refine_diff_density_min -1.011 _refine_diff_density_rms 0.132