# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email PAKHING@ntu.edu.sg _publ_contact_author_name 'Pak-Hing Leung' loop_ _publ_author_name 'Pak-Hing Leung' 'Sumod Pullarkat' 'Yongxin Li' 'Kennard Chen' 'Mengtao Ma' data_leung381 _database_code_depnum_ccdc_archive 'CCDC 857605' #TrackingRef '- leung381-344-475.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_absolute_configuration ad _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H24 Cl2 N O4 P Pd' _chemical_formula_sum 'C20 H24 Cl2 N O4 P Pd' _chemical_formula_weight 550.67 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 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 10.8879(2) _cell_length_b 12.1286(3) _cell_length_c 17.4097(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2299.04(9) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8262 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 28.15 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.591 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1112 _exptl_absorpt_coefficient_mu 1.134 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6990 _exptl_absorpt_correction_T_max 0.8393 _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 28298 _diffrn_reflns_av_R_equivalents 0.0473 _diffrn_reflns_av_sigmaI/netI 0.0582 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 31.58 _reflns_number_total 7490 _reflns_number_gt 6567 _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^)+(0.0155P)^2^+0.3591P] 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 -0.049(19) _refine_ls_number_reflns 7490 _refine_ls_number_parameters 266 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0474 _refine_ls_R_factor_gt 0.0359 _refine_ls_wR_factor_ref 0.0578 _refine_ls_wR_factor_gt 0.0534 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _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 0.459593(17) 0.238732(13) 0.130665(11) 0.01651(4) Uani 1 1 d . . . C1 C 0.3356(3) 0.1127(2) 0.00929(15) 0.0245(6) Uani 1 1 d . . . H1A H 0.4187 0.1128 -0.0124 0.037 Uiso 1 1 calc R . . H1B H 0.2929 0.1805 -0.0058 0.037 Uiso 1 1 calc R . . H1C H 0.2902 0.0487 -0.0100 0.037 Uiso 1 1 calc R . . C2 C 0.3992(2) -0.00011(19) 0.11806(18) 0.0257(6) Uani 1 1 d . . . H2A H 0.3471 -0.0609 0.1005 0.039 Uiso 1 1 calc R . . H2B H 0.4064 -0.0026 0.1741 0.039 Uiso 1 1 calc R . . H2C H 0.4810 -0.0071 0.0950 0.039 Uiso 1 1 calc R . . C3 C -0.0588(3) 0.0439(2) 0.01593(18) 0.0327(7) Uani 1 1 d . . . H3A H -0.0308 -0.0188 -0.0150 0.049 Uiso 1 1 calc R . . H3B H -0.1054 0.0948 -0.0166 0.049 Uiso 1 1 calc R . . H3C H -0.1114 0.0173 0.0577 0.049 Uiso 1 1 calc R . . C4 C 0.1223(3) 0.0423(2) 0.09169(16) 0.0227(6) Uani 1 1 d . . . C5 C 0.2172(2) 0.11631(17) 0.13104(17) 0.0186(5) Uani 1 1 d . . . H5 H 0.2249 0.0909 0.1855 0.022 Uiso 1 1 calc R . . C6 C 0.1741(2) 0.23647(17) 0.13285(15) 0.0173(4) Uani 1 1 d . . . H6 H 0.1669 0.2645 0.0790 0.021 Uiso 1 1 calc R . . C7 C 0.0503(2) 0.2450(2) 0.17193(14) 0.0225(5) Uani 1 1 d . . . C8 C -0.1182(3) 0.3658(3) 0.1915(2) 0.0453(9) Uani 1 1 d . . . H8A H -0.1785 0.3137 0.1708 0.068 Uiso 1 1 calc R . . H8B H -0.1437 0.4413 0.1794 0.068 Uiso 1 1 calc R . . H8C H -0.1130 0.3569 0.2474 0.068 Uiso 1 1 calc R . . C9 C 0.2654(2) 0.45897(19) 0.17102(16) 0.0190(5) Uani 1 1 d . . . C10 C 0.2100(2) 0.4971(2) 0.10375(16) 0.0213(6) Uani 1 1 d . . . H10 H 0.1829 0.4465 0.0657 0.026 Uiso 1 1 calc R . . C11 C 0.1949(3) 0.6095(2) 0.09303(18) 0.0303(7) Uani 1 1 d . . . H11 H 0.1568 0.6359 0.0475 0.036 Uiso 1 1 calc R . . C12 C 0.2346(3) 0.6832(2) 0.14805(19) 0.0336(8) Uani 1 1 d . . . H12 H 0.2241 0.7601 0.1401 0.040 Uiso 1 1 calc R . . C13 C 0.2899(3) 0.6457(2) 0.21478(19) 0.0313(7) Uani 1 1 d . . . H13 H 0.3170 0.6967 0.2526 0.038 Uiso 1 1 calc R . . C14 C 0.3053(3) 0.5335(2) 0.22617(17) 0.0249(6) Uani 1 1 d . . . H14 H 0.3434 0.5075 0.2718 0.030 Uiso 1 1 calc R . . C15 C 0.2781(2) 0.27958(19) 0.28364(15) 0.0218(6) Uani 1 1 d . . . C16 C 0.1771(3) 0.3184(2) 0.32566(17) 0.0309(7) Uani 1 1 d . . . H16 H 0.1231 0.3713 0.3038 0.037 Uiso 1 1 calc R . . C17 C 0.1570(3) 0.2791(2) 0.39904(19) 0.0427(8) Uani 1 1 d . . . H17 H 0.0879 0.3043 0.4274 0.051 Uiso 1 1 calc R . . C18 C 0.2361(4) 0.2038(3) 0.4314(2) 0.0551(11) Uani 1 1 d . . . H18 H 0.2216 0.1775 0.4820 0.066 Uiso 1 1 calc R . . C19 C 0.3364(4) 0.1666(3) 0.3907(2) 0.0600(11) Uani 1 1 d . . . H19 H 0.3914 0.1154 0.4135 0.072 Uiso 1 1 calc R . . C20 C 0.3569(3) 0.2033(2) 0.31686(19) 0.0396(8) Uani 1 1 d . . . H20 H 0.4253 0.1763 0.2886 0.047 Uiso 1 1 calc R . . Cl1 Cl 0.63614(6) 0.15885(5) 0.07224(4) 0.02572(15) Uani 1 1 d . . . Cl2 Cl 0.56891(6) 0.38675(5) 0.17596(4) 0.02775(16) Uani 1 1 d . . . N1 N 0.34329(19) 0.10712(16) 0.09441(12) 0.0172(4) Uani 1 1 d . . . O1 O 0.11720(19) -0.05577(14) 0.10072(13) 0.0378(6) Uani 1 1 d . . . O2 O 0.04631(18) 0.10041(13) 0.04784(11) 0.0268(4) Uani 1 1 d . . . O3 O 0.00428(18) 0.17423(16) 0.20955(13) 0.0369(5) Uani 1 1 d . . . O4 O 0.00131(15) 0.34416(15) 0.15747(12) 0.0265(5) Uani 1 1 d . . . P1 P 0.29599(6) 0.31407(5) 0.18333(4) 0.01641(13) 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 0.01350(9) 0.01626(8) 0.01976(9) -0.00100(7) 0.00046(7) 0.00112(7) C1 0.0266(16) 0.0261(13) 0.0207(15) -0.0041(11) 0.0002(11) 0.0035(11) C2 0.0231(16) 0.0158(11) 0.0382(19) 0.0001(12) -0.0008(12) 0.0038(10) C3 0.0252(18) 0.0344(15) 0.0385(18) 0.0012(13) -0.0122(14) -0.0088(12) C4 0.0190(15) 0.0233(13) 0.0257(16) 0.0007(11) 0.0029(11) -0.0029(10) C5 0.0197(14) 0.0146(10) 0.0215(13) 0.0017(11) -0.0001(12) -0.0002(8) C6 0.0148(12) 0.0179(10) 0.0191(11) -0.0010(12) 0.0020(10) 0.0002(9) C7 0.0168(13) 0.0280(12) 0.0228(12) -0.0011(11) -0.0002(10) -0.0030(12) C8 0.026(2) 0.056(2) 0.053(2) 0.0075(17) 0.0188(16) 0.0167(15) C9 0.0152(14) 0.0171(12) 0.0245(15) -0.0016(10) 0.0021(11) 0.0015(9) C10 0.0204(15) 0.0205(12) 0.0231(14) 0.0000(10) 0.0019(11) -0.0002(10) C11 0.0343(18) 0.0249(14) 0.0318(18) 0.0056(12) -0.0008(13) 0.0068(12) C12 0.0354(19) 0.0178(13) 0.048(2) 0.0030(13) 0.0077(14) 0.0035(11) C13 0.0310(19) 0.0217(13) 0.0411(19) -0.0103(12) -0.0005(14) 0.0001(12) C14 0.0242(17) 0.0203(13) 0.0301(16) -0.0048(11) -0.0038(12) 0.0034(11) C15 0.0271(16) 0.0185(12) 0.0197(14) -0.0018(10) -0.0024(10) 0.0027(10) C16 0.043(2) 0.0261(14) 0.0240(16) -0.0029(12) 0.0047(13) 0.0051(13) C17 0.068(2) 0.0315(17) 0.0284(17) -0.0036(13) 0.0198(16) 0.0031(15) C18 0.112(4) 0.0320(17) 0.0218(18) 0.0053(14) 0.011(2) 0.0074(19) C19 0.103(3) 0.045(2) 0.032(2) 0.0104(16) -0.001(2) 0.037(2) C20 0.051(2) 0.0395(18) 0.0285(18) 0.0006(14) -0.0015(15) 0.0208(14) Cl1 0.0205(4) 0.0283(3) 0.0284(4) -0.0031(3) 0.0059(3) 0.0045(3) Cl2 0.0174(4) 0.0223(3) 0.0435(4) -0.0072(3) -0.0047(3) -0.0015(2) N1 0.0184(12) 0.0133(9) 0.0198(12) 0.0006(8) 0.0007(9) 0.0021(8) O1 0.0351(13) 0.0165(9) 0.0617(16) 0.0040(9) -0.0134(11) -0.0068(8) O2 0.0255(11) 0.0233(9) 0.0315(11) 0.0047(8) -0.0103(9) -0.0087(9) O3 0.0283(13) 0.0378(11) 0.0445(14) 0.0107(10) 0.0139(9) -0.0029(8) O4 0.0157(11) 0.0294(10) 0.0344(12) 0.0018(8) 0.0061(8) 0.0055(7) P1 0.0149(4) 0.0163(3) 0.0180(3) -0.0010(3) -0.0005(3) 0.0014(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 Pd1 N1 2.133(2) . ? Pd1 P1 2.2020(7) . ? Pd1 Cl2 2.2938(6) . ? Pd1 Cl1 2.3808(7) . ? C1 N1 1.486(3) . ? C2 N1 1.494(3) . ? C3 O2 1.445(3) . ? C4 O1 1.201(3) . ? C4 O2 1.328(3) . ? C4 C5 1.531(3) . ? C5 N1 1.518(3) . ? C5 C6 1.531(3) . ? C6 C7 1.513(3) . ? C6 P1 1.849(2) . ? C7 O3 1.191(3) . ? C7 O4 1.339(3) . ? C8 O4 1.454(3) . ? C9 C14 1.389(4) . ? C9 C10 1.397(4) . ? C9 P1 1.802(2) . ? C10 C11 1.385(4) . ? C11 C12 1.381(4) . ? C12 C13 1.385(4) . ? C13 C14 1.385(4) . ? C15 C20 1.388(4) . ? C15 C16 1.402(4) . ? C15 P1 1.806(3) . ? C16 C17 1.381(4) . ? C17 C18 1.376(5) . ? C18 C19 1.378(5) . ? C19 C20 1.378(5) . ? 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 N1 Pd1 P1 87.33(6) . . ? N1 Pd1 Cl2 174.54(6) . . ? P1 Pd1 Cl2 87.24(2) . . ? N1 Pd1 Cl1 92.77(6) . . ? P1 Pd1 Cl1 179.22(3) . . ? Cl2 Pd1 Cl1 92.66(2) . . ? O1 C4 O2 124.9(2) . . ? O1 C4 C5 123.6(2) . . ? O2 C4 C5 111.5(2) . . ? N1 C5 C4 112.3(2) . . ? N1 C5 C6 110.83(18) . . ? C4 C5 C6 111.2(2) . . ? C7 C6 C5 110.33(19) . . ? C7 C6 P1 112.98(16) . . ? C5 C6 P1 105.93(16) . . ? O3 C7 O4 125.6(2) . . ? O3 C7 C6 124.9(2) . . ? O4 C7 C6 109.4(2) . . ? C14 C9 C10 120.0(2) . . ? C14 C9 P1 119.7(2) . . ? C10 C9 P1 120.2(2) . . ? C11 C10 C9 119.4(3) . . ? C12 C11 C10 120.5(3) . . ? C11 C12 C13 120.3(3) . . ? C12 C13 C14 119.7(3) . . ? C13 C14 C9 120.2(3) . . ? C20 C15 C16 119.4(3) . . ? C20 C15 P1 119.4(2) . . ? C16 C15 P1 120.8(2) . . ? C17 C16 C15 119.4(3) . . ? C18 C17 C16 120.5(3) . . ? C17 C18 C19 120.2(3) . . ? C18 C19 C20 120.2(3) . . ? C19 C20 C15 120.2(3) . . ? C1 N1 C2 109.7(2) . . ? C1 N1 C5 111.4(2) . . ? C2 N1 C5 108.48(19) . . ? C1 N1 Pd1 107.10(15) . . ? C2 N1 Pd1 109.14(15) . . ? C5 N1 Pd1 110.96(14) . . ? C4 O2 C3 117.5(2) . . ? C7 O4 C8 116.2(2) . . ? C9 P1 C15 108.72(12) . . ? C9 P1 C6 107.89(11) . . ? C15 P1 C6 105.32(12) . . ? C9 P1 Pd1 120.33(9) . . ? C15 P1 Pd1 113.18(9) . . ? C6 P1 Pd1 99.87(7) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 31.58 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.442 _refine_diff_density_min -0.704 _refine_diff_density_rms 0.101 # = = = = = end data_leung344 _database_code_depnum_ccdc_archive 'CCDC 857606' #TrackingRef '- leung381-344-475.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_absolute_configuration ad _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C41 H46 N2 O4 P Pd, C H2 Cl2 Cl O4' _chemical_formula_sum 'C42 H48 Cl3 N2 O8 P Pd' _chemical_formula_weight 952.54 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) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.2143(4) _cell_length_b 17.4999(6) _cell_length_c 11.5906(4) _cell_angle_alpha 90.00 _cell_angle_beta 111.861(2) _cell_angle_gamma 90.00 _cell_volume 2111.07(13) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7948 _cell_measurement_theta_min 3.04 _cell_measurement_theta_max 34.43 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.499 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 980 _exptl_absorpt_coefficient_mu 0.722 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7915 _exptl_absorpt_correction_T_max 0.8346 _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 50086 _diffrn_reflns_av_R_equivalents 0.0377 _diffrn_reflns_av_sigmaI/netI 0.0603 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 36.86 _reflns_number_total 20717 _reflns_number_gt 17450 _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^)+(0.0557P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.019(15) _refine_ls_number_reflns 20717 _refine_ls_number_parameters 525 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0584 _refine_ls_R_factor_gt 0.0415 _refine_ls_wR_factor_ref 0.1122 _refine_ls_wR_factor_gt 0.0918 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.084 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.582341(13) 0.750223(9) 0.923395(13) 0.01534(3) Uani 1 1 d . . . C1 C 0.4980(2) 0.68885(13) 0.7676(2) 0.0181(4) Uani 1 1 d . . . C2 C 0.5570(2) 0.63691(13) 0.7105(2) 0.0210(4) Uani 1 1 d . . . H2 H 0.6469 0.6282 0.7477 0.025 Uiso 1 1 calc R . . C3 C 0.4865(2) 0.59923(15) 0.6029(2) 0.0232(4) Uani 1 1 d . . . H3 H 0.5288 0.5659 0.5657 0.028 Uiso 1 1 calc R . . C4 C 0.3524(2) 0.60910(15) 0.5464(2) 0.0242(4) Uani 1 1 d . . . C5 C 0.2778(3) 0.56914(18) 0.4355(3) 0.0345(6) Uani 1 1 d . . . H5 H 0.3189 0.5347 0.3987 0.041 Uiso 1 1 calc R . . C6 C 0.1482(3) 0.5799(2) 0.3818(3) 0.0410(7) Uani 1 1 d . . . H6 H 0.0996 0.5528 0.3083 0.049 Uiso 1 1 calc R . . C7 C 0.0861(3) 0.6314(2) 0.4353(3) 0.0406(8) Uani 1 1 d . . . H7 H -0.0042 0.6386 0.3975 0.049 Uiso 1 1 calc R . . C8 C 0.1558(3) 0.67117(19) 0.5417(3) 0.0319(6) Uani 1 1 d . . . H8 H 0.1131 0.7063 0.5757 0.038 Uiso 1 1 calc R . . C9 C 0.2908(2) 0.66035(15) 0.6016(2) 0.0217(4) Uani 1 1 d . . . C10 C 0.3663(2) 0.69911(14) 0.7135(2) 0.0194(4) Uani 1 1 d . . . C11 C 0.30593(19) 0.75690(17) 0.7713(2) 0.0212(4) Uani 1 1 d . . . H11 H 0.2173 0.7393 0.7596 0.025 Uiso 1 1 calc R . . C12 C 0.2965(3) 0.83412(17) 0.7066(3) 0.0337(6) Uani 1 1 d . . . H12A H 0.2475 0.8698 0.7370 0.051 Uiso 1 1 calc R . . H12B H 0.2529 0.8275 0.6166 0.051 Uiso 1 1 calc R . . H12C H 0.3830 0.8545 0.7248 0.051 Uiso 1 1 calc R . . C13 C 0.3572(3) 0.68959(18) 0.9681(3) 0.0278(6) Uani 1 1 d . . . H13A H 0.4122 0.6889 1.0565 0.042 Uiso 1 1 calc R . . H13B H 0.3735 0.6438 0.9276 0.042 Uiso 1 1 calc R . . H13C H 0.2668 0.6904 0.9593 0.042 Uiso 1 1 calc R . . C14 C 0.3512(3) 0.82669(19) 0.9662(3) 0.0299(6) Uani 1 1 d . . . H14A H 0.2575 0.8301 0.9388 0.045 Uiso 1 1 calc R . . H14B H 0.3843 0.8730 0.9410 0.045 Uiso 1 1 calc R . . H14C H 0.3887 0.8218 1.0569 0.045 Uiso 1 1 calc R . . C15 C 0.6306(2) 0.81894(14) 1.1980(2) 0.0187(4) Uani 1 1 d D . . C16 C 0.5846(2) 0.88600(15) 1.2346(2) 0.0233(4) Uani 1 1 d . . . C17 C 0.5697(3) 0.96188(16) 1.1697(3) 0.0321(6) Uani 1 1 d . . . H17A H 0.5123 0.9562 1.0825 0.048 Uiso 1 1 calc RD . . H17B H 0.6540 0.9798 1.1736 0.048 Uiso 1 1 calc RD . . H17C H 0.5333 0.9991 1.2106 0.048 Uiso 1 1 calc R . . C18 C 0.5415(3) 0.88094(16) 1.3328(2) 0.0258(5) Uani 1 1 d . . . H18 H 0.5116 0.9260 1.3591 0.031 Uiso 1 1 calc R . . C19 C 0.5406(3) 0.81275(18) 1.3935(2) 0.0278(5) Uani 1 1 d . . . C20 C 0.4950(3) 0.8088(2) 1.5007(3) 0.0362(6) Uani 1 1 d . . . H20A H 0.5212 0.8552 1.5511 0.054 Uiso 1 1 calc R . . H20B H 0.5331 0.7641 1.5522 0.054 Uiso 1 1 calc R . . H20C H 0.4012 0.8044 1.4684 0.054 Uiso 1 1 calc R . . C21 C 0.5834(2) 0.7470(2) 1.3530(2) 0.0255(4) Uani 1 1 d . . . H21 H 0.5807 0.6996 1.3918 0.031 Uiso 1 1 calc R . . C22 C 0.63016(18) 0.74904(19) 1.25691(18) 0.0213(3) Uani 1 1 d . . . C23 C 0.6751(3) 0.67484(15) 1.2221(3) 0.0267(5) Uani 1 1 d . . . H23A H 0.6567 0.6743 1.1325 0.040 Uiso 1 1 calc R . . H23B H 0.6300 0.6324 1.2432 0.040 Uiso 1 1 calc R . . H23C H 0.7678 0.6694 1.2678 0.040 Uiso 1 1 calc R . . C24 C 0.8232(2) 0.81243(13) 1.1476(2) 0.0188(4) Uani 1 1 d D . . H24 H 0.8459 0.7628 1.1935 0.023 Uiso 1 1 calc R . . C25 C 0.8854(2) 0.87779(16) 1.2390(2) 0.0255(5) Uani 1 1 d . . . C26 C 0.8916(4) 1.0126(2) 1.2602(4) 0.0542(10) Uani 1 1 d . . . H26A H 0.8667 1.0066 1.3322 0.081 Uiso 1 1 calc R . . H26B H 0.8486 1.0576 1.2123 0.081 Uiso 1 1 calc R . . H26C H 0.9849 1.0193 1.2887 0.081 Uiso 1 1 calc R . . C27 C 0.8722(2) 0.81103(13) 1.0407(2) 0.0177(4) Uani 1 1 d . . . H27 H 0.8513 0.8619 0.9985 0.021 Uiso 1 1 calc R . . C28 C 1.0162(2) 0.79988(14) 1.0802(2) 0.0211(4) Uani 1 1 d . . . C29 C 1.2038(2) 0.7497(3) 1.2343(3) 0.0402(6) Uani 1 1 d . . . H29A H 1.2200 0.7099 1.1825 0.060 Uiso 1 1 calc R . . H29B H 1.2337 0.7322 1.3208 0.060 Uiso 1 1 calc R . . H29C H 1.2501 0.7963 1.2293 0.060 Uiso 1 1 calc R . . C30 C 0.8548(2) 0.64529(13) 0.9774(2) 0.0212(4) Uani 1 1 d . . . C31 C 0.7821(3) 0.58768(14) 1.0027(3) 0.0264(5) Uani 1 1 d . . . H31 H 0.6954 0.5973 0.9925 0.032 Uiso 1 1 calc R . . C32 C 0.8359(3) 0.51633(16) 1.0427(3) 0.0384(7) Uani 1 1 d . . . H32 H 0.7857 0.4775 1.0601 0.046 Uiso 1 1 calc R . . C33 C 0.9605(4) 0.50148(18) 1.0573(3) 0.0415(8) Uani 1 1 d . . . H33 H 0.9964 0.4525 1.0852 0.050 Uiso 1 1 calc R . . C34 C 1.0344(3) 0.55730(18) 1.0319(3) 0.0374(7) Uani 1 1 d . . . H34 H 1.1208 0.5466 1.0423 0.045 Uiso 1 1 calc R . . C35 C 0.9826(2) 0.62931(16) 0.9909(3) 0.0274(5) Uani 1 1 d . . . H35 H 1.0331 0.6674 0.9723 0.033 Uiso 1 1 calc R . . C36 C 0.8168(2) 0.76225(13) 0.7884(2) 0.0194(4) Uani 1 1 d . . . C37 C 0.8553(2) 0.70684(16) 0.7225(2) 0.0267(5) Uani 1 1 d . . . H37 H 0.8635 0.6550 0.7485 0.032 Uiso 1 1 calc R . . C38 C 0.8815(3) 0.72802(19) 0.6186(3) 0.0348(6) Uani 1 1 d . . . H38 H 0.9067 0.6903 0.5733 0.042 Uiso 1 1 calc R . . C39 C 0.8712(3) 0.8036(2) 0.5807(3) 0.0428(8) Uani 1 1 d . . . H39 H 0.8919 0.8179 0.5113 0.051 Uiso 1 1 calc R . . C40 C 0.8307(3) 0.8577(2) 0.6442(3) 0.0389(7) Uani 1 1 d . . . H40 H 0.8224 0.9094 0.6174 0.047 Uiso 1 1 calc R . . C41 C 0.8019(3) 0.83788(16) 0.7466(3) 0.0281(5) Uani 1 1 d . . . H41 H 0.7720 0.8756 0.7883 0.034 Uiso 1 1 calc R . . C42 C 0.2367(4) 0.9583(2) 0.4454(4) 0.0588(11) Uani 1 1 d . . . H42A H 0.1728 0.9206 0.4499 0.071 Uiso 1 1 calc R . . H42B H 0.3234 0.9378 0.4935 0.071 Uiso 1 1 calc R . . Cl1 Cl 0.21953(11) 0.97039(7) 0.28887(12) 0.0621(3) Uani 1 1 d . . . Cl2 Cl 0.21577(17) 1.04310(10) 0.51112(14) 0.0975(6) Uani 1 1 d . . . Cl3 Cl 0.43264(6) 0.49482(4) 0.17767(6) 0.02798(12) Uani 1 1 d . . . N1 N 0.38604(17) 0.75902(14) 0.90870(17) 0.0200(4) Uani 1 1 d . . . N2 N 0.67969(18) 0.82095(11) 1.09666(18) 0.0176(3) Uani 1 1 d D . . H2A H 0.667(2) 0.8666(12) 1.065(3) 0.026 Uiso 1 1 d D . . O1 O 0.8540(2) 0.94522(12) 1.1823(2) 0.0370(5) Uani 1 1 d . . . O2 O 0.9513(2) 0.86840(14) 1.34659(19) 0.0394(5) Uani 1 1 d . . . O3 O 1.06719(16) 0.76555(11) 1.19039(17) 0.0286(4) Uani 1 1 d . . . O4 O 1.07528(18) 0.81810(13) 1.0170(2) 0.0316(4) Uani 1 1 d . . . O5 O 0.3722(3) 0.56728(15) 0.1675(3) 0.0622(8) Uani 1 1 d . . . O6 O 0.3442(3) 0.4412(2) 0.0967(3) 0.0681(10) Uani 1 1 d . . . O7 O 0.5433(2) 0.50030(17) 0.1451(3) 0.0489(6) Uani 1 1 d . . . O8 O 0.4677(3) 0.46935(18) 0.3032(2) 0.0550(7) Uani 1 1 d . . . P1 P 0.78071(5) 0.73767(3) 0.92398(5) 0.01635(11) 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 0.01446(5) 0.01667(6) 0.01734(6) -0.00090(7) 0.00874(4) 0.00026(7) C1 0.0176(9) 0.0193(9) 0.0205(9) -0.0010(7) 0.0107(7) -0.0016(7) C2 0.0199(9) 0.0217(10) 0.0233(10) -0.0005(8) 0.0101(8) 0.0005(8) C3 0.0252(11) 0.0243(10) 0.0231(11) -0.0023(8) 0.0124(9) 0.0006(8) C4 0.0255(11) 0.0271(11) 0.0197(10) -0.0021(8) 0.0081(9) -0.0014(9) C5 0.0398(15) 0.0377(15) 0.0234(12) -0.0113(11) 0.0088(11) -0.0069(12) C6 0.0358(15) 0.054(2) 0.0265(14) -0.0127(13) 0.0033(11) -0.0069(14) C7 0.0251(13) 0.060(2) 0.0294(15) -0.0075(13) 0.0017(11) -0.0016(12) C8 0.0222(11) 0.0451(16) 0.0263(12) -0.0068(11) 0.0067(9) -0.0005(11) C9 0.0180(9) 0.0294(11) 0.0184(10) -0.0015(8) 0.0075(8) -0.0019(8) C10 0.0179(9) 0.0232(10) 0.0189(9) -0.0002(8) 0.0091(7) -0.0003(8) C11 0.0160(7) 0.0278(12) 0.0211(8) -0.0006(10) 0.0083(6) 0.0021(9) C12 0.0406(15) 0.0302(13) 0.0327(14) 0.0065(11) 0.0163(12) 0.0111(11) C13 0.0225(12) 0.0367(14) 0.0277(13) 0.0021(11) 0.0133(10) -0.0054(10) C14 0.0234(12) 0.0372(15) 0.0337(15) -0.0089(12) 0.0160(11) 0.0051(11) C15 0.0188(10) 0.0220(10) 0.0169(9) -0.0019(8) 0.0086(8) -0.0009(8) C16 0.0259(11) 0.0250(11) 0.0221(10) -0.0022(8) 0.0125(9) 0.0005(8) C17 0.0446(16) 0.0218(11) 0.0371(15) -0.0004(10) 0.0236(13) 0.0041(11) C18 0.0274(11) 0.0316(12) 0.0234(11) -0.0061(9) 0.0154(9) 0.0003(9) C19 0.0237(11) 0.0425(15) 0.0203(10) -0.0033(10) 0.0118(9) -0.0042(10) C20 0.0398(15) 0.0506(17) 0.0263(12) -0.0042(12) 0.0215(11) -0.0048(13) C21 0.0247(9) 0.0322(11) 0.0218(8) 0.0016(12) 0.0111(7) -0.0045(13) C22 0.0202(7) 0.0242(8) 0.0201(8) 0.0004(12) 0.0080(6) -0.0033(12) C23 0.0325(13) 0.0215(11) 0.0297(13) 0.0037(9) 0.0157(11) 0.0027(10) C24 0.0193(9) 0.0218(10) 0.0175(9) -0.0012(7) 0.0095(7) -0.0010(7) C25 0.0235(11) 0.0326(12) 0.0233(11) -0.0075(9) 0.0123(9) -0.0072(9) C26 0.051(2) 0.0300(16) 0.072(3) -0.0253(16) 0.0119(18) -0.0060(14) C27 0.0183(9) 0.0168(9) 0.0219(10) -0.0001(7) 0.0118(8) -0.0015(7) C28 0.0189(9) 0.0208(10) 0.0251(11) -0.0033(8) 0.0098(8) -0.0031(7) C29 0.0211(9) 0.0548(16) 0.0382(13) 0.0035(19) 0.0037(9) 0.0029(18) C30 0.0213(10) 0.0186(9) 0.0234(10) -0.0012(8) 0.0079(8) 0.0025(7) C31 0.0298(12) 0.0171(10) 0.0307(13) 0.0001(9) 0.0096(10) -0.0008(8) C32 0.0502(18) 0.0191(11) 0.0417(16) 0.0015(11) 0.0122(14) -0.0011(11) C33 0.0546(19) 0.0249(13) 0.0324(15) -0.0010(11) 0.0018(13) 0.0154(13) C34 0.0317(14) 0.0341(14) 0.0366(15) -0.0067(12) 0.0013(11) 0.0148(11) C35 0.0203(10) 0.0286(12) 0.0306(13) -0.0050(10) 0.0064(9) 0.0062(9) C36 0.0167(8) 0.0248(13) 0.0180(8) -0.0010(7) 0.0082(6) -0.0008(7) C37 0.0251(11) 0.0335(13) 0.0271(12) -0.0033(10) 0.0162(9) 0.0009(9) C38 0.0338(13) 0.0498(18) 0.0293(13) -0.0071(11) 0.0215(11) -0.0026(11) C39 0.0406(17) 0.067(2) 0.0257(14) 0.0026(14) 0.0180(12) -0.0117(16) C40 0.0466(17) 0.0408(16) 0.0320(15) 0.0112(12) 0.0178(13) -0.0006(13) C41 0.0320(13) 0.0293(12) 0.0244(12) 0.0038(9) 0.0120(10) 0.0020(10) C42 0.051(2) 0.043(2) 0.067(3) 0.0071(18) 0.004(2) 0.0033(17) Cl1 0.0524(5) 0.0631(6) 0.0735(7) 0.0056(5) 0.0266(5) -0.0020(5) Cl2 0.1050(11) 0.0905(10) 0.0662(8) -0.0273(7) -0.0037(7) 0.0250(9) Cl3 0.0330(3) 0.0225(2) 0.0286(3) -0.0034(2) 0.0117(2) -0.0045(2) N1 0.0166(7) 0.0263(12) 0.0211(7) -0.0015(8) 0.0117(6) -0.0005(8) N2 0.0189(8) 0.0180(8) 0.0180(8) -0.0008(6) 0.0092(7) -0.0003(6) O1 0.0421(12) 0.0245(9) 0.0379(12) -0.0090(8) 0.0073(9) -0.0040(8) O2 0.0412(12) 0.0532(14) 0.0208(9) -0.0046(9) 0.0080(8) -0.0120(10) O3 0.0182(7) 0.0403(13) 0.0262(8) 0.0052(7) 0.0072(6) 0.0015(7) O4 0.0211(8) 0.0425(11) 0.0363(10) 0.0036(9) 0.0166(8) -0.0034(8) O5 0.0691(19) 0.0381(14) 0.095(2) 0.0230(15) 0.0481(18) 0.0177(13) O6 0.092(2) 0.077(2) 0.0491(15) -0.0351(15) 0.0418(16) -0.0589(18) O7 0.0443(13) 0.0517(15) 0.0607(16) -0.0135(13) 0.0309(12) -0.0091(12) O8 0.0637(18) 0.0710(19) 0.0298(12) 0.0100(12) 0.0169(12) 0.0218(15) P1 0.01476(19) 0.0176(3) 0.0186(2) -0.00111(18) 0.00845(17) 0.00065(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C1 2.009(2) . ? Pd1 N1 2.1493(17) . ? Pd1 P1 2.2329(5) . ? Pd1 N2 2.2637(19) . ? C1 C10 1.385(3) . ? C1 C2 1.424(3) . ? C2 C3 1.372(3) . ? C3 C4 1.410(4) . ? C4 C9 1.421(4) . ? C4 C5 1.428(4) . ? C5 C6 1.365(5) . ? C6 C7 1.415(5) . ? C7 C8 1.379(4) . ? C8 C9 1.424(3) . ? C9 C10 1.429(3) . ? C10 C11 1.505(3) . ? C11 N1 1.510(3) . ? C11 C12 1.530(4) . ? C13 N1 1.490(4) . ? C14 N1 1.481(4) . ? C15 C22 1.402(4) . ? C15 C16 1.409(3) . ? C15 N2 1.472(3) . ? C16 C18 1.395(4) . ? C16 C17 1.505(4) . ? C18 C19 1.387(4) . ? C19 C21 1.393(4) . ? C19 C20 1.512(4) . ? C21 C22 1.398(3) . ? C22 C23 1.501(4) . ? C24 N2 1.501(3) . ? C24 C27 1.532(3) . ? C24 C25 1.538(3) . ? C25 O2 1.201(3) . ? C25 O1 1.332(4) . ? C26 O1 1.449(4) . ? C27 C28 1.518(3) . ? C27 P1 1.870(2) . ? C28 O4 1.200(3) . ? C28 O3 1.332(3) . ? C29 O3 1.450(3) . ? C30 C31 1.394(4) . ? C30 C35 1.411(3) . ? C30 P1 1.818(2) . ? C31 C32 1.389(4) . ? C32 C33 1.368(5) . ? C33 C34 1.382(5) . ? C34 C35 1.395(4) . ? C36 C41 1.398(4) . ? C36 C37 1.398(3) . ? C36 P1 1.815(2) . ? C37 C38 1.392(4) . ? C38 C39 1.384(5) . ? C39 C40 1.376(5) . ? C40 C41 1.386(4) . ? C42 Cl2 1.723(5) . ? C42 Cl1 1.765(5) . ? Cl3 O5 1.422(3) . ? Cl3 O7 1.429(3) . ? Cl3 O8 1.429(3) . ? Cl3 O6 1.433(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 C1 Pd1 N1 80.88(8) . . ? C1 Pd1 P1 94.90(6) . . ? N1 Pd1 P1 175.67(5) . . ? C1 Pd1 N2 178.71(9) . . ? N1 Pd1 N2 99.93(7) . . ? P1 Pd1 N2 84.28(5) . . ? C10 C1 C2 118.3(2) . . ? C10 C1 Pd1 113.80(16) . . ? C2 C1 Pd1 127.89(17) . . ? C3 C2 C1 121.3(2) . . ? C2 C3 C4 121.2(2) . . ? C3 C4 C9 118.8(2) . . ? C3 C4 C5 121.6(2) . . ? C9 C4 C5 119.6(2) . . ? C6 C5 C4 120.6(3) . . ? C5 C6 C7 120.2(3) . . ? C8 C7 C6 120.4(3) . . ? C7 C8 C9 121.0(3) . . ? C4 C9 C8 118.1(2) . . ? C4 C9 C10 119.1(2) . . ? C8 C9 C10 122.8(2) . . ? C1 C10 C9 121.4(2) . . ? C1 C10 C11 117.8(2) . . ? C9 C10 C11 120.7(2) . . ? C10 C11 N1 107.23(18) . . ? C10 C11 C12 109.7(2) . . ? N1 C11 C12 113.6(2) . . ? C22 C15 C16 120.8(2) . . ? C22 C15 N2 118.7(2) . . ? C16 C15 N2 120.5(2) . . ? C18 C16 C15 118.0(2) . . ? C18 C16 C17 117.2(2) . . ? C15 C16 C17 124.7(2) . . ? C19 C18 C16 122.6(2) . . ? C18 C19 C21 118.1(2) . . ? C18 C19 C20 121.7(3) . . ? C21 C19 C20 120.2(3) . . ? C19 C21 C22 121.7(3) . . ? C21 C22 C15 118.7(3) . . ? C21 C22 C23 117.1(3) . . ? C15 C22 C23 124.16(19) . . ? N2 C24 C27 109.77(17) . . ? N2 C24 C25 110.00(19) . . ? C27 C24 C25 111.20(19) . . ? O2 C25 O1 125.5(3) . . ? O2 C25 C24 124.0(3) . . ? O1 C25 C24 110.5(2) . . ? C28 C27 C24 114.80(19) . . ? C28 C27 P1 111.45(15) . . ? C24 C27 P1 109.31(15) . . ? O4 C28 O3 124.5(2) . . ? O4 C28 C27 123.3(2) . . ? O3 C28 C27 112.1(2) . . ? C31 C30 C35 118.8(2) . . ? C31 C30 P1 119.08(18) . . ? C35 C30 P1 122.1(2) . . ? C32 C31 C30 120.4(3) . . ? C33 C32 C31 120.5(3) . . ? C32 C33 C34 120.3(3) . . ? C33 C34 C35 120.3(3) . . ? C34 C35 C30 119.6(3) . . ? C41 C36 C37 119.3(2) . . ? C41 C36 P1 119.19(18) . . ? C37 C36 P1 121.50(18) . . ? C38 C37 C36 119.7(3) . . ? C39 C38 C37 120.6(3) . . ? C40 C39 C38 119.5(3) . . ? C39 C40 C41 121.0(3) . . ? C40 C41 C36 119.8(3) . . ? Cl2 C42 Cl1 111.7(2) . . ? O5 Cl3 O7 110.65(17) . . ? O5 Cl3 O8 107.72(19) . . ? O7 Cl3 O8 110.64(18) . . ? O5 Cl3 O6 109.8(2) . . ? O7 Cl3 O6 109.17(17) . . ? O8 Cl3 O6 108.86(19) . . ? C14 N1 C13 107.74(19) . . ? C14 N1 C11 110.0(2) . . ? C13 N1 C11 108.7(2) . . ? C14 N1 Pd1 117.12(17) . . ? C13 N1 Pd1 107.30(16) . . ? C11 N1 Pd1 105.74(12) . . ? C15 N2 C24 110.37(17) . . ? C15 N2 Pd1 119.68(14) . . ? C24 N2 Pd1 112.77(13) . . ? C25 O1 C26 116.9(3) . . ? C28 O3 C29 116.3(2) . . ? C36 P1 C30 106.53(11) . . ? C36 P1 C27 102.97(10) . . ? C30 P1 C27 107.84(11) . . ? C36 P1 Pd1 121.16(7) . . ? C30 P1 Pd1 114.64(8) . . ? C27 P1 Pd1 102.26(7) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 36.86 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.569 _refine_diff_density_min -1.050 _refine_diff_density_rms 0.253 # = = = = = end data_leung475 _database_code_depnum_ccdc_archive 'CCDC 857607' #TrackingRef '- leung381-344-475.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_absolute_configuration ad _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H26 Cl2 N O4 P Pd' _chemical_formula_sum 'C25 H26 Cl2 N O4 P Pd' _chemical_formula_weight 612.74 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' 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' O O 0.0106 0.0060 '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) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.5919(14) _cell_length_b 20.528(3) _cell_length_c 12.6956(16) _cell_angle_alpha 90.00 _cell_angle_beta 109.676(8) _cell_angle_gamma 90.00 _cell_volume 2599.2(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8919 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 32.90 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.566 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1240 _exptl_absorpt_coefficient_mu 1.013 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7510 _exptl_absorpt_correction_T_max 0.8387 _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 65855 _diffrn_reflns_av_R_equivalents 0.0396 _diffrn_reflns_av_sigmaI/netI 0.0406 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 33.30 _reflns_number_total 19720 _reflns_number_gt 17544 _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^)+(0.0432P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.018(12) _refine_ls_number_reflns 19720 _refine_ls_number_parameters 625 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0377 _refine_ls_R_factor_gt 0.0287 _refine_ls_wR_factor_ref 0.0811 _refine_ls_wR_factor_gt 0.0701 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.089 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.597929(17) 0.765121(8) 1.084913(13) 0.02077(4) Uani 1 1 d D . . Pd2 Pd 0.933183(18) 0.735231(8) 0.417093(14) 0.02167(4) Uani 1 1 d D . . C1 C 0.8420(2) 0.72817(12) 1.02568(19) 0.0233(4) Uani 1 1 d . . . C2 C 0.9711(3) 0.70981(13) 1.0903(2) 0.0275(5) Uani 1 1 d . . . H2 H 1.0194 0.7340 1.1551 0.033 Uiso 1 1 calc R . . C3 C 1.0288(3) 0.65540(14) 1.0590(2) 0.0323(5) Uani 1 1 d . . . H3 H 1.1173 0.6428 1.1027 0.039 Uiso 1 1 calc R . . C4 C 0.9581(3) 0.61903(13) 0.9638(2) 0.0310(5) Uani 1 1 d . . . C5 C 1.0179(4) 0.55748(15) 0.9354(3) 0.0425(7) Uani 1 1 d . . . H5A H 1.0009 0.5210 0.9786 0.064 Uiso 1 1 calc R . . H5B H 1.1148 0.5632 0.9538 0.064 Uiso 1 1 calc R . . H5C H 0.9769 0.5483 0.8553 0.064 Uiso 1 1 calc R . . C6 C 0.8305(3) 0.64006(14) 0.8992(2) 0.0338(6) Uani 1 1 d . . . H6 H 0.7824 0.6169 0.8330 0.041 Uiso 1 1 calc R . . C7 C 0.7725(3) 0.69388(13) 0.9293(2) 0.0303(5) Uani 1 1 d . . . H7 H 0.6852 0.7075 0.8842 0.036 Uiso 1 1 calc R . . C8 C 0.7691(2) 0.84070(11) 0.98166(19) 0.0220(4) Uani 1 1 d . . . H8 H 0.7117 0.8281 0.9042 0.026 Uiso 1 1 calc R . . C9 C 0.9095(2) 0.85799(12) 0.9813(2) 0.0256(4) Uani 1 1 d . . . C10 C 1.0658(3) 0.8403(2) 0.8885(3) 0.0484(8) Uani 1 1 d . . . H10A H 1.0872 0.8867 0.8865 0.073 Uiso 1 1 calc R . . H10B H 1.0718 0.8187 0.8215 0.073 Uiso 1 1 calc R . . H10C H 1.1295 0.8202 0.9553 0.073 Uiso 1 1 calc R . . C11 C 0.7033(2) 0.89775(11) 1.0210(2) 0.0237(4) Uani 1 1 d . . . H11 H 0.7630 0.9114 1.0971 0.028 Uiso 1 1 calc R . . C12 C 0.6881(3) 0.95413(13) 0.9417(2) 0.0287(5) Uani 1 1 d . . . C13 C 0.6017(4) 1.05988(16) 0.8920(4) 0.0523(9) Uani 1 1 d . . . H13A H 0.6839 1.0734 0.8789 0.078 Uiso 1 1 calc R . . H13B H 0.5659 1.0966 0.9226 0.078 Uiso 1 1 calc R . . H13C H 0.5352 1.0459 0.8211 0.078 Uiso 1 1 calc R . . C14 C 0.4195(3) 0.87572(13) 0.8944(2) 0.0271(5) Uani 1 1 d . . . C15 C 0.3898(3) 0.82213(14) 0.8244(2) 0.0343(6) Uani 1 1 d . . . H15 H 0.4329 0.7817 0.8501 0.041 Uiso 1 1 calc R . . C16 C 0.2972(3) 0.82680(17) 0.7165(2) 0.0436(7) Uani 1 1 d . . . H16 H 0.2785 0.7900 0.6683 0.052 Uiso 1 1 calc R . . C17 C 0.2333(3) 0.88468(19) 0.6804(3) 0.0445(8) Uani 1 1 d . . . H17 H 0.1688 0.8877 0.6074 0.053 Uiso 1 1 calc R . . C18 C 0.2619(3) 0.93910(17) 0.7493(3) 0.0402(7) Uani 1 1 d . . . H18 H 0.2180 0.9792 0.7227 0.048 Uiso 1 1 calc R . . C19 C 0.3544(3) 0.93508(14) 0.8569(2) 0.0328(5) Uani 1 1 d . . . H19 H 0.3733 0.9721 0.9045 0.039 Uiso 1 1 calc R . . C20 C 0.4947(3) 0.91861(12) 1.1265(2) 0.0263(5) Uani 1 1 d . . . C21 C 0.5879(3) 0.94993(13) 1.2174(2) 0.0322(5) Uani 1 1 d . . . H21 H 0.6811 0.9468 1.2288 0.039 Uiso 1 1 calc R . . C22 C 0.5435(3) 0.98537(16) 1.2904(3) 0.0403(7) Uani 1 1 d . . . H22 H 0.6071 1.0068 1.3519 0.048 Uiso 1 1 calc R . . C23 C 0.4106(3) 0.99041(16) 1.2764(3) 0.0413(7) Uani 1 1 d . . . H23 H 0.3815 1.0156 1.3267 0.050 Uiso 1 1 calc R . . C24 C 0.3193(4) 0.9584(2) 1.1885(3) 0.0510(9) Uani 1 1 d . . . H24 H 0.2265 0.9612 1.1787 0.061 Uiso 1 1 calc R . . C25 C 0.3603(3) 0.92234(18) 1.1141(3) 0.0417(7) Uani 1 1 d . . . H25 H 0.2959 0.9000 1.0542 0.050 Uiso 1 1 calc R . . C26 C 0.6806(2) 0.75932(12) 0.46399(18) 0.0230(4) Uani 1 1 d . . . C27 C 0.5617(3) 0.78874(14) 0.4015(2) 0.0340(6) Uani 1 1 d . . . H27 H 0.5163 0.7750 0.3269 0.041 Uiso 1 1 calc R . . C28 C 0.5088(3) 0.83845(16) 0.4481(3) 0.0385(6) Uani 1 1 d . . . H28 H 0.4271 0.8586 0.4046 0.046 Uiso 1 1 calc R . . C29 C 0.5727(3) 0.85914(14) 0.5565(3) 0.0329(5) Uani 1 1 d . . . C30 C 0.5194(4) 0.91633(18) 0.6032(4) 0.0513(9) Uani 1 1 d . . . H30A H 0.5314 0.9082 0.6821 0.077 Uiso 1 1 calc R . . H30B H 0.4239 0.9221 0.5610 0.077 Uiso 1 1 calc R . . H30C H 0.5684 0.9558 0.5970 0.077 Uiso 1 1 calc R . . C31 C 0.6892(3) 0.82721(14) 0.6193(2) 0.0314(5) Uani 1 1 d . . . H31 H 0.7317 0.8393 0.6953 0.038 Uiso 1 1 calc R . . C32 C 0.7450(3) 0.77817(12) 0.5742(2) 0.0276(5) Uani 1 1 d . . . H32 H 0.8262 0.7577 0.6180 0.033 Uiso 1 1 calc R . . C33 C 0.7270(2) 0.64047(11) 0.44043(18) 0.0216(4) Uani 1 1 d . . . H33 H 0.7265 0.6132 0.3750 0.026 Uiso 1 1 calc R . . C34 C 0.5938(3) 0.62931(12) 0.4594(2) 0.0272(5) Uani 1 1 d . . . C35 C 0.3620(3) 0.6342(3) 0.3692(3) 0.0634(12) Uani 1 1 d . . . H35A H 0.3398 0.5897 0.3851 0.095 Uiso 1 1 calc R . . H35B H 0.2975 0.6487 0.2977 0.095 Uiso 1 1 calc R . . H35C H 0.3579 0.6633 0.4291 0.095 Uiso 1 1 calc R . . C36 C 0.8449(2) 0.61843(11) 0.54069(19) 0.0230(4) Uani 1 1 d . . . H36 H 0.8407 0.6402 0.6099 0.028 Uiso 1 1 calc R . . C37 C 0.8377(3) 0.54517(12) 0.5530(2) 0.0263(5) Uani 1 1 d . . . C38 C 0.9207(4) 0.45297(15) 0.6636(3) 0.0495(9) Uani 1 1 d . . . H38A H 0.8298 0.4365 0.6506 0.074 Uiso 1 1 calc R . . H38B H 0.9784 0.4412 0.7393 0.074 Uiso 1 1 calc R . . H38C H 0.9565 0.4337 0.6088 0.074 Uiso 1 1 calc R . . C39 C 1.0434(2) 0.57883(12) 0.43705(19) 0.0234(4) Uani 1 1 d . . . C40 C 1.0098(3) 0.58370(13) 0.3208(2) 0.0293(5) Uani 1 1 d . . . H40 H 0.9665 0.6216 0.2824 0.035 Uiso 1 1 calc R . . C41 C 1.0405(3) 0.53236(15) 0.2621(2) 0.0370(6) Uani 1 1 d . . . H41 H 1.0180 0.5353 0.1832 0.044 Uiso 1 1 calc R . . C42 C 1.1034(3) 0.47711(15) 0.3174(3) 0.0385(6) Uani 1 1 d . . . H42 H 1.1246 0.4426 0.2763 0.046 Uiso 1 1 calc R . . C43 C 1.1359(3) 0.47165(15) 0.4323(3) 0.0370(6) Uani 1 1 d . . . H43 H 1.1786 0.4335 0.4701 0.044 Uiso 1 1 calc R . . C44 C 1.1053(3) 0.52252(13) 0.4913(2) 0.0306(5) Uani 1 1 d . . . H44 H 1.1270 0.5189 0.5701 0.037 Uiso 1 1 calc R . . C45 C 1.1375(3) 0.64900(12) 0.6455(2) 0.0251(5) Uani 1 1 d . . . C46 C 1.1164(3) 0.66255(15) 0.7461(2) 0.0353(6) Uani 1 1 d . . . H46 H 1.0281 0.6688 0.7475 0.042 Uiso 1 1 calc R . . C47 C 1.2262(3) 0.66678(17) 0.8445(2) 0.0440(7) Uani 1 1 d . . . H47 H 1.2125 0.6765 0.9130 0.053 Uiso 1 1 calc R . . C48 C 1.3540(4) 0.65700(16) 0.8434(3) 0.0435(8) Uani 1 1 d . . . H48 H 1.4276 0.6581 0.9116 0.052 Uiso 1 1 calc R . . C49 C 1.3761(3) 0.64567(16) 0.7442(3) 0.0415(7) Uani 1 1 d . . . H49 H 1.4649 0.6404 0.7435 0.050 Uiso 1 1 calc R . . C50 C 1.2677(3) 0.64203(15) 0.6450(2) 0.0355(6) Uani 1 1 d . . . H50 H 1.2830 0.6347 0.5763 0.043 Uiso 1 1 calc R . . Cl1 Cl 0.67412(7) 0.66052(3) 1.15752(5) 0.02886(12) Uani 1 1 d . . . Cl2 Cl 0.39060(6) 0.75106(3) 1.10212(5) 0.03129(13) Uani 1 1 d . . . Cl3 Cl 0.84701(7) 0.83054(3) 0.31191(5) 0.02940(12) Uani 1 1 d . . . Cl4 Cl 1.14766(7) 0.75658(4) 0.42456(6) 0.03987(15) Uani 1 1 d . . . N1 N 0.7801(2) 0.78377(9) 1.05874(17) 0.0215(4) Uani 1 1 d D . . H1N H 0.822(2) 0.7941(17) 1.1212(17) 0.032 Uiso 1 1 d D . . N2 N 0.7393(2) 0.71089(9) 0.41022(17) 0.0221(4) Uani 1 1 d D . . H2N H 0.699(2) 0.7102(17) 0.3430(16) 0.033 Uiso 1 1 d D . . O1 O 0.9914(2) 0.88708(11) 1.0563(2) 0.0391(5) Uani 1 1 d . . . O2 O 0.93040(19) 0.83348(11) 0.89162(17) 0.0331(4) Uani 1 1 d . . . O3 O 0.7226(3) 0.95180(11) 0.8605(2) 0.0441(5) Uani 1 1 d . . . O4 O 0.6318(2) 1.00559(9) 0.9717(2) 0.0383(5) Uani 1 1 d . . . O5 O 0.5818(2) 0.61842(12) 0.54791(19) 0.0397(5) Uani 1 1 d . . . O6 O 0.4947(2) 0.63533(12) 0.36286(17) 0.0380(5) Uani 1 1 d . . . O7 O 0.7696(2) 0.51079(10) 0.47886(18) 0.0394(5) Uani 1 1 d . . . O8 O 0.9168(2) 0.52425(10) 0.65173(17) 0.0366(5) Uani 1 1 d . . . P1 P 0.54358(6) 0.86684(3) 1.03171(5) 0.02294(11) Uani 1 1 d . . . P2 P 1.00059(6) 0.64491(3) 0.51344(5) 0.02147(11) 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 0.02186(7) 0.02170(7) 0.01844(7) 0.00054(6) 0.00638(5) -0.00234(6) Pd2 0.02433(8) 0.01989(7) 0.02041(7) 0.00092(6) 0.00705(5) -0.00003(6) C1 0.0241(10) 0.0220(10) 0.0248(10) 0.0010(8) 0.0097(8) 0.0001(8) C2 0.0292(11) 0.0255(11) 0.0250(11) -0.0014(9) 0.0054(9) 0.0032(9) C3 0.0336(14) 0.0313(13) 0.0312(12) 0.0023(10) 0.0099(10) 0.0082(10) C4 0.0391(14) 0.0232(11) 0.0360(13) -0.0021(10) 0.0195(11) 0.0014(10) C5 0.0539(19) 0.0315(14) 0.0462(17) -0.0053(12) 0.0221(15) 0.0083(13) C6 0.0358(14) 0.0320(13) 0.0332(13) -0.0109(10) 0.0113(11) -0.0030(10) C7 0.0273(12) 0.0310(12) 0.0293(12) -0.0061(10) 0.0049(9) -0.0006(9) C8 0.0218(10) 0.0223(10) 0.0229(10) 0.0015(8) 0.0086(8) -0.0013(8) C9 0.0238(11) 0.0229(10) 0.0299(11) 0.0040(9) 0.0088(9) 0.0004(8) C10 0.0301(15) 0.068(2) 0.0530(19) -0.0017(17) 0.0219(14) -0.0018(15) C11 0.0225(10) 0.0216(10) 0.0275(11) 0.0013(8) 0.0090(8) -0.0013(8) C12 0.0263(12) 0.0226(11) 0.0366(13) 0.0049(10) 0.0098(10) -0.0010(9) C13 0.0486(19) 0.0291(15) 0.075(3) 0.0201(15) 0.0153(18) 0.0122(13) C14 0.0244(11) 0.0325(12) 0.0240(10) 0.0025(9) 0.0075(9) -0.0016(9) C15 0.0375(14) 0.0310(13) 0.0292(12) 0.0022(10) 0.0043(10) -0.0059(11) C16 0.0454(17) 0.0485(17) 0.0277(13) 0.0010(12) 0.0002(12) -0.0114(14) C17 0.0322(15) 0.066(2) 0.0288(13) 0.0119(13) 0.0015(11) -0.0052(14) C18 0.0325(14) 0.0487(16) 0.0383(15) 0.0151(13) 0.0104(11) 0.0083(12) C19 0.0272(12) 0.0361(14) 0.0346(13) 0.0032(11) 0.0096(10) 0.0037(10) C20 0.0253(11) 0.0254(11) 0.0296(12) -0.0033(9) 0.0109(9) 0.0001(8) C21 0.0302(13) 0.0308(12) 0.0334(13) -0.0054(10) 0.0078(10) 0.0003(10) C22 0.0422(16) 0.0395(15) 0.0388(15) -0.0149(12) 0.0131(12) -0.0042(13) C23 0.0477(18) 0.0379(15) 0.0429(16) -0.0117(12) 0.0212(13) 0.0050(13) C24 0.0344(16) 0.078(3) 0.0441(17) -0.0125(17) 0.0182(13) 0.0061(16) C25 0.0265(13) 0.060(2) 0.0390(15) -0.0165(14) 0.0118(11) -0.0031(13) C26 0.0262(10) 0.0202(10) 0.0222(9) 0.0017(8) 0.0075(7) 0.0015(8) C27 0.0331(13) 0.0359(13) 0.0270(12) -0.0019(10) 0.0024(10) 0.0095(11) C28 0.0319(14) 0.0390(15) 0.0409(15) -0.0006(12) 0.0076(11) 0.0131(11) C29 0.0340(14) 0.0288(13) 0.0404(14) -0.0059(11) 0.0186(11) 0.0009(10) C30 0.0504(19) 0.0457(18) 0.065(2) -0.0128(16) 0.0288(17) 0.0101(15) C31 0.0369(14) 0.0305(12) 0.0270(11) -0.0064(10) 0.0112(10) -0.0027(10) C32 0.0301(11) 0.0262(11) 0.0233(10) 0.0009(8) 0.0049(8) 0.0025(8) C33 0.0248(10) 0.0193(9) 0.0205(9) 0.0003(7) 0.0076(8) 0.0014(8) C34 0.0269(11) 0.0236(10) 0.0324(12) 0.0026(9) 0.0118(9) 0.0011(9) C35 0.0262(15) 0.108(4) 0.057(2) 0.000(2) 0.0152(15) 0.0054(18) C36 0.0274(11) 0.0205(10) 0.0219(10) 0.0026(8) 0.0092(8) 0.0027(8) C37 0.0295(12) 0.0235(11) 0.0282(12) 0.0034(9) 0.0128(9) 0.0038(9) C38 0.078(3) 0.0296(14) 0.0444(18) 0.0159(13) 0.0252(17) 0.0211(15) C39 0.0233(10) 0.0249(10) 0.0230(10) -0.0020(8) 0.0093(8) 0.0015(8) C40 0.0350(13) 0.0293(12) 0.0241(11) -0.0012(9) 0.0106(9) -0.0003(10) C41 0.0472(17) 0.0390(15) 0.0274(12) -0.0076(11) 0.0158(11) -0.0033(13) C42 0.0427(16) 0.0338(14) 0.0450(16) -0.0137(12) 0.0229(13) -0.0007(12) C43 0.0358(14) 0.0312(13) 0.0448(16) -0.0047(12) 0.0147(12) 0.0077(11) C44 0.0334(13) 0.0302(12) 0.0276(11) 0.0000(9) 0.0095(10) 0.0086(10) C45 0.0301(12) 0.0206(10) 0.0213(10) 0.0013(8) 0.0044(8) 0.0019(8) C46 0.0389(15) 0.0425(15) 0.0234(11) -0.0035(10) 0.0090(10) -0.0055(12) C47 0.0501(18) 0.0527(19) 0.0248(12) -0.0039(12) 0.0068(12) -0.0156(15) C48 0.0461(17) 0.0366(15) 0.0337(14) 0.0017(12) -0.0051(13) -0.0098(13) C49 0.0318(14) 0.0376(15) 0.0432(16) -0.0050(12) -0.0029(12) 0.0014(11) C50 0.0279(13) 0.0400(15) 0.0328(13) -0.0063(11) 0.0025(10) 0.0044(11) Cl1 0.0344(3) 0.0236(3) 0.0289(3) 0.0041(2) 0.0109(2) -0.0037(2) Cl2 0.0249(3) 0.0421(4) 0.0277(3) -0.0018(2) 0.0100(2) -0.0072(2) Cl3 0.0373(3) 0.0207(2) 0.0270(3) 0.0039(2) 0.0065(2) -0.0019(2) Cl4 0.0292(3) 0.0447(4) 0.0475(4) 0.0075(3) 0.0152(3) -0.0023(3) N1 0.0248(9) 0.0189(8) 0.0215(8) 0.0020(7) 0.0086(7) -0.0012(7) N2 0.0263(9) 0.0169(8) 0.0217(8) 0.0009(7) 0.0063(7) 0.0012(7) O1 0.0295(10) 0.0408(12) 0.0449(12) -0.0109(9) 0.0099(9) -0.0102(8) O2 0.0278(9) 0.0423(11) 0.0322(9) 0.0005(8) 0.0138(7) -0.0017(8) O3 0.0551(14) 0.0396(12) 0.0453(12) 0.0151(10) 0.0270(11) 0.0101(10) O4 0.0389(11) 0.0237(9) 0.0541(13) 0.0049(8) 0.0179(10) 0.0062(8) O5 0.0400(12) 0.0475(13) 0.0366(11) 0.0110(9) 0.0195(9) 0.0031(9) O6 0.0247(9) 0.0571(13) 0.0323(10) -0.0009(9) 0.0097(7) -0.0019(9) O7 0.0528(13) 0.0225(9) 0.0390(11) -0.0023(8) 0.0105(9) -0.0040(8) O8 0.0518(13) 0.0259(9) 0.0303(9) 0.0072(7) 0.0115(9) 0.0125(9) P1 0.0220(3) 0.0236(3) 0.0238(3) 0.0001(2) 0.0085(2) -0.0003(2) P2 0.0230(3) 0.0215(3) 0.0196(2) 0.0011(2) 0.0067(2) 0.0030(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 Pd1 N1 2.100(2) . ? Pd1 P1 2.2103(7) . ? Pd1 Cl2 2.2971(7) . ? Pd1 Cl1 2.3686(7) . ? Pd2 N2 2.087(2) . ? Pd2 P2 2.2034(6) . ? Pd2 Cl4 2.2840(8) . ? Pd2 Cl3 2.3714(7) . ? C1 C2 1.389(3) . ? C1 C7 1.389(3) . ? C1 N1 1.447(3) . ? C2 C3 1.394(4) . ? C2 H2 0.9500 . ? C3 C4 1.403(4) . ? C3 H3 0.9500 . ? C4 C6 1.393(4) . ? C4 C5 1.511(4) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.379(4) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 N1 1.503(3) . ? C8 C11 1.530(3) . ? C8 C9 1.531(3) . ? C8 H8 1.0000 . ? C9 O1 1.208(3) . ? C9 O2 1.330(3) . ? C10 O2 1.455(4) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.507(4) . ? C11 P1 1.854(2) . ? C11 H11 1.0000 . ? C12 O3 1.204(4) . ? C12 O4 1.331(3) . ? C13 O4 1.467(4) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.382(4) . ? C14 C19 1.402(4) . ? C14 P1 1.805(3) . ? C15 C16 1.395(4) . ? C15 H15 0.9500 . ? C16 C17 1.367(5) . ? C16 H16 0.9500 . ? C17 C18 1.388(5) . ? C17 H17 0.9500 . ? C18 C19 1.390(4) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C25 1.381(4) . ? C20 C21 1.397(4) . ? C20 P1 1.807(3) . ? C21 C22 1.379(4) . ? C21 H21 0.9500 . ? C22 C23 1.363(5) . ? C22 H22 0.9500 . ? C23 C24 1.373(5) . ? C23 H23 0.9500 . ? C24 C25 1.381(5) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C27 1.381(3) . ? C26 C32 1.389(3) . ? C26 N2 1.458(3) . ? C27 C28 1.388(4) . ? C27 H27 0.9500 . ? C28 C29 1.380(4) . ? C28 H28 0.9500 . ? C29 C31 1.387(4) . ? C29 C30 1.509(4) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.385(4) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 N2 1.512(3) . ? C33 C36 1.521(3) . ? C33 C34 1.526(4) . ? C33 H33 1.0000 . ? C34 O5 1.194(3) . ? C34 O6 1.324(3) . ? C35 O6 1.435(4) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 C37 1.517(3) . ? C36 P2 1.876(3) . ? C36 H36 1.0000 . ? C37 O7 1.203(3) . ? C37 O8 1.323(3) . ? C38 O8 1.470(4) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C44 1.392(3) . ? C39 C40 1.401(3) . ? C39 P2 1.812(2) . ? C40 C41 1.391(4) . ? C40 H40 0.9500 . ? C41 C42 1.382(5) . ? C41 H41 0.9500 . ? C42 C43 1.386(5) . ? C42 H42 0.9500 . ? C43 C44 1.386(4) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 C50 1.389(4) . ? C45 C46 1.397(4) . ? C45 P2 1.812(2) . ? C46 C47 1.393(4) . ? C46 H46 0.9500 . ? C47 C48 1.373(5) . ? C47 H47 0.9500 . ? C48 C49 1.376(5) . ? C48 H48 0.9500 . ? C49 C50 1.392(4) . ? C49 H49 0.9500 . ? C50 H50 0.9500 . ? N1 H1N 0.794(17) . ? N2 H2N 0.817(17) . ? 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 N1 Pd1 P1 86.45(6) . . ? N1 Pd1 Cl2 175.21(6) . . ? P1 Pd1 Cl2 89.36(2) . . ? N1 Pd1 Cl1 90.92(6) . . ? P1 Pd1 Cl1 174.16(2) . . ? Cl2 Pd1 Cl1 93.47(2) . . ? N2 Pd2 P2 87.26(6) . . ? N2 Pd2 Cl4 177.21(6) . . ? P2 Pd2 Cl4 90.38(3) . . ? N2 Pd2 Cl3 89.27(6) . . ? P2 Pd2 Cl3 176.51(3) . . ? Cl4 Pd2 Cl3 93.09(3) . . ? C2 C1 C7 120.5(2) . . ? C2 C1 N1 119.7(2) . . ? C7 C1 N1 119.8(2) . . ? C1 C2 C3 119.2(2) . . ? C1 C2 H2 120.4 . . ? C3 C2 H2 120.4 . . ? C2 C3 C4 120.9(3) . . ? C2 C3 H3 119.6 . . ? C4 C3 H3 119.6 . . ? C6 C4 C3 118.3(2) . . ? C6 C4 C5 121.3(3) . . ? C3 C4 C5 120.4(3) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 C4 121.3(2) . . ? C7 C6 H6 119.4 . . ? C4 C6 H6 119.4 . . ? C6 C7 C1 119.8(2) . . ? C6 C7 H7 120.1 . . ? C1 C7 H7 120.1 . . ? N1 C8 C11 109.07(19) . . ? N1 C8 C9 108.64(18) . . ? C11 C8 C9 111.90(19) . . ? N1 C8 H8 109.1 . . ? C11 C8 H8 109.1 . . ? C9 C8 H8 109.1 . . ? O1 C9 O2 125.4(2) . . ? O1 C9 C8 123.6(2) . . ? O2 C9 C8 110.9(2) . . ? O2 C10 H10A 109.5 . . ? O2 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? O2 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C8 109.1(2) . . ? C12 C11 P1 114.65(17) . . ? C8 C11 P1 106.79(16) . . ? C12 C11 H11 108.7 . . ? C8 C11 H11 108.7 . . ? P1 C11 H11 108.7 . . ? O3 C12 O4 124.8(3) . . ? O3 C12 C11 123.1(3) . . ? O4 C12 C11 112.0(2) . . ? O4 C13 H13A 109.5 . . ? O4 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? O4 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 C19 119.6(2) . . ? C15 C14 P1 118.3(2) . . ? C19 C14 P1 122.1(2) . . ? C14 C15 C16 120.6(3) . . ? C14 C15 H15 119.7 . . ? C16 C15 H15 119.7 . . ? C17 C16 C15 119.6(3) . . ? C17 C16 H16 120.2 . . ? C15 C16 H16 120.2 . . ? C16 C17 C18 120.7(3) . . ? C16 C17 H17 119.7 . . ? C18 C17 H17 119.7 . . ? C17 C18 C19 120.2(3) . . ? C17 C18 H18 119.9 . . ? C19 C18 H18 119.9 . . ? C18 C19 C14 119.2(3) . . ? C18 C19 H19 120.4 . . ? C14 C19 H19 120.4 . . ? C25 C20 C21 118.9(3) . . ? C25 C20 P1 118.2(2) . . ? C21 C20 P1 122.7(2) . . ? C22 C21 C20 119.5(3) . . ? C22 C21 H21 120.3 . . ? C20 C21 H21 120.3 . . ? C23 C22 C21 121.6(3) . . ? C23 C22 H22 119.2 . . ? C21 C22 H22 119.2 . . ? C22 C23 C24 118.9(3) . . ? C22 C23 H23 120.5 . . ? C24 C23 H23 120.5 . . ? C23 C24 C25 121.0(3) . . ? C23 C24 H24 119.5 . . ? C25 C24 H24 119.5 . . ? C20 C25 C24 120.1(3) . . ? C20 C25 H25 120.0 . . ? C24 C25 H25 120.0 . . ? C27 C26 C32 120.0(2) . . ? C27 C26 N2 118.6(2) . . ? C32 C26 N2 121.3(2) . . ? C26 C27 C28 119.9(2) . . ? C26 C27 H27 120.1 . . ? C28 C27 H27 120.1 . . ? C29 C28 C27 121.2(3) . . ? C29 C28 H28 119.4 . . ? C27 C28 H28 119.4 . . ? C28 C29 C31 118.1(3) . . ? C28 C29 C30 120.6(3) . . ? C31 C29 C30 121.3(3) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 C31 C29 121.8(2) . . ? C32 C31 H31 119.1 . . ? C29 C31 H31 119.1 . . ? C31 C32 C26 119.0(2) . . ? C31 C32 H32 120.5 . . ? C26 C32 H32 120.5 . . ? N2 C33 C36 112.33(19) . . ? N2 C33 C34 110.27(19) . . ? C36 C33 C34 111.4(2) . . ? N2 C33 H33 107.5 . . ? C36 C33 H33 107.5 . . ? C34 C33 H33 107.5 . . ? O5 C34 O6 125.9(3) . . ? O5 C34 C33 125.0(2) . . ? O6 C34 C33 109.1(2) . . ? O6 C35 H35A 109.5 . . ? O6 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? O6 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C37 C36 C33 109.0(2) . . ? C37 C36 P2 112.60(17) . . ? C33 C36 P2 106.53(16) . . ? C37 C36 H36 109.5 . . ? C33 C36 H36 109.5 . . ? P2 C36 H36 109.5 . . ? O7 C37 O8 124.9(2) . . ? O7 C37 C36 122.6(2) . . ? O8 C37 C36 112.5(2) . . ? O8 C38 H38A 109.5 . . ? O8 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? O8 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C44 C39 C40 119.4(2) . . ? C44 C39 P2 121.19(19) . . ? C40 C39 P2 119.34(19) . . ? C41 C40 C39 119.2(3) . . ? C41 C40 H40 120.4 . . ? C39 C40 H40 120.4 . . ? C42 C41 C40 120.6(3) . . ? C42 C41 H41 119.7 . . ? C40 C41 H41 119.7 . . ? C41 C42 C43 120.5(3) . . ? C41 C42 H42 119.7 . . ? C43 C42 H42 119.7 . . ? C42 C43 C44 119.2(3) . . ? C42 C43 H43 120.4 . . ? C44 C43 H43 120.4 . . ? C43 C44 C39 121.0(3) . . ? C43 C44 H44 119.5 . . ? C39 C44 H44 119.5 . . ? C50 C45 C46 119.3(2) . . ? C50 C45 P2 118.5(2) . . ? C46 C45 P2 122.1(2) . . ? C47 C46 C45 119.4(3) . . ? C47 C46 H46 120.3 . . ? C45 C46 H46 120.3 . . ? C48 C47 C46 120.6(3) . . ? C48 C47 H47 119.7 . . ? C46 C47 H47 119.7 . . ? C47 C48 C49 120.4(3) . . ? C47 C48 H48 119.8 . . ? C49 C48 H48 119.8 . . ? C48 C49 C50 119.7(3) . . ? C48 C49 H49 120.2 . . ? C50 C49 H49 120.2 . . ? C45 C50 C49 120.5(3) . . ? C45 C50 H50 119.7 . . ? C49 C50 H50 119.7 . . ? C1 N1 C8 111.57(18) . . ? C1 N1 Pd1 115.63(15) . . ? C8 N1 Pd1 111.75(14) . . ? C1 N1 H1N 110(2) . . ? C8 N1 H1N 110(3) . . ? Pd1 N1 H1N 97(2) . . ? C26 N2 C33 116.53(19) . . ? C26 N2 Pd2 112.67(14) . . ? C33 N2 Pd2 112.69(14) . . ? C26 N2 H2N 110(2) . . ? C33 N2 H2N 101(2) . . ? Pd2 N2 H2N 102(2) . . ? C9 O2 C10 115.9(2) . . ? C12 O4 C13 114.8(3) . . ? C34 O6 C35 115.6(3) . . ? C37 O8 C38 114.0(2) . . ? C14 P1 C20 107.77(12) . . ? C14 P1 C11 106.27(12) . . ? C20 P1 C11 108.70(11) . . ? C14 P1 Pd1 114.87(9) . . ? C20 P1 Pd1 117.11(9) . . ? C11 P1 Pd1 101.27(8) . . ? C39 P2 C45 105.27(11) . . ? C39 P2 C36 106.01(11) . . ? C45 P2 C36 108.79(12) . . ? C39 P2 Pd2 115.19(8) . . ? C45 P2 Pd2 118.91(8) . . ? C36 P2 Pd2 101.86(7) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 33.30 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.704 _refine_diff_density_min -0.941 _refine_diff_density_rms 0.220