# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Pak-Hing Leung' _publ_contact_author_email PAKHING@NTU.EDU.SG _publ_section_title ; Controllable synthesis of P-chiral 1,2- and 1,3-diphosphines via asymmetric Diels-Alder reactions involving functionalized allylic phosphines as dienophiles ; loop_ _publ_author_name 'Pak-Hing Leung' 'Deepa Krishnan' 'Yongxin Li' 'Sumod A Pullarkat' 'Crystal Huixian Yeong' 'Mingjun Yuan' # Attachment 'complex_41.cif' data_leung328 _database_code_depnum_ccdc_archive 'CCDC 711830' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_absolute_configuration ad _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C29 H30 Cl2 O2 P2 Pd, C4 H10 O' _chemical_formula_sum 'C33 H40 Cl2 O3 P2 Pd' _chemical_formula_weight 723.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 9.9121(3) _cell_length_b 15.1031(4) _cell_length_c 22.4411(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3359.51(16) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8435 _cell_measurement_theta_min 2.62 _cell_measurement_theta_max 30.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.431 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1488 _exptl_absorpt_coefficient_mu 0.838 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7871 _exptl_absorpt_correction_T_max 0.9360 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 75867 _diffrn_reflns_av_R_equivalents 0.0396 _diffrn_reflns_av_sigmaI/netI 0.0257 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 30.58 _reflns_number_total 10294 _reflns_number_gt 9593 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0358P)^2^+7.7000P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.02(3) _refine_ls_number_reflns 10294 _refine_ls_number_parameters 430 _refine_ls_number_restraints 331 _refine_ls_R_factor_all 0.0482 _refine_ls_R_factor_gt 0.0415 _refine_ls_wR_factor_ref 0.1068 _refine_ls_wR_factor_gt 0.1003 _refine_ls_goodness_of_fit_ref 1.147 _refine_ls_restrained_S_all 1.157 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd -0.06100(2) 0.220454(16) 0.197394(11) 0.01822(6) Uani 1 1 d . A . C1 C -0.1059(4) 0.0979(3) 0.07156(16) 0.0238(7) Uani 1 1 d . A . C2 C -0.0952(5) 0.1359(3) 0.01496(18) 0.0331(9) Uani 1 1 d . . . H2 H -0.0229 0.1751 0.0063 0.040 Uiso 1 1 calc R . . C3 C -0.1896(6) 0.1166(3) -0.0283(2) 0.0402(10) Uani 1 1 d . . . H3 H -0.1807 0.1413 -0.0670 0.048 Uiso 1 1 calc R . . C4 C -0.2982(6) 0.0609(4) -0.0156(2) 0.0451(12) Uani 1 1 d . . . H4 H -0.3634 0.0479 -0.0453 0.054 Uiso 1 1 calc R . . C5 C -0.3100(5) 0.0249(4) 0.0408(2) 0.0440(12) Uani 1 1 d . . . H5 H -0.3841 -0.0127 0.0499 0.053 Uiso 1 1 calc R . . C6 C -0.2145(5) 0.0431(3) 0.0843(2) 0.0332(9) Uani 1 1 d . . . H6 H -0.2234 0.0179 0.1229 0.040 Uiso 1 1 calc R . . C7 C 0.1803(4) 0.1501(2) 0.10219(16) 0.0214(6) Uani 1 1 d . A . H7 H 0.1888 0.2075 0.0803 0.026 Uiso 1 1 calc R . . C8 C 0.2146(4) 0.0679(3) 0.06685(17) 0.0270(8) Uani 1 1 d . . . C9 C 0.3012(6) 0.0743(4) 0.0121(2) 0.0433(12) Uani 1 1 d . . . H9A H 0.3827 0.1085 0.0212 0.065 Uiso 1 1 calc R . . H9B H 0.2507 0.1039 -0.0198 0.065 Uiso 1 1 calc R . . H9C H 0.3268 0.0147 -0.0010 0.065 Uiso 1 1 calc R . . C10 C 0.1661(4) -0.0046(3) 0.09363(17) 0.0270(7) Uani 1 1 d . . . C11 C 0.1792(7) -0.0990(3) 0.0759(2) 0.0454(12) Uani 1 1 d . . . H11A H 0.2377 -0.1034 0.0408 0.068 Uiso 1 1 calc R . . H11B H 0.0899 -0.1229 0.0663 0.068 Uiso 1 1 calc R . . H11C H 0.2187 -0.1328 0.1088 0.068 Uiso 1 1 calc R . . C12 C 0.0956(4) 0.0195(2) 0.15193(16) 0.0209(6) Uani 1 1 d . A . H12 H 0.0360 -0.0272 0.1694 0.025 Uiso 1 1 calc R . . C13 C 0.2070(3) 0.0571(2) 0.19402(18) 0.0221(6) Uani 1 1 d . . . H13 H 0.2839 0.0142 0.1944 0.027 Uiso 1 1 calc R . . C14 C 0.2569(4) 0.1445(3) 0.16313(16) 0.0226(7) Uani 1 1 d . . . H14 H 0.2299 0.1962 0.1883 0.027 Uiso 1 1 calc R . . C15 C 0.4079(4) 0.1483(3) 0.15260(18) 0.0278(8) Uani 1 1 d . . . C16 C 0.5840(4) 0.2454(4) 0.1226(3) 0.0451(12) Uani 1 1 d . . . H16A H 0.6375 0.2266 0.1571 0.068 Uiso 1 1 calc R . . H16B H 0.5978 0.3088 0.1156 0.068 Uiso 1 1 calc R . . H16C H 0.6126 0.2121 0.0873 0.068 Uiso 1 1 calc R . . C17 C 0.1601(4) 0.0707(3) 0.25898(16) 0.0244(7) Uani 1 1 d . A . H17A H 0.2298 0.1057 0.2800 0.029 Uiso 1 1 calc R . . H17B H 0.1560 0.0120 0.2785 0.029 Uiso 1 1 calc R . . C18 C -0.1301(4) 0.0404(3) 0.27763(16) 0.0246(7) Uani 1 1 d . A . C19 C -0.2596(5) 0.0564(3) 0.2557(2) 0.0407(11) Uani 1 1 d . . . H19 H -0.2793 0.1103 0.2357 0.049 Uiso 1 1 calc R . . C20 C -0.3603(5) -0.0076(4) 0.2635(3) 0.0568(17) Uani 1 1 d . . . H20 H -0.4482 0.0022 0.2479 0.068 Uiso 1 1 calc R . . C21 C -0.3320(5) -0.0851(3) 0.2938(2) 0.0442(12) Uani 1 1 d . . . H21 H -0.4013 -0.1276 0.2998 0.053 Uiso 1 1 calc R . . C22 C -0.2058(5) -0.1011(3) 0.3152(2) 0.0363(10) Uani 1 1 d . . . H22 H -0.1874 -0.1550 0.3354 0.044 Uiso 1 1 calc R . . C23 C -0.1036(4) -0.0389(3) 0.30745(19) 0.0296(8) Uani 1 1 d . . . H23 H -0.0157 -0.0504 0.3225 0.036 Uiso 1 1 calc R . . C24 C 0.017(3) 0.1620(14) 0.3465(6) 0.025(3) Uani 0.38(2) 1 d PDU A 1 C25 C 0.123(2) 0.2184(14) 0.3590(9) 0.041(4) Uani 0.38(2) 1 d PDU A 1 H25 H 0.1772 0.2413 0.3276 0.049 Uiso 0.38(2) 1 calc PR A 1 C26 C 0.1507(19) 0.2410(16) 0.4170(7) 0.053(4) Uani 0.38(2) 1 d PDU A 1 H26 H 0.2333 0.2693 0.4269 0.063 Uiso 0.38(2) 1 calc PR A 1 C27 C 0.056(2) 0.2219(18) 0.4612(7) 0.052(4) Uani 0.38(2) 1 d PDU A 1 H27 H 0.0695 0.2432 0.5006 0.063 Uiso 0.38(2) 1 calc PR A 1 C28 C -0.058(3) 0.1718(15) 0.4478(9) 0.047(4) Uani 0.38(2) 1 d PDU A 1 H28 H -0.1235 0.1607 0.4776 0.056 Uiso 0.38(2) 1 calc PR A 1 C29 C -0.074(2) 0.138(2) 0.3908(8) 0.036(4) Uani 0.38(2) 1 d PDU A 1 H29 H -0.1470 0.0994 0.3822 0.043 Uiso 0.38(2) 1 calc PR A 1 C24A C 0.0224(16) 0.1789(10) 0.3430(4) 0.029(3) Uani 0.62(2) 1 d PDU A 2 C25A C 0.1159(14) 0.2447(8) 0.3491(5) 0.033(2) Uani 0.62(2) 1 d PDU A 2 H25A H 0.1585 0.2685 0.3147 0.040 Uiso 0.62(2) 1 calc PR A 2 C26A C 0.1488(11) 0.2768(10) 0.4048(5) 0.047(2) Uani 0.62(2) 1 d PDU A 2 H26A H 0.2104 0.3248 0.4081 0.057 Uiso 0.62(2) 1 calc PR A 2 C27A C 0.0950(18) 0.2412(10) 0.4551(5) 0.055(3) Uani 0.62(2) 1 d PDU A 2 H27A H 0.1231 0.2617 0.4932 0.066 Uiso 0.62(2) 1 calc PR A 2 C28A C -0.0011(18) 0.1750(10) 0.4505(6) 0.052(3) Uani 0.62(2) 1 d PDU A 2 H28A H -0.0412 0.1504 0.4852 0.062 Uiso 0.62(2) 1 calc PR A 2 C29A C -0.0378(19) 0.1451(14) 0.3941(6) 0.045(3) Uani 0.62(2) 1 d PDU A 2 H29A H -0.1054 0.1008 0.3904 0.054 Uiso 0.62(2) 1 calc PR A 2 C30 C -0.0044(10) 0.6650(7) 0.8561(5) 0.124(4) Uani 1 1 d DU . . H30A H 0.0735 0.6311 0.8418 0.186 Uiso 1 1 calc R . . H30B H -0.0865 0.6295 0.8514 0.186 Uiso 1 1 calc R . . H30C H 0.0081 0.6796 0.8983 0.186 Uiso 1 1 calc R . . C31 C -0.0188(12) 0.7587(8) 0.8164(7) 0.206(6) Uani 1 1 d DU . . H31A H 0.0203 0.7494 0.7762 0.247 Uiso 1 1 calc R . . H31B H -0.1155 0.7733 0.8114 0.247 Uiso 1 1 calc R . . C32 C -0.0066(15) 0.8687(11) 0.8947(5) 0.167(5) Uani 1 1 d DU . . H32A H 0.0009 0.8293 0.9299 0.201 Uiso 1 1 calc R . . H32B H -0.1018 0.8862 0.8885 0.201 Uiso 1 1 calc R . . C33 C 0.0980(14) 0.9561(10) 0.8985(5) 0.161(6) Uani 1 1 d DU . . H33A H 0.1916 0.9356 0.8963 0.242 Uiso 1 1 calc R . . H33B H 0.0837 0.9874 0.9363 0.242 Uiso 1 1 calc R . . H33C H 0.0795 0.9963 0.8652 0.242 Uiso 1 1 calc R . . Cl1 Cl -0.09443(9) 0.31177(6) 0.11348(4) 0.02635(18) Uani 1 1 d . . . Cl2 Cl -0.15337(12) 0.32381(7) 0.26393(5) 0.0332(2) Uani 1 1 d . . . O1 O 0.4422(3) 0.22862(19) 0.13401(15) 0.0356(6) Uani 1 1 d . . . O2 O 0.4857(3) 0.0886(2) 0.15768(18) 0.0464(9) Uani 1 1 d . . . O3 O 0.0501(9) 0.8335(7) 0.8453(5) 0.173(4) Uani 1 1 d DU . . P1 P -0.00342(10) 0.12573(6) 0.27001(4) 0.02016(17) Uani 1 1 d D . . P2 P 0.01156(9) 0.12340(6) 0.13012(4) 0.01775(16) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.01671(10) 0.01781(10) 0.02013(10) 0.00181(9) -0.00058(9) -0.00006(9) C1 0.0222(17) 0.0273(17) 0.0221(16) -0.0026(13) -0.0035(13) 0.0018(13) C2 0.036(2) 0.038(2) 0.0248(18) 0.0057(16) -0.0057(15) -0.0055(17) C3 0.047(3) 0.047(3) 0.0265(19) 0.0044(18) -0.0113(19) -0.001(2) C4 0.044(3) 0.050(3) 0.042(3) -0.015(2) -0.019(2) -0.002(2) C5 0.036(2) 0.050(3) 0.046(3) -0.011(2) -0.002(2) -0.020(2) C6 0.031(2) 0.038(2) 0.031(2) -0.0004(16) -0.0004(16) -0.0082(17) C7 0.0160(15) 0.0239(16) 0.0242(16) 0.0086(12) 0.0015(12) 0.0027(12) C8 0.0246(18) 0.034(2) 0.0226(16) 0.0001(14) 0.0052(14) 0.0074(15) C9 0.043(3) 0.057(3) 0.030(2) 0.006(2) 0.016(2) 0.008(2) C10 0.0290(19) 0.0287(18) 0.0233(16) -0.0009(14) 0.0051(14) 0.0041(15) C11 0.063(3) 0.029(2) 0.044(3) -0.0023(19) 0.019(2) 0.008(2) C12 0.0179(16) 0.0225(15) 0.0222(15) 0.0052(12) 0.0056(12) 0.0042(12) C13 0.0195(15) 0.0226(15) 0.0242(15) 0.0064(14) 0.0043(14) 0.0048(12) C14 0.0160(15) 0.0283(17) 0.0236(16) 0.0070(13) 0.0013(12) 0.0016(13) C15 0.0188(18) 0.034(2) 0.0305(18) 0.0074(15) 0.0016(13) 0.0003(14) C16 0.018(2) 0.050(3) 0.067(3) 0.014(2) 0.0051(19) -0.0054(17) C17 0.0190(16) 0.0339(19) 0.0203(15) 0.0066(14) -0.0012(12) 0.0055(14) C18 0.0240(18) 0.0303(18) 0.0196(15) 0.0069(13) 0.0032(13) 0.0018(14) C19 0.031(2) 0.044(3) 0.047(3) 0.025(2) -0.0060(19) -0.0050(19) C20 0.030(2) 0.074(4) 0.066(4) 0.041(3) -0.015(2) -0.015(2) C21 0.040(3) 0.048(3) 0.045(3) 0.017(2) 0.000(2) -0.017(2) C22 0.036(2) 0.038(2) 0.035(2) 0.0111(17) 0.0074(17) -0.0024(18) C23 0.0297(18) 0.0293(17) 0.0298(18) 0.0070(16) 0.0045(16) 0.0058(14) C24 0.042(6) 0.006(5) 0.027(6) -0.004(4) -0.005(5) 0.001(4) C25 0.038(6) 0.041(8) 0.044(7) -0.008(6) -0.006(6) 0.007(7) C26 0.057(7) 0.057(8) 0.044(6) 0.006(6) -0.029(6) -0.012(7) C27 0.071(10) 0.055(9) 0.030(6) 0.006(6) -0.016(6) 0.008(8) C28 0.070(10) 0.046(6) 0.025(5) 0.003(5) 0.006(7) 0.009(8) C29 0.051(8) 0.042(7) 0.014(5) 0.002(5) 0.003(5) -0.007(7) C24A 0.032(4) 0.038(7) 0.017(3) 0.005(3) -0.005(3) 0.015(4) C25A 0.039(4) 0.032(4) 0.030(4) -0.005(3) -0.007(3) -0.004(4) C26A 0.053(4) 0.040(5) 0.049(5) -0.012(4) -0.020(4) 0.015(5) C27A 0.074(8) 0.055(7) 0.036(5) -0.012(5) -0.024(5) 0.009(5) C28A 0.078(8) 0.052(5) 0.026(4) -0.002(4) -0.006(6) 0.004(7) C29A 0.070(8) 0.039(5) 0.027(4) 0.000(3) -0.003(5) -0.003(6) C30 0.061(5) 0.149(9) 0.162(10) -0.076(8) -0.035(6) 0.031(6) C31 0.112(7) 0.146(10) 0.359(14) -0.046(11) -0.164(9) 0.020(7) C32 0.151(11) 0.271(14) 0.080(7) -0.050(9) -0.030(7) 0.073(10) C33 0.159(13) 0.224(15) 0.100(8) -0.058(9) -0.034(8) 0.079(12) Cl1 0.0286(5) 0.0217(4) 0.0287(4) 0.0078(3) -0.0074(3) -0.0023(3) Cl2 0.0416(6) 0.0249(4) 0.0330(5) -0.0042(4) 0.0096(4) 0.0034(4) O1 0.0176(11) 0.0314(14) 0.0577(18) 0.0101(13) 0.0027(13) -0.0026(13) O2 0.0240(15) 0.0421(19) 0.073(2) 0.0259(18) 0.0085(15) 0.0077(13) O3 0.097(6) 0.178(8) 0.244(10) -0.031(7) -0.058(7) 0.053(6) P1 0.0207(4) 0.0220(4) 0.0178(4) 0.0019(3) -0.0009(3) 0.0022(3) P2 0.0175(4) 0.0178(4) 0.0179(4) 0.0028(3) 0.0009(3) -0.0001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 P2 2.2237(9) . ? Pd1 P1 2.2424(9) . ? Pd1 Cl2 2.3462(10) . ? Pd1 Cl1 2.3576(9) . ? C1 C6 1.387(6) . ? C1 C2 1.398(5) . ? C1 P2 1.798(4) . ? C2 C3 1.380(6) . ? C3 C4 1.395(8) . ? C4 C5 1.383(8) . ? C5 C6 1.386(6) . ? C7 C8 1.512(5) . ? C7 C14 1.566(5) . ? C7 P2 1.832(4) . ? C8 C10 1.338(6) . ? C8 C9 1.503(6) . ? C10 C11 1.487(6) . ? C10 C12 1.527(5) . ? C12 C13 1.560(5) . ? C12 P2 1.843(4) . ? C13 C17 1.544(5) . ? C13 C14 1.571(5) . ? C14 C15 1.517(5) . ? C15 O2 1.192(5) . ? C15 O1 1.326(5) . ? C16 O1 1.451(5) . ? C17 P1 1.838(4) . ? C18 C19 1.396(6) . ? C18 C23 1.397(5) . ? C18 P1 1.808(4) . ? C19 C20 1.401(7) . ? C20 C21 1.381(7) . ? C21 C22 1.361(7) . ? C22 C23 1.392(6) . ? C24 C25 1.387(14) . ? C24 C29 1.389(14) . ? C24 P1 1.812(12) . ? C25 C26 1.372(14) . ? C26 C27 1.396(15) . ? C27 C28 1.389(15) . ? C28 C29 1.386(14) . ? C24A C25A 1.366(11) . ? C24A C29A 1.389(12) . ? C24A P1 1.842(8) . ? C25A C26A 1.381(10) . ? C26A C27A 1.359(11) . ? C27A C28A 1.385(12) . ? C28A C29A 1.393(11) . ? C30 C31 1.679(14) . ? C31 O3 1.470(11) . ? C32 O3 1.353(12) . ? C32 C33 1.681(15) . ? 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 89.45(3) . . ? P2 Pd1 Cl2 175.45(4) . . ? P1 Pd1 Cl2 93.51(4) . . ? P2 Pd1 Cl1 83.62(3) . . ? P1 Pd1 Cl1 171.69(4) . . ? Cl2 Pd1 Cl1 93.69(4) . . ? C6 C1 C2 119.4(4) . . ? C6 C1 P2 118.7(3) . . ? C2 C1 P2 121.8(3) . . ? C3 C2 C1 120.1(4) . . ? C2 C3 C4 120.4(4) . . ? C5 C4 C3 119.3(4) . . ? C4 C5 C6 120.6(4) . . ? C5 C6 C1 120.2(4) . . ? C8 C7 C14 107.7(3) . . ? C8 C7 P2 101.7(3) . . ? C14 C7 P2 97.6(2) . . ? C10 C8 C9 128.7(4) . . ? C10 C8 C7 110.8(3) . . ? C9 C8 C7 120.3(4) . . ? C8 C10 C11 129.3(4) . . ? C8 C10 C12 110.8(3) . . ? C11 C10 C12 119.9(4) . . ? C10 C12 C13 106.3(3) . . ? C10 C12 P2 100.5(2) . . ? C13 C12 P2 99.9(2) . . ? C17 C13 C12 114.0(3) . . ? C17 C13 C14 113.5(3) . . ? C12 C13 C14 105.1(3) . . ? C15 C14 C7 109.9(3) . . ? C15 C14 C13 114.3(3) . . ? C7 C14 C13 106.2(3) . . ? O2 C15 O1 123.8(4) . . ? O2 C15 C14 126.5(4) . . ? O1 C15 C14 109.7(3) . . ? C13 C17 P1 117.0(2) . . ? C19 C18 C23 119.4(4) . . ? C19 C18 P1 118.8(3) . . ? C23 C18 P1 121.7(3) . . ? C18 C19 C20 119.5(4) . . ? C21 C20 C19 120.1(5) . . ? C22 C21 C20 120.7(4) . . ? C21 C22 C23 120.3(4) . . ? C22 C23 C18 120.1(4) . . ? C25 C24 C29 120.5(15) . . ? C25 C24 P1 117.4(13) . . ? C29 C24 P1 122.0(14) . . ? C26 C25 C24 119.7(17) . . ? C25 C26 C27 119.4(17) . . ? C28 C27 C26 120.2(15) . . ? C29 C28 C27 119.7(18) . . ? C28 C29 C24 119.3(18) . . ? C25A C24A C29A 118.5(9) . . ? C25A C24A P1 120.0(8) . . ? C29A C24A P1 120.9(9) . . ? C24A C25A C26A 120.4(10) . . ? C27A C26A C25A 121.4(10) . . ? C26A C27A C28A 119.5(10) . . ? C27A C28A C29A 118.8(12) . . ? C24A C29A C28A 121.2(12) . . ? O3 C31 C30 111.9(9) . . ? O3 C32 C33 95.4(11) . . ? C15 O1 C16 117.6(3) . . ? C32 O3 C31 118.1(12) . . ? C18 P1 C24 101.6(6) . . ? C18 P1 C17 107.62(18) . . ? C24 P1 C17 99.7(9) . . ? C18 P1 C24A 108.9(4) . . ? C24 P1 C24A 8.5(9) . . ? C17 P1 C24A 101.2(5) . . ? C18 P1 Pd1 110.30(12) . . ? C24 P1 Pd1 121.6(8) . . ? C17 P1 Pd1 114.52(12) . . ? C24A P1 Pd1 113.8(5) . . ? C1 P2 C7 112.88(17) . . ? C1 P2 C12 107.72(18) . . ? C7 P2 C12 82.29(16) . . ? C1 P2 Pd1 115.34(13) . . ? C7 P2 Pd1 112.48(13) . . ? C12 P2 Pd1 121.82(12) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.58 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.162 _refine_diff_density_min -0.828 _refine_diff_density_rms 0.111 # Attachment 'complex_71.cif' data_leung355 _database_code_depnum_ccdc_archive 'CCDC 711831' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_absolute_configuration ad _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C29 H30 Cl2 O2 P2 Pd' _chemical_formula_sum 'C29 H30 Cl2 O2 P2 Pd' _chemical_formula_weight 649.77 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 8.8932(2) _cell_length_b 15.1804(3) _cell_length_c 20.1229(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2716.64(10) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9130 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 31.93 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.589 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1320 _exptl_absorpt_coefficient_mu 1.024 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7487 _exptl_absorpt_correction_T_max 0.9602 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43231 _diffrn_reflns_av_R_equivalents 0.0314 _diffrn_reflns_av_sigmaI/netI 0.0283 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 31.96 _reflns_number_total 9379 _reflns_number_gt 8789 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0310P)^2^+0.2765P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.007(14) _refine_ls_number_reflns 9379 _refine_ls_number_parameters 328 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0259 _refine_ls_R_factor_gt 0.0220 _refine_ls_wR_factor_ref 0.0633 _refine_ls_wR_factor_gt 0.0515 _refine_ls_goodness_of_fit_ref 1.141 _refine_ls_restrained_S_all 1.141 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.381210(14) -0.043556(9) 0.178188(6) 0.01590(3) Uani 1 1 d . . . C1 C 0.4092(2) -0.09742(12) 0.00963(9) 0.0181(3) Uani 1 1 d . . . C2 C 0.3023(2) -0.05802(15) -0.03103(10) 0.0267(4) Uani 1 1 d . . . H2 H 0.2693 0.0004 -0.0223 0.032 Uiso 1 1 calc R . . C3 C 0.2439(3) -0.10457(16) -0.08457(11) 0.0290(4) Uani 1 1 d . . . H3 H 0.1710 -0.0779 -0.1126 0.035 Uiso 1 1 calc R . . C4 C 0.2918(2) -0.18993(15) -0.09725(10) 0.0261(4) Uani 1 1 d . . . H4 H 0.2510 -0.2217 -0.1337 0.031 Uiso 1 1 calc R . . C5 C 0.3988(3) -0.22884(14) -0.05691(10) 0.0256(4) Uani 1 1 d . . . H5 H 0.4328 -0.2869 -0.0662 0.031 Uiso 1 1 calc R . . C6 C 0.4567(2) -0.18327(13) -0.00292(10) 0.0224(4) Uani 1 1 d . . . H6 H 0.5284 -0.2105 0.0254 0.027 Uiso 1 1 calc R . . C7 C 0.69236(19) -0.05836(12) 0.08148(9) 0.0158(3) Uani 1 1 d . . . H7 H 0.7225 -0.1206 0.0907 0.019 Uiso 1 1 calc R . . C8 C 0.7393(2) -0.02266(12) 0.01333(9) 0.0180(3) Uani 1 1 d . . . C9 C 0.8654(2) -0.06437(13) -0.02395(9) 0.0238(4) Uani 1 1 d . . . H9A H 0.8732 -0.0376 -0.0681 0.036 Uiso 1 1 calc R . . H9B H 0.8463 -0.1277 -0.0285 0.036 Uiso 1 1 calc R . . H9C H 0.9597 -0.0553 0.0003 0.036 Uiso 1 1 calc R . . C10 C 0.65485(18) 0.04709(13) -0.00371(8) 0.0174(3) Uani 1 1 d . . . C11 C 0.6492(3) 0.09721(14) -0.06741(10) 0.0259(4) Uani 1 1 d . . . H11A H 0.7231 0.0728 -0.0985 0.039 Uiso 1 1 calc R . . H11B H 0.6724 0.1593 -0.0589 0.039 Uiso 1 1 calc R . . H11C H 0.5483 0.0924 -0.0867 0.039 Uiso 1 1 calc R . . C12 C 0.5520(2) 0.07290(12) 0.05304(9) 0.0165(3) Uani 1 1 d . . . H12 H 0.4708 0.1160 0.0418 0.020 Uiso 1 1 calc R . . C13 C 0.6533(2) 0.09752(12) 0.11441(9) 0.0166(3) Uani 1 1 d . . . H13 H 0.5883 0.1218 0.1506 0.020 Uiso 1 1 calc R . . C14 C 0.7246(2) 0.00802(12) 0.13839(9) 0.0155(3) Uani 1 1 d . . . H14 H 0.8347 0.0139 0.1474 0.019 Uiso 1 1 calc R . . C15 C 0.7793(2) 0.16303(13) 0.09955(10) 0.0211(4) Uani 1 1 d . . . H15A H 0.8310 0.1765 0.1419 0.025 Uiso 1 1 calc R . . H15B H 0.8533 0.1333 0.0704 0.025 Uiso 1 1 calc R . . C16 C 0.7373(2) 0.24851(13) 0.06761(10) 0.0233(4) Uani 1 1 d . . . C17 C 0.5506(3) 0.35633(16) 0.05599(14) 0.0368(6) Uani 1 1 d . . . H17A H 0.5929 0.4039 0.0831 0.055 Uiso 1 1 calc R . . H17B H 0.4406 0.3600 0.0567 0.055 Uiso 1 1 calc R . . H17C H 0.5865 0.3622 0.0101 0.055 Uiso 1 1 calc R . . C18 C 0.6615(2) 0.05805(12) 0.27143(8) 0.0176(3) Uani 1 1 d . . . C19 C 0.8091(2) 0.06617(14) 0.29473(11) 0.0256(4) Uani 1 1 d . . . H19 H 0.8813 0.0219 0.2850 0.031 Uiso 1 1 calc R . . C20 C 0.8492(3) 0.13920(16) 0.33204(12) 0.0328(5) Uani 1 1 d . . . H20 H 0.9491 0.1444 0.3483 0.039 Uiso 1 1 calc R . . C21 C 0.7451(3) 0.20479(15) 0.34591(11) 0.0300(5) Uani 1 1 d . . . H21 H 0.7744 0.2553 0.3706 0.036 Uiso 1 1 calc R . . C22 C 0.5981(3) 0.19636(13) 0.32360(11) 0.0268(4) Uani 1 1 d . . . H22 H 0.5263 0.2408 0.3335 0.032 Uiso 1 1 calc R . . C23 C 0.5556(2) 0.12256(13) 0.28668(9) 0.0213(4) Uani 1 1 d . . . H23 H 0.4546 0.1164 0.2720 0.026 Uiso 1 1 calc R . . C25 C 0.7119(2) -0.12679(12) 0.24461(9) 0.0172(3) Uani 1 1 d . . . C26 C 0.8662(2) -0.14206(13) 0.23514(10) 0.0229(4) Uani 1 1 d . . . H26 H 0.9243 -0.1026 0.2090 0.027 Uiso 1 1 calc R . . C27 C 0.9334(3) -0.21493(15) 0.26418(11) 0.0290(5) Uani 1 1 d . . . H27 H 1.0378 -0.2251 0.2579 0.035 Uiso 1 1 calc R . . C28 C 0.8500(3) -0.27299(15) 0.30225(11) 0.0297(5) Uani 1 1 d . . . H28 H 0.8966 -0.3234 0.3211 0.036 Uiso 1 1 calc R . . C29 C 0.6991(3) -0.25745(14) 0.31274(11) 0.0285(4) Uani 1 1 d . . . H29 H 0.6428 -0.2966 0.3399 0.034 Uiso 1 1 calc R . . C30 C 0.6285(2) -0.18523(13) 0.28400(10) 0.0225(4) Uani 1 1 d . . . H30 H 0.5242 -0.1755 0.2910 0.027 Uiso 1 1 calc R . . Cl1 Cl 0.14277(5) -0.03897(5) 0.12592(2) 0.03268(11) Uani 1 1 d . . . Cl2 Cl 0.27984(6) -0.05401(4) 0.28598(2) 0.03360(12) Uani 1 1 d . . . O1 O 0.59752(18) 0.27257(10) 0.08238(8) 0.0284(3) Uani 1 1 d . . . O2 O 0.8201(2) 0.29045(12) 0.03279(11) 0.0455(5) Uani 1 1 d . . . P1 P 0.48780(5) -0.03805(3) 0.07889(2) 0.01503(8) Uani 1 1 d . . . P2 P 0.62050(5) -0.02913(3) 0.21272(2) 0.01508(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.01180(5) 0.02101(6) 0.01490(5) -0.00010(5) 0.00093(5) -0.00165(5) C1 0.0169(8) 0.0203(8) 0.0169(8) -0.0006(6) 0.0007(7) -0.0022(6) C2 0.0241(9) 0.0317(11) 0.0244(9) -0.0044(8) -0.0077(8) 0.0061(8) C3 0.0245(10) 0.0409(12) 0.0217(9) -0.0012(8) -0.0075(8) 0.0012(9) C4 0.0231(10) 0.0332(11) 0.0220(9) -0.0038(8) -0.0005(8) -0.0103(9) C5 0.0303(11) 0.0210(9) 0.0254(9) -0.0017(7) 0.0006(9) -0.0070(8) C6 0.0243(9) 0.0198(9) 0.0231(9) 0.0014(7) -0.0034(8) -0.0017(7) C7 0.0142(7) 0.0168(9) 0.0162(7) 0.0010(6) 0.0001(6) 0.0011(6) C8 0.0170(8) 0.0234(9) 0.0136(7) -0.0011(6) 0.0014(6) -0.0009(7) C9 0.0226(9) 0.0298(10) 0.0189(8) -0.0010(7) 0.0046(8) 0.0039(8) C10 0.0164(7) 0.0223(8) 0.0136(7) 0.0016(7) 0.0001(6) -0.0016(7) C11 0.0301(11) 0.0300(10) 0.0176(8) 0.0062(7) 0.0010(8) 0.0016(8) C12 0.0154(8) 0.0180(8) 0.0160(8) 0.0020(6) -0.0001(6) 0.0017(6) C13 0.0150(8) 0.0179(8) 0.0170(8) 0.0010(6) 0.0006(6) 0.0008(6) C14 0.0129(7) 0.0200(8) 0.0136(7) 0.0009(6) -0.0007(6) 0.0002(6) C15 0.0168(8) 0.0225(9) 0.0240(9) 0.0014(7) 0.0000(7) -0.0030(7) C16 0.0245(10) 0.0213(9) 0.0239(9) 0.0011(7) 0.0006(8) -0.0046(8) C17 0.0364(13) 0.0249(11) 0.0491(15) 0.0086(10) -0.0044(11) 0.0037(10) C18 0.0174(8) 0.0218(9) 0.0137(7) -0.0003(6) -0.0004(6) -0.0032(6) C19 0.0197(9) 0.0297(11) 0.0272(10) -0.0054(8) -0.0044(8) -0.0014(7) C20 0.0262(11) 0.0364(12) 0.0357(12) -0.0089(9) -0.0073(9) -0.0088(9) C21 0.0377(12) 0.0248(10) 0.0274(10) -0.0066(8) -0.0013(10) -0.0090(9) C22 0.0358(11) 0.0212(8) 0.0233(9) -0.0020(8) 0.0003(10) 0.0002(8) C23 0.0224(9) 0.0237(9) 0.0178(8) 0.0008(7) -0.0005(7) 0.0004(7) C25 0.0174(8) 0.0195(8) 0.0147(7) -0.0013(6) -0.0011(6) -0.0008(7) C26 0.0192(9) 0.0260(9) 0.0234(9) 0.0025(7) 0.0037(8) 0.0023(8) C27 0.0219(10) 0.0333(12) 0.0319(11) 0.0016(9) 0.0002(8) 0.0058(8) C28 0.0306(12) 0.0248(10) 0.0338(11) 0.0050(8) -0.0072(9) 0.0045(8) C29 0.0293(10) 0.0240(10) 0.0322(11) 0.0081(8) -0.0044(9) -0.0057(8) C30 0.0183(8) 0.0252(9) 0.0239(8) 0.0039(7) -0.0008(8) -0.0043(8) Cl1 0.01334(19) 0.0587(3) 0.0260(2) 0.0022(2) -0.00136(16) -0.0011(2) Cl2 0.0269(2) 0.0542(4) 0.0197(2) -0.0011(2) 0.00746(18) -0.0056(2) O1 0.0253(8) 0.0202(7) 0.0397(8) 0.0066(6) 0.0039(7) 0.0002(6) O2 0.0397(10) 0.0372(10) 0.0597(12) 0.0190(9) 0.0175(9) -0.0040(8) P1 0.01307(18) 0.0180(2) 0.01406(17) 0.00014(18) -0.00065(15) -0.00038(18) P2 0.01314(17) 0.0191(2) 0.01305(17) -0.00016(14) -0.00036(17) -0.00064(18) _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 P1 2.2132(4) . ? Pd1 P2 2.2493(5) . ? Pd1 Cl2 2.3543(5) . ? Pd1 Cl1 2.3680(5) . ? C1 C2 1.390(3) . ? C1 C6 1.393(3) . ? C1 P1 1.8008(19) . ? C2 C3 1.389(3) . ? C3 C4 1.388(3) . ? C4 C5 1.383(3) . ? C5 C6 1.387(3) . ? C7 C8 1.532(2) . ? C7 C14 1.552(3) . ? C7 P1 1.8458(18) . ? C8 C10 1.343(3) . ? C8 C9 1.491(3) . ? C10 C11 1.491(3) . ? C10 C12 1.515(2) . ? C12 C13 1.574(3) . ? C12 P1 1.8529(19) . ? C13 C15 1.527(3) . ? C13 C14 1.575(3) . ? C14 P2 1.8469(18) . ? C15 C16 1.495(3) . ? C16 O2 1.199(3) . ? C16 O1 1.329(3) . ? C17 O1 1.440(3) . ? C18 C23 1.393(3) . ? C18 C19 1.399(3) . ? C18 P2 1.8111(19) . ? C19 C20 1.386(3) . ? C20 C21 1.388(3) . ? C21 C22 1.389(3) . ? C22 C23 1.396(3) . ? C25 C30 1.402(3) . ? C25 C26 1.405(3) . ? C25 P2 1.8085(19) . ? C26 C27 1.386(3) . ? C27 C28 1.383(3) . ? C28 C29 1.379(3) . ? C29 C30 1.389(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 Pd1 P2 82.529(16) . . ? P1 Pd1 Cl2 176.72(2) . . ? P2 Pd1 Cl2 94.833(17) . . ? P1 Pd1 Cl1 88.938(17) . . ? P2 Pd1 Cl1 168.974(19) . . ? Cl2 Pd1 Cl1 93.915(18) . . ? C2 C1 C6 120.22(18) . . ? C2 C1 P1 120.38(15) . . ? C6 C1 P1 119.40(15) . . ? C3 C2 C1 119.6(2) . . ? C4 C3 C2 120.2(2) . . ? C5 C4 C3 120.14(19) . . ? C4 C5 C6 120.1(2) . . ? C5 C6 C1 119.74(19) . . ? C8 C7 C14 112.36(14) . . ? C8 C7 P1 100.62(12) . . ? C14 C7 P1 95.40(11) . . ? C10 C8 C9 128.86(17) . . ? C10 C8 C7 110.79(15) . . ? C9 C8 C7 120.34(16) . . ? C8 C10 C11 129.85(17) . . ? C8 C10 C12 110.44(15) . . ? C11 C10 C12 119.70(17) . . ? C10 C12 C13 107.87(14) . . ? C10 C12 P1 99.35(13) . . ? C13 C12 P1 99.90(12) . . ? C15 C13 C12 114.90(15) . . ? C15 C13 C14 109.08(15) . . ? C12 C13 C14 105.42(14) . . ? C7 C14 C13 105.06(14) . . ? C7 C14 P2 107.88(12) . . ? C13 C14 P2 108.06(12) . . ? C16 C15 C13 117.77(17) . . ? O2 C16 O1 124.0(2) . . ? O2 C16 C15 123.9(2) . . ? O1 C16 C15 112.07(17) . . ? C23 C18 C19 119.91(18) . . ? C23 C18 P2 121.41(14) . . ? C19 C18 P2 118.15(14) . . ? C20 C19 C18 119.6(2) . . ? C19 C20 C21 120.7(2) . . ? C20 C21 C22 119.80(19) . . ? C21 C22 C23 120.1(2) . . ? C18 C23 C22 119.87(19) . . ? C30 C25 C26 119.27(18) . . ? C30 C25 P2 118.81(15) . . ? C26 C25 P2 121.74(15) . . ? C27 C26 C25 119.67(19) . . ? C28 C27 C26 120.7(2) . . ? C29 C28 C27 119.8(2) . . ? C28 C29 C30 120.7(2) . . ? C29 C30 C25 119.7(2) . . ? C16 O1 C17 115.53(18) . . ? C1 P1 C7 108.70(8) . . ? C1 P1 C12 110.92(8) . . ? C7 P1 C12 81.74(8) . . ? C1 P1 Pd1 120.91(6) . . ? C7 P1 Pd1 112.98(6) . . ? C12 P1 Pd1 114.81(6) . . ? C25 P2 C18 106.09(8) . . ? C25 P2 C14 108.21(8) . . ? C18 P2 C14 101.79(8) . . ? C25 P2 Pd1 117.06(6) . . ? C18 P2 Pd1 117.59(6) . . ? C14 P2 Pd1 104.69(6) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 31.96 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.431 _refine_diff_density_min -0.446 _refine_diff_density_rms 0.121