# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Jonathan Iggo' _publ_contact_author_email IGGO@LIV.AC.UK loop_ _publ_author_name 'Jonathan Iggo' 'Jamie F. Bickley' 'B. Heaton' 'Chacko Jacob' 'Jianke Liu.' 'Mark Matthews' ; J.Pelletier ; 'Kelly J. Sheridan' 'Alexander Steiner' 'Robin Whyman' data_1 _database_code_depnum_ccdc_archive 'CCDC 746623' #TrackingRef 'data.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H32 Cl6 N2 P2 Pd' _chemical_formula_weight 873.68 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' Cl Cl 0.1484 0.1585 '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' 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 Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 20.0004(10) _cell_length_b 7.9187(4) _cell_length_c 22.9503(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3634.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 373(2) _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.597 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1760 _exptl_absorpt_coefficient_mu 1.070 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; _diffrn_ambient_temperature 373(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 'Bruker Apex' _diffrn_measurement_method /w _diffrn_reflns_number 21122 _diffrn_reflns_av_R_equivalents 0.0200 _diffrn_reflns_av_sigmaI/netI 0.0171 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 28.30 _reflns_number_total 4310 _reflns_number_gt 3857 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0278P)^2^+2.1992P] 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_number_reflns 4310 _refine_ls_number_parameters 215 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0269 _refine_ls_R_factor_gt 0.0229 _refine_ls_wR_factor_ref 0.0578 _refine_ls_wR_factor_gt 0.0560 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _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 C1 C 0.88581(8) 0.00218(18) 0.38914(7) 0.0162(3) Uani 1 1 d . . . C2 C 0.85286(8) 0.0608(2) 0.33999(7) 0.0211(3) Uani 1 1 d . . . H2 H 0.8556 0.1743 0.3298 0.025 Uiso 1 1 calc R . . C3 C 0.81592(8) -0.0496(2) 0.30614(7) 0.0252(3) Uani 1 1 d . . . H3 H 0.7941 -0.0103 0.2730 0.030 Uiso 1 1 calc R . . C4 C 0.81134(8) -0.2183(2) 0.32129(7) 0.0261(4) Uani 1 1 d . . . H4 H 0.7864 -0.2919 0.2984 0.031 Uiso 1 1 calc R . . C5 C 0.84367(9) -0.2773(2) 0.37026(8) 0.0281(4) Uani 1 1 d . . . H5 H 0.8402 -0.3906 0.3805 0.034 Uiso 1 1 calc R . . C6 C 0.88137(8) -0.1679(2) 0.40428(7) 0.0225(3) Uani 1 1 d . . . H6 H 0.9036 -0.2080 0.4371 0.027 Uiso 1 1 calc R . . C7 C 0.88018(7) 0.29363(19) 0.46795(6) 0.0164(3) Uani 1 1 d . . . C9 C 0.86981(10) 0.5140(2) 0.53665(8) 0.0281(4) Uani 1 1 d . . . H9 H 0.8891 0.5884 0.5631 0.034 Uiso 1 1 calc R A 1 C10 C 0.80171(9) 0.5185(2) 0.52729(8) 0.0270(4) Uani 1 1 d . C . H10 H 0.7752 0.5955 0.5474 0.032 Uiso 1 1 calc R . . C11 C 0.77315(9) 0.4085(2) 0.48817(8) 0.0281(4) Uani 1 1 d . . . H11 H 0.7271 0.4097 0.4823 0.034 Uiso 1 1 calc R C . C12 C 0.81272(8) 0.2962(2) 0.45753(7) 0.0206(3) Uani 1 1 d . C . H12 H 0.7938 0.2235 0.4303 0.025 Uiso 1 1 calc R . . C13 C 0.97970(7) 0.2718(2) 0.37777(6) 0.0168(3) Uani 1 1 d . . . C14 C 1.01560(8) 0.1911(2) 0.33397(7) 0.0228(3) Uani 1 1 d . C . H14 H 1.0172 0.0738 0.3325 0.027 Uiso 1 1 calc R . . C15 C 1.04889(9) 0.2862(2) 0.29256(7) 0.0269(4) Uani 1 1 d . . . H15 H 1.0728 0.2330 0.2631 0.032 Uiso 1 1 calc R C . C16 C 1.04644(9) 0.4605(2) 0.29516(8) 0.0295(4) Uani 1 1 d . C . H16 H 1.0684 0.5253 0.2673 0.035 Uiso 1 1 calc R . . C17 C 1.01104(10) 0.5374(3) 0.33940(10) 0.0342(4) Uani 1 1 d . . . H17 H 1.0096 0.6547 0.3412 0.041 Uiso 1 1 calc R B 1 C18 C 0.17898(11) 0.7793(3) 0.34471(9) 0.0439(5) Uani 1 1 d . . . H18A H 0.1728 0.8577 0.3767 0.053 Uiso 1 1 calc R . . H18B H 0.1565 0.6747 0.3548 0.053 Uiso 1 1 calc R . . C8 C 0.90939(8) 0.4008(2) 0.50727(7) 0.0259(4) Uani 0.500(17) 1 d P C 1 H8 H 0.9552 0.3970 0.5140 0.031 Uiso 0.500(17) 1 calc PR C 1 N1 N 0.97784(8) 0.4442(2) 0.38088(7) 0.0276(4) Uani 0.500(17) 1 d P C 1 C8' C 0.97784(8) 0.4442(2) 0.38088(7) 0.0276(4) Uani 0.500(17) 1 d P C 2 H8' H 0.9544 0.4977 0.4106 0.033 Uiso 0.500(17) 1 calc PR C 2 N1' N 0.90939(8) 0.4008(2) 0.50727(7) 0.0259(4) Uani 0.500(17) 1 d P C 2 Cl1 Cl 1.097110(18) 0.03864(5) 0.448226(16) 0.02089(8) Uani 1 1 d . C . Cl2 Cl 0.26465(3) 0.73967(7) 0.33580(2) 0.04027(12) Uani 1 1 d . . . Cl3 Cl 0.14203(3) 0.86386(6) 0.28143(2) 0.03722(11) Uani 1 1 d . . . P1 P 0.936381(18) 0.14537(5) 0.432449(16) 0.01424(8) Uani 1 1 d . C . Pd1 Pd 1.0000 0.0000 0.5000 0.01397(5) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0142(7) 0.0178(7) 0.0167(7) -0.0018(5) 0.0012(6) -0.0009(5) C2 0.0213(8) 0.0200(8) 0.0221(8) -0.0007(6) -0.0030(6) 0.0007(6) C3 0.0209(8) 0.0311(9) 0.0236(8) -0.0056(7) -0.0035(6) 0.0026(7) C4 0.0207(8) 0.0312(9) 0.0265(8) -0.0099(7) 0.0041(6) -0.0082(7) C5 0.0374(10) 0.0207(8) 0.0263(8) -0.0022(7) 0.0059(7) -0.0097(7) C6 0.0283(8) 0.0207(8) 0.0186(7) 0.0010(6) 0.0011(6) -0.0019(6) C7 0.0185(7) 0.0142(7) 0.0164(7) 0.0030(5) 0.0008(5) 0.0005(6) C9 0.0351(10) 0.0218(9) 0.0275(9) -0.0031(7) -0.0043(7) 0.0001(7) C10 0.0328(9) 0.0237(9) 0.0244(8) 0.0001(7) 0.0061(7) 0.0088(7) C11 0.0201(8) 0.0288(9) 0.0355(9) 0.0001(8) -0.0003(7) 0.0044(7) C12 0.0198(7) 0.0199(8) 0.0221(7) -0.0005(6) -0.0036(6) 0.0007(6) C13 0.0144(7) 0.0203(7) 0.0156(7) 0.0048(6) -0.0026(5) -0.0010(6) C14 0.0246(8) 0.0242(8) 0.0196(7) 0.0017(6) 0.0018(6) -0.0020(7) C15 0.0254(8) 0.0355(10) 0.0197(8) 0.0016(7) 0.0049(6) -0.0023(7) C16 0.0257(9) 0.0343(10) 0.0284(9) 0.0115(8) 0.0013(7) -0.0065(7) C17 0.0335(10) 0.0248(9) 0.0442(12) 0.0058(8) 0.0065(8) -0.0012(8) C18 0.0400(11) 0.0636(15) 0.0281(10) -0.0002(10) 0.0080(8) 0.0042(10) C8 0.0233(8) 0.0229(8) 0.0316(8) -0.0025(6) -0.0038(6) 0.0006(6) N1 0.0262(8) 0.0257(8) 0.0307(9) 0.0022(7) 0.0051(7) 0.0004(7) C8' 0.0262(8) 0.0257(8) 0.0307(9) 0.0022(7) 0.0051(7) 0.0004(7) N1' 0.0233(8) 0.0229(8) 0.0316(8) -0.0025(6) -0.0038(6) 0.0006(6) Cl1 0.01622(17) 0.02685(19) 0.01960(17) 0.00490(15) 0.00347(14) 0.00165(14) Cl2 0.0421(3) 0.0453(3) 0.0333(2) -0.0027(2) 0.0084(2) 0.0099(2) Cl3 0.0439(3) 0.0326(2) 0.0352(2) -0.00300(19) -0.0020(2) -0.0028(2) P1 0.01359(17) 0.01525(18) 0.01388(17) 0.00135(14) -0.00046(13) 0.00022(14) Pd1 0.01273(9) 0.01623(9) 0.01293(8) 0.00186(5) 0.00003(5) 0.00097(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.387(2) . ? C1 C6 1.394(2) . ? C1 P1 1.8157(15) . ? C2 C3 1.383(2) . ? C3 C4 1.383(3) . ? C4 C5 1.378(3) . ? C5 C6 1.389(2) . ? C7 C8 1.370(2) . ? C7 C12 1.370(2) . ? C7 P1 1.8181(15) . ? C9 C8 1.373(2) . ? C9 C10 1.379(3) . ? C10 C11 1.375(3) . ? C11 C12 1.383(2) . ? C13 N1 1.367(2) . ? C13 C14 1.391(2) . ? C13 P1 1.8244(15) . ? C14 C15 1.383(2) . ? C15 C16 1.383(3) . ? C16 C17 1.379(3) . ? C17 N1 1.375(3) . ? C18 Cl2 1.754(2) . ? C18 Cl3 1.762(2) . ? Cl1 Pd1 2.2973(4) . ? P1 Pd1 2.3125(4) . ? Pd1 Cl1 2.2973(4) 5_756 ? Pd1 P1 2.3125(4) 5_756 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 119.75(15) . . ? C2 C1 P1 120.07(12) . . ? C6 C1 P1 120.16(12) . . ? C3 C2 C1 119.92(16) . . ? C4 C3 C2 120.31(16) . . ? C5 C4 C3 120.10(16) . . ? C4 C5 C6 120.09(16) . . ? C5 C6 C1 119.82(15) . . ? C8 C7 C12 121.71(15) . . ? C8 C7 P1 115.58(12) . . ? C12 C7 P1 122.68(12) . . ? C8 C9 C10 120.64(16) . . ? C11 C10 C9 119.72(16) . . ? C10 C11 C12 120.11(16) . . ? C7 C12 C11 118.96(15) . . ? N1 C13 C14 120.71(15) . . ? N1 C13 P1 119.94(12) . . ? C14 C13 P1 119.33(12) . . ? C15 C14 C13 119.66(16) . . ? C16 C15 C14 119.78(16) . . ? C17 C16 C15 119.37(17) . . ? N1 C17 C16 121.37(18) . . ? Cl2 C18 Cl3 112.44(11) . . ? C7 C8 C9 118.83(15) . . ? C13 N1 C17 119.10(16) . . ? C1 P1 C7 107.71(7) . . ? C1 P1 C13 103.35(7) . . ? C7 P1 C13 104.32(7) . . ? C1 P1 Pd1 111.27(5) . . ? C7 P1 Pd1 111.17(5) . . ? C13 P1 Pd1 118.23(5) . . ? Cl1 Pd1 Cl1 180.0 . 5_756 ? Cl1 Pd1 P1 92.988(13) . . ? Cl1 Pd1 P1 87.012(13) 5_756 . ? Cl1 Pd1 P1 87.012(13) . 5_756 ? Cl1 Pd1 P1 92.988(13) 5_756 5_756 ? P1 Pd1 P1 180.000(13) . 5_756 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -0.2(2) . . . . ? P1 C1 C2 C3 178.15(12) . . . . ? C1 C2 C3 C4 0.4(2) . . . . ? C2 C3 C4 C5 -0.1(3) . . . . ? C3 C4 C5 C6 -0.5(3) . . . . ? C4 C5 C6 C1 0.7(3) . . . . ? C2 C1 C6 C5 -0.4(2) . . . . ? P1 C1 C6 C5 -178.71(13) . . . . ? C8 C9 C10 C11 0.0(3) . . . . ? C9 C10 C11 C12 -1.2(3) . . . . ? C8 C7 C12 C11 -0.9(2) . . . . ? P1 C7 C12 C11 177.38(13) . . . . ? C10 C11 C12 C7 1.7(3) . . . . ? N1 C13 C14 C15 -1.0(2) . . . . ? P1 C13 C14 C15 -179.63(13) . . . . ? C13 C14 C15 C16 0.2(3) . . . . ? C14 C15 C16 C17 0.4(3) . . . . ? C15 C16 C17 N1 -0.3(3) . . . . ? C12 C7 C8 C9 -0.3(2) . . . . ? P1 C7 C8 C9 -178.70(13) . . . . ? C10 C9 C8 C7 0.8(3) . . . . ? C14 C13 N1 C17 1.1(3) . . . . ? P1 C13 N1 C17 179.72(14) . . . . ? C16 C17 N1 C13 -0.5(3) . . . . ? C2 C1 P1 C7 68.81(14) . . . . ? C6 C1 P1 C7 -112.87(13) . . . . ? C2 C1 P1 C13 -41.22(14) . . . . ? C6 C1 P1 C13 137.10(13) . . . . ? C2 C1 P1 Pd1 -169.11(11) . . . . ? C6 C1 P1 Pd1 9.21(14) . . . . ? C8 C7 P1 C1 173.61(12) . . . . ? C12 C7 P1 C1 -4.74(15) . . . . ? C8 C7 P1 C13 -77.02(13) . . . . ? C12 C7 P1 C13 104.63(14) . . . . ? C8 C7 P1 Pd1 51.48(13) . . . . ? C12 C7 P1 Pd1 -126.88(12) . . . . ? N1 C13 P1 C1 128.21(14) . . . . ? C14 C13 P1 C1 -53.19(14) . . . . ? N1 C13 P1 C7 15.68(15) . . . . ? C14 C13 P1 C7 -165.72(12) . . . . ? N1 C13 P1 Pd1 -108.39(13) . . . . ? C14 C13 P1 Pd1 70.21(13) . . . . ? C1 P1 Pd1 Cl1 105.72(5) . . . . ? C7 P1 Pd1 Cl1 -134.23(5) . . . . ? C13 P1 Pd1 Cl1 -13.63(6) . . . . ? C1 P1 Pd1 Cl1 -74.28(5) . . . 5_756 ? C7 P1 Pd1 Cl1 45.77(5) . . . 5_756 ? C13 P1 Pd1 Cl1 166.37(6) . . . 5_756 ? C1 P1 Pd1 P1 177(8) . . . 5_756 ? C7 P1 Pd1 P1 -63(8) . . . 5_756 ? C13 P1 Pd1 P1 57(8) . . . 5_756 ? _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.954 _refine_diff_density_max 0.443 _refine_diff_density_min -0.210 _refine_diff_density_rms 0.061 #===END data_2b _database_code_depnum_ccdc_archive 'CCDC 746624' #TrackingRef 'data.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H40 Cl6 N2 O6 P2 Pd S2' _chemical_formula_weight 1065.88 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' S S 0.1246 0.1234 '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)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 23.972(3) _cell_length_b 10.0239(14) _cell_length_c 18.270(3) _cell_angle_alpha 90.00 _cell_angle_beta 95.549(3) _cell_angle_gamma 90.00 _cell_volume 4369.6(10) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.620 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2160 _exptl_absorpt_coefficient_mu 1.008 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.735 _exptl_absorpt_correction_T_max 0.817 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker Apex' _diffrn_reflns_number 21748 _diffrn_reflns_av_R_equivalents 0.0532 _diffrn_reflns_av_sigmaI/netI 0.0655 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 0.85 _diffrn_reflns_theta_max 25.03 _reflns_number_total 7680 _reflns_number_gt 5630 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0977P)^2^+10.4693P] 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_number_reflns 7680 _refine_ls_number_parameters 516 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0896 _refine_ls_R_factor_gt 0.0627 _refine_ls_wR_factor_ref 0.1680 _refine_ls_wR_factor_gt 0.1528 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3338(2) 0.2176(6) 0.1996(3) 0.0147(13) Uani 1 1 d . . . C2 C 0.3719(2) 0.1603(6) 0.1554(3) 0.0134(13) Uani 1 1 d . . . H2 H 0.3843 0.2099 0.1158 0.016 Uiso 1 1 calc R . . C3 C 0.3914(3) 0.0322(6) 0.1691(3) 0.0168(13) Uani 1 1 d . . . H3 H 0.4174 -0.0058 0.1390 0.020 Uiso 1 1 calc R . . C4 C 0.3731(3) -0.0414(6) 0.2266(3) 0.0213(14) Uani 1 1 d . . . H4 H 0.3863 -0.1298 0.2358 0.026 Uiso 1 1 calc R . . C5 C 0.3352(3) 0.0153(6) 0.2709(3) 0.0210(14) Uani 1 1 d . . . H5 H 0.3231 -0.0349 0.3105 0.025 Uiso 1 1 calc R . . C6 C 0.3150(3) 0.1435(6) 0.2581(3) 0.0179(14) Uani 1 1 d . . . H6 H 0.2888 0.1809 0.2882 0.021 Uiso 1 1 calc R . . C7 C 0.4642(3) 0.5129(6) 0.2615(3) 0.0188(14) Uani 1 1 d . . . H7 H 0.4860 0.5006 0.3073 0.023 Uiso 1 1 calc R . . C8 C 0.4850(3) 0.5885(6) 0.2071(3) 0.0211(14) Uani 1 1 d . . . H8 H 0.5208 0.6297 0.2153 0.025 Uiso 1 1 calc R . . C9 C 0.4530(3) 0.6034(6) 0.1405(3) 0.0227(15) Uani 1 1 d . . . H9 H 0.4663 0.6562 0.1026 0.027 Uiso 1 1 calc R . . C10 C 0.4013(3) 0.5407(6) 0.1294(3) 0.0188(14) Uani 1 1 d . . . H10 H 0.3798 0.5481 0.0830 0.023 Uiso 1 1 calc R . . C11 C 0.3808(2) 0.4679(6) 0.1848(3) 0.0120(12) Uani 1 1 d . . . C12 C 0.2841(2) 0.4035(6) 0.0863(3) 0.0134(13) Uani 1 1 d . . . C13 C 0.2732(3) 0.2923(6) 0.0414(3) 0.0199(14) Uani 1 1 d . . . H13 H 0.2807 0.2050 0.0601 0.024 Uiso 1 1 calc R . . C14 C 0.2512(3) 0.3107(7) -0.0316(3) 0.0258(16) Uani 1 1 d . . . H14 H 0.2433 0.2354 -0.0625 0.031 Uiso 1 1 calc R . . C15 C 0.2410(3) 0.4360(7) -0.0589(3) 0.0228(15) Uani 1 1 d . . . H15 H 0.2270 0.4472 -0.1090 0.027 Uiso 1 1 calc R . . C16 C 0.2508(3) 0.5478(7) -0.0141(3) 0.0231(15) Uani 1 1 d . . . H16 H 0.2434 0.6347 -0.0334 0.028 Uiso 1 1 calc R . . C17 C 0.2714(3) 0.5311(6) 0.0586(3) 0.0203(14) Uani 1 1 d . . . H17 H 0.2770 0.6066 0.0899 0.024 Uiso 1 1 calc R . . C18 C 0.2148(3) 0.5914(6) 0.4284(3) 0.0128(12) Uani 1 1 d . . . C19 C 0.2694(3) 0.5566(6) 0.4497(3) 0.0151(13) Uani 1 1 d . . . H19 H 0.2931 0.5293 0.4138 0.018 Uiso 1 1 calc R . . C20 C 0.2902(3) 0.5610(6) 0.5240(3) 0.0151(13) Uani 1 1 d . . . H20 H 0.3280 0.5367 0.5387 0.018 Uiso 1 1 calc R . . C21 C 0.2550(3) 0.6014(6) 0.5761(3) 0.0171(13) Uani 1 1 d . . . H21 H 0.2689 0.6061 0.6265 0.021 Uiso 1 1 calc R . . C22 C 0.2002(3) 0.6345(6) 0.5549(3) 0.0173(13) Uani 1 1 d . . . H22 H 0.1762 0.6602 0.5909 0.021 Uiso 1 1 calc R . . C23 C 0.1795(3) 0.6305(6) 0.4813(3) 0.0147(13) Uani 1 1 d . . . H23 H 0.1417 0.6542 0.4669 0.018 Uiso 1 1 calc R . . C24 C 0.1263(3) 0.4959(5) 0.3256(3) 0.0133(12) Uani 1 1 d . . . C25 C 0.1158(3) 0.4003(6) 0.3769(3) 0.0187(14) Uani 1 1 d . . . H25 H 0.1411 0.3888 0.4198 0.022 Uiso 1 1 calc R . . C26 C 0.0681(3) 0.3210(6) 0.3658(3) 0.0220(15) Uani 1 1 d . . . H26 H 0.0605 0.2554 0.4011 0.026 Uiso 1 1 calc R . . C27 C 0.0317(3) 0.3382(7) 0.3031(3) 0.0235(15) Uani 1 1 d . . . H27 H -0.0012 0.2853 0.2948 0.028 Uiso 1 1 calc R . . C28 C 0.0440(3) 0.4333(7) 0.2529(3) 0.0241(15) Uani 1 1 d . . . H28 H 0.0196 0.4458 0.2093 0.029 Uiso 1 1 calc R . . C29 C 0.1668(2) 0.7606(6) 0.3073(3) 0.0152(13) Uani 1 1 d . . . C30 C 0.1205(3) 0.8151(6) 0.3392(3) 0.0178(13) Uani 1 1 d . . . H30 H 0.1015 0.7635 0.3726 0.021 Uiso 1 1 calc R . . C31 C 0.1030(3) 0.9436(6) 0.3219(3) 0.0201(14) Uani 1 1 d . . . H31 H 0.0723 0.9808 0.3440 0.024 Uiso 1 1 calc R . . C32 C 0.1304(3) 1.0188(6) 0.2717(3) 0.0188(14) Uani 1 1 d . . . H32 H 0.1181 1.1069 0.2595 0.023 Uiso 1 1 calc R . . C33 C 0.1750(3) 0.9657(6) 0.2401(3) 0.0158(13) Uani 1 1 d . . . H33 H 0.1937 1.0172 0.2063 0.019 Uiso 1 1 calc R . . C34 C 0.1928(3) 0.8374(6) 0.2573(3) 0.0153(13) Uani 1 1 d . . . H34 H 0.2234 0.8011 0.2345 0.018 Uiso 1 1 calc R . . C35 C 0.0497(3) 0.0981(8) 0.0650(4) 0.0359(18) Uani 1 1 d . . . H35A H 0.0294 0.1199 0.0167 0.043 Uiso 1 1 calc R . . H35B H 0.0527 -0.0002 0.0688 0.043 Uiso 1 1 calc R . . C36 C 0.9032(3) 0.0347(7) 0.4700(4) 0.0356(19) Uani 1 1 d . . . H36A H 0.9295 0.0060 0.5113 0.053 Uiso 1 1 calc R . . H36B H 0.8903 -0.0432 0.4406 0.053 Uiso 1 1 calc R . . H36C H 0.8709 0.0786 0.4889 0.053 Uiso 1 1 calc R . . C37 C 0.4084(3) 0.3480(6) 0.9455(4) 0.0278(16) Uani 1 1 d . . . H37A H 0.3698 0.3635 0.9567 0.042 Uiso 1 1 calc R . . H37B H 0.4156 0.3985 0.9015 0.042 Uiso 1 1 calc R . . H37C H 0.4344 0.3772 0.9871 0.042 Uiso 1 1 calc R . . C38 C 0.4368(3) 0.6915(7) 0.4293(4) 0.0326(17) Uani 1 1 d . . . H38A H 0.4181 0.6214 0.3976 0.039 Uiso 1 1 calc R . . H38B H 0.4588 0.6472 0.4711 0.039 Uiso 1 1 calc R . . Cl1 Cl 0.19333(7) 0.32415(16) 0.22141(9) 0.0242(4) Uani 1 1 d . . . Cl2 Cl 0.31696(6) 0.66273(14) 0.28501(8) 0.0165(3) Uani 1 1 d . . . Cl3 Cl 0.01161(9) 0.1584(2) 0.13519(11) 0.0472(5) Uani 1 1 d . . . Cl4 Cl 0.11726(8) 0.16781(18) 0.07014(9) 0.0325(4) Uani 1 1 d . . . Cl5 Cl 0.48231(9) 0.7844(2) 0.37830(10) 0.0404(5) Uani 1 1 d . . . Cl6 Cl 0.38612(9) 0.7951(2) 0.46253(10) 0.0417(5) Uani 1 1 d . . . N1 N 0.4136(2) 0.4570(5) 0.2497(2) 0.0143(11) Uani 1 1 d . . . H1N H 0.4008 0.4110 0.2856 0.017 Uiso 1 1 calc R . . N2 N 0.0900(2) 0.5082(5) 0.2650(3) 0.0164(11) Uani 1 1 d . . . H2N H 0.0969 0.5681 0.2319 0.020 Uiso 1 1 calc R . . O1 O 0.4094(2) 0.1080(4) 0.9977(2) 0.0265(11) Uani 1 1 d . . . O2 O 0.47423(18) 0.1595(4) 0.9076(2) 0.0244(11) Uani 1 1 d . . . O3 O 0.37545(19) 0.1396(5) 0.8693(2) 0.0230(10) Uani 1 1 d . . . O4 O 0.9453(2) 0.2688(5) 0.4561(3) 0.0326(12) Uani 1 1 d . . . O5 O 0.98811(18) 0.0819(4) 0.3975(2) 0.0240(10) Uani 1 1 d . . . O6 O 0.89784(19) 0.1676(5) 0.3481(2) 0.0273(11) Uani 1 1 d . . . P1 P 0.31185(7) 0.38817(15) 0.18214(8) 0.0120(3) Uani 1 1 d . . . P2 P 0.19098(6) 0.59286(15) 0.33054(7) 0.0112(3) Uani 1 1 d . . . Pd1 Pd 0.253945(18) 0.49320(4) 0.25737(2) 0.01133(15) Uani 1 1 d . . . S1 S 0.41828(7) 0.17591(15) 0.92973(8) 0.0171(3) Uani 1 1 d . . . S2 S 0.93663(7) 0.14702(16) 0.41494(8) 0.0188(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.020(3) 0.015(3) 0.009(3) -0.002(2) 0.001(2) -0.001(2) C2 0.020(3) 0.015(3) 0.006(3) 0.000(2) 0.004(2) -0.001(2) C3 0.022(4) 0.013(3) 0.015(3) -0.002(2) -0.001(3) -0.001(2) C4 0.025(4) 0.014(3) 0.023(3) 0.003(3) -0.006(3) -0.004(3) C5 0.034(4) 0.017(3) 0.012(3) 0.005(3) 0.003(3) -0.006(3) C6 0.031(4) 0.016(3) 0.008(3) 0.003(2) 0.010(3) -0.007(3) C7 0.026(4) 0.019(3) 0.012(3) -0.002(3) 0.003(2) 0.001(3) C8 0.024(4) 0.025(4) 0.015(3) 0.002(3) 0.006(3) -0.005(3) C9 0.036(4) 0.022(4) 0.011(3) 0.002(3) 0.006(3) -0.009(3) C10 0.031(4) 0.015(3) 0.011(3) 0.002(2) 0.001(3) 0.002(3) C11 0.021(3) 0.009(3) 0.007(3) -0.002(2) 0.004(2) 0.001(2) C12 0.021(3) 0.011(3) 0.009(3) -0.001(2) 0.004(2) 0.000(2) C13 0.031(4) 0.014(3) 0.014(3) -0.002(3) 0.000(3) -0.001(3) C14 0.036(4) 0.030(4) 0.011(3) -0.006(3) -0.003(3) -0.004(3) C15 0.024(4) 0.033(4) 0.011(3) -0.002(3) -0.003(3) 0.003(3) C16 0.033(4) 0.020(4) 0.017(3) 0.008(3) 0.003(3) 0.009(3) C17 0.028(4) 0.015(3) 0.018(3) -0.007(3) 0.001(3) 0.003(3) C18 0.023(3) 0.009(3) 0.007(3) 0.005(2) 0.004(2) -0.001(2) C19 0.026(4) 0.015(3) 0.006(3) 0.002(2) 0.008(2) 0.000(3) C20 0.022(3) 0.017(3) 0.007(3) 0.005(2) -0.002(2) 0.003(3) C21 0.028(4) 0.018(3) 0.007(3) -0.001(2) 0.005(2) -0.003(3) C22 0.029(4) 0.018(3) 0.006(3) -0.001(2) 0.007(3) 0.001(3) C23 0.018(3) 0.019(3) 0.008(3) -0.001(2) 0.004(2) 0.002(2) C24 0.022(3) 0.006(3) 0.012(3) 0.000(2) 0.005(2) -0.001(2) C25 0.024(4) 0.024(4) 0.009(3) 0.000(3) 0.004(2) 0.000(3) C26 0.032(4) 0.019(4) 0.017(3) 0.001(3) 0.014(3) -0.007(3) C27 0.031(4) 0.025(4) 0.015(3) -0.002(3) 0.003(3) -0.013(3) C28 0.029(4) 0.030(4) 0.012(3) 0.001(3) 0.001(3) -0.004(3) C29 0.019(3) 0.019(3) 0.007(3) 0.000(2) -0.003(2) 0.001(3) C30 0.023(3) 0.019(3) 0.012(3) 0.002(3) 0.004(2) 0.000(3) C31 0.024(4) 0.024(4) 0.012(3) 0.002(3) 0.003(3) 0.002(3) C32 0.029(4) 0.014(3) 0.013(3) 0.004(2) -0.004(3) 0.002(3) C33 0.025(4) 0.013(3) 0.009(3) 0.005(2) 0.004(2) 0.003(2) C34 0.027(4) 0.015(3) 0.004(3) 0.001(2) 0.003(2) -0.002(3) C35 0.047(5) 0.028(4) 0.031(4) 0.001(3) -0.005(3) -0.008(3) C36 0.045(5) 0.031(4) 0.034(4) 0.016(3) 0.021(4) 0.003(3) C37 0.042(5) 0.019(4) 0.024(4) -0.008(3) 0.012(3) 0.003(3) C38 0.051(5) 0.015(4) 0.031(4) -0.004(3) -0.002(3) -0.003(3) Cl1 0.0256(9) 0.0191(8) 0.0296(9) -0.0128(7) 0.0106(7) -0.0077(7) Cl2 0.0234(8) 0.0130(8) 0.0136(7) -0.0026(6) 0.0042(6) -0.0041(6) Cl3 0.0453(13) 0.0567(14) 0.0418(12) 0.0055(10) 0.0156(9) 0.0054(10) Cl4 0.0363(11) 0.0370(11) 0.0242(9) -0.0019(8) 0.0024(7) 0.0006(8) Cl5 0.0469(12) 0.0382(11) 0.0364(10) 0.0033(9) 0.0047(9) -0.0078(9) Cl6 0.0508(13) 0.0420(12) 0.0340(10) -0.0170(9) 0.0136(9) -0.0065(9) N1 0.026(3) 0.013(3) 0.004(2) 0.0032(19) 0.005(2) -0.002(2) N2 0.024(3) 0.017(3) 0.009(2) 0.003(2) 0.004(2) -0.005(2) O1 0.048(3) 0.022(3) 0.010(2) 0.0046(19) 0.008(2) -0.004(2) O2 0.023(3) 0.025(3) 0.027(3) -0.009(2) 0.010(2) -0.005(2) O3 0.029(3) 0.032(3) 0.009(2) -0.0053(19) 0.0039(18) 0.002(2) O4 0.043(3) 0.028(3) 0.027(3) -0.010(2) 0.001(2) 0.002(2) O5 0.018(2) 0.028(3) 0.026(2) 0.001(2) 0.0036(19) 0.005(2) O6 0.035(3) 0.034(3) 0.012(2) 0.000(2) -0.0030(19) 0.012(2) P1 0.0213(9) 0.0108(8) 0.0045(7) -0.0009(6) 0.0045(6) -0.0013(6) P2 0.0194(8) 0.0116(8) 0.0032(7) 0.0006(6) 0.0035(6) -0.0014(6) Pd1 0.0206(3) 0.0095(3) 0.0047(2) -0.00193(17) 0.00504(17) -0.00235(18) S1 0.0278(9) 0.0146(8) 0.0101(7) -0.0047(6) 0.0073(6) -0.0037(6) S2 0.0256(9) 0.0196(9) 0.0114(7) -0.0006(6) 0.0035(6) 0.0014(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.399(8) . ? C1 C6 1.410(8) . ? C1 P1 1.808(6) . ? C2 C3 1.382(8) . ? C3 C4 1.390(9) . ? C4 C5 1.393(9) . ? C5 C6 1.386(9) . ? C7 N1 1.336(8) . ? C7 C8 1.380(8) . ? C8 C9 1.383(9) . ? C9 C10 1.388(9) . ? C10 C11 1.377(8) . ? C11 N1 1.362(7) . ? C11 P1 1.832(6) . ? C12 C13 1.394(8) . ? C12 C17 1.399(8) . ? C12 P1 1.819(6) . ? C13 C14 1.398(8) . ? C14 C15 1.365(9) . ? C15 C16 1.395(9) . ? C16 C17 1.381(9) . ? C18 C19 1.372(8) . ? C18 C23 1.402(8) . ? C18 P2 1.823(6) . ? C19 C20 1.402(8) . ? C20 C21 1.393(8) . ? C21 C22 1.374(9) . ? C22 C23 1.387(8) . ? C24 N2 1.346(8) . ? C24 C25 1.381(8) . ? C24 P2 1.824(6) . ? C25 C26 1.392(9) . ? C26 C27 1.381(9) . ? C27 C28 1.374(9) . ? C28 N2 1.335(8) . ? C29 C34 1.388(8) . ? C29 C30 1.412(8) . ? C29 P2 1.815(6) . ? C30 C31 1.382(9) . ? C31 C32 1.399(9) . ? C32 C33 1.372(9) . ? C33 C34 1.381(8) . ? C35 Cl3 1.752(8) . ? C35 Cl4 1.758(8) . ? C36 S2 1.755(7) . ? C37 S1 1.768(6) . ? C38 Cl6 1.752(8) . ? C38 Cl5 1.766(7) . ? Cl1 Pd1 2.2870(16) . ? Cl2 Pd1 2.2972(15) . ? O1 S1 1.450(4) . ? O2 S1 1.447(4) . ? O3 S1 1.479(4) . ? O4 S2 1.438(5) . ? O5 S2 1.459(5) . ? O6 S2 1.476(4) . ? P1 Pd1 2.3008(15) . ? P2 Pd1 2.3352(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 C2 C1 C6 119.7(5) . . ? C2 C1 P1 118.7(4) . . ? C6 C1 P1 121.5(5) . . ? C3 C2 C1 120.4(5) . . ? C2 C3 C4 120.3(6) . . ? C3 C4 C5 119.6(6) . . ? C6 C5 C4 121.2(6) . . ? C5 C6 C1 118.9(6) . . ? N1 C7 C8 120.0(6) . . ? C7 C8 C9 119.0(6) . . ? C8 C9 C10 119.5(6) . . ? C11 C10 C9 120.6(6) . . ? N1 C11 C10 117.8(5) . . ? N1 C11 P1 115.6(4) . . ? C10 C11 P1 126.6(5) . . ? C13 C12 C17 119.8(5) . . ? C13 C12 P1 122.0(4) . . ? C17 C12 P1 118.2(4) . . ? C12 C13 C14 119.2(6) . . ? C15 C14 C13 120.6(6) . . ? C14 C15 C16 120.7(6) . . ? C17 C16 C15 119.5(6) . . ? C16 C17 C12 120.3(6) . . ? C19 C18 C23 119.8(5) . . ? C19 C18 P2 118.7(4) . . ? C23 C18 P2 121.4(5) . . ? C18 C19 C20 120.6(5) . . ? C21 C20 C19 119.2(6) . . ? C22 C21 C20 120.3(5) . . ? C21 C22 C23 120.6(5) . . ? C22 C23 C18 119.6(6) . . ? N2 C24 C25 118.4(5) . . ? N2 C24 P2 118.1(4) . . ? C25 C24 P2 123.1(5) . . ? C24 C25 C26 119.9(6) . . ? C27 C26 C25 119.5(6) . . ? C28 C27 C26 118.8(6) . . ? N2 C28 C27 120.4(6) . . ? C34 C29 C30 118.5(5) . . ? C34 C29 P2 120.9(5) . . ? C30 C29 P2 120.6(4) . . ? C31 C30 C29 120.0(6) . . ? C30 C31 C32 120.0(6) . . ? C33 C32 C31 120.1(6) . . ? C32 C33 C34 120.1(6) . . ? C33 C34 C29 121.2(6) . . ? Cl3 C35 Cl4 111.5(4) . . ? Cl6 C38 Cl5 110.8(4) . . ? C7 N1 C11 123.1(5) . . ? C28 N2 C24 122.9(5) . . ? C1 P1 C12 108.9(3) . . ? C1 P1 C11 99.3(3) . . ? C12 P1 C11 103.6(3) . . ? C1 P1 Pd1 120.59(19) . . ? C12 P1 Pd1 110.5(2) . . ? C11 P1 Pd1 112.29(18) . . ? C29 P2 C18 107.4(3) . . ? C29 P2 C24 103.4(3) . . ? C18 P2 C24 103.2(3) . . ? C29 P2 Pd1 118.2(2) . . ? C18 P2 Pd1 113.5(2) . . ? C24 P2 Pd1 109.68(19) . . ? Cl1 Pd1 Cl2 175.82(5) . . ? Cl1 Pd1 P1 83.83(6) . . ? Cl2 Pd1 P1 92.75(5) . . ? Cl1 Pd1 P2 93.07(6) . . ? Cl2 Pd1 P2 90.31(5) . . ? P1 Pd1 P2 176.78(6) . . ? O2 S1 O1 113.7(3) . . ? O2 S1 O3 111.0(3) . . ? O1 S1 O3 112.0(3) . . ? O2 S1 C37 107.4(3) . . ? O1 S1 C37 106.6(3) . . ? O3 S1 C37 105.5(3) . . ? O4 S2 O5 114.3(3) . . ? O4 S2 O6 111.2(3) . . ? O5 S2 O6 111.1(3) . . ? O4 S2 C36 107.2(3) . . ? O5 S2 C36 106.4(3) . . ? O6 S2 C36 106.1(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -0.5(9) . . . . ? P1 C1 C2 C3 177.3(5) . . . . ? C1 C2 C3 C4 0.4(9) . . . . ? C2 C3 C4 C5 -0.5(9) . . . . ? C3 C4 C5 C6 0.6(10) . . . . ? C4 C5 C6 C1 -0.7(10) . . . . ? C2 C1 C6 C5 0.7(9) . . . . ? P1 C1 C6 C5 -177.1(5) . . . . ? N1 C7 C8 C9 -0.9(9) . . . . ? C7 C8 C9 C10 -1.0(10) . . . . ? C8 C9 C10 C11 2.3(10) . . . . ? C9 C10 C11 N1 -1.6(9) . . . . ? C9 C10 C11 P1 175.6(5) . . . . ? C17 C12 C13 C14 1.8(9) . . . . ? P1 C12 C13 C14 179.2(5) . . . . ? C12 C13 C14 C15 0.6(10) . . . . ? C13 C14 C15 C16 -1.8(10) . . . . ? C14 C15 C16 C17 0.4(10) . . . . ? C15 C16 C17 C12 2.1(10) . . . . ? C13 C12 C17 C16 -3.2(10) . . . . ? P1 C12 C17 C16 179.3(5) . . . . ? C23 C18 C19 C20 -0.6(9) . . . . ? P2 C18 C19 C20 176.6(5) . . . . ? C18 C19 C20 C21 -0.1(9) . . . . ? C19 C20 C21 C22 1.0(9) . . . . ? C20 C21 C22 C23 -1.2(9) . . . . ? C21 C22 C23 C18 0.5(9) . . . . ? C19 C18 C23 C22 0.4(9) . . . . ? P2 C18 C23 C22 -176.8(5) . . . . ? N2 C24 C25 C26 -1.0(9) . . . . ? P2 C24 C25 C26 -173.6(5) . . . . ? C24 C25 C26 C27 0.3(9) . . . . ? C25 C26 C27 C28 0.4(10) . . . . ? C26 C27 C28 N2 -0.5(10) . . . . ? C34 C29 C30 C31 -1.7(9) . . . . ? P2 C29 C30 C31 179.1(5) . . . . ? C29 C30 C31 C32 1.1(9) . . . . ? C30 C31 C32 C33 -0.5(9) . . . . ? C31 C32 C33 C34 0.4(9) . . . . ? C32 C33 C34 C29 -1.0(9) . . . . ? C30 C29 C34 C33 1.6(9) . . . . ? P2 C29 C34 C33 -179.2(5) . . . . ? C8 C7 N1 C11 1.6(9) . . . . ? C10 C11 N1 C7 -0.3(9) . . . . ? P1 C11 N1 C7 -177.9(5) . . . . ? C27 C28 N2 C24 -0.2(10) . . . . ? C25 C24 N2 C28 0.9(9) . . . . ? P2 C24 N2 C28 173.9(5) . . . . ? C2 C1 P1 C12 54.8(5) . . . . ? C6 C1 P1 C12 -127.4(5) . . . . ? C2 C1 P1 C11 -53.1(5) . . . . ? C6 C1 P1 C11 124.7(5) . . . . ? C2 C1 P1 Pd1 -176.0(4) . . . . ? C6 C1 P1 Pd1 1.8(6) . . . . ? C13 C12 P1 C1 10.7(6) . . . . ? C17 C12 P1 C1 -171.8(5) . . . . ? C13 C12 P1 C11 115.7(5) . . . . ? C17 C12 P1 C11 -66.9(5) . . . . ? C13 C12 P1 Pd1 -123.9(5) . . . . ? C17 C12 P1 Pd1 53.6(5) . . . . ? N1 C11 P1 C1 -60.9(5) . . . . ? C10 C11 P1 C1 121.8(5) . . . . ? N1 C11 P1 C12 -173.0(4) . . . . ? C10 C11 P1 C12 9.7(6) . . . . ? N1 C11 P1 Pd1 67.7(4) . . . . ? C10 C11 P1 Pd1 -109.6(5) . . . . ? C34 C29 P2 C18 117.5(5) . . . . ? C30 C29 P2 C18 -63.3(5) . . . . ? C34 C29 P2 C24 -133.8(5) . . . . ? C30 C29 P2 C24 45.4(5) . . . . ? C34 C29 P2 Pd1 -12.5(6) . . . . ? C30 C29 P2 Pd1 166.7(4) . . . . ? C19 C18 P2 C29 -121.1(5) . . . . ? C23 C18 P2 C29 56.1(5) . . . . ? C19 C18 P2 C24 130.1(5) . . . . ? C23 C18 P2 C24 -52.7(5) . . . . ? C19 C18 P2 Pd1 11.4(5) . . . . ? C23 C18 P2 Pd1 -171.4(4) . . . . ? N2 C24 P2 C29 50.0(5) . . . . ? C25 C24 P2 C29 -137.4(5) . . . . ? N2 C24 P2 C18 161.8(4) . . . . ? C25 C24 P2 C18 -25.5(6) . . . . ? N2 C24 P2 Pd1 -76.9(5) . . . . ? C25 C24 P2 Pd1 95.8(5) . . . . ? C1 P1 Pd1 Cl1 -59.9(2) . . . . ? C12 P1 Pd1 Cl1 68.6(2) . . . . ? C11 P1 Pd1 Cl1 -176.3(2) . . . . ? C1 P1 Pd1 Cl2 122.5(2) . . . . ? C12 P1 Pd1 Cl2 -109.0(2) . . . . ? C11 P1 Pd1 Cl2 6.1(2) . . . . ? C1 P1 Pd1 P2 -75.7(10) . . . . ? C12 P1 Pd1 P2 52.7(10) . . . . ? C11 P1 Pd1 P2 167.8(9) . . . . ? C29 P2 Pd1 Cl1 -118.1(2) . . . . ? C18 P2 Pd1 Cl1 114.9(2) . . . . ? C24 P2 Pd1 Cl1 0.0(2) . . . . ? C29 P2 Pd1 Cl2 59.5(2) . . . . ? C18 P2 Pd1 Cl2 -67.6(2) . . . . ? C24 P2 Pd1 Cl2 177.5(2) . . . . ? C29 P2 Pd1 P1 -102.3(10) . . . . ? C18 P2 Pd1 P1 130.6(10) . . . . ? C24 P2 Pd1 P1 15.7(10) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 2.800 _refine_diff_density_min -1.823 _refine_diff_density_rms 0.169 #===END data_3BF4 _database_code_depnum_ccdc_archive 'CCDC 746625' #TrackingRef 'data.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H28 B Cl F4 N2 P2 Pd' _chemical_formula_weight 755.18 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 '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 Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 17.704(2) _cell_length_b 18.156(2) _cell_length_c 20.149(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6476.4(14) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.549 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3040 _exptl_absorpt_coefficient_mu 0.805 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.873 _exptl_absorpt_correction_T_max 0.965 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker APEX' _diffrn_measurement_method /w _diffrn_reflns_number 38516 _diffrn_reflns_av_R_equivalents 0.0170 _diffrn_reflns_av_sigmaI/netI 0.0144 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 28.28 _reflns_number_total 7687 _reflns_number_gt 6783 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0342P)^2^+3.6754P] 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_number_reflns 7687 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0284 _refine_ls_R_factor_gt 0.0235 _refine_ls_wR_factor_ref 0.0638 _refine_ls_wR_factor_gt 0.0607 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _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 B1 B 0.03470(10) 0.26593(10) 0.88496(8) 0.0203(3) Uani 1 1 d . . . C1 C 0.12870(9) 0.22142(8) 0.72718(7) 0.0182(3) Uani 1 1 d . . . H1 H 0.1495 0.2272 0.7703 0.022 Uiso 1 1 calc R . . C2 C 0.05946(9) 0.25338(8) 0.71206(7) 0.0199(3) Uani 1 1 d . . . H2 H 0.0328 0.2806 0.7448 0.024 Uiso 1 1 calc R . . C3 C 0.02961(9) 0.24517(9) 0.64896(8) 0.0205(3) Uani 1 1 d . . . H3 H -0.0178 0.2666 0.6383 0.025 Uiso 1 1 calc R . . C4 C 0.06925(8) 0.20548(8) 0.60099(7) 0.0187(3) Uani 1 1 d . . . H4 H 0.0499 0.1994 0.5574 0.022 Uiso 1 1 calc R . . C5 C 0.13790(8) 0.17528(7) 0.61935(7) 0.0152(3) Uani 1 1 d . . . C6 C 0.25497(8) 0.18031(8) 0.52174(7) 0.0158(3) Uani 1 1 d . . . C7 C 0.21183(9) 0.22360(8) 0.47864(7) 0.0195(3) Uani 1 1 d . . . H7 H 0.1584 0.2190 0.4784 0.023 Uiso 1 1 calc R . . C8 C 0.24685(9) 0.27324(9) 0.43629(8) 0.0224(3) Uani 1 1 d . . . H8 H 0.2175 0.3019 0.4064 0.027 Uiso 1 1 calc R . . C9 C 0.32475(10) 0.28097(9) 0.43770(8) 0.0249(3) Uani 1 1 d . . . H9 H 0.3488 0.3146 0.4084 0.030 Uiso 1 1 calc R . . C10 C 0.36764(9) 0.23966(10) 0.48174(8) 0.0272(3) Uani 1 1 d . . . H10 H 0.4209 0.2460 0.4832 0.033 Uiso 1 1 calc R . . C11 C 0.33303(9) 0.18903(9) 0.52375(8) 0.0213(3) Uani 1 1 d . . . H11 H 0.3625 0.1606 0.5536 0.026 Uiso 1 1 calc R . . C12 C 0.15396(8) 0.04927(8) 0.53181(7) 0.0165(3) Uani 1 1 d . . . C13 C 0.14310(9) 0.05306(9) 0.46333(7) 0.0225(3) Uani 1 1 d . . . H13 H 0.1641 0.0925 0.4385 0.027 Uiso 1 1 calc R . . C14 C 0.10122(10) -0.00151(9) 0.43170(8) 0.0270(4) Uani 1 1 d . . . H14 H 0.0934 0.0008 0.3851 0.032 Uiso 1 1 calc R . . C15 C 0.07088(9) -0.05908(9) 0.46784(9) 0.0270(3) Uani 1 1 d . . . H15 H 0.0428 -0.0964 0.4458 0.032 Uiso 1 1 calc R . . C16 C 0.08117(9) -0.06285(9) 0.53603(9) 0.0264(3) Uani 1 1 d . . . H16 H 0.0600 -0.1023 0.5607 0.032 Uiso 1 1 calc R . . C17 C 0.12261(9) -0.00859(8) 0.56791(8) 0.0209(3) Uani 1 1 d . . . H17 H 0.1297 -0.0109 0.6146 0.025 Uiso 1 1 calc R . . C18 C 0.34955(9) -0.02084(8) 0.58474(7) 0.0204(3) Uani 1 1 d . . . C19 C 0.39927(12) -0.07845(10) 0.57142(9) 0.0348(4) Uani 1 1 d . . . H19 H 0.4225 -0.1048 0.6067 0.042 Uiso 1 1 calc R . . C20 C 0.41428(13) -0.09675(11) 0.50603(10) 0.0384(5) Uani 1 1 d . . . H20 H 0.4475 -0.1362 0.4956 0.046 Uiso 1 1 calc R . . C21 C 0.37998(11) -0.05650(10) 0.45630(9) 0.0333(4) Uani 1 1 d . . . H21 H 0.3892 -0.0676 0.4109 0.040 Uiso 1 1 calc R . . C22 C 0.33197(11) 0.00031(10) 0.47386(8) 0.0305(4) Uani 1 1 d . . . H22 H 0.3088 0.0280 0.4395 0.037 Uiso 1 1 calc R . . C23 C 0.27491(9) -0.07681(8) 0.70192(8) 0.0196(3) Uani 1 1 d . . . C24 C 0.26457(9) -0.08537(10) 0.76991(9) 0.0243(3) Uani 1 1 d . . . H24 H 0.2863 -0.0510 0.7999 0.029 Uiso 1 1 calc R . . C25 C 0.22229(11) -0.14452(9) 0.79410(10) 0.0316(4) Uani 1 1 d . . . H25 H 0.2163 -0.1510 0.8406 0.038 Uiso 1 1 calc R . . C26 C 0.18907(10) -0.19370(9) 0.75037(11) 0.0350(4) Uani 1 1 d . . . H26 H 0.1601 -0.2337 0.7670 0.042 Uiso 1 1 calc R . . C27 C 0.19783(10) -0.18484(9) 0.68286(11) 0.0333(4) Uani 1 1 d . . . H27 H 0.1743 -0.2184 0.6532 0.040 Uiso 1 1 calc R . . C28 C 0.24092(9) -0.12713(10) 0.65791(10) 0.0260(3) Uani 1 1 d . . . H28 H 0.2474 -0.1217 0.6114 0.031 Uiso 1 1 calc R . . C29 C 0.41768(8) 0.00474(8) 0.70961(7) 0.0167(3) Uani 1 1 d . . . C30 C 0.46473(10) 0.06459(9) 0.69554(8) 0.0227(3) Uani 1 1 d . . . H30 H 0.4455 0.1060 0.6722 0.027 Uiso 1 1 calc R . . C31 C 0.53983(10) 0.06307(9) 0.71588(8) 0.0251(3) Uani 1 1 d . . . H31 H 0.5721 0.1034 0.7060 0.030 Uiso 1 1 calc R . . C32 C 0.56773(9) 0.00309(9) 0.75045(8) 0.0257(3) Uani 1 1 d . . . H32 H 0.6194 0.0019 0.7632 0.031 Uiso 1 1 calc R . . C33 C 0.52060(9) -0.05529(9) 0.76660(8) 0.0244(3) Uani 1 1 d . . . H33 H 0.5395 -0.0955 0.7918 0.029 Uiso 1 1 calc R . . C34 C 0.44558(9) -0.05476(8) 0.74583(7) 0.0195(3) Uani 1 1 d . . . H34 H 0.4134 -0.0950 0.7564 0.023 Uiso 1 1 calc R . . Cl1 Cl 0.27804(3) 0.10485(2) 0.794847(18) 0.02590(9) Uani 1 1 d . . . F1 F 0.07041(7) 0.19882(6) 0.87890(5) 0.0400(3) Uani 1 1 d . . . F2 F -0.03457(6) 0.26385(9) 0.85393(6) 0.0541(4) Uani 1 1 d . . . F3 F 0.02578(6) 0.28236(6) 0.95242(5) 0.0322(2) Uani 1 1 d . . . F4 F 0.08003(7) 0.31888(6) 0.85582(5) 0.0409(3) Uani 1 1 d . . . N1 N 0.16636(7) 0.18258(7) 0.68147(6) 0.0158(2) Uani 1 1 d . . . N2 N 0.31645(8) 0.01831(7) 0.53705(6) 0.0224(3) Uani 1 1 d . . . P1 P 0.20800(2) 0.116909(19) 0.577250(17) 0.01411(8) Uani 1 1 d . . . P2 P 0.32558(2) 0.00286(2) 0.670600(18) 0.01603(8) Uani 1 1 d . . . Pd1 Pd 0.252021(6) 0.101979(6) 0.681902(5) 0.01412(4) 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 B1 0.0208(8) 0.0254(9) 0.0148(7) -0.0007(6) -0.0015(6) 0.0029(7) C1 0.0245(7) 0.0152(6) 0.0150(6) -0.0014(5) 0.0006(6) -0.0005(6) C2 0.0250(7) 0.0169(7) 0.0178(7) 0.0002(5) 0.0043(6) 0.0022(6) C3 0.0191(7) 0.0200(7) 0.0223(7) 0.0017(6) 0.0006(6) 0.0029(6) C4 0.0207(7) 0.0193(7) 0.0162(7) 0.0004(5) -0.0009(6) -0.0008(6) C5 0.0194(7) 0.0124(6) 0.0139(6) 0.0004(5) 0.0019(5) -0.0014(5) C6 0.0203(7) 0.0144(7) 0.0127(6) -0.0001(5) 0.0019(5) -0.0014(5) C7 0.0181(7) 0.0214(7) 0.0189(7) 0.0028(6) -0.0007(6) -0.0004(6) C8 0.0275(8) 0.0207(7) 0.0192(7) 0.0044(6) -0.0021(6) -0.0007(6) C9 0.0286(8) 0.0246(8) 0.0214(7) 0.0044(6) 0.0011(6) -0.0100(6) C10 0.0197(7) 0.0345(9) 0.0275(8) 0.0048(7) -0.0007(7) -0.0082(7) C11 0.0194(7) 0.0252(7) 0.0194(7) 0.0024(6) -0.0029(6) -0.0006(6) C12 0.0171(7) 0.0150(6) 0.0174(7) -0.0025(5) 0.0000(5) 0.0015(5) C13 0.0264(8) 0.0234(8) 0.0176(7) -0.0012(6) 0.0008(6) -0.0029(6) C14 0.0295(9) 0.0294(9) 0.0222(8) -0.0083(7) -0.0042(6) 0.0003(7) C15 0.0233(8) 0.0207(7) 0.0372(9) -0.0109(7) -0.0036(7) -0.0008(6) C16 0.0245(8) 0.0179(7) 0.0370(9) 0.0013(7) 0.0015(7) -0.0030(6) C17 0.0228(7) 0.0185(7) 0.0216(7) 0.0015(6) 0.0009(6) -0.0001(6) C18 0.0253(8) 0.0190(7) 0.0170(7) -0.0030(5) -0.0017(6) 0.0026(6) C19 0.0478(11) 0.0326(9) 0.0241(8) -0.0046(7) -0.0051(8) 0.0211(8) C20 0.0506(12) 0.0355(10) 0.0290(9) -0.0085(7) -0.0004(9) 0.0216(9) C21 0.0446(11) 0.0350(9) 0.0202(8) -0.0055(7) 0.0034(7) 0.0090(8) C22 0.0400(10) 0.0332(9) 0.0183(7) 0.0017(7) 0.0020(7) 0.0110(8) C23 0.0172(7) 0.0133(7) 0.0283(8) 0.0013(6) -0.0042(6) 0.0020(6) C24 0.0216(8) 0.0217(8) 0.0297(8) 0.0022(7) 0.0006(6) 0.0001(6) C25 0.0268(9) 0.0249(9) 0.0431(11) 0.0103(7) 0.0080(8) 0.0019(7) C26 0.0208(8) 0.0184(8) 0.0657(13) 0.0059(8) 0.0055(8) -0.0007(6) C27 0.0211(8) 0.0182(8) 0.0606(13) -0.0057(8) -0.0088(8) 0.0005(6) C28 0.0249(8) 0.0184(8) 0.0348(9) -0.0032(7) -0.0091(7) 0.0033(6) C29 0.0189(7) 0.0161(7) 0.0151(6) -0.0016(5) -0.0006(5) 0.0011(5) C30 0.0318(9) 0.0176(7) 0.0189(7) 0.0013(6) -0.0026(6) -0.0034(6) C31 0.0287(8) 0.0261(8) 0.0205(7) -0.0020(6) 0.0005(6) -0.0105(7) C32 0.0200(7) 0.0347(9) 0.0223(7) -0.0039(7) -0.0017(6) -0.0037(7) C33 0.0234(8) 0.0249(8) 0.0248(8) 0.0032(6) -0.0042(6) 0.0022(6) C34 0.0210(7) 0.0168(7) 0.0208(7) 0.0011(6) -0.0009(6) -0.0008(6) Cl1 0.0409(2) 0.02316(19) 0.01363(17) -0.00283(13) -0.00639(16) 0.00849(16) F1 0.0645(8) 0.0236(5) 0.0318(5) -0.0023(4) -0.0064(5) 0.0131(5) F2 0.0217(5) 0.1127(12) 0.0278(6) -0.0102(7) -0.0080(5) 0.0083(6) F3 0.0255(5) 0.0548(7) 0.0161(4) -0.0062(4) 0.0015(4) 0.0044(5) F4 0.0682(8) 0.0312(6) 0.0234(5) 0.0038(4) 0.0000(5) -0.0175(5) N1 0.0203(6) 0.0129(5) 0.0144(6) 0.0007(4) 0.0003(5) -0.0002(5) N2 0.0281(7) 0.0227(6) 0.0164(6) 0.0001(5) 0.0004(5) 0.0054(5) P1 0.01711(17) 0.01386(16) 0.01137(16) 0.00020(13) 0.00021(13) 0.00007(13) P2 0.02017(18) 0.01321(17) 0.01470(16) -0.00008(13) -0.00240(14) 0.00211(14) Pd1 0.01881(7) 0.01236(7) 0.01119(6) -0.00019(3) -0.00116(4) 0.00171(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag B1 F2 1.377(2) . ? B1 F1 1.378(2) . ? B1 F4 1.383(2) . ? B1 F3 1.4006(19) . ? C1 N1 1.3379(18) . ? C1 C2 1.390(2) . ? C2 C3 1.385(2) . ? C3 C4 1.395(2) . ? C4 C5 1.384(2) . ? C5 N1 1.3558(18) . ? C5 P1 1.8393(14) . ? C6 C11 1.392(2) . ? C6 C7 1.398(2) . ? C6 P1 1.8076(15) . ? C7 C8 1.387(2) . ? C8 C9 1.387(2) . ? C9 C10 1.388(2) . ? C10 C11 1.392(2) . ? C12 C17 1.393(2) . ? C12 C13 1.395(2) . ? C12 P1 1.8060(15) . ? C13 C14 1.392(2) . ? C14 C15 1.382(2) . ? C15 C16 1.388(2) . ? C16 C17 1.386(2) . ? C18 N2 1.331(2) . ? C18 C19 1.393(2) . ? C18 P2 1.8325(15) . ? C19 C20 1.385(3) . ? C20 C21 1.381(3) . ? C21 C22 1.382(2) . ? C22 N2 1.343(2) . ? C23 C24 1.391(2) . ? C23 C28 1.408(2) . ? C23 P2 1.8151(16) . ? C24 C25 1.397(2) . ? C25 C26 1.385(3) . ? C26 C27 1.379(3) . ? C27 C28 1.390(3) . ? C29 C34 1.394(2) . ? C29 C30 1.398(2) . ? C29 P2 1.8105(15) . ? C30 C31 1.392(2) . ? C31 C32 1.384(2) . ? C32 C33 1.388(2) . ? C33 C34 1.392(2) . ? Cl1 Pd1 2.3225(5) . ? N1 Pd1 2.1075(12) . ? N2 P1 2.7472(14) . ? P1 Pd1 2.2644(4) . ? P2 Pd1 2.2330(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F2 B1 F1 110.12(14) . . ? F2 B1 F4 110.06(14) . . ? F1 B1 F4 108.11(14) . . ? F2 B1 F3 110.25(13) . . ? F1 B1 F3 109.03(13) . . ? F4 B1 F3 109.23(13) . . ? N1 C1 C2 120.57(14) . . ? C3 C2 C1 119.53(14) . . ? C2 C3 C4 119.98(14) . . ? C5 C4 C3 117.47(14) . . ? N1 C5 C4 122.30(13) . . ? N1 C5 P1 103.38(10) . . ? C4 C5 P1 134.24(11) . . ? C11 C6 C7 119.77(14) . . ? C11 C6 P1 120.75(11) . . ? C7 C6 P1 119.41(11) . . ? C8 C7 C6 120.20(14) . . ? C9 C8 C7 119.85(15) . . ? C8 C9 C10 120.16(15) . . ? C9 C10 C11 120.33(15) . . ? C6 C11 C10 119.64(14) . . ? C17 C12 C13 119.92(14) . . ? C17 C12 P1 117.32(11) . . ? C13 C12 P1 122.76(12) . . ? C14 C13 C12 119.43(15) . . ? C15 C14 C13 120.25(15) . . ? C14 C15 C16 120.52(15) . . ? C17 C16 C15 119.55(15) . . ? C16 C17 C12 120.32(14) . . ? N2 C18 C19 122.67(15) . . ? N2 C18 P2 117.01(11) . . ? C19 C18 P2 120.30(12) . . ? C20 C19 C18 119.01(16) . . ? C21 C20 C19 118.62(16) . . ? C20 C21 C22 118.65(16) . . ? N2 C22 C21 123.36(16) . . ? C24 C23 C28 119.43(16) . . ? C24 C23 P2 119.77(12) . . ? C28 C23 P2 120.62(13) . . ? C23 C24 C25 120.01(17) . . ? C26 C25 C24 120.07(18) . . ? C27 C26 C25 120.31(17) . . ? C26 C27 C28 120.42(17) . . ? C27 C28 C23 119.73(18) . . ? C34 C29 C30 119.82(14) . . ? C34 C29 P2 122.12(11) . . ? C30 C29 P2 117.59(11) . . ? C31 C30 C29 119.61(15) . . ? C32 C31 C30 120.32(15) . . ? C31 C32 C33 120.29(15) . . ? C32 C33 C34 119.86(15) . . ? C33 C34 C29 120.03(14) . . ? C1 N1 C5 120.13(13) . . ? C1 N1 Pd1 136.20(10) . . ? C5 N1 Pd1 101.73(9) . . ? C18 N2 C22 117.68(14) . . ? C18 N2 P1 116.28(10) . . ? C22 N2 P1 125.53(11) . . ? C12 P1 C6 111.28(7) . . ? C12 P1 C5 105.55(7) . . ? C6 P1 C5 103.23(6) . . ? C12 P1 Pd1 124.97(5) . . ? C6 P1 Pd1 119.61(5) . . ? C5 P1 Pd1 82.63(5) . . ? C12 P1 N2 77.15(5) . . ? C6 P1 N2 84.90(6) . . ? C5 P1 N2 169.43(5) . . ? Pd1 P1 N2 87.48(3) . . ? C29 P2 C23 108.01(7) . . ? C29 P2 C18 101.87(7) . . ? C23 P2 C18 104.81(7) . . ? C29 P2 Pd1 117.76(5) . . ? C23 P2 Pd1 108.58(5) . . ? C18 P2 Pd1 114.87(5) . . ? N1 Pd1 P2 168.19(3) . . ? N1 Pd1 P1 70.45(3) . . ? P2 Pd1 P1 101.666(14) . . ? N1 Pd1 Cl1 97.54(3) . . ? P2 Pd1 Cl1 90.134(14) . . ? P1 Pd1 Cl1 167.983(15) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 -0.4(2) . . . . ? C1 C2 C3 C4 -0.4(2) . . . . ? C2 C3 C4 C5 0.3(2) . . . . ? C3 C4 C5 N1 0.7(2) . . . . ? C3 C4 C5 P1 177.09(12) . . . . ? C11 C6 C7 C8 2.3(2) . . . . ? P1 C6 C7 C8 179.17(12) . . . . ? C6 C7 C8 C9 -1.3(2) . . . . ? C7 C8 C9 C10 -0.6(3) . . . . ? C8 C9 C10 C11 1.4(3) . . . . ? C7 C6 C11 C10 -1.4(2) . . . . ? P1 C6 C11 C10 -178.26(12) . . . . ? C9 C10 C11 C6 -0.4(3) . . . . ? C17 C12 C13 C14 -0.3(2) . . . . ? P1 C12 C13 C14 179.49(12) . . . . ? C12 C13 C14 C15 -0.2(2) . . . . ? C13 C14 C15 C16 0.6(3) . . . . ? C14 C15 C16 C17 -0.4(3) . . . . ? C15 C16 C17 C12 -0.2(2) . . . . ? C13 C12 C17 C16 0.6(2) . . . . ? P1 C12 C17 C16 -179.30(12) . . . . ? N2 C18 C19 C20 -1.0(3) . . . . ? P2 C18 C19 C20 177.77(16) . . . . ? C18 C19 C20 C21 0.8(3) . . . . ? C19 C20 C21 C22 -0.1(3) . . . . ? C20 C21 C22 N2 -0.4(3) . . . . ? C28 C23 C24 C25 1.5(2) . . . . ? P2 C23 C24 C25 176.70(13) . . . . ? C23 C24 C25 C26 -1.6(3) . . . . ? C24 C25 C26 C27 0.3(3) . . . . ? C25 C26 C27 C28 0.9(3) . . . . ? C26 C27 C28 C23 -0.9(3) . . . . ? C24 C23 C28 C27 -0.3(2) . . . . ? P2 C23 C28 C27 -175.41(12) . . . . ? C34 C29 C30 C31 2.2(2) . . . . ? P2 C29 C30 C31 -170.14(12) . . . . ? C29 C30 C31 C32 -0.7(2) . . . . ? C30 C31 C32 C33 -1.6(2) . . . . ? C31 C32 C33 C34 2.4(2) . . . . ? C32 C33 C34 C29 -0.8(2) . . . . ? C30 C29 C34 C33 -1.5(2) . . . . ? P2 C29 C34 C33 170.52(12) . . . . ? C2 C1 N1 C5 1.3(2) . . . . ? C2 C1 N1 Pd1 -159.51(11) . . . . ? C4 C5 N1 C1 -1.5(2) . . . . ? P1 C5 N1 C1 -178.86(11) . . . . ? C4 C5 N1 Pd1 165.10(12) . . . . ? P1 C5 N1 Pd1 -12.27(9) . . . . ? C19 C18 N2 C22 0.5(3) . . . . ? P2 C18 N2 C22 -178.32(13) . . . . ? C19 C18 N2 P1 172.68(14) . . . . ? P2 C18 N2 P1 -6.11(16) . . . . ? C21 C22 N2 C18 0.2(3) . . . . ? C21 C22 N2 P1 -171.17(14) . . . . ? C17 C12 P1 C6 172.08(11) . . . . ? C13 C12 P1 C6 -7.76(15) . . . . ? C17 C12 P1 C5 -76.61(13) . . . . ? C13 C12 P1 C5 103.55(13) . . . . ? C17 C12 P1 Pd1 15.23(14) . . . . ? C13 C12 P1 Pd1 -164.61(11) . . . . ? C17 C12 P1 N2 92.84(12) . . . . ? C13 C12 P1 N2 -87.00(13) . . . . ? C11 C6 P1 C12 -122.70(13) . . . . ? C7 C6 P1 C12 60.45(14) . . . . ? C11 C6 P1 C5 124.52(13) . . . . ? C7 C6 P1 C5 -52.33(13) . . . . ? C11 C6 P1 Pd1 35.55(14) . . . . ? C7 C6 P1 Pd1 -141.30(10) . . . . ? C11 C6 P1 N2 -48.62(12) . . . . ? C7 C6 P1 N2 134.53(12) . . . . ? N1 C5 P1 C12 135.58(9) . . . . ? C4 C5 P1 C12 -41.31(16) . . . . ? N1 C5 P1 C6 -107.51(10) . . . . ? C4 C5 P1 C6 75.59(16) . . . . ? N1 C5 P1 Pd1 11.26(8) . . . . ? C4 C5 P1 Pd1 -165.63(15) . . . . ? N1 C5 P1 N2 32.1(4) . . . . ? C4 C5 P1 N2 -144.8(3) . . . . ? C18 N2 P1 C12 -112.50(13) . . . . ? C22 N2 P1 C12 59.02(15) . . . . ? C18 N2 P1 C6 134.28(12) . . . . ? C22 N2 P1 C6 -54.20(15) . . . . ? C18 N2 P1 C5 -6.4(4) . . . . ? C22 N2 P1 C5 165.1(3) . . . . ? C18 N2 P1 Pd1 14.25(11) . . . . ? C22 N2 P1 Pd1 -174.23(14) . . . . ? C34 C29 P2 C23 11.67(14) . . . . ? C30 C29 P2 C23 -176.16(12) . . . . ? C34 C29 P2 C18 -98.39(13) . . . . ? C30 C29 P2 C18 73.79(13) . . . . ? C34 C29 P2 Pd1 135.01(11) . . . . ? C30 C29 P2 Pd1 -52.82(13) . . . . ? C24 C23 P2 C29 56.09(14) . . . . ? C28 C23 P2 C29 -128.81(13) . . . . ? C24 C23 P2 C18 164.13(13) . . . . ? C28 C23 P2 C18 -20.77(15) . . . . ? C24 C23 P2 Pd1 -72.65(13) . . . . ? C28 C23 P2 Pd1 102.44(13) . . . . ? N2 C18 P2 C29 -134.07(13) . . . . ? C19 C18 P2 C29 47.12(16) . . . . ? N2 C18 P2 C23 113.45(13) . . . . ? C19 C18 P2 C23 -65.37(16) . . . . ? N2 C18 P2 Pd1 -5.61(15) . . . . ? C19 C18 P2 Pd1 175.58(13) . . . . ? C1 N1 Pd1 P2 123.96(17) . . . . ? C5 N1 Pd1 P2 -39.2(2) . . . . ? C1 N1 Pd1 P1 173.42(15) . . . . ? C5 N1 Pd1 P1 10.27(8) . . . . ? C1 N1 Pd1 Cl1 -6.17(15) . . . . ? C5 N1 Pd1 Cl1 -169.33(8) . . . . ? C29 P2 Pd1 N1 -177.54(17) . . . . ? C23 P2 Pd1 N1 -54.48(17) . . . . ? C18 P2 Pd1 N1 62.45(18) . . . . ? C29 P2 Pd1 P1 135.47(5) . . . . ? C23 P2 Pd1 P1 -101.47(6) . . . . ? C18 P2 Pd1 P1 15.46(6) . . . . ? C29 P2 Pd1 Cl1 -46.82(6) . . . . ? C23 P2 Pd1 Cl1 76.24(6) . . . . ? C18 P2 Pd1 Cl1 -166.83(6) . . . . ? C12 P1 Pd1 N1 -111.31(7) . . . . ? C6 P1 Pd1 N1 93.61(7) . . . . ? C5 P1 Pd1 N1 -7.45(6) . . . . ? N2 P1 Pd1 N1 176.29(5) . . . . ? C12 P1 Pd1 P2 59.56(6) . . . . ? C6 P1 Pd1 P2 -95.52(6) . . . . ? C5 P1 Pd1 P2 163.41(4) . . . . ? N2 P1 Pd1 P2 -12.84(3) . . . . ? C12 P1 Pd1 Cl1 -109.38(9) . . . . ? C6 P1 Pd1 Cl1 95.54(9) . . . . ? C5 P1 Pd1 Cl1 -5.52(9) . . . . ? N2 P1 Pd1 Cl1 178.22(7) . . . . ? _diffrn_measured_fraction_theta_max 0.957 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.957 _refine_diff_density_max 0.633 _refine_diff_density_min -0.431 _refine_diff_density_rms 0.064 #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 746626' #TrackingRef 'data.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H46 Cl2 N3 O2 P3 Pd' _chemical_formula_weight 1003.12 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' Pd Pd -0.9988 1.0072 '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' 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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.8634(16) _cell_length_b 11.1293(15) _cell_length_c 35.892(5) _cell_angle_alpha 90.00 _cell_angle_beta 94.840(2) _cell_angle_gamma 90.00 _cell_volume 4722.0(11) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.411 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2056 _exptl_absorpt_coefficient_mu 0.651 _exptl_absorpt_correction_type semi-empirical _exptl_absorpt_correction_T_min 0.762 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker Apex' _diffrn_measurement_method /w _diffrn_reflns_number 23535 _diffrn_reflns_av_R_equivalents 0.0387 _diffrn_reflns_av_sigmaI/netI 0.0477 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 4.11 _diffrn_reflns_theta_max 25.03 _reflns_number_total 8280 _reflns_number_gt 7303 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0796P)^2^+32.5085P] 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_number_reflns 8280 _refine_ls_number_parameters 558 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0742 _refine_ls_R_factor_gt 0.0649 _refine_ls_wR_factor_ref 0.1708 _refine_ls_wR_factor_gt 0.1653 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3367(4) 0.0674(5) 0.10633(15) 0.0178(11) Uani 1 1 d . . . C2 C 0.3395(5) -0.0503(5) 0.11909(17) 0.0253(13) Uani 1 1 d . . . H2 H 0.3175 -0.0680 0.1433 0.030 Uiso 1 1 calc R . . C3 C 0.3739(6) -0.1412(6) 0.0969(2) 0.0368(16) Uani 1 1 d . . . H3 H 0.3770 -0.2213 0.1061 0.044 Uiso 1 1 calc R . . C4 C 0.4040(5) -0.1177(6) 0.0614(2) 0.0372(17) Uani 1 1 d . . . H4 H 0.4265 -0.1813 0.0461 0.045 Uiso 1 1 calc R . . C5 C 0.4014(5) -0.0017(6) 0.04845(17) 0.0310(15) Uani 1 1 d . . . H5 H 0.4229 0.0151 0.0241 0.037 Uiso 1 1 calc R . . C6 C 0.3674(4) 0.0915(6) 0.07081(15) 0.0211(12) Uani 1 1 d . . . H6 H 0.3653 0.1716 0.0617 0.025 Uiso 1 1 calc R . . C7 C 0.3391(5) 0.3238(5) 0.11766(15) 0.0198(11) Uani 1 1 d . . . C8 C 0.2662(5) 0.4139(5) 0.10569(16) 0.0223(12) Uani 1 1 d . . . H8 H 0.1872 0.4056 0.1077 0.027 Uiso 1 1 calc R . . C9 C 0.3092(6) 0.5181(6) 0.09058(18) 0.0301(14) Uani 1 1 d . . . H9 H 0.2592 0.5805 0.0818 0.036 Uiso 1 1 calc R . . C10 C 0.4248(6) 0.5307(6) 0.08839(19) 0.0334(15) Uani 1 1 d . . . H10 H 0.4537 0.6026 0.0786 0.040 Uiso 1 1 calc R . . C11 C 0.4981(5) 0.4395(6) 0.10042(18) 0.0308(14) Uani 1 1 d . . . H11 H 0.5771 0.4486 0.0988 0.037 Uiso 1 1 calc R . . C12 C 0.4565(5) 0.3362(5) 0.11462(16) 0.0230(12) Uani 1 1 d . . . H12 H 0.5066 0.2728 0.1225 0.028 Uiso 1 1 calc R . . C13 C 0.3646(4) 0.1577(5) 0.18165(15) 0.0187(12) Uani 1 1 d . . . C14 C 0.4486(5) 0.2324(6) 0.19828(16) 0.0267(13) Uani 1 1 d . . . H14 H 0.4704 0.3033 0.1861 0.032 Uiso 1 1 calc R . . C15 C 0.4998(5) 0.2008(7) 0.23315(18) 0.0377(17) Uani 1 1 d . . . H15 H 0.5574 0.2501 0.2450 0.045 Uiso 1 1 calc R . . C16 C 0.4669(6) 0.0983(7) 0.25034(18) 0.0399(18) Uani 1 1 d . . . H16 H 0.5017 0.0751 0.2741 0.048 Uiso 1 1 calc R . . C17 C 0.3821(7) 0.0295(7) 0.23247(19) 0.0437(18) Uani 1 1 d . . . H17 H 0.3589 -0.0411 0.2446 0.052 Uiso 1 1 calc R . . C18 C -0.1687(4) 0.0676(5) 0.18166(14) 0.0177(11) Uani 1 1 d . . . C19 C -0.2826(5) 0.0924(6) 0.17152(16) 0.0234(12) Uani 1 1 d . . . H19 H -0.3078 0.1732 0.1689 0.028 Uiso 1 1 calc R . . C20 C -0.3585(5) -0.0014(6) 0.16525(18) 0.0314(15) Uani 1 1 d . . . H20 H -0.4363 0.0152 0.1589 0.038 Uiso 1 1 calc R . . C21 C -0.3214(5) -0.1191(6) 0.16815(18) 0.0311(14) Uani 1 1 d . . . H21 H -0.3728 -0.1835 0.1629 0.037 Uiso 1 1 calc R . . C22 C -0.2085(6) -0.1418(6) 0.17875(18) 0.0316(14) Uani 1 1 d . . . H22 H -0.1831 -0.2226 0.1814 0.038 Uiso 1 1 calc R . . C23 C -0.1325(5) -0.0494(5) 0.18558(16) 0.0236(12) Uani 1 1 d . . . H23 H -0.0553 -0.0664 0.1930 0.028 Uiso 1 1 calc R . . C24 C -0.1409(4) 0.3244(5) 0.18863(16) 0.0178(11) Uani 1 1 d . . . C25 C -0.2155(5) 0.3431(5) 0.21585(17) 0.0218(12) Uani 1 1 d . . . H25 H -0.2201 0.2863 0.2354 0.026 Uiso 1 1 calc R . . C26 C -0.2838(5) 0.4454(6) 0.21448(18) 0.0299(14) Uani 1 1 d . . . H26 H -0.3332 0.4599 0.2335 0.036 Uiso 1 1 calc R . . C27 C -0.2791(5) 0.5247(6) 0.18553(19) 0.0316(15) Uani 1 1 d . . . H27 H -0.3269 0.5933 0.1843 0.038 Uiso 1 1 calc R . . C28 C -0.2053(5) 0.5064(6) 0.15781(19) 0.0302(14) Uani 1 1 d . . . H28 H -0.2030 0.5622 0.1378 0.036 Uiso 1 1 calc R . . C29 C -0.1350(5) 0.4062(5) 0.15954(16) 0.0219(12) Uani 1 1 d . . . H29 H -0.0835 0.3937 0.1410 0.026 Uiso 1 1 calc R . . C30 C 0.0034(4) 0.1576(5) 0.23568(15) 0.0166(11) Uani 1 1 d . . . C31 C 0.0054(5) 0.2394(7) 0.26476(17) 0.0320(14) Uani 1 1 d . . . H31 H -0.0318 0.3147 0.2614 0.038 Uiso 1 1 calc R . . C32 C 0.0623(6) 0.2102(8) 0.29884(19) 0.046(2) Uani 1 1 d . . . H32 H 0.0647 0.2657 0.3190 0.055 Uiso 1 1 calc R . . C33 C 0.1157(5) 0.1000(8) 0.3035(2) 0.043(2) Uani 1 1 d . . . H33 H 0.1540 0.0781 0.3268 0.051 Uiso 1 1 calc R . . C34 C 0.1118(6) 0.0244(7) 0.2739(2) 0.0449(19) Uani 1 1 d . . . H34 H 0.1488 -0.0510 0.2772 0.054 Uiso 1 1 calc R . . C35 C -0.1193(4) 0.0766(5) 0.09494(15) 0.0203(12) Uani 1 1 d . . . C36 C -0.2021(5) -0.0124(6) 0.08994(15) 0.0229(12) Uani 1 1 d . . . H36 H -0.1847 -0.0935 0.0964 0.028 Uiso 1 1 calc R . . C37 C -0.3102(5) 0.0193(6) 0.07546(16) 0.0277(14) Uani 1 1 d . . . H37 H -0.3673 -0.0404 0.0719 0.033 Uiso 1 1 calc R . . C38 C -0.3351(5) 0.1385(7) 0.06622(19) 0.0354(16) Uani 1 1 d . . . H38 H -0.4082 0.1604 0.0555 0.043 Uiso 1 1 calc R . . C39 C -0.2521(6) 0.2237(7) 0.0728(2) 0.0432(18) Uani 1 1 d . . . H39 H -0.2698 0.3054 0.0673 0.052 Uiso 1 1 calc R . . C40 C -0.1442(5) 0.1951(6) 0.08717(19) 0.0285(14) Uani 1 1 d . . . H40 H -0.0883 0.2557 0.0916 0.034 Uiso 1 1 calc R . . C41 C 0.1082(4) -0.1299(6) 0.15718(16) 0.0252(13) Uani 1 1 d . . . H41 H 0.1360 -0.0647 0.1724 0.030 Uiso 1 1 calc R . . C42 C 0.1266(5) -0.2474(6) 0.16966(18) 0.0287(14) Uani 1 1 d . . . H42 H 0.1667 -0.2627 0.1932 0.034 Uiso 1 1 calc R . . C43 C 0.0851(5) -0.3421(6) 0.1471(2) 0.0345(16) Uani 1 1 d . . . H43 H 0.0969 -0.4224 0.1555 0.041 Uiso 1 1 calc R . . C44 C 0.0278(5) -0.3213(6) 0.11306(19) 0.0333(15) Uani 1 1 d . . . H44 H 0.0003 -0.3871 0.0981 0.040 Uiso 1 1 calc R . . C45 C 0.0096(5) -0.2054(5) 0.10038(17) 0.0229(12) Uani 1 1 d . . . H45 H -0.0300 -0.1918 0.0766 0.027 Uiso 1 1 calc R . . C46 C 0.0495(4) -0.1068(5) 0.12252(15) 0.0186(11) Uani 1 1 d . . . C47 C 0.0881(4) 0.0751(5) 0.06459(15) 0.0193(11) Uani 1 1 d . . . C48 C 0.1146(4) -0.0145(5) 0.04026(16) 0.0218(12) Uani 1 1 d . . . H48 H 0.1067 -0.0966 0.0469 0.026 Uiso 1 1 calc R . . C49 C 0.1534(5) 0.0166(6) 0.00574(16) 0.0266(13) Uani 1 1 d . . . H49 H 0.1717 -0.0440 -0.0114 0.032 Uiso 1 1 calc R . . C50 C 0.1646(5) 0.1362(7) -0.00302(17) 0.0321(15) Uani 1 1 d . . . H50 H 0.1910 0.1592 -0.0263 0.039 Uiso 1 1 calc R . . C51 C 0.1374(6) 0.2215(7) 0.0221(2) 0.0393(17) Uani 1 1 d . . . H51 H 0.1444 0.3038 0.0157 0.047 Uiso 1 1 calc R . . Cl1 Cl 0.15561(11) 0.34914(12) 0.19017(4) 0.0192(3) Uani 1 1 d . . . Cl2 Cl 0.6999(2) 0.6786(3) 0.07220(8) 0.0930(11) Uani 1 1 d . . . N1 N 0.3303(5) 0.0577(5) 0.19849(15) 0.0385(14) Uani 1 1 d . . . N2 N 0.0583(5) 0.0494(6) 0.23967(18) 0.0419(14) Uani 1 1 d . . . N3 N 0.1004(5) 0.1937(5) 0.05628(16) 0.0378(14) Uani 1 1 d . . . P1 P 0.28504(11) 0.18469(13) 0.13625(4) 0.0155(3) Uani 1 1 d . . . P2 P -0.06037(11) 0.18452(13) 0.18813(4) 0.0155(3) Uani 1 1 d . . . P3 P 0.02956(11) 0.04904(13) 0.10940(4) 0.0156(3) Uani 1 1 d . . . Pd1 Pd 0.09714(3) 0.18571(4) 0.152516(11) 0.01355(14) Uani 1 1 d . . . O1 O 0.4493(7) 0.2808(10) 0.0026(2) 0.116(4) Uani 1 1 d . . . O2 O 0.8637(13) 0.4847(14) 0.0632(4) 0.091(3) Uiso 0.552(12) 1 d P . . O2' O 0.8963(16) 0.4839(17) 0.0360(6) 0.091(3) Uiso 0.448(12) 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.005(2) 0.018(3) 0.030(3) 0.001(2) -0.001(2) 0.000(2) C2 0.021(3) 0.024(3) 0.030(3) -0.001(3) -0.003(2) -0.003(2) C3 0.034(4) 0.020(3) 0.054(4) -0.002(3) -0.009(3) 0.003(3) C4 0.025(3) 0.032(4) 0.052(4) -0.022(3) -0.007(3) 0.008(3) C5 0.013(3) 0.051(4) 0.030(3) -0.013(3) 0.004(2) -0.001(3) C6 0.009(2) 0.026(3) 0.028(3) -0.002(2) 0.000(2) -0.002(2) C7 0.020(3) 0.015(3) 0.024(3) -0.003(2) 0.006(2) -0.005(2) C8 0.024(3) 0.016(3) 0.028(3) 0.000(2) 0.007(2) 0.001(2) C9 0.037(3) 0.019(3) 0.036(3) 0.005(3) 0.013(3) 0.004(3) C10 0.041(4) 0.019(3) 0.043(4) 0.003(3) 0.017(3) -0.007(3) C11 0.024(3) 0.026(3) 0.044(4) -0.003(3) 0.011(3) -0.012(3) C12 0.019(3) 0.017(3) 0.034(3) 0.002(2) 0.005(2) -0.002(2) C13 0.015(3) 0.021(3) 0.020(3) 0.001(2) 0.004(2) 0.005(2) C14 0.020(3) 0.034(4) 0.026(3) 0.000(3) -0.001(2) -0.003(3) C15 0.020(3) 0.058(5) 0.034(3) -0.015(3) -0.005(3) 0.005(3) C16 0.047(4) 0.047(5) 0.026(3) 0.009(3) 0.008(3) 0.026(4) C17 0.064(5) 0.036(4) 0.033(4) 0.015(3) 0.014(3) 0.006(4) C18 0.016(3) 0.020(3) 0.018(3) 0.000(2) 0.005(2) -0.001(2) C19 0.019(3) 0.021(3) 0.030(3) -0.004(2) 0.002(2) -0.001(2) C20 0.012(3) 0.038(4) 0.044(4) -0.006(3) 0.005(3) -0.002(3) C21 0.024(3) 0.031(4) 0.039(4) -0.004(3) 0.007(3) -0.013(3) C22 0.041(4) 0.020(3) 0.033(3) -0.003(3) -0.001(3) 0.003(3) C23 0.015(3) 0.029(3) 0.027(3) -0.004(3) 0.000(2) 0.004(2) C24 0.012(2) 0.008(3) 0.033(3) -0.004(2) 0.000(2) -0.003(2) C25 0.018(3) 0.014(3) 0.033(3) -0.001(2) 0.001(2) 0.002(2) C26 0.023(3) 0.027(3) 0.041(4) -0.009(3) 0.009(3) 0.004(3) C27 0.022(3) 0.018(3) 0.055(4) -0.003(3) 0.002(3) 0.005(2) C28 0.027(3) 0.020(3) 0.043(4) 0.007(3) 0.003(3) 0.004(3) C29 0.020(3) 0.016(3) 0.029(3) 0.000(2) 0.001(2) -0.003(2) C30 0.010(2) 0.013(3) 0.027(3) 0.004(2) 0.003(2) -0.001(2) C31 0.026(3) 0.039(4) 0.031(3) -0.006(3) -0.002(3) 0.002(3) C32 0.026(3) 0.084(6) 0.026(3) -0.016(4) -0.001(3) -0.006(4) C33 0.017(3) 0.066(5) 0.043(4) 0.031(4) -0.008(3) -0.010(3) C34 0.033(4) 0.029(4) 0.068(5) 0.019(4) -0.021(3) 0.000(3) C35 0.010(2) 0.028(3) 0.023(3) -0.002(2) 0.002(2) -0.001(2) C36 0.020(3) 0.029(3) 0.020(3) 0.000(2) 0.003(2) -0.002(2) C37 0.010(3) 0.044(4) 0.029(3) -0.001(3) 0.002(2) -0.005(3) C38 0.013(3) 0.053(4) 0.040(4) 0.010(3) 0.001(3) 0.006(3) C39 0.024(3) 0.036(4) 0.071(5) 0.009(4) 0.013(3) 0.014(3) C40 0.014(3) 0.020(3) 0.052(4) -0.002(3) 0.004(3) 0.003(2) C41 0.012(3) 0.041(4) 0.023(3) -0.001(3) 0.005(2) -0.003(2) C42 0.023(3) 0.026(4) 0.038(3) 0.013(3) 0.003(3) 0.008(3) C43 0.031(3) 0.017(3) 0.058(4) 0.005(3) 0.018(3) 0.004(3) C44 0.028(3) 0.027(4) 0.046(4) -0.007(3) 0.015(3) -0.006(3) C45 0.019(3) 0.013(3) 0.037(3) -0.004(2) 0.007(2) -0.002(2) C46 0.013(2) 0.015(3) 0.029(3) 0.000(2) 0.006(2) -0.001(2) C47 0.014(2) 0.021(3) 0.022(3) 0.002(2) 0.001(2) -0.003(2) C48 0.013(2) 0.024(3) 0.029(3) -0.002(2) 0.003(2) -0.002(2) C49 0.019(3) 0.035(4) 0.025(3) -0.006(3) 0.001(2) -0.003(3) C50 0.024(3) 0.050(4) 0.023(3) 0.008(3) 0.005(2) -0.002(3) C51 0.039(4) 0.035(4) 0.047(4) 0.012(3) 0.018(3) -0.004(3) Cl1 0.0173(6) 0.0132(6) 0.0273(7) -0.0056(5) 0.0035(5) -0.0030(5) Cl2 0.0724(16) 0.111(2) 0.0898(18) 0.0611(17) -0.0251(14) -0.0561(16) N1 0.041(3) 0.040(4) 0.035(3) 0.010(3) 0.007(2) -0.002(3) N2 0.029(3) 0.040(4) 0.056(4) 0.009(3) -0.006(3) 0.003(3) N3 0.039(3) 0.032(3) 0.046(3) 0.002(3) 0.018(3) 0.001(3) P1 0.0099(6) 0.0148(7) 0.0220(7) 0.0013(6) 0.0022(5) -0.0010(5) P2 0.0112(6) 0.0154(7) 0.0203(7) -0.0001(6) 0.0029(5) 0.0016(5) P3 0.0099(6) 0.0171(7) 0.0197(7) -0.0005(6) 0.0013(5) -0.0004(5) Pd1 0.0090(2) 0.0129(2) 0.0189(2) -0.00043(16) 0.00212(14) -0.00005(15) O1 0.067(5) 0.196(10) 0.089(6) 0.058(6) 0.025(4) 0.032(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C6 1.381(8) . ? C1 C2 1.387(8) . ? C1 P1 1.829(6) . ? C2 C3 1.372(9) . ? C3 C4 1.374(10) . ? C4 C5 1.372(10) . ? C5 C6 1.392(8) . ? C7 C8 1.370(8) . ? C7 C12 1.414(8) . ? C7 P1 1.823(6) . ? C8 C9 1.395(8) . ? C9 C10 1.387(9) . ? C10 C11 1.382(9) . ? C11 C12 1.366(8) . ? C13 N1 1.345(8) . ? C13 C14 1.392(8) . ? C13 P1 1.838(5) . ? C14 C15 1.390(9) . ? C15 C16 1.369(11) . ? C16 C17 1.378(11) . ? C17 N1 1.355(9) . ? C18 C23 1.376(8) . ? C18 C19 1.396(8) . ? C18 P2 1.830(5) . ? C19 C20 1.384(9) . ? C20 C21 1.383(9) . ? C21 C22 1.384(9) . ? C22 C23 1.376(9) . ? C24 C25 1.388(8) . ? C24 C29 1.392(8) . ? C24 P2 1.827(5) . ? C25 C26 1.397(8) . ? C26 C27 1.368(9) . ? C27 C28 1.395(9) . ? C28 C29 1.391(8) . ? C30 N2 1.371(8) . ? C30 C31 1.384(8) . ? C30 P2 1.832(5) . ? C31 C32 1.385(9) . ? C32 C33 1.383(11) . ? C33 C34 1.354(11) . ? C34 N2 1.362(9) . ? C35 C40 1.375(8) . ? C35 C36 1.396(8) . ? C35 P3 1.824(5) . ? C36 C37 1.388(8) . ? C37 C38 1.393(10) . ? C38 C39 1.374(10) . ? C39 C40 1.376(9) . ? C41 C42 1.394(9) . ? C41 C46 1.397(8) . ? C42 C43 1.393(10) . ? C43 C44 1.367(10) . ? C44 C45 1.378(9) . ? C45 C46 1.413(8) . ? C46 P3 1.808(6) . ? C47 N3 1.364(8) . ? C47 C48 1.379(8) . ? C47 P3 1.828(5) . ? C48 C49 1.401(8) . ? C49 C50 1.377(9) . ? C50 C51 1.368(10) . ? C51 N3 1.372(8) . ? Cl1 Pd1 2.3361(13) . ? P1 Pd1 2.3515(13) . ? P2 Pd1 2.3515(13) . ? P3 Pd1 2.2675(14) . ? O2 O2' 1.08(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 C1 C2 119.2(5) . . ? C6 C1 P1 122.1(4) . . ? C2 C1 P1 118.7(4) . . ? C3 C2 C1 120.3(6) . . ? C2 C3 C4 120.7(6) . . ? C5 C4 C3 119.6(6) . . ? C4 C5 C6 120.3(6) . . ? C1 C6 C5 119.9(6) . . ? C8 C7 C12 120.3(5) . . ? C8 C7 P1 120.3(4) . . ? C12 C7 P1 119.4(4) . . ? C7 C8 C9 119.3(5) . . ? C10 C9 C8 120.1(6) . . ? C11 C10 C9 120.4(6) . . ? C12 C11 C10 119.8(6) . . ? C11 C12 C7 120.0(6) . . ? N1 C13 C14 122.2(5) . . ? N1 C13 P1 112.4(4) . . ? C14 C13 P1 125.3(4) . . ? C15 C14 C13 118.5(6) . . ? C16 C15 C14 119.8(6) . . ? C15 C16 C17 118.5(6) . . ? N1 C17 C16 123.2(7) . . ? C23 C18 C19 120.1(5) . . ? C23 C18 P2 116.7(4) . . ? C19 C18 P2 123.1(4) . . ? C20 C19 C18 119.7(6) . . ? C21 C20 C19 120.2(5) . . ? C20 C21 C22 119.3(6) . . ? C23 C22 C21 121.1(6) . . ? C18 C23 C22 119.6(5) . . ? C25 C24 C29 120.3(5) . . ? C25 C24 P2 120.0(4) . . ? C29 C24 P2 119.4(4) . . ? C24 C25 C26 120.0(6) . . ? C27 C26 C25 119.5(6) . . ? C26 C27 C28 121.1(6) . . ? C29 C28 C27 119.7(6) . . ? C28 C29 C24 119.4(5) . . ? N2 C30 C31 121.4(5) . . ? N2 C30 P2 113.3(4) . . ? C31 C30 P2 125.0(4) . . ? C30 C31 C32 119.2(7) . . ? C33 C32 C31 119.9(7) . . ? C34 C33 C32 118.1(6) . . ? C33 C34 N2 124.3(7) . . ? C40 C35 C36 121.2(5) . . ? C40 C35 P3 113.9(4) . . ? C36 C35 P3 124.8(5) . . ? C37 C36 C35 119.1(6) . . ? C36 C37 C38 120.1(6) . . ? C39 C38 C37 118.8(6) . . ? C38 C39 C40 122.4(7) . . ? C35 C40 C39 118.4(6) . . ? C42 C41 C46 120.7(6) . . ? C43 C42 C41 119.0(6) . . ? C44 C43 C42 121.1(6) . . ? C43 C44 C45 120.4(6) . . ? C44 C45 C46 120.3(6) . . ? C41 C46 C45 118.5(5) . . ? C41 C46 P3 116.9(4) . . ? C45 C46 P3 124.6(4) . . ? N3 C47 C48 121.8(5) . . ? N3 C47 P3 113.7(4) . . ? C48 C47 P3 124.5(4) . . ? C47 C48 C49 119.4(6) . . ? C50 C49 C48 119.1(6) . . ? C51 C50 C49 119.2(6) . . ? C50 C51 N3 123.0(7) . . ? C13 N1 C17 117.7(6) . . ? C34 N2 C30 117.0(6) . . ? C47 N3 C51 117.5(6) . . ? C7 P1 C1 104.2(2) . . ? C7 P1 C13 107.0(3) . . ? C1 P1 C13 103.4(2) . . ? C7 P1 Pd1 117.17(18) . . ? C1 P1 Pd1 121.40(17) . . ? C13 P1 Pd1 101.98(17) . . ? C24 P2 C18 104.2(2) . . ? C24 P2 C30 107.8(2) . . ? C18 P2 C30 103.4(2) . . ? C24 P2 Pd1 116.14(18) . . ? C18 P2 Pd1 121.13(17) . . ? C30 P2 Pd1 102.88(16) . . ? C46 P3 C35 109.8(3) . . ? C46 P3 C47 109.3(3) . . ? C35 P3 C47 98.8(2) . . ? C46 P3 Pd1 115.78(19) . . ? C35 P3 Pd1 111.07(19) . . ? C47 P3 Pd1 110.80(18) . . ? P3 Pd1 Cl1 171.00(5) . . ? P3 Pd1 P2 96.65(5) . . ? Cl1 Pd1 P2 84.30(5) . . ? P3 Pd1 P1 96.62(5) . . ? Cl1 Pd1 P1 84.61(5) . . ? P2 Pd1 P1 161.51(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 1.0(8) . . . . ? P1 C1 C2 C3 177.7(4) . . . . ? C1 C2 C3 C4 -1.3(9) . . . . ? C2 C3 C4 C5 1.1(10) . . . . ? C3 C4 C5 C6 -0.7(9) . . . . ? C2 C1 C6 C5 -0.5(8) . . . . ? P1 C1 C6 C5 -177.1(4) . . . . ? C4 C5 C6 C1 0.4(8) . . . . ? C12 C7 C8 C9 -0.1(8) . . . . ? P1 C7 C8 C9 -178.2(4) . . . . ? C7 C8 C9 C10 -1.2(9) . . . . ? C8 C9 C10 C11 1.3(10) . . . . ? C9 C10 C11 C12 -0.1(10) . . . . ? C10 C11 C12 C7 -1.2(9) . . . . ? C8 C7 C12 C11 1.4(9) . . . . ? P1 C7 C12 C11 179.4(5) . . . . ? N1 C13 C14 C15 1.2(9) . . . . ? P1 C13 C14 C15 178.8(4) . . . . ? C13 C14 C15 C16 -0.2(9) . . . . ? C14 C15 C16 C17 -0.7(10) . . . . ? C15 C16 C17 N1 0.7(11) . . . . ? C23 C18 C19 C20 -0.3(8) . . . . ? P2 C18 C19 C20 176.6(5) . . . . ? C18 C19 C20 C21 -1.5(9) . . . . ? C19 C20 C21 C22 2.4(10) . . . . ? C20 C21 C22 C23 -1.5(10) . . . . ? C19 C18 C23 C22 1.3(8) . . . . ? P2 C18 C23 C22 -175.9(5) . . . . ? C21 C22 C23 C18 -0.3(9) . . . . ? C29 C24 C25 C26 -1.0(8) . . . . ? P2 C24 C25 C26 -174.8(4) . . . . ? C24 C25 C26 C27 2.1(9) . . . . ? C25 C26 C27 C28 -1.5(10) . . . . ? C26 C27 C28 C29 -0.1(10) . . . . ? C27 C28 C29 C24 1.1(9) . . . . ? C25 C24 C29 C28 -0.5(8) . . . . ? P2 C24 C29 C28 173.2(4) . . . . ? N2 C30 C31 C32 -1.3(9) . . . . ? P2 C30 C31 C32 -176.2(5) . . . . ? C30 C31 C32 C33 -0.3(10) . . . . ? C31 C32 C33 C34 1.0(10) . . . . ? C32 C33 C34 N2 -0.2(11) . . . . ? C40 C35 C36 C37 2.6(9) . . . . ? P3 C35 C36 C37 -174.0(4) . . . . ? C35 C36 C37 C38 -0.2(9) . . . . ? C36 C37 C38 C39 -2.1(10) . . . . ? C37 C38 C39 C40 2.1(11) . . . . ? C36 C35 C40 C39 -2.6(9) . . . . ? P3 C35 C40 C39 174.3(5) . . . . ? C38 C39 C40 C35 0.2(11) . . . . ? C46 C41 C42 C43 -0.2(8) . . . . ? C41 C42 C43 C44 0.4(9) . . . . ? C42 C43 C44 C45 -0.1(9) . . . . ? C43 C44 C45 C46 -0.3(9) . . . . ? C42 C41 C46 C45 -0.2(8) . . . . ? C42 C41 C46 P3 179.4(4) . . . . ? C44 C45 C46 C41 0.5(8) . . . . ? C44 C45 C46 P3 -179.1(4) . . . . ? N3 C47 C48 C49 -1.1(8) . . . . ? P3 C47 C48 C49 176.6(4) . . . . ? C47 C48 C49 C50 0.3(8) . . . . ? C48 C49 C50 C51 -0.2(9) . . . . ? C49 C50 C51 N3 0.9(10) . . . . ? C14 C13 N1 C17 -1.3(9) . . . . ? P1 C13 N1 C17 -179.2(5) . . . . ? C16 C17 N1 C13 0.3(10) . . . . ? C33 C34 N2 C30 -1.4(10) . . . . ? C31 C30 N2 C34 2.1(9) . . . . ? P2 C30 N2 C34 177.6(5) . . . . ? C48 C47 N3 C51 1.7(9) . . . . ? P3 C47 N3 C51 -176.2(5) . . . . ? C50 C51 N3 C47 -1.6(10) . . . . ? C8 C7 P1 C1 122.4(5) . . . . ? C12 C7 P1 C1 -55.6(5) . . . . ? C8 C7 P1 C13 -128.5(5) . . . . ? C12 C7 P1 C13 53.5(5) . . . . ? C8 C7 P1 Pd1 -14.8(5) . . . . ? C12 C7 P1 Pd1 167.2(4) . . . . ? C6 C1 P1 C7 -22.1(5) . . . . ? C2 C1 P1 C7 161.3(4) . . . . ? C6 C1 P1 C13 -133.9(4) . . . . ? C2 C1 P1 C13 49.5(5) . . . . ? C6 C1 P1 Pd1 112.8(4) . . . . ? C2 C1 P1 Pd1 -63.8(5) . . . . ? N1 C13 P1 C7 178.8(4) . . . . ? C14 C13 P1 C7 1.0(6) . . . . ? N1 C13 P1 C1 -71.5(4) . . . . ? C14 C13 P1 C1 110.7(5) . . . . ? N1 C13 P1 Pd1 55.3(4) . . . . ? C14 C13 P1 Pd1 -122.6(5) . . . . ? C25 C24 P2 C18 60.9(5) . . . . ? C29 C24 P2 C18 -112.9(4) . . . . ? C25 C24 P2 C30 -48.5(5) . . . . ? C29 C24 P2 C30 137.7(4) . . . . ? C25 C24 P2 Pd1 -163.3(4) . . . . ? C29 C24 P2 Pd1 22.9(5) . . . . ? C23 C18 P2 C24 -170.9(4) . . . . ? C19 C18 P2 C24 12.0(5) . . . . ? C23 C18 P2 C30 -58.4(5) . . . . ? C19 C18 P2 C30 124.6(5) . . . . ? C23 C18 P2 Pd1 56.0(5) . . . . ? C19 C18 P2 Pd1 -121.1(4) . . . . ? N2 C30 P2 C24 174.7(4) . . . . ? C31 C30 P2 C24 -10.0(6) . . . . ? N2 C30 P2 C18 64.8(4) . . . . ? C31 C30 P2 C18 -119.9(5) . . . . ? N2 C30 P2 Pd1 -62.1(4) . . . . ? C31 C30 P2 Pd1 113.2(5) . . . . ? C41 C46 P3 C35 -129.1(4) . . . . ? C45 C46 P3 C35 50.5(5) . . . . ? C41 C46 P3 C47 123.5(4) . . . . ? C45 C46 P3 C47 -56.8(5) . . . . ? C41 C46 P3 Pd1 -2.4(5) . . . . ? C45 C46 P3 Pd1 177.2(4) . . . . ? C40 C35 P3 C46 175.2(4) . . . . ? C36 C35 P3 C46 -8.0(6) . . . . ? C40 C35 P3 C47 -70.5(5) . . . . ? C36 C35 P3 C47 106.3(5) . . . . ? C40 C35 P3 Pd1 45.9(5) . . . . ? C36 C35 P3 Pd1 -137.3(4) . . . . ? N3 C47 P3 C46 -166.1(4) . . . . ? C48 C47 P3 C46 16.1(5) . . . . ? N3 C47 P3 C35 79.3(5) . . . . ? C48 C47 P3 C35 -98.6(5) . . . . ? N3 C47 P3 Pd1 -37.4(5) . . . . ? C48 C47 P3 Pd1 144.8(4) . . . . ? C46 P3 Pd1 Cl1 -179(15) . . . . ? C35 P3 Pd1 Cl1 -52.8(4) . . . . ? C47 P3 Pd1 Cl1 56.0(4) . . . . ? C46 P3 Pd1 P2 -83.28(19) . . . . ? C35 P3 Pd1 P2 42.8(2) . . . . ? C47 P3 Pd1 P2 151.57(19) . . . . ? C46 P3 Pd1 P1 83.82(19) . . . . ? C35 P3 Pd1 P1 -150.1(2) . . . . ? C47 P3 Pd1 P1 -41.34(19) . . . . ? C24 P2 Pd1 P3 -114.7(2) . . . . ? C18 P2 Pd1 P3 13.3(2) . . . . ? C30 P2 Pd1 P3 127.87(18) . . . . ? C24 P2 Pd1 Cl1 56.3(2) . . . . ? C18 P2 Pd1 Cl1 -175.7(2) . . . . ? C30 P2 Pd1 Cl1 -61.13(18) . . . . ? C24 P2 Pd1 P1 109.7(2) . . . . ? C18 P2 Pd1 P1 -122.3(2) . . . . ? C30 P2 Pd1 P1 -7.7(3) . . . . ? C7 P1 Pd1 P3 115.6(2) . . . . ? C1 P1 Pd1 P3 -13.9(2) . . . . ? C13 P1 Pd1 P3 -127.92(19) . . . . ? C7 P1 Pd1 Cl1 -55.4(2) . . . . ? C1 P1 Pd1 Cl1 175.0(2) . . . . ? C13 P1 Pd1 Cl1 61.05(19) . . . . ? C7 P1 Pd1 P2 -108.8(2) . . . . ? C1 P1 Pd1 P2 121.7(3) . . . . ? C13 P1 Pd1 P2 7.7(3) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.651 _refine_diff_density_min -2.181 _refine_diff_density_rms 0.123 #===END data_7 _database_code_depnum_ccdc_archive 'CCDC 746627' #TrackingRef 'data.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H34 Cl2 N2 O2 P2 Pd' _chemical_formula_weight 825.94 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' Pd Pd -0.9988 1.0072 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.5706(9) _cell_length_b 9.5072(10) _cell_length_c 22.614(2) _cell_angle_alpha 85.134(2) _cell_angle_beta 80.784(2) _cell_angle_gamma 78.237(2) _cell_volume 1778.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.543 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 840 _exptl_absorpt_coefficient_mu 0.802 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6178 _exptl_absorpt_correction_T_max 0.7457 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker Apex' _diffrn_measurement_method /w _diffrn_reflns_number 9230 _diffrn_reflns_av_R_equivalents 0.0184 _diffrn_reflns_av_sigmaI/netI 0.0363 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.74 _diffrn_reflns_theta_max 25.03 _reflns_number_total 6163 _reflns_number_gt 5686 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0795P)^2^+16.3994P] 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_number_reflns 6163 _refine_ls_number_parameters 449 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0697 _refine_ls_R_factor_gt 0.0653 _refine_ls_wR_factor_ref 0.1639 _refine_ls_wR_factor_gt 0.1607 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.8026(6) 0.5196(6) 0.9180(3) 0.0179(11) Uani 1 1 d . . . C2 C 0.9187(7) 0.6064(6) 0.9063(3) 0.0210(12) Uani 1 1 d . . . H2 H 0.9825 0.6090 0.8679 0.025 Uiso 1 1 calc R . . C3 C 0.9406(7) 0.6886(7) 0.9510(3) 0.0240(13) Uani 1 1 d . . . H3 H 1.0187 0.7483 0.9430 0.029 Uiso 1 1 calc R . . C4 C 0.8491(7) 0.6842(6) 1.0073(3) 0.0238(13) Uani 1 1 d . . . H4 H 0.8641 0.7408 1.0378 0.029 Uiso 1 1 calc R . . C5 C 0.7356(7) 0.5964(7) 1.0187(3) 0.0234(12) Uani 1 1 d . . . H5 H 0.6737 0.5919 1.0574 0.028 Uiso 1 1 calc R . . C6 C 0.7120(7) 0.5161(6) 0.9744(3) 0.0215(12) Uani 1 1 d . . . H6 H 0.6327 0.4576 0.9825 0.026 Uiso 1 1 calc R . . C7 C 0.7072(7) 0.2589(6) 0.8924(3) 0.0187(11) Uani 1 1 d . . . C8 C 0.7795(7) 0.1863(6) 0.9404(3) 0.0225(12) Uani 1 1 d . . . H8 H 0.8554 0.2256 0.9569 0.027 Uiso 1 1 calc R . . C9 C 0.7400(7) 0.0567(7) 0.9638(3) 0.0250(13) Uani 1 1 d . . . H9 H 0.7887 0.0071 0.9965 0.030 Uiso 1 1 calc R . . C10 C 0.6304(7) -0.0004(7) 0.9399(3) 0.0259(13) Uani 1 1 d . . . H10 H 0.6043 -0.0902 0.9553 0.031 Uiso 1 1 calc R . . C11 C 0.5582(7) 0.0756(7) 0.8928(3) 0.0257(13) Uani 1 1 d . . . H11 H 0.4798 0.0382 0.8770 0.031 Uiso 1 1 calc R . . C12 C 0.5976(6) 0.2029(6) 0.8688(2) 0.0165(11) Uani 1 1 d . . . H12 H 0.5491 0.2519 0.8360 0.020 Uiso 1 1 calc R . . C13 C 0.5818(6) 0.5250(6) 0.8340(3) 0.0186(11) Uani 1 1 d . . . C14 C 0.4871(7) 0.6396(6) 0.8651(3) 0.0233(12) Uani 1 1 d . . . H14 H 0.5210 0.6715 0.8988 0.028 Uiso 1 1 calc R . . C15 C 0.3418(7) 0.7075(7) 0.8463(3) 0.0289(14) Uani 1 1 d . . . H15 H 0.2747 0.7847 0.8677 0.035 Uiso 1 1 calc R . . C16 C 0.2960(8) 0.6623(7) 0.7966(3) 0.0318(15) Uani 1 1 d . . . H16 H 0.1980 0.7083 0.7830 0.038 Uiso 1 1 calc R . . C17 C 0.3948(9) 0.5490(7) 0.7672(3) 0.0359(16) Uani 1 1 d . . . H17 H 0.3621 0.5165 0.7334 0.043 Uiso 1 1 calc R . . C18 C 1.2215(7) 0.2286(6) 0.7559(3) 0.0233(13) Uani 1 1 d . . . H18 H 1.3118 0.2782 0.7382 0.028 Uiso 1 1 calc R . . C19 C 1.1806(8) 0.1265(6) 0.7193(3) 0.0288(14) Uani 1 1 d . . . C20 C 1.0762(8) 0.0283(7) 0.7511(3) 0.0301(14) Uani 1 1 d . . . H20 H 1.0275 -0.0254 0.7283 0.036 Uiso 1 1 calc R . . C21 C 1.0496(8) 0.0140(6) 0.8102(3) 0.0272(14) Uani 1 1 d . . . H21 H 0.9816 -0.0496 0.8287 0.033 Uiso 1 1 calc R . . C22 C 1.1219(7) 0.0934(6) 0.8487(3) 0.0219(12) Uani 1 1 d . . . C23 C 1.1887(7) 0.2140(6) 0.8197(3) 0.0230(13) Uani 1 1 d . . . H23 H 1.2563 0.2568 0.8427 0.028 Uiso 1 1 calc R . . C24 C 0.8578(7) 0.4152(6) 0.6441(3) 0.0217(12) Uani 1 1 d . . . C25 C 0.7997(8) 0.2899(7) 0.6615(3) 0.0305(14) Uani 1 1 d . . . H25 H 0.7940 0.2541 0.7022 0.037 Uiso 1 1 calc R . . C26 C 0.7498(10) 0.2165(8) 0.6196(4) 0.0428(18) Uani 1 1 d . . . H26 H 0.7092 0.1312 0.6319 0.051 Uiso 1 1 calc R . . C27 C 0.7587(9) 0.2659(8) 0.5608(3) 0.0372(16) Uani 1 1 d . . . H27 H 0.7258 0.2144 0.5323 0.045 Uiso 1 1 calc R . . C28 C 0.8159(8) 0.3916(8) 0.5430(3) 0.0329(15) Uani 1 1 d . . . H28 H 0.8205 0.4269 0.5023 0.040 Uiso 1 1 calc R . . C29 C 0.8663(7) 0.4661(7) 0.5841(3) 0.0258(13) Uani 1 1 d . . . H29 H 0.9066 0.5515 0.5716 0.031 Uiso 1 1 calc R . . C30 C 1.2306(8) 0.4629(8) 0.6282(3) 0.0316(15) Uani 1 1 d . . . H30 H 1.2223 0.3643 0.6319 0.038 Uiso 1 1 calc R . . C31 C 1.3675(8) 0.5051(9) 0.5955(3) 0.0401(18) Uani 1 1 d . . . H31 H 1.4533 0.4352 0.5774 0.048 Uiso 1 1 calc R . . C32 C 1.3778(10) 0.6492(11) 0.5897(3) 0.049(2) Uani 1 1 d . . . H32 H 1.4709 0.6781 0.5674 0.059 Uiso 1 1 calc R . . C33 C 1.2553(10) 0.7494(9) 0.6158(4) 0.048(2) Uani 1 1 d . . . H33 H 1.2636 0.8480 0.6113 0.057 Uiso 1 1 calc R . . C34 C 1.1183(8) 0.7101(8) 0.6488(3) 0.0344(15) Uani 1 1 d . . . H34 H 1.0337 0.7812 0.6670 0.041 Uiso 1 1 calc R . . C35 C 1.1063(7) 0.5659(7) 0.6552(3) 0.0231(13) Uani 1 1 d . . . C36 C 0.7904(7) 0.6748(6) 0.7117(3) 0.0215(12) Uani 1 1 d . . . C37 C 0.6675(8) 0.7292(7) 0.6785(3) 0.0311(15) Uani 1 1 d . . . H37 H 0.6498 0.6765 0.6472 0.037 Uiso 1 1 calc R . . C38 C 0.5710(8) 0.8605(8) 0.6914(4) 0.0396(17) Uani 1 1 d . . . H38 H 0.4864 0.8995 0.6687 0.048 Uiso 1 1 calc R . . C39 C 0.5975(8) 0.9346(7) 0.7369(3) 0.0359(16) Uani 1 1 d . . . H39 H 0.5317 1.0251 0.7468 0.043 Uiso 1 1 calc R . . C40 C 0.7230(9) 0.8735(8) 0.7682(3) 0.0380(16) Uani 1 1 d . . . H40 H 0.7426 0.9250 0.7995 0.046 Uiso 1 1 calc R . . C41 C 0.7910(17) -0.138(4) 0.4691(9) 0.135(2) Uiso 0.613(8) 1 d PDU A 1 H41A H 0.8248 -0.2371 0.4554 0.161 Uiso 0.613(8) 1 calc PR A 1 H41B H 0.8449 -0.0731 0.4398 0.161 Uiso 0.613(8) 1 calc PR A 1 Cl1 Cl 0.8437(11) -0.1305(11) 0.5387(4) 0.1236(18) Uiso 0.613(8) 1 d PDU A 1 Cl2 Cl 0.5858(11) -0.0850(11) 0.4747(4) 0.152(2) Uiso 0.613(8) 1 d PDU . 1 C41' C 0.829(3) -0.115(4) 0.4725(9) 0.132(2) Uiso 0.387(8) 1 d PDU A 2 H41C H 0.7832 -0.0131 0.4620 0.159 Uiso 0.387(8) 1 calc PR A 2 H41D H 0.9166 -0.1504 0.4399 0.159 Uiso 0.387(8) 1 calc PR A 2 Cl1' Cl 0.9044(17) -0.1269(16) 0.5391(6) 0.119(2) Uiso 0.387(8) 1 d PDU A 2 Cl2' Cl 0.6830(17) -0.2168(16) 0.4810(6) 0.146(2) Uiso 0.387(8) 1 d PDU A 2 N1 N 0.8181(7) 0.7462(6) 0.7566(3) 0.0319(12) Uani 1 1 d . . . N2 N 0.5382(7) 0.4812(6) 0.7845(3) 0.0355(13) Uani 1 1 d . . . O1 O 1.1244(5) 0.0544(5) 0.90197(19) 0.0278(10) Uani 1 1 d . . . O2 O 1.2291(7) 0.1158(5) 0.6654(2) 0.0441(13) Uani 1 1 d . . . P1 P 0.77111(16) 0.42240(15) 0.85627(6) 0.0158(3) Uani 1 1 d . . . P2 P 0.93177(17) 0.50398(16) 0.69928(6) 0.0182(3) Uani 1 1 d . . . Pd1 Pd 0.99204(5) 0.36190(4) 0.783175(18) 0.01550(15) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.014(3) 0.016(3) 0.022(3) -0.001(2) -0.006(2) 0.002(2) C2 0.017(3) 0.024(3) 0.021(3) -0.002(2) -0.001(2) -0.002(2) C3 0.019(3) 0.024(3) 0.029(3) 0.001(2) -0.005(2) -0.006(2) C4 0.027(3) 0.017(3) 0.028(3) -0.005(2) -0.012(3) 0.000(2) C5 0.023(3) 0.026(3) 0.019(3) -0.003(2) -0.001(2) 0.001(2) C6 0.015(3) 0.020(3) 0.028(3) -0.002(2) -0.001(2) -0.001(2) C7 0.017(3) 0.016(3) 0.022(3) -0.001(2) -0.002(2) 0.001(2) C8 0.019(3) 0.022(3) 0.025(3) -0.002(2) -0.006(2) 0.001(2) C9 0.026(3) 0.024(3) 0.023(3) 0.004(2) -0.004(2) 0.001(2) C10 0.025(3) 0.018(3) 0.032(3) 0.001(2) -0.001(3) -0.002(2) C11 0.021(3) 0.024(3) 0.033(3) -0.003(3) -0.006(3) -0.002(2) C12 0.017(3) 0.013(3) 0.018(3) 0.000(2) -0.006(2) 0.001(2) C13 0.012(3) 0.020(3) 0.024(3) 0.001(2) -0.004(2) -0.001(2) C14 0.019(3) 0.023(3) 0.026(3) 0.002(2) -0.005(2) -0.002(2) C15 0.019(3) 0.025(3) 0.038(4) 0.004(3) -0.002(3) 0.003(2) C16 0.025(3) 0.028(3) 0.044(4) 0.014(3) -0.016(3) -0.007(3) C17 0.049(4) 0.028(4) 0.037(4) 0.006(3) -0.026(3) -0.009(3) C18 0.014(3) 0.018(3) 0.034(3) 0.001(2) -0.003(2) 0.003(2) C19 0.034(4) 0.016(3) 0.031(4) -0.002(2) -0.007(3) 0.011(3) C20 0.041(4) 0.017(3) 0.035(4) -0.006(3) -0.017(3) -0.001(3) C21 0.030(3) 0.017(3) 0.037(4) 0.000(3) -0.016(3) -0.002(2) C22 0.018(3) 0.018(3) 0.027(3) -0.001(2) -0.007(2) 0.005(2) C23 0.015(3) 0.017(3) 0.036(3) -0.003(2) -0.015(2) 0.007(2) C24 0.020(3) 0.022(3) 0.021(3) -0.002(2) -0.004(2) 0.001(2) C25 0.038(4) 0.031(4) 0.025(3) 0.000(3) -0.008(3) -0.013(3) C26 0.059(5) 0.031(4) 0.044(4) -0.008(3) -0.009(4) -0.017(4) C27 0.043(4) 0.043(4) 0.030(4) -0.013(3) -0.011(3) -0.008(3) C28 0.032(4) 0.041(4) 0.025(3) -0.003(3) -0.007(3) -0.002(3) C29 0.023(3) 0.031(3) 0.023(3) 0.002(3) -0.003(2) -0.005(3) C30 0.023(3) 0.042(4) 0.026(3) 0.005(3) -0.005(3) 0.000(3) C31 0.021(3) 0.069(5) 0.028(4) 0.003(3) -0.004(3) -0.005(3) C32 0.036(4) 0.088(7) 0.034(4) 0.017(4) -0.016(3) -0.034(4) C33 0.039(4) 0.051(5) 0.060(5) 0.003(4) -0.011(4) -0.025(4) C34 0.028(3) 0.034(4) 0.047(4) 0.000(3) -0.011(3) -0.016(3) C35 0.018(3) 0.028(3) 0.025(3) 0.004(2) -0.008(2) -0.006(2) C36 0.017(3) 0.020(3) 0.027(3) 0.000(2) -0.002(2) -0.002(2) C37 0.025(3) 0.029(3) 0.041(4) -0.005(3) -0.013(3) -0.001(3) C38 0.027(4) 0.034(4) 0.055(5) -0.002(3) -0.016(3) 0.006(3) C39 0.024(3) 0.026(3) 0.055(4) -0.011(3) 0.003(3) 0.000(3) C40 0.036(4) 0.036(4) 0.044(4) -0.015(3) -0.002(3) -0.010(3) N1 0.029(3) 0.031(3) 0.036(3) -0.006(2) -0.008(2) -0.002(2) N2 0.042(3) 0.029(3) 0.037(3) 0.001(2) -0.019(3) -0.002(3) O1 0.030(2) 0.027(2) 0.026(2) 0.0008(18) -0.0123(18) 0.0026(18) O2 0.067(4) 0.030(3) 0.028(3) -0.007(2) -0.002(2) 0.007(2) P1 0.0133(7) 0.0149(7) 0.0188(7) -0.0016(5) -0.0036(5) -0.0007(5) P2 0.0169(7) 0.0179(7) 0.0193(7) 0.0003(6) -0.0048(6) -0.0007(6) Pd1 0.0133(2) 0.0149(2) 0.0175(2) -0.00155(15) -0.00434(15) 0.00130(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C6 1.385(8) . ? C1 C2 1.398(8) . ? C1 P1 1.820(6) . ? C2 C3 1.386(9) . ? C3 C4 1.386(9) . ? C4 C5 1.387(9) . ? C5 C6 1.373(9) . ? C7 C12 1.365(8) . ? C7 C8 1.397(8) . ? C7 P1 1.837(6) . ? C8 C9 1.383(9) . ? C9 C10 1.374(9) . ? C10 C11 1.392(9) . ? C11 C12 1.367(8) . ? C13 N2 1.356(8) . ? C13 C14 1.388(8) . ? C13 P1 1.836(6) . ? C14 C15 1.394(8) . ? C15 C16 1.376(10) . ? C16 C17 1.374(10) . ? C17 N2 1.367(9) . ? C18 C23 1.426(9) . ? C18 C19 1.455(9) . ? C18 Pd1 2.141(6) . ? C19 O2 1.228(8) . ? C19 C20 1.487(10) . ? C20 C21 1.320(9) . ? C21 C22 1.478(9) . ? C22 O1 1.233(7) . ? C22 C23 1.446(9) . ? C23 Pd1 2.187(5) . ? C24 C25 1.386(9) . ? C24 C29 1.395(8) . ? C24 P2 1.823(6) . ? C25 C26 1.389(10) . ? C26 C27 1.368(11) . ? C27 C28 1.387(10) . ? C28 C29 1.385(9) . ? C30 C35 1.390(9) . ? C30 C31 1.395(10) . ? C31 C32 1.385(12) . ? C32 C33 1.359(13) . ? C33 C34 1.389(10) . ? C34 C35 1.390(9) . ? C35 P2 1.833(6) . ? C36 N1 1.346(8) . ? C36 C37 1.380(9) . ? C36 P2 1.831(6) . ? C37 C38 1.375(10) . ? C38 C39 1.369(11) . ? C39 C40 1.383(11) . ? C40 N1 1.334(9) . ? C41 Cl1 1.716(13) . ? C41 Cl2 1.716(13) . ? Cl2 Cl2 2.21(2) 2_656 ? C41' Cl2' 1.716(13) . ? C41' Cl1' 1.716(13) . ? P1 Pd1 2.3159(14) . ? P2 Pd1 2.2991(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 C6 C1 C2 119.3(5) . . ? C6 C1 P1 122.9(4) . . ? C2 C1 P1 117.8(4) . . ? C3 C2 C1 119.8(5) . . ? C4 C3 C2 120.4(6) . . ? C3 C4 C5 119.5(6) . . ? C6 C5 C4 120.4(6) . . ? C5 C6 C1 120.7(6) . . ? C12 C7 C8 120.3(5) . . ? C12 C7 P1 119.1(4) . . ? C8 C7 P1 120.4(4) . . ? C9 C8 C7 119.6(6) . . ? C10 C9 C8 120.2(6) . . ? C9 C10 C11 118.9(6) . . ? C12 C11 C10 121.5(6) . . ? C7 C12 C11 119.5(5) . . ? N2 C13 C14 121.2(5) . . ? N2 C13 P1 115.6(4) . . ? C14 C13 P1 123.3(4) . . ? C13 C14 C15 119.3(6) . . ? C16 C15 C14 119.8(6) . . ? C17 C16 C15 118.6(6) . . ? N2 C17 C16 122.7(6) . . ? C23 C18 C19 120.4(6) . . ? C23 C18 Pd1 72.5(3) . . ? C19 C18 Pd1 102.4(4) . . ? O2 C19 C18 124.3(7) . . ? O2 C19 C20 119.6(6) . . ? C18 C19 C20 116.1(6) . . ? C21 C20 C19 121.7(6) . . ? C20 C21 C22 122.3(6) . . ? O1 C22 C23 123.9(6) . . ? O1 C22 C21 120.0(6) . . ? C23 C22 C21 116.1(5) . . ? C18 C23 C22 120.2(5) . . ? C18 C23 Pd1 69.0(3) . . ? C22 C23 Pd1 106.5(4) . . ? C25 C24 C29 119.4(6) . . ? C25 C24 P2 119.0(5) . . ? C29 C24 P2 121.5(5) . . ? C24 C25 C26 120.1(6) . . ? C27 C26 C25 120.7(7) . . ? C26 C27 C28 119.6(6) . . ? C29 C28 C27 120.5(6) . . ? C28 C29 C24 119.7(6) . . ? C35 C30 C31 119.7(7) . . ? C32 C31 C30 119.8(7) . . ? C33 C32 C31 120.2(7) . . ? C32 C33 C34 121.1(8) . . ? C33 C34 C35 119.3(7) . . ? C34 C35 C30 119.8(6) . . ? C34 C35 P2 122.3(5) . . ? C30 C35 P2 117.9(5) . . ? N1 C36 C37 121.9(6) . . ? N1 C36 P2 113.4(4) . . ? C37 C36 P2 124.7(5) . . ? C38 C37 C36 119.2(6) . . ? C39 C38 C37 119.7(6) . . ? C38 C39 C40 117.9(6) . . ? N1 C40 C39 123.6(7) . . ? Cl1 C41 Cl2 108.0(13) . . ? C41 Cl2 Cl2 131.7(12) . 2_656 ? Cl2' C41' Cl1' 108.1(13) . . ? C40 N1 C36 117.7(6) . . ? C13 N2 C17 118.4(6) . . ? C1 P1 C13 103.9(3) . . ? C1 P1 C7 104.6(3) . . ? C13 P1 C7 101.4(3) . . ? C1 P1 Pd1 115.98(19) . . ? C13 P1 Pd1 119.10(19) . . ? C7 P1 Pd1 110.06(18) . . ? C24 P2 C36 106.2(3) . . ? C24 P2 C35 102.5(3) . . ? C36 P2 C35 101.2(3) . . ? C24 P2 Pd1 114.8(2) . . ? C36 P2 Pd1 116.8(2) . . ? C35 P2 Pd1 113.54(19) . . ? C18 Pd1 C23 38.5(2) . . ? C18 Pd1 P2 105.25(17) . . ? C23 Pd1 P2 142.41(17) . . ? C18 Pd1 P1 149.08(17) . . ? C23 Pd1 P1 111.50(17) . . ? P2 Pd1 P1 105.56(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -0.6(8) . . . . ? P1 C1 C2 C3 176.4(4) . . . . ? C1 C2 C3 C4 0.6(9) . . . . ? C2 C3 C4 C5 0.2(9) . . . . ? C3 C4 C5 C6 -1.0(9) . . . . ? C4 C5 C6 C1 1.0(9) . . . . ? C2 C1 C6 C5 -0.2(8) . . . . ? P1 C1 C6 C5 -177.1(4) . . . . ? C12 C7 C8 C9 0.3(9) . . . . ? P1 C7 C8 C9 -174.5(5) . . . . ? C7 C8 C9 C10 0.1(9) . . . . ? C8 C9 C10 C11 -1.2(9) . . . . ? C9 C10 C11 C12 2.0(9) . . . . ? C8 C7 C12 C11 0.5(8) . . . . ? P1 C7 C12 C11 175.3(4) . . . . ? C10 C11 C12 C7 -1.6(9) . . . . ? N2 C13 C14 C15 2.3(9) . . . . ? P1 C13 C14 C15 -177.4(5) . . . . ? C13 C14 C15 C16 -1.4(9) . . . . ? C14 C15 C16 C17 0.9(10) . . . . ? C15 C16 C17 N2 -1.2(10) . . . . ? C23 C18 C19 O2 -166.7(6) . . . . ? Pd1 C18 C19 O2 116.4(6) . . . . ? C23 C18 C19 C20 11.7(8) . . . . ? Pd1 C18 C19 C20 -65.1(6) . . . . ? O2 C19 C20 C21 165.2(6) . . . . ? C18 C19 C20 C21 -13.4(9) . . . . ? C19 C20 C21 C22 -0.3(10) . . . . ? C20 C21 C22 O1 -163.7(6) . . . . ? C20 C21 C22 C23 15.4(9) . . . . ? C19 C18 C23 C22 3.1(8) . . . . ? Pd1 C18 C23 C22 97.5(5) . . . . ? C19 C18 C23 Pd1 -94.3(5) . . . . ? O1 C22 C23 C18 162.6(5) . . . . ? C21 C22 C23 C18 -16.5(8) . . . . ? O1 C22 C23 Pd1 -122.4(5) . . . . ? C21 C22 C23 Pd1 58.5(6) . . . . ? C29 C24 C25 C26 -0.4(10) . . . . ? P2 C24 C25 C26 -176.9(6) . . . . ? C24 C25 C26 C27 0.6(12) . . . . ? C25 C26 C27 C28 -0.9(12) . . . . ? C26 C27 C28 C29 1.0(11) . . . . ? C27 C28 C29 C24 -0.8(10) . . . . ? C25 C24 C29 C28 0.4(9) . . . . ? P2 C24 C29 C28 176.9(5) . . . . ? C35 C30 C31 C32 -0.7(10) . . . . ? C30 C31 C32 C33 0.1(11) . . . . ? C31 C32 C33 C34 0.3(12) . . . . ? C32 C33 C34 C35 -0.2(11) . . . . ? C33 C34 C35 C30 -0.4(10) . . . . ? C33 C34 C35 P2 178.7(6) . . . . ? C31 C30 C35 C34 0.8(9) . . . . ? C31 C30 C35 P2 -178.3(5) . . . . ? N1 C36 C37 C38 0.5(10) . . . . ? P2 C36 C37 C38 -178.7(6) . . . . ? C36 C37 C38 C39 -0.5(11) . . . . ? C37 C38 C39 C40 0.5(11) . . . . ? C38 C39 C40 N1 -0.7(11) . . . . ? Cl1 C41 Cl2 Cl2 39(3) . . . 2_656 ? C39 C40 N1 C36 0.7(11) . . . . ? C37 C36 N1 C40 -0.6(10) . . . . ? P2 C36 N1 C40 178.6(5) . . . . ? C14 C13 N2 C17 -2.6(9) . . . . ? P1 C13 N2 C17 177.1(5) . . . . ? C16 C17 N2 C13 2.1(10) . . . . ? C6 C1 P1 C13 72.9(5) . . . . ? C2 C1 P1 C13 -104.0(5) . . . . ? C6 C1 P1 C7 -33.1(5) . . . . ? C2 C1 P1 C7 150.0(4) . . . . ? C6 C1 P1 Pd1 -154.5(4) . . . . ? C2 C1 P1 Pd1 28.6(5) . . . . ? N2 C13 P1 C1 174.4(5) . . . . ? C14 C13 P1 C1 -5.9(6) . . . . ? N2 C13 P1 C7 -77.3(5) . . . . ? C14 C13 P1 C7 102.4(5) . . . . ? N2 C13 P1 Pd1 43.6(5) . . . . ? C14 C13 P1 Pd1 -136.8(4) . . . . ? C12 C7 P1 C1 145.4(4) . . . . ? C8 C7 P1 C1 -39.7(5) . . . . ? C12 C7 P1 C13 37.7(5) . . . . ? C8 C7 P1 C13 -147.5(5) . . . . ? C12 C7 P1 Pd1 -89.4(4) . . . . ? C8 C7 P1 Pd1 85.5(5) . . . . ? C25 C24 P2 C36 -112.7(5) . . . . ? C29 C24 P2 C36 70.8(5) . . . . ? C25 C24 P2 C35 141.6(5) . . . . ? C29 C24 P2 C35 -34.9(6) . . . . ? C25 C24 P2 Pd1 18.0(6) . . . . ? C29 C24 P2 Pd1 -158.4(4) . . . . ? N1 C36 P2 C24 172.8(5) . . . . ? C37 C36 P2 C24 -8.0(6) . . . . ? N1 C36 P2 C35 -80.6(5) . . . . ? C37 C36 P2 C35 98.7(6) . . . . ? N1 C36 P2 Pd1 43.2(5) . . . . ? C37 C36 P2 Pd1 -137.6(5) . . . . ? C34 C35 P2 C24 121.3(5) . . . . ? C30 C35 P2 C24 -59.5(5) . . . . ? C34 C35 P2 C36 11.8(6) . . . . ? C30 C35 P2 C36 -169.1(5) . . . . ? C34 C35 P2 Pd1 -114.2(5) . . . . ? C30 C35 P2 Pd1 64.9(5) . . . . ? C19 C18 Pd1 C23 118.3(6) . . . . ? C23 C18 Pd1 P2 167.8(3) . . . . ? C19 C18 Pd1 P2 -73.9(4) . . . . ? C23 C18 Pd1 P1 -17.1(6) . . . . ? C19 C18 Pd1 P1 101.2(5) . . . . ? C22 C23 Pd1 C18 -116.6(6) . . . . ? C18 C23 Pd1 P2 -19.6(5) . . . . ? C22 C23 Pd1 P2 -136.2(3) . . . . ? C18 C23 Pd1 P1 170.7(3) . . . . ? C22 C23 Pd1 P1 54.0(4) . . . . ? C24 P2 Pd1 C18 78.2(3) . . . . ? C36 P2 Pd1 C18 -156.4(3) . . . . ? C35 P2 Pd1 C18 -39.2(3) . . . . ? C24 P2 Pd1 C23 90.7(3) . . . . ? C36 P2 Pd1 C23 -144.0(3) . . . . ? C35 P2 Pd1 C23 -26.8(4) . . . . ? C24 P2 Pd1 P1 -99.2(2) . . . . ? C36 P2 Pd1 P1 26.2(2) . . . . ? C35 P2 Pd1 P1 143.3(2) . . . . ? C1 P1 Pd1 C18 74.6(4) . . . . ? C13 P1 Pd1 C18 -160.2(4) . . . . ? C7 P1 Pd1 C18 -43.8(4) . . . . ? C1 P1 Pd1 C23 63.3(3) . . . . ? C13 P1 Pd1 C23 -171.5(3) . . . . ? C7 P1 Pd1 C23 -55.1(3) . . . . ? C1 P1 Pd1 P2 -110.3(2) . . . . ? C13 P1 Pd1 P2 14.9(2) . . . . ? C7 P1 Pd1 P2 131.3(2) . . . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 3.686 _refine_diff_density_min -1.961 _refine_diff_density_rms 0.153 #===END