Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Nicholas Long' _publ_contact_author_address ; Department of Chemistry Imperial College of Science, Techno South Kensington LONDON SW7 2AY UNITED KINGDOM ; _publ_contact_author_email N.LONG@IC.AC.UK _publ_section_title ; Steric control over the formation of cis and trans bischelated palladium(II) complexes using a new series of flexible N,P pyridyl-phosphine ligands ; loop_ _publ_author_name 'Nicholas Long' 'Deborah A. Clarke' 'Philip W. Miller' 'Andrew J. P. White' data_Compound_1 _database_code_depnum_ccdc_archive 'CCDC 650212' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H34 B N2 P' _chemical_formula_sum 'C19 H34 B N2 P' _chemical_formula_weight 332.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 '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 13.6292(13) _cell_length_b 9.5466(7) _cell_length_c 15.4193(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.817(7) _cell_angle_gamma 90.00 _cell_volume 2006.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.8637 _cell_measurement_theta_max 70.3384 _exptl_crystal_description 'prismatic needles' _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.100 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 728 _exptl_absorpt_coefficient_mu 1.196 _exptl_absorpt_correction_type 'numeric analytical' _exptl_absorpt_correction_T_min 0.78556 _exptl_absorpt_correction_T_max 0.86992 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.27p5 beta (release 01-04-2005 CrysAlis171 .NET) (compiled Apr 1 2005,17:53:34) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54248 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance Ultra (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur PX Ultra' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 8.2556 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9718 _diffrn_reflns_av_R_equivalents 0.0206 _diffrn_reflns_av_sigmaI/netI 0.0224 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 5.45 _diffrn_reflns_theta_max 70.50 _reflns_number_total 3706 _reflns_number_gt 3060 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0729P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3706 _refine_ls_number_parameters 221 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0468 _refine_ls_R_factor_gt 0.0393 _refine_ls_wR_factor_ref 0.1173 _refine_ls_wR_factor_gt 0.1129 _refine_ls_goodness_of_fit_ref 1.164 _refine_ls_restrained_S_all 1.164 _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 B B 0.14105(15) -0.0608(3) 0.67107(14) 0.0461(5) Uani 1 1 d D . . H0A H 0.1416(15) -0.1732(5) 0.6867(13) 0.074(6) Uiso 1 1 d D . . H0B H 0.2034(9) 0.0026(17) 0.6944(13) 0.069(7) Uiso 1 1 d D . . H0C H 0.1281(14) -0.042(2) 0.6015(3) 0.065(6) Uiso 1 1 d D . . P P 0.02929(3) 0.01565(4) 0.72925(2) 0.02790(14) Uani 1 1 d . . . C1 C 0.04252(12) 0.01069(16) 0.84876(9) 0.0337(4) Uani 1 1 d . . . H1D H 0.1069 0.0515 0.8654 0.040 Uiso 1 1 calc R . . H1E H -0.0091 0.0702 0.8743 0.040 Uiso 1 1 calc R . . N2 N 0.03573(10) -0.12884(14) 0.88555(8) 0.0385(3) Uani 1 1 d . . . C3 C -0.04696(12) -0.16814(17) 0.92957(9) 0.0365(4) Uani 1 1 d . . . N4 N -0.12278(10) -0.07827(16) 0.92731(8) 0.0423(3) Uani 1 1 d . . . C5 C -0.20556(14) -0.1152(2) 0.96789(11) 0.0544(5) Uani 1 1 d . . . H5A H -0.2590 -0.0513 0.9658 0.065 Uiso 1 1 calc R . . C6 C -0.21845(17) -0.2378(2) 1.01181(12) 0.0624(6) Uani 1 1 d . . . H6A H -0.2786 -0.2591 1.0393 0.075 Uiso 1 1 calc R . . C7 C -0.14068(19) -0.3290(2) 1.01458(11) 0.0645(6) Uani 1 1 d . . . H7A H -0.1468 -0.4154 1.0446 0.077 Uiso 1 1 calc R . . C8 C -0.05302(16) -0.29676(19) 0.97396(11) 0.0515(5) Uani 1 1 d . . . H8A H 0.0011 -0.3595 0.9761 0.062 Uiso 1 1 calc R . . C9 C 0.12553(14) -0.2104(2) 0.89158(12) 0.0576(5) Uani 1 1 d . . . H9A H 0.1497 -0.2105 0.9517 0.086 Uiso 1 1 calc R . . H9B H 0.1752 -0.1688 0.8541 0.086 Uiso 1 1 calc R . . H9C H 0.1123 -0.3068 0.8730 0.086 Uiso 1 1 calc R . . C10 C -0.08562(10) -0.07808(15) 0.70531(9) 0.0289(3) Uani 1 1 d . . . H10A H -0.0867 -0.1593 0.7462 0.035 Uiso 1 1 calc R . . C11 C -0.17964(11) 0.00425(16) 0.72233(10) 0.0317(3) Uani 1 1 d . . . H11A H -0.1774 0.0424 0.7820 0.038 Uiso 1 1 calc R . . H11B H -0.1844 0.0840 0.6815 0.038 Uiso 1 1 calc R . . C12 C -0.26961(12) -0.08955(19) 0.71119(11) 0.0421(4) Uani 1 1 d . . . H12A H -0.2683 -0.1629 0.7566 0.051 Uiso 1 1 calc R . . H12B H -0.3296 -0.0328 0.7190 0.051 Uiso 1 1 calc R . . C13 C -0.27352(13) -0.15892(19) 0.62218(11) 0.0456(4) Uani 1 1 d . . . H13A H -0.3293 -0.2252 0.6196 0.055 Uiso 1 1 calc R . . H13B H -0.2846 -0.0865 0.5771 0.055 Uiso 1 1 calc R . . C14 C -0.17914(13) -0.23701(18) 0.60357(10) 0.0449(4) Uani 1 1 d . . . H14A H -0.1821 -0.2745 0.5437 0.054 Uiso 1 1 calc R . . H14B H -0.1726 -0.3172 0.6439 0.054 Uiso 1 1 calc R . . C15 C -0.08916(12) -0.14223(17) 0.61352(9) 0.0375(4) Uani 1 1 d . . . H15A H -0.0923 -0.0665 0.5697 0.045 Uiso 1 1 calc R . . H15B H -0.0288 -0.1974 0.6037 0.045 Uiso 1 1 calc R . . C16 C 0.01063(10) 0.20252(16) 0.70839(9) 0.0296(3) Uani 1 1 d . . . H16A H -0.0505 0.2314 0.7387 0.035 Uiso 1 1 calc R . . C17 C -0.00462(13) 0.23263(17) 0.61160(10) 0.0411(4) Uani 1 1 d . . . H17A H 0.0538 0.2013 0.5794 0.049 Uiso 1 1 calc R . . H17B H -0.0620 0.1792 0.5896 0.049 Uiso 1 1 calc R . . C18 C -0.02125(15) 0.38857(19) 0.59580(12) 0.0533(5) Uani 1 1 d . . . H18A H -0.0829 0.4178 0.6237 0.064 Uiso 1 1 calc R . . H18B H -0.0283 0.4058 0.5327 0.064 Uiso 1 1 calc R . . C19 C 0.06387(15) 0.47603(19) 0.63216(13) 0.0536(5) Uani 1 1 d . . . H19A H 0.1247 0.4529 0.6009 0.064 Uiso 1 1 calc R . . H19B H 0.0498 0.5768 0.6233 0.064 Uiso 1 1 calc R . . C20 C 0.07855(14) 0.44686(19) 0.72830(12) 0.0470(4) Uani 1 1 d . . . H20A H 0.0200 0.4785 0.7601 0.056 Uiso 1 1 calc R . . H20B H 0.1358 0.5007 0.7503 0.056 Uiso 1 1 calc R . . C21 C 0.09536(12) 0.29080(18) 0.74553(10) 0.0406(4) Uani 1 1 d . . . H21A H 0.1012 0.2747 0.8088 0.049 Uiso 1 1 calc R . . H21B H 0.1576 0.2612 0.7187 0.049 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 B 0.0362(10) 0.0548(13) 0.0475(11) -0.0024(10) 0.0054(9) 0.0111(10) P 0.0273(2) 0.0322(2) 0.0242(2) 0.00075(14) 0.00006(15) 0.00100(15) C1 0.0372(9) 0.0374(9) 0.0263(8) 0.0034(6) -0.0038(6) -0.0041(7) N2 0.0427(8) 0.0391(8) 0.0336(7) 0.0097(6) -0.0044(6) 0.0048(6) C3 0.0516(10) 0.0349(9) 0.0228(7) 0.0014(6) -0.0062(6) -0.0070(7) N4 0.0422(8) 0.0528(9) 0.0319(7) 0.0093(6) -0.0017(6) -0.0053(7) C5 0.0470(11) 0.0788(15) 0.0374(9) 0.0062(9) -0.0007(8) -0.0150(10) C6 0.0699(14) 0.0765(16) 0.0408(10) 0.0029(10) 0.0014(9) -0.0322(13) C7 0.1112(19) 0.0480(12) 0.0344(9) 0.0041(8) 0.0002(10) -0.0395(13) C8 0.0843(14) 0.0353(10) 0.0347(9) 0.0031(7) -0.0037(9) -0.0063(10) C9 0.0585(12) 0.0640(13) 0.0503(11) 0.0130(9) -0.0055(9) 0.0216(10) C10 0.0339(8) 0.0263(8) 0.0265(7) 0.0006(6) -0.0001(6) -0.0022(6) C11 0.0314(8) 0.0324(8) 0.0314(8) -0.0020(6) -0.0003(6) -0.0018(6) C12 0.0346(9) 0.0453(10) 0.0464(9) -0.0005(8) -0.0011(7) -0.0072(8) C13 0.0453(10) 0.0469(11) 0.0444(9) 0.0017(8) -0.0127(7) -0.0153(8) C14 0.0602(11) 0.0387(10) 0.0355(8) -0.0065(7) -0.0061(7) -0.0114(8) C15 0.0467(9) 0.0355(9) 0.0301(8) -0.0064(6) -0.0008(7) -0.0027(7) C16 0.0296(7) 0.0309(8) 0.0282(7) 0.0022(6) 0.0006(6) -0.0031(6) C17 0.0546(10) 0.0382(9) 0.0303(8) 0.0070(7) -0.0069(7) -0.0102(8) C18 0.0680(13) 0.0444(11) 0.0469(10) 0.0164(8) -0.0162(9) -0.0135(9) C19 0.0614(12) 0.0371(10) 0.0621(12) 0.0130(8) -0.0061(10) -0.0129(9) C20 0.0463(10) 0.0389(10) 0.0556(11) -0.0028(8) -0.0101(8) -0.0099(8) C21 0.0386(9) 0.0408(10) 0.0421(9) 0.0034(7) -0.0102(7) -0.0086(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 B P 1.9227(19) . ? P C16 1.8298(15) . ? P C10 1.8366(15) . ? P C1 1.8496(15) . ? C1 N2 1.4512(18) . ? N2 C3 1.376(2) . ? N2 C9 1.452(2) . ? C3 N4 1.343(2) . ? C3 C8 1.409(2) . ? N4 C5 1.345(2) . ? C5 C6 1.365(3) . ? C6 C7 1.372(3) . ? C7 C8 1.391(3) . ? C10 C11 1.529(2) . ? C10 C15 1.5422(18) . ? C11 C12 1.526(2) . ? C12 C13 1.524(2) . ? C13 C14 1.518(2) . ? C14 C15 1.530(2) . ? C16 C17 1.5311(19) . ? C16 C21 1.534(2) . ? C17 C18 1.525(2) . ? C18 C19 1.529(2) . ? C19 C20 1.519(3) . ? C20 C21 1.530(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 C16 P C10 108.89(7) . . ? C16 P C1 102.21(7) . . ? C10 P C1 104.98(7) . . ? C16 P B 113.40(9) . . ? C10 P B 113.59(9) . . ? C1 P B 112.86(9) . . ? N2 C1 P 114.02(10) . . ? C3 N2 C1 120.03(13) . . ? C3 N2 C9 121.18(14) . . ? C1 N2 C9 117.28(14) . . ? N4 C3 N2 116.63(14) . . ? N4 C3 C8 121.26(16) . . ? N2 C3 C8 122.11(16) . . ? C3 N4 C5 118.06(16) . . ? N4 C5 C6 124.8(2) . . ? C5 C6 C7 117.04(19) . . ? C6 C7 C8 120.91(18) . . ? C7 C8 C3 117.92(19) . . ? C11 C10 C15 110.26(12) . . ? C11 C10 P 115.42(10) . . ? C15 C10 P 113.16(10) . . ? C12 C11 C10 110.67(13) . . ? C13 C12 C11 111.97(13) . . ? C14 C13 C12 111.40(13) . . ? C13 C14 C15 111.77(14) . . ? C14 C15 C10 109.96(12) . . ? C17 C16 C21 110.59(12) . . ? C17 C16 P 111.78(10) . . ? C21 C16 P 111.60(11) . . ? C18 C17 C16 110.91(14) . . ? C17 C18 C19 111.36(16) . . ? C20 C19 C18 110.26(14) . . ? C19 C20 C21 111.43(15) . . ? C20 C21 C16 111.10(13) . . ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 70.50 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 0.269 _refine_diff_density_min -0.295 _refine_diff_density_rms 0.041 #===END data_Compound_2 _database_code_depnum_ccdc_archive 'CCDC 650213' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H31 Cl2 N2 P Pd, C H2 Cl2' _chemical_formula_sum 'C20 H33 Cl4 N2 P Pd' _chemical_formula_weight 580.65 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' _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 11.5230(13) _cell_length_b 15.8628(19) _cell_length_c 13.3819(12) _cell_angle_alpha 90.00 _cell_angle_beta 97.806(8) _cell_angle_gamma 90.00 _cell_volume 2423.4(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 23736 _cell_measurement_theta_min 3.7541 _cell_measurement_theta_max 32.0182 _exptl_crystal_description blocks _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.592 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1184 _exptl_absorpt_coefficient_mu 1.283 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.92687 _exptl_absorpt_correction_T_max 1.04984 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET) (compiled Jan 20 2006,12:36:28) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur 3' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 15.9863 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39028 _diffrn_reflns_av_R_equivalents 0.0277 _diffrn_reflns_av_sigmaI/netI 0.0232 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.79 _diffrn_reflns_theta_max 32.06 _reflns_number_total 7934 _reflns_number_gt 6141 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET) (compiled Jan 20 2006,12:36:28) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET) (compiled Jan 20 2006,12:36:28) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET) (compiled Jan 20 2006,12:36:28) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0611P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7934 _refine_ls_number_parameters 254 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0474 _refine_ls_R_factor_gt 0.0344 _refine_ls_wR_factor_ref 0.0963 _refine_ls_wR_factor_gt 0.0924 _refine_ls_goodness_of_fit_ref 1.131 _refine_ls_restrained_S_all 1.131 _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 Pd Pd 0.539738(11) 0.218831(8) 0.412172(10) 0.02046(5) Uani 1 1 d . . . Cl1 Cl 0.43513(4) 0.15565(3) 0.26229(3) 0.03054(11) Uani 1 1 d . . . C1 C 0.72096(17) 0.20627(10) 0.61679(15) 0.0241(4) Uani 1 1 d . . . H1A H 0.7899 0.1940 0.5824 0.029 Uiso 1 1 calc R . . H1B H 0.7496 0.2285 0.6848 0.029 Uiso 1 1 calc R . . Cl2 Cl 0.44040(5) 0.34273(3) 0.37563(4) 0.03895(13) Uani 1 1 d . . . P P 0.63005(4) 0.28589(3) 0.54521(4) 0.01966(9) Uani 1 1 d . . . N2 N 0.65512(14) 0.12807(9) 0.62653(11) 0.0237(3) Uani 1 1 d . . . C3 C 0.64758(15) 0.07366(10) 0.54609(14) 0.0211(3) Uani 1 1 d . . . N4 N 0.63057(13) 0.10628(9) 0.45124(11) 0.0218(3) Uani 1 1 d . . . C5 C 0.64280(16) 0.05410(12) 0.37331(15) 0.0269(4) Uani 1 1 d . . . H5A H 0.6386 0.0777 0.3077 0.032 Uiso 1 1 calc R . . C6 C 0.66100(18) -0.03119(13) 0.38429(16) 0.0330(4) Uani 1 1 d . . . H6A H 0.6706 -0.0655 0.3278 0.040 Uiso 1 1 calc R . . C7 C 0.66504(19) -0.06579(12) 0.47956(18) 0.0338(5) Uani 1 1 d . . . H7A H 0.6716 -0.1251 0.4885 0.041 Uiso 1 1 calc R . . C8 C 0.65953(17) -0.01418(11) 0.56111(16) 0.0278(4) Uani 1 1 d . . . H8A H 0.6637 -0.0373 0.6270 0.033 Uiso 1 1 calc R . . C9 C 0.6643(2) 0.09327(13) 0.72858(14) 0.0323(4) Uani 1 1 d . . . H9A H 0.5994 0.0540 0.7327 0.048 Uiso 1 1 calc R . . H9B H 0.6607 0.1392 0.7771 0.048 Uiso 1 1 calc R . . H9C H 0.7389 0.0633 0.7443 0.048 Uiso 1 1 calc R . . C10 C 0.73675(15) 0.36635(11) 0.51904(14) 0.0222(3) Uani 1 1 d . . . H10A H 0.7999 0.3670 0.5782 0.027 Uiso 1 1 calc R . . C11 C 0.79503(17) 0.34074(12) 0.42637(15) 0.0280(4) Uani 1 1 d . . . H11A H 0.8288 0.2835 0.4369 0.034 Uiso 1 1 calc R . . H11B H 0.7352 0.3391 0.3659 0.034 Uiso 1 1 calc R . . C12 C 0.89099(19) 0.40264(14) 0.40918(18) 0.0356(5) Uani 1 1 d . . . H12A H 0.9239 0.3868 0.3472 0.043 Uiso 1 1 calc R . . H12B H 0.9549 0.3997 0.4666 0.043 Uiso 1 1 calc R . . C13 C 0.8442(2) 0.49261(14) 0.39877(17) 0.0360(5) Uani 1 1 d . . . H13A H 0.9093 0.5318 0.3914 0.043 Uiso 1 1 calc R . . H13B H 0.7859 0.4971 0.3374 0.043 Uiso 1 1 calc R . . C14 C 0.7873(2) 0.51733(12) 0.49078(16) 0.0334(4) Uani 1 1 d . . . H14A H 0.7554 0.5752 0.4817 0.040 Uiso 1 1 calc R . . H14B H 0.8471 0.5171 0.5514 0.040 Uiso 1 1 calc R . . C15 C 0.68886(18) 0.45648(11) 0.50639(16) 0.0281(4) Uani 1 1 d . . . H15A H 0.6267 0.4590 0.4476 0.034 Uiso 1 1 calc R . . H15B H 0.6541 0.4730 0.5672 0.034 Uiso 1 1 calc R . . C16 C 0.53716(16) 0.33352(11) 0.63064(14) 0.0232(3) Uani 1 1 d . . . H16A H 0.5005 0.3847 0.5960 0.028 Uiso 1 1 calc R . . C17 C 0.60843(17) 0.36338(13) 0.72965(15) 0.0287(4) Uani 1 1 d . . . H17A H 0.6442 0.3142 0.7676 0.034 Uiso 1 1 calc R . . H17B H 0.6723 0.4011 0.7146 0.034 Uiso 1 1 calc R . . C18 C 0.52926(19) 0.41031(14) 0.79355(16) 0.0352(5) Uani 1 1 d . . . H18A H 0.5756 0.4284 0.8577 0.042 Uiso 1 1 calc R . . H18B H 0.4974 0.4614 0.7572 0.042 Uiso 1 1 calc R . . C19 C 0.42866(19) 0.35425(16) 0.81602(17) 0.0373(5) Uani 1 1 d . . . H19A H 0.3761 0.3869 0.8542 0.045 Uiso 1 1 calc R . . H19B H 0.4603 0.3063 0.8586 0.045 Uiso 1 1 calc R . . C20 C 0.35874(18) 0.32060(15) 0.71921(16) 0.0348(5) Uani 1 1 d . . . H20A H 0.3183 0.3681 0.6811 0.042 Uiso 1 1 calc R . . H20B H 0.2982 0.2810 0.7367 0.042 Uiso 1 1 calc R . . C21 C 0.43645(17) 0.27543(12) 0.65251(16) 0.0281(4) Uani 1 1 d . . . H21A H 0.3891 0.2588 0.5882 0.034 Uiso 1 1 calc R . . H21B H 0.4691 0.2236 0.6868 0.034 Uiso 1 1 calc R . . C30 C 0.5733(3) 0.31333(18) 1.1304(2) 0.0534(7) Uani 1 1 d . . . H30A H 0.5189 0.2818 1.1678 0.064 Uiso 1 1 calc R . . H30B H 0.6421 0.3299 1.1790 0.064 Uiso 1 1 calc R . . Cl3 Cl 0.61976(7) 0.24716(4) 1.03721(6) 0.0642(2) Uani 1 1 d . . . Cl4 Cl 0.50344(7) 0.40376(4) 1.07801(5) 0.05589(17) 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 Pd 0.02234(8) 0.02044(8) 0.01748(8) 0.00032(5) -0.00129(5) 0.00038(4) Cl1 0.0362(2) 0.0298(2) 0.0225(2) 0.00158(17) -0.00761(18) -0.00567(18) C1 0.0254(9) 0.0212(8) 0.0236(9) -0.0004(6) -0.0035(7) -0.0009(6) Cl2 0.0464(3) 0.0311(2) 0.0346(3) -0.0016(2) -0.0112(2) 0.0151(2) P 0.0222(2) 0.01800(19) 0.0182(2) -0.00082(15) 0.00059(16) 0.00064(15) N2 0.0314(8) 0.0210(7) 0.0180(7) 0.0022(5) 0.0002(6) -0.0011(6) C3 0.0185(7) 0.0202(7) 0.0243(9) 0.0016(6) 0.0016(6) -0.0008(6) N4 0.0232(7) 0.0222(7) 0.0198(7) 0.0001(5) 0.0022(5) -0.0003(5) C5 0.0271(9) 0.0290(9) 0.0248(9) -0.0047(7) 0.0041(7) 0.0014(7) C6 0.0360(11) 0.0286(9) 0.0338(11) -0.0094(8) 0.0025(9) 0.0052(8) C7 0.0375(11) 0.0212(8) 0.0418(12) -0.0033(8) 0.0021(9) 0.0008(8) C8 0.0306(9) 0.0209(8) 0.0314(10) 0.0040(7) 0.0014(8) -0.0009(7) C9 0.0455(12) 0.0306(9) 0.0196(9) 0.0042(7) 0.0002(8) 0.0012(9) C10 0.0246(8) 0.0212(8) 0.0210(8) 0.0004(6) 0.0036(6) 0.0011(6) C11 0.0324(10) 0.0284(9) 0.0244(9) -0.0022(7) 0.0082(7) 0.0033(7) C12 0.0350(11) 0.0387(11) 0.0354(11) 0.0019(9) 0.0136(9) -0.0013(9) C13 0.0447(12) 0.0339(10) 0.0313(11) 0.0068(8) 0.0119(9) -0.0058(9) C14 0.0455(12) 0.0244(9) 0.0321(11) 0.0021(8) 0.0113(9) -0.0049(8) C15 0.0349(10) 0.0203(8) 0.0304(10) -0.0001(7) 0.0095(8) 0.0015(7) C16 0.0253(8) 0.0232(8) 0.0213(9) -0.0014(7) 0.0041(7) -0.0007(6) C17 0.0291(9) 0.0341(10) 0.0235(9) -0.0051(7) 0.0051(7) -0.0056(8) C18 0.0391(11) 0.0415(11) 0.0260(10) -0.0098(8) 0.0076(8) 0.0005(9) C19 0.0286(10) 0.0587(14) 0.0258(10) -0.0022(9) 0.0079(8) 0.0029(9) C20 0.0263(9) 0.0489(12) 0.0298(11) -0.0012(9) 0.0055(8) -0.0012(9) C21 0.0241(9) 0.0316(9) 0.0286(10) -0.0025(8) 0.0038(7) -0.0030(7) C30 0.0622(17) 0.0543(15) 0.0409(14) 0.0127(12) -0.0037(12) -0.0079(13) Cl3 0.0662(4) 0.0439(3) 0.0735(5) -0.0075(3) -0.0233(4) 0.0127(3) Cl4 0.0847(5) 0.0363(3) 0.0493(4) -0.0030(3) 0.0186(3) 0.0007(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd N4 2.0995(15) . ? Pd P 2.2092(5) . ? Pd Cl2 2.2935(5) . ? Pd Cl1 2.4132(5) . ? C1 N2 1.469(2) . ? C1 P 1.8269(18) . ? P C16 1.8320(19) . ? P C10 1.8386(18) . ? N2 C3 1.373(2) . ? N2 C9 1.463(2) . ? C3 N4 1.360(2) . ? C3 C8 1.412(2) . ? N4 C5 1.354(2) . ? C5 C6 1.374(3) . ? C6 C7 1.383(3) . ? C7 C8 1.373(3) . ? C10 C15 1.534(2) . ? C10 C11 1.543(3) . ? C11 C12 1.520(3) . ? C12 C13 1.525(3) . ? C13 C14 1.523(3) . ? C14 C15 1.525(3) . ? C16 C17 1.536(3) . ? C16 C21 1.541(3) . ? C17 C18 1.526(3) . ? C18 C19 1.523(3) . ? C19 C20 1.526(3) . ? C20 C21 1.526(3) . ? C30 Cl4 1.745(3) . ? C30 Cl3 1.768(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Pd P 92.55(4) . . ? N4 Pd Cl2 177.91(4) . . ? P Pd Cl2 85.759(19) . . ? N4 Pd Cl1 91.70(4) . . ? P Pd Cl1 175.700(17) . . ? Cl2 Pd Cl1 90.013(19) . . ? N2 C1 P 111.35(12) . . ? C1 P C16 107.46(9) . . ? C1 P C10 103.25(8) . . ? C16 P C10 107.16(8) . . ? C1 P Pd 105.27(6) . . ? C16 P Pd 116.76(6) . . ? C10 P Pd 115.77(6) . . ? C3 N2 C9 118.90(15) . . ? C3 N2 C1 116.07(15) . . ? C9 N2 C1 115.38(15) . . ? N4 C3 N2 118.57(15) . . ? N4 C3 C8 120.48(17) . . ? N2 C3 C8 120.93(17) . . ? C5 N4 C3 118.00(15) . . ? C5 N4 Pd 115.39(12) . . ? C3 N4 Pd 124.03(12) . . ? N4 C5 C6 123.38(19) . . ? C5 C6 C7 118.35(19) . . ? C8 C7 C6 119.79(18) . . ? C7 C8 C3 119.31(19) . . ? C15 C10 C11 110.26(15) . . ? C15 C10 P 115.36(13) . . ? C11 C10 P 110.21(12) . . ? C12 C11 C10 110.89(16) . . ? C11 C12 C13 111.28(17) . . ? C14 C13 C12 110.66(17) . . ? C13 C14 C15 110.97(17) . . ? C14 C15 C10 109.99(16) . . ? C17 C16 C21 110.42(15) . . ? C17 C16 P 112.10(13) . . ? C21 C16 P 113.01(12) . . ? C18 C17 C16 110.09(16) . . ? C19 C18 C17 110.78(18) . . ? C18 C19 C20 111.40(18) . . ? C19 C20 C21 112.12(17) . . ? C20 C21 C16 110.32(16) . . ? Cl4 C30 Cl3 111.84(15) . . ? _diffrn_measured_fraction_theta_max 0.939 _diffrn_reflns_theta_full 32.06 _diffrn_measured_fraction_theta_full 0.939 _refine_diff_density_max 1.348 _refine_diff_density_min -0.986 _refine_diff_density_rms 0.099 #===END data_Compound_3 _database_code_depnum_ccdc_archive 'CCDC 650214' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H27 Cl2 N2 P Pd' _chemical_formula_sum 'C15 H27 Cl2 N2 P Pd' _chemical_formula_weight 443.66 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' _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 8.5961(13) _cell_length_b 13.265(2) _cell_length_c 16.3961(3) _cell_angle_alpha 90.00 _cell_angle_beta 105.141(5) _cell_angle_gamma 90.00 _cell_volume 1804.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 23948 _cell_measurement_theta_min 3.8521 _cell_measurement_theta_max 31.9408 _exptl_crystal_description prisms _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.633 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 904 _exptl_absorpt_coefficient_mu 1.408 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.69159 _exptl_absorpt_correction_T_max 0.81759 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET) (compiled Jan 20 2006,12:36:28) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur 3' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 15.9863 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29195 _diffrn_reflns_av_R_equivalents 0.0328 _diffrn_reflns_av_sigmaI/netI 0.0157 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.93 _diffrn_reflns_theta_max 32.01 _reflns_number_total 5755 _reflns_number_gt 5342 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0206P)^2^+1.1359P] 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 SHELXL _refine_ls_extinction_coef 0.0032(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5755 _refine_ls_number_parameters 192 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0228 _refine_ls_R_factor_gt 0.0205 _refine_ls_wR_factor_ref 0.0515 _refine_ls_wR_factor_gt 0.0505 _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_restrained_S_all 1.107 _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 Pd Pd 0.140979(11) 0.265494(7) 0.482941(6) 0.01627(4) Uani 1 1 d . . . Cl1 Cl 0.00110(4) 0.22694(3) 0.33992(2) 0.02674(7) Uani 1 1 d . . . Cl2 Cl 0.33452(5) 0.34179(4) 0.43166(2) 0.03706(10) Uani 1 1 d . . . P P 0.27151(4) 0.30802(2) 0.61578(2) 0.01668(6) Uani 1 1 d . . . C1 C 0.17225(17) 0.23019(10) 0.68007(8) 0.0209(2) Uani 1 1 d . . . H1A H 0.2399 0.2290 0.7391 0.025 Uiso 1 1 calc R . . H1B H 0.0676 0.2612 0.6802 0.025 Uiso 1 1 calc R . . N2 N 0.14474(15) 0.12636(9) 0.64879(7) 0.0217(2) Uani 1 1 d . . . C3 C 0.00732(16) 0.11162(10) 0.58487(8) 0.0189(2) Uani 1 1 d . . . N4 N -0.03368(13) 0.18428(8) 0.52468(7) 0.01830(19) Uani 1 1 d . . . C5 C -0.18238(16) 0.17974(12) 0.46966(9) 0.0237(3) Uani 1 1 d . . . H5A H -0.2159 0.2339 0.4312 0.028 Uiso 1 1 calc R . . C6 C -0.28667(18) 0.10031(13) 0.46710(9) 0.0291(3) Uani 1 1 d . . . H6A H -0.3906 0.1003 0.4286 0.035 Uiso 1 1 calc R . . C7 C -0.23603(19) 0.02021(12) 0.52232(10) 0.0296(3) Uani 1 1 d . . . H7A H -0.3017 -0.0381 0.5188 0.036 Uiso 1 1 calc R . . C8 C -0.09053(18) 0.02567(10) 0.58204(9) 0.0247(3) Uani 1 1 d . . . H8A H -0.0562 -0.0279 0.6210 0.030 Uiso 1 1 calc R . . C9 C 0.1932(2) 0.04777(12) 0.71308(10) 0.0324(3) Uani 1 1 d . . . H9A H 0.1175 0.0463 0.7486 0.049 Uiso 1 1 calc R . . H9B H 0.3019 0.0622 0.7483 0.049 Uiso 1 1 calc R . . H9C H 0.1928 -0.0178 0.6855 0.049 Uiso 1 1 calc R . . C10 C 0.22410(18) 0.44025(11) 0.64190(10) 0.0259(3) Uani 1 1 d . . . C11 C 0.0393(2) 0.45010(13) 0.61664(13) 0.0380(4) Uani 1 1 d . . . H11A H 0.0091 0.5184 0.6295 0.057 Uiso 1 1 calc R . . H11B H -0.0068 0.4010 0.6484 0.057 Uiso 1 1 calc R . . H11C H -0.0020 0.4372 0.5560 0.057 Uiso 1 1 calc R . . C12 C 0.2927(2) 0.51722(12) 0.59094(13) 0.0384(4) Uani 1 1 d . . . H12A H 0.2666 0.5855 0.6059 0.058 Uiso 1 1 calc R . . H12B H 0.2454 0.5060 0.5305 0.058 Uiso 1 1 calc R . . H12C H 0.4100 0.5094 0.6038 0.058 Uiso 1 1 calc R . . C13 C 0.2867(3) 0.46300(14) 0.73677(12) 0.0401(4) Uani 1 1 d . . . H13A H 0.2595 0.5326 0.7477 0.060 Uiso 1 1 calc R . . H13B H 0.4040 0.4543 0.7542 0.060 Uiso 1 1 calc R . . H13C H 0.2365 0.4166 0.7689 0.060 Uiso 1 1 calc R . . C14 C 0.49096(17) 0.27425(11) 0.65394(9) 0.0245(3) Uani 1 1 d . . . C15 C 0.60252(19) 0.35377(15) 0.63083(12) 0.0379(4) Uani 1 1 d . . . H15A H 0.7150 0.3325 0.6524 0.057 Uiso 1 1 calc R . . H15B H 0.5866 0.4187 0.6561 0.057 Uiso 1 1 calc R . . H15C H 0.5771 0.3608 0.5693 0.057 Uiso 1 1 calc R . . C16 C 0.5435(2) 0.25754(16) 0.74980(11) 0.0376(4) Uani 1 1 d . . . H16A H 0.6584 0.2404 0.7670 0.056 Uiso 1 1 calc R . . H16B H 0.4808 0.2022 0.7649 0.056 Uiso 1 1 calc R . . H16C H 0.5249 0.3193 0.7787 0.056 Uiso 1 1 calc R . . C17 C 0.5113(2) 0.17428(13) 0.61038(11) 0.0330(3) Uani 1 1 d . . . H17A H 0.6243 0.1530 0.6283 0.049 Uiso 1 1 calc R . . H17B H 0.4795 0.1836 0.5490 0.049 Uiso 1 1 calc R . . H17C H 0.4431 0.1225 0.6261 0.049 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd 0.01824(5) 0.01702(5) 0.01395(5) 0.00096(3) 0.00494(3) -0.00196(3) Cl1 0.02992(16) 0.03522(18) 0.01482(13) -0.00026(11) 0.00538(11) -0.00740(13) Cl2 0.03147(18) 0.0553(3) 0.02579(16) 0.00628(16) 0.00986(14) -0.01777(17) P 0.01734(14) 0.01681(14) 0.01612(13) -0.00192(10) 0.00478(10) -0.00177(10) C1 0.0271(6) 0.0217(6) 0.0154(5) -0.0028(4) 0.0080(5) -0.0037(5) N2 0.0283(6) 0.0187(5) 0.0169(5) 0.0025(4) 0.0037(4) -0.0032(4) C3 0.0235(6) 0.0176(5) 0.0176(5) -0.0015(4) 0.0091(4) -0.0015(4) N4 0.0207(5) 0.0185(5) 0.0166(4) -0.0004(4) 0.0066(4) -0.0026(4) C5 0.0223(6) 0.0305(7) 0.0193(6) -0.0005(5) 0.0069(5) -0.0015(5) C6 0.0233(6) 0.0405(8) 0.0245(6) -0.0068(6) 0.0081(5) -0.0092(6) C7 0.0323(7) 0.0299(7) 0.0305(7) -0.0087(6) 0.0149(6) -0.0142(6) C8 0.0327(7) 0.0191(6) 0.0261(6) -0.0019(5) 0.0145(5) -0.0058(5) C9 0.0433(9) 0.0270(7) 0.0239(7) 0.0100(6) 0.0036(6) -0.0015(6) C10 0.0286(7) 0.0178(6) 0.0322(7) -0.0054(5) 0.0098(5) -0.0028(5) C11 0.0316(8) 0.0262(7) 0.0577(11) -0.0045(7) 0.0143(7) 0.0069(6) C12 0.0447(9) 0.0207(7) 0.0520(10) 0.0033(7) 0.0161(8) -0.0049(6) C13 0.0538(11) 0.0311(8) 0.0361(9) -0.0165(7) 0.0131(8) -0.0055(7) C14 0.0188(6) 0.0322(7) 0.0212(6) -0.0033(5) 0.0030(5) 0.0007(5) C15 0.0220(7) 0.0482(10) 0.0422(9) -0.0024(8) 0.0062(6) -0.0093(6) C16 0.0289(8) 0.0571(11) 0.0219(7) -0.0012(7) -0.0022(6) 0.0062(7) C17 0.0292(7) 0.0359(8) 0.0336(8) -0.0044(6) 0.0079(6) 0.0106(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 Pd N4 2.1024(11) . ? Pd P 2.2460(3) . ? Pd Cl2 2.2869(4) . ? Pd Cl1 2.3945(4) . ? P C1 1.8372(14) . ? P C10 1.8754(15) . ? P C14 1.8799(15) . ? C1 N2 1.4671(17) . ? N2 C3 1.3731(17) . ? N2 C9 1.4636(18) . ? C3 N4 1.3585(16) . ? C3 C8 1.4104(18) . ? N4 C5 1.3597(17) . ? C5 C6 1.377(2) . ? C6 C7 1.390(2) . ? C7 C8 1.374(2) . ? C10 C12 1.532(2) . ? C10 C13 1.537(2) . ? C10 C11 1.539(2) . ? C14 C16 1.534(2) . ? C14 C17 1.538(2) . ? C14 C15 1.538(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 N4 Pd P 91.80(3) . . ? N4 Pd Cl2 175.16(3) . . ? P Pd Cl2 91.044(15) . . ? N4 Pd Cl1 89.47(3) . . ? P Pd Cl1 177.781(13) . . ? Cl2 Pd Cl1 87.817(15) . . ? C1 P C10 103.50(6) . . ? C1 P C14 104.54(7) . . ? C10 P C14 113.95(7) . . ? C1 P Pd 103.06(4) . . ? C10 P Pd 111.90(5) . . ? C14 P Pd 117.82(5) . . ? N2 C1 P 112.56(9) . . ? C3 N2 C9 118.34(12) . . ? C3 N2 C1 115.37(11) . . ? C9 N2 C1 115.30(11) . . ? N4 C3 N2 117.50(11) . . ? N4 C3 C8 120.68(12) . . ? N2 C3 C8 121.80(12) . . ? C3 N4 C5 118.11(11) . . ? C3 N4 Pd 121.89(9) . . ? C5 N4 Pd 115.74(9) . . ? N4 C5 C6 123.08(14) . . ? C5 C6 C7 118.32(14) . . ? C8 C7 C6 119.72(13) . . ? C7 C8 C3 119.34(14) . . ? C12 C10 C13 109.77(14) . . ? C12 C10 C11 108.31(14) . . ? C13 C10 C11 108.64(14) . . ? C12 C10 P 111.18(11) . . ? C13 C10 P 112.03(11) . . ? C11 C10 P 106.77(10) . . ? C16 C14 C17 108.22(14) . . ? C16 C14 C15 108.42(14) . . ? C17 C14 C15 108.86(14) . . ? C16 C14 P 112.13(11) . . ? C17 C14 P 106.07(10) . . ? C15 C14 P 112.98(11) . . ? _diffrn_measured_fraction_theta_max 0.916 _diffrn_reflns_theta_full 32.01 _diffrn_measured_fraction_theta_full 0.916 _refine_diff_density_max 0.563 _refine_diff_density_min -0.736 _refine_diff_density_rms 0.067 #===END data_Compound_4 _database_code_depnum_ccdc_archive 'CCDC 650215' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H62 Cl2 N4 P2 Pd' _chemical_formula_sum 'C38 H62 Cl2 N4 P2 Pd' _chemical_formula_weight 814.16 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.171(4) _cell_length_b 20.345(4) _cell_length_c 9.4447(8) _cell_angle_alpha 90.00 _cell_angle_beta 104.668(12) _cell_angle_gamma 90.00 _cell_volume 3935.4(11) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 15930 _cell_measurement_theta_min 3.8892 _cell_measurement_theta_max 31.9904 _exptl_crystal_description needles _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.374 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1712 _exptl_absorpt_coefficient_mu 0.721 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.98522 _exptl_absorpt_correction_T_max 1.01999 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET) (compiled Jan 20 2006,12:36:28) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur 3' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 15.9863 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28365 _diffrn_reflns_av_R_equivalents 0.0300 _diffrn_reflns_av_sigmaI/netI 0.0303 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.90 _diffrn_reflns_theta_max 32.06 _reflns_number_total 6437 _reflns_number_gt 4982 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET) (compiled Jan 20 2006,12:36:28) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET) (compiled Jan 20 2006,12:36:28) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET) (compiled Jan 20 2006,12:36:28) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0460P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6437 _refine_ls_number_parameters 214 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0413 _refine_ls_R_factor_gt 0.0293 _refine_ls_wR_factor_ref 0.0756 _refine_ls_wR_factor_gt 0.0734 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _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 Pd Pd 0.0000 0.280666(7) 0.7500 0.01940(5) Uani 1 2 d S . . Cl Cl 0.078793(17) 0.29031(2) 0.96771(4) 0.03081(9) Uani 1 1 d . . . P P 0.081945(16) 0.274559(16) 0.62472(4) 0.01839(7) Uani 1 1 d . . . C1 C 0.05660(8) 0.23045(7) 0.44610(16) 0.0255(3) Uani 1 1 d . . . H1A H 0.0138 0.2481 0.3911 0.031 Uiso 1 1 calc R . . H1B H 0.0886 0.2405 0.3888 0.031 Uiso 1 1 calc R . . N2 N 0.05110(7) 0.15964(6) 0.45552(15) 0.0318(3) Uani 1 1 d . . . C3 C 0.08551(7) 0.11861(7) 0.38686(16) 0.0286(3) Uani 1 1 d . . . N4 N 0.12828(7) 0.14645(7) 0.32092(16) 0.0384(3) Uani 1 1 d . . . C5 C 0.16072(9) 0.10670(11) 0.2505(2) 0.0501(5) Uani 1 1 d . . . H5A H 0.1908 0.1260 0.2033 0.060 Uiso 1 1 calc R . . C6 C 0.15281(10) 0.03939(11) 0.2427(2) 0.0599(6) Uani 1 1 d . . . H6A H 0.1763 0.0130 0.1906 0.072 Uiso 1 1 calc R . . C7 C 0.11017(10) 0.01206(10) 0.3124(3) 0.0594(6) Uani 1 1 d . . . H7A H 0.1039 -0.0342 0.3095 0.071 Uiso 1 1 calc R . . C8 C 0.07613(9) 0.05061(8) 0.3868(2) 0.0416(4) Uani 1 1 d . . . H8A H 0.0470 0.0316 0.4369 0.050 Uiso 1 1 calc R . . C9 C -0.00028(9) 0.13321(9) 0.5152(2) 0.0397(4) Uani 1 1 d . . . H9A H -0.0298 0.1064 0.4408 0.060 Uiso 1 1 calc R . . H9B H -0.0248 0.1694 0.5445 0.060 Uiso 1 1 calc R . . H9C H 0.0190 0.1059 0.6008 0.060 Uiso 1 1 calc R . . C10 C 0.15950(7) 0.23658(7) 0.72697(15) 0.0216(3) Uani 1 1 d . . . H10A H 0.1762 0.2648 0.8152 0.026 Uiso 1 1 calc R . . C11 C 0.15048(7) 0.16739(7) 0.78538(17) 0.0288(3) Uani 1 1 d . . . H11A H 0.1176 0.1690 0.8435 0.035 Uiso 1 1 calc R . . H11B H 0.1344 0.1370 0.7022 0.035 Uiso 1 1 calc R . . C12 C 0.21526(8) 0.14211(8) 0.88103(19) 0.0360(4) Uani 1 1 d . . . H12A H 0.2293 0.1706 0.9683 0.043 Uiso 1 1 calc R . . H12B H 0.2091 0.0971 0.9150 0.043 Uiso 1 1 calc R . . C13 C 0.26788(8) 0.14128(8) 0.7980(2) 0.0387(4) Uani 1 1 d . . . H13A H 0.2556 0.1099 0.7156 0.046 Uiso 1 1 calc R . . H13B H 0.3096 0.1264 0.8639 0.046 Uiso 1 1 calc R . . C14 C 0.27681(7) 0.20950(8) 0.73945(18) 0.0310(3) Uani 1 1 d . . . H14A H 0.3095 0.2073 0.6810 0.037 Uiso 1 1 calc R . . H14B H 0.2936 0.2397 0.8226 0.037 Uiso 1 1 calc R . . C15 C 0.21285(7) 0.23652(8) 0.64440(16) 0.0260(3) Uani 1 1 d . . . H15A H 0.1987 0.2093 0.5551 0.031 Uiso 1 1 calc R . . H15B H 0.2198 0.2819 0.6139 0.031 Uiso 1 1 calc R . . C16 C 0.10651(7) 0.35509(6) 0.56734(14) 0.0215(3) Uani 1 1 d . . . H16A H 0.1389 0.3468 0.5085 0.026 Uiso 1 1 calc R . . C17 C 0.14033(8) 0.39757(7) 0.69819(16) 0.0285(3) Uani 1 1 d . . . H17A H 0.1093 0.4075 0.7580 0.034 Uiso 1 1 calc R . . H17B H 0.1776 0.3731 0.7602 0.034 Uiso 1 1 calc R . . C18 C 0.16480(8) 0.46181(8) 0.64688(19) 0.0362(4) Uani 1 1 d . . . H18A H 0.1846 0.4894 0.7330 0.043 Uiso 1 1 calc R . . H18B H 0.1991 0.4519 0.5955 0.043 Uiso 1 1 calc R . . C19 C 0.10971(9) 0.49957(8) 0.54478(19) 0.0368(4) Uani 1 1 d . . . H19A H 0.0784 0.5147 0.5998 0.044 Uiso 1 1 calc R . . H19B H 0.1277 0.5388 0.5070 0.044 Uiso 1 1 calc R . . C20 C 0.07450(9) 0.45711(8) 0.41775(17) 0.0379(4) Uani 1 1 d . . . H20A H 0.1046 0.4464 0.3561 0.046 Uiso 1 1 calc R . . H20B H 0.0372 0.4819 0.3568 0.046 Uiso 1 1 calc R . . C21 C 0.04957(8) 0.39345(8) 0.46998(17) 0.0305(3) Uani 1 1 d . . . H21A H 0.0279 0.3663 0.3845 0.037 Uiso 1 1 calc R . . H21B H 0.0170 0.4038 0.5258 0.037 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd 0.01500(7) 0.02425(8) 0.01867(7) 0.000 0.00376(5) 0.000 Cl 0.01872(16) 0.0511(2) 0.02078(16) -0.00131(14) 0.00161(12) -0.00099(14) P 0.01543(15) 0.02059(17) 0.01951(16) -0.00077(12) 0.00506(12) -0.00006(12) C1 0.0264(7) 0.0264(7) 0.0249(7) -0.0050(5) 0.0086(6) -0.0025(5) N2 0.0354(7) 0.0265(6) 0.0383(7) -0.0105(5) 0.0182(6) -0.0083(5) C3 0.0253(7) 0.0287(7) 0.0284(7) -0.0081(6) 0.0007(6) -0.0003(6) N4 0.0326(7) 0.0430(8) 0.0420(8) -0.0125(6) 0.0137(6) -0.0003(6) C5 0.0328(9) 0.0656(13) 0.0533(11) -0.0190(10) 0.0136(8) 0.0056(9) C6 0.0374(10) 0.0641(14) 0.0725(14) -0.0360(12) 0.0032(10) 0.0182(10) C7 0.0451(11) 0.0330(10) 0.0897(16) -0.0194(10) -0.0018(11) 0.0107(8) C8 0.0383(9) 0.0282(8) 0.0542(11) -0.0033(8) 0.0045(8) 0.0011(7) C9 0.0404(9) 0.0366(9) 0.0473(9) -0.0115(8) 0.0204(8) -0.0147(7) C10 0.0192(6) 0.0203(6) 0.0257(6) 0.0011(5) 0.0062(5) 0.0007(5) C11 0.0261(7) 0.0233(7) 0.0369(8) 0.0054(6) 0.0076(6) -0.0007(5) C12 0.0345(8) 0.0250(8) 0.0449(9) 0.0103(7) 0.0032(7) 0.0023(6) C13 0.0271(8) 0.0300(8) 0.0545(10) 0.0026(8) 0.0020(7) 0.0087(6) C14 0.0184(7) 0.0352(8) 0.0392(8) 0.0013(6) 0.0069(6) 0.0030(6) C15 0.0196(7) 0.0300(7) 0.0298(7) 0.0014(6) 0.0089(6) 0.0018(5) C16 0.0208(6) 0.0218(6) 0.0224(6) 0.0006(5) 0.0063(5) -0.0002(5) C17 0.0323(8) 0.0228(7) 0.0256(7) 0.0012(5) -0.0018(6) -0.0013(6) C18 0.0351(9) 0.0254(7) 0.0409(8) 0.0032(7) -0.0035(7) -0.0072(6) C19 0.0423(9) 0.0237(7) 0.0399(8) 0.0080(6) 0.0021(7) -0.0013(7) C20 0.0427(9) 0.0342(9) 0.0311(8) 0.0119(7) -0.0013(7) -0.0026(7) C21 0.0286(8) 0.0292(8) 0.0276(7) 0.0052(6) -0.0040(6) -0.0021(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 Pd Cl 2.3048(5) . ? Pd Cl 2.3048(5) 2_556 ? Pd P 2.3376(5) 2_556 ? Pd P 2.3376(5) . ? P C16 1.8415(14) . ? P C10 1.8500(14) . ? P C1 1.8657(14) . ? C1 N2 1.4499(18) . ? N2 C3 1.3738(19) . ? N2 C9 1.450(2) . ? C3 N4 1.347(2) . ? C3 C8 1.398(2) . ? N4 C5 1.341(2) . ? C5 C6 1.379(3) . ? C6 C7 1.363(3) . ? C7 C8 1.373(3) . ? C10 C15 1.526(2) . ? C10 C11 1.5412(19) . ? C11 C12 1.528(2) . ? C12 C13 1.516(2) . ? C13 C14 1.524(2) . ? C14 C15 1.525(2) . ? C16 C17 1.5293(19) . ? C16 C21 1.532(2) . ? C17 C18 1.529(2) . ? C18 C19 1.520(2) . ? C19 C20 1.513(2) . ? C20 C21 1.527(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 Cl Pd Cl 170.23(2) . 2_556 ? Cl Pd P 90.870(18) . 2_556 ? Cl Pd P 89.649(18) 2_556 2_556 ? Cl Pd P 89.649(18) . . ? Cl Pd P 90.870(18) 2_556 . ? P Pd P 173.907(17) 2_556 . ? C16 P C10 104.23(6) . . ? C16 P C1 101.52(6) . . ? C10 P C1 106.57(7) . . ? C16 P Pd 113.75(4) . . ? C10 P Pd 115.61(5) . . ? C1 P Pd 113.76(5) . . ? N2 C1 P 115.57(10) . . ? C3 N2 C9 119.88(13) . . ? C3 N2 C1 120.96(13) . . ? C9 N2 C1 118.18(13) . . ? N4 C3 N2 117.49(14) . . ? N4 C3 C8 121.89(15) . . ? N2 C3 C8 120.62(15) . . ? C5 N4 C3 117.66(17) . . ? N4 C5 C6 123.7(2) . . ? C7 C6 C5 117.75(18) . . ? C6 C7 C8 120.77(19) . . ? C7 C8 C3 118.22(18) . . ? C15 C10 C11 110.91(12) . . ? C15 C10 P 114.04(10) . . ? C11 C10 P 113.23(10) . . ? C12 C11 C10 110.19(12) . . ? C13 C12 C11 111.42(13) . . ? C12 C13 C14 110.66(13) . . ? C13 C14 C15 111.64(13) . . ? C14 C15 C10 111.17(12) . . ? C17 C16 C21 109.47(12) . . ? C17 C16 P 111.98(9) . . ? C21 C16 P 113.08(10) . . ? C18 C17 C16 110.71(12) . . ? C19 C18 C17 111.47(13) . . ? C20 C19 C18 111.06(14) . . ? C19 C20 C21 111.67(13) . . ? C20 C21 C16 110.02(13) . . ? _diffrn_measured_fraction_theta_max 0.938 _diffrn_reflns_theta_full 32.06 _diffrn_measured_fraction_theta_full 0.938 _refine_diff_density_max 1.204 _refine_diff_density_min -0.619 _refine_diff_density_rms 0.067 #===END data_Compound_5 _database_code_depnum_ccdc_archive 'CCDC 650216' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H38 N4 P2 Pd, 2(Cl O4), C H2 Cl2' _chemical_formula_sum 'C39 H40 Cl4 N4 O8 P2 Pd' _chemical_formula_weight 1002.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd 0.1215 3.9337 '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 9.8852(1) _cell_length_b 19.9719(1) _cell_length_c 21.5616(1) _cell_angle_alpha 90.00 _cell_angle_beta 98.528(1) _cell_angle_gamma 90.00 _cell_volume 4209.76(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 32907 _cell_measurement_theta_min 3.0278 _cell_measurement_theta_max 71.2804 _exptl_crystal_description blocks _exptl_crystal_colour 'Pale yellow' _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.582 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2040 _exptl_absorpt_coefficient_mu 7.086 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.78823 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54248 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance Ultra (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur PX Ultra' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.2556 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 60736 _diffrn_reflns_av_R_equivalents 0.0358 _diffrn_reflns_av_sigmaI/netI 0.0205 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 71.47 _reflns_number_total 8162 _reflns_number_gt 6763 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0574P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00019(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8162 _refine_ls_number_parameters 566 _refine_ls_number_restraints 101 _refine_ls_R_factor_all 0.0372 _refine_ls_R_factor_gt 0.0305 _refine_ls_wR_factor_ref 0.0839 _refine_ls_wR_factor_gt 0.0814 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.243 _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 Pd Pd 0.812560(19) 0.277058(9) 0.491568(8) 0.02261(8) Uani 1 1 d . . . P1 P 0.76908(7) 0.17807(3) 0.44481(3) 0.02492(15) Uani 1 1 d . . . C1 C 0.6050(3) 0.19703(15) 0.39737(13) 0.0313(6) Uani 1 1 d . . . H1A H 0.5774 0.1578 0.3704 0.038 Uiso 1 1 calc R . . H1B H 0.5361 0.2024 0.4260 0.038 Uiso 1 1 calc R . . N2 N 0.5988(3) 0.25600(14) 0.35741(11) 0.0354(6) Uani 1 1 d . . . C3 C 0.7042(3) 0.29683(15) 0.34931(13) 0.0288(6) Uani 1 1 d . . . N4 N 0.8059(2) 0.30738(11) 0.39789(10) 0.0264(5) Uani 1 1 d . . . C5 C 0.9159(3) 0.34491(15) 0.38893(14) 0.0327(6) Uani 1 1 d . . . H5A H 0.9898 0.3483 0.4224 0.039 Uiso 1 1 calc R . . C6 C 0.9260(3) 0.37779(16) 0.33488(14) 0.0387(7) Uani 1 1 d . . . H6A H 1.0036 0.4045 0.3307 0.046 Uiso 1 1 calc R . . C7 C 0.8186(4) 0.37104(17) 0.28577(14) 0.0418(8) Uani 1 1 d . . . H7A H 0.8207 0.3946 0.2477 0.050 Uiso 1 1 calc R . . C8 C 0.7101(3) 0.33075(16) 0.29209(14) 0.0375(7) Uani 1 1 d . . . H8A H 0.6382 0.3254 0.2580 0.045 Uiso 1 1 calc R . . C9 C 0.4730(3) 0.25812(19) 0.31213(15) 0.0442(8) Uani 1 1 d . . . H9A H 0.4535 0.3045 0.2988 0.066 Uiso 1 1 calc R . . H9B H 0.3968 0.2406 0.3317 0.066 Uiso 1 1 calc R . . H9C H 0.4843 0.2306 0.2756 0.066 Uiso 1 1 calc R . . C10 C 0.7319(3) 0.10428(14) 0.48739(13) 0.0299(6) Uani 1 1 d . . . C11 C 0.8133(3) 0.04679(16) 0.48729(14) 0.0358(7) Uani 1 1 d . . . H11A H 0.8867 0.0457 0.4635 0.043 Uiso 1 1 calc R . . C12 C 0.7857(4) -0.00819(16) 0.52207(16) 0.0432(8) Uani 1 1 d . . . H12A H 0.8403 -0.0473 0.5218 0.052 Uiso 1 1 calc R . . C13 C 0.6802(4) -0.00708(17) 0.55714(16) 0.0448(8) Uani 1 1 d . . . H13A H 0.6631 -0.0451 0.5813 0.054 Uiso 1 1 calc R . . C14 C 0.5987(4) 0.04943(17) 0.55720(15) 0.0426(8) Uani 1 1 d . . . H14A H 0.5255 0.0500 0.5812 0.051 Uiso 1 1 calc R . . C15 C 0.6242(3) 0.10493(16) 0.52233(14) 0.0348(7) Uani 1 1 d . . . H15A H 0.5681 0.1436 0.5222 0.042 Uiso 1 1 calc R . . C16 C 0.8865(3) 0.15536(14) 0.39167(13) 0.0290(6) Uani 1 1 d . . . C17 C 0.8393(3) 0.12197(16) 0.33577(14) 0.0380(7) Uani 1 1 d . . . H17A H 0.7458 0.1095 0.3261 0.046 Uiso 1 1 calc R . . C18 C 0.9301(4) 0.10711(17) 0.29444(15) 0.0481(9) Uani 1 1 d . . . H18A H 0.8980 0.0853 0.2559 0.058 Uiso 1 1 calc R . . C19 C 1.0666(4) 0.12373(18) 0.30886(17) 0.0502(9) Uani 1 1 d . . . H19A H 1.1282 0.1128 0.2805 0.060 Uiso 1 1 calc R . . C20 C 1.1141(4) 0.15625(17) 0.36442(18) 0.0468(8) Uani 1 1 d . . . H20A H 1.2083 0.1673 0.3743 0.056 Uiso 1 1 calc R . . C21 C 1.0241(3) 0.17288(16) 0.40603(16) 0.0385(7) Uani 1 1 d . . . H21A H 1.0563 0.1960 0.4439 0.046 Uiso 1 1 calc R . . P31 P 0.84781(7) 0.24417(3) 0.59205(3) 0.02479(15) Uani 1 1 d . . . C31 C 0.9381(3) 0.31422(14) 0.63626(12) 0.0295(6) Uani 1 1 d . . . H31A H 0.8710 0.3407 0.6558 0.035 Uiso 1 1 calc R . . H31B H 1.0056 0.2957 0.6704 0.035 Uiso 1 1 calc R . . N32 N 1.0091(2) 0.35895(12) 0.59776(11) 0.0294(5) Uani 1 1 d . . . C33 C 0.9226(3) 0.40413(14) 0.56258(13) 0.0275(6) Uani 1 1 d . . . N34 N 0.8207(2) 0.37788(11) 0.52150(11) 0.0264(5) Uani 1 1 d . . . C35 C 0.7256(3) 0.41897(15) 0.48913(14) 0.0333(6) Uani 1 1 d . . . H35A H 0.6516 0.3997 0.4618 0.040 Uiso 1 1 calc R . . C36 C 0.7331(3) 0.48736(16) 0.49462(16) 0.0400(7) Uani 1 1 d . . . H36A H 0.6653 0.5152 0.4718 0.048 Uiso 1 1 calc R . . C37 C 0.8420(4) 0.51456(16) 0.53426(17) 0.0442(8) Uani 1 1 d . . . H37A H 0.8512 0.5618 0.5379 0.053 Uiso 1 1 calc R . . C38 C 0.9371(3) 0.47358(15) 0.56838(16) 0.0382(7) Uani 1 1 d . . . H38A H 1.0119 0.4923 0.5956 0.046 Uiso 1 1 calc R . . C39 C 1.1394(3) 0.38461(17) 0.63035(15) 0.0396(7) Uani 1 1 d . . . H39A H 1.1866 0.4094 0.6007 0.059 Uiso 1 1 calc R . . H39B H 1.1967 0.3471 0.6478 0.059 Uiso 1 1 calc R . . H39C H 1.1221 0.4145 0.6644 0.059 Uiso 1 1 calc R . . C40 C 0.9624(3) 0.17361(15) 0.60865(13) 0.0321(6) Uani 1 1 d . . . C41 C 0.9237(4) 0.11392(16) 0.63459(16) 0.0468(8) Uani 1 1 d . . . H41A H 0.8338 0.1081 0.6443 0.056 Uiso 1 1 calc R . . C42 C 1.0203(5) 0.06315(19) 0.64588(19) 0.0670(13) Uani 1 1 d . . . H42A H 0.9954 0.0221 0.6635 0.080 Uiso 1 1 calc R . . C43 C 1.1496(5) 0.0706(2) 0.63240(19) 0.0692(14) Uani 1 1 d . . . H43A H 1.2142 0.0354 0.6412 0.083 Uiso 1 1 calc R . . C44 C 1.1868(4) 0.1296(2) 0.60580(19) 0.0607(11) Uani 1 1 d . . . H44A H 1.2767 0.1346 0.5958 0.073 Uiso 1 1 calc R . . C45 C 1.0936(4) 0.18125(18) 0.59376(16) 0.0441(8) Uani 1 1 d . . . H45A H 1.1190 0.2217 0.5754 0.053 Uiso 1 1 calc R . . C46 C 0.6977(3) 0.23491(15) 0.62950(14) 0.0315(6) Uani 1 1 d . . . C47 C 0.5739(3) 0.25898(16) 0.59785(16) 0.0387(7) Uani 1 1 d . . . H47A H 0.5678 0.2735 0.5556 0.046 Uiso 1 1 calc R . . C48 C 0.4597(4) 0.26163(19) 0.6282(2) 0.0518(9) Uani 1 1 d . . . H48A H 0.3752 0.2777 0.6065 0.062 Uiso 1 1 calc R . . C49 C 0.4685(4) 0.2411(2) 0.6894(2) 0.0592(11) Uani 1 1 d . . . H49A H 0.3902 0.2436 0.7100 0.071 Uiso 1 1 calc R . . C50 C 0.5894(4) 0.2171(2) 0.72109(17) 0.0603(11) Uani 1 1 d . . . H50A H 0.5944 0.2031 0.7635 0.072 Uiso 1 1 calc R . . C51 C 0.7053(4) 0.21322(19) 0.69100(15) 0.0470(9) Uani 1 1 d . . . H51A H 0.7886 0.1958 0.7126 0.056 Uiso 1 1 calc R . . Cl1 Cl 1.30395(8) 0.31035(4) 0.45887(4) 0.04243(19) Uani 1 1 d . . . O11 O 1.3469(3) 0.24218(14) 0.46388(15) 0.0633(8) Uani 1 1 d . . . O12 O 1.4160(3) 0.35334(17) 0.47847(18) 0.0859(11) Uani 1 1 d . . . O13 O 1.2008(3) 0.31966(14) 0.49864(12) 0.0581(7) Uani 1 1 d . . . O14 O 1.2449(3) 0.32654(16) 0.39562(12) 0.0633(8) Uani 1 1 d . . . Cl2 Cl 1.05166(12) 0.53074(5) 0.22194(4) 0.0572(2) Uani 1 1 d D . . O21 O 1.1773(5) 0.4942(3) 0.2107(2) 0.089(2) Uani 0.684(7) 1 d PD A 1 O22 O 1.0570(7) 0.5267(3) 0.2873(2) 0.113(3) Uani 0.684(7) 1 d PD A 1 O23 O 1.0805(8) 0.5961(3) 0.2075(4) 0.145(4) Uani 0.684(7) 1 d PD A 1 O24 O 0.9442(5) 0.5066(4) 0.1849(4) 0.142(4) Uani 0.684(7) 1 d PD A 1 O21' O 1.1017(13) 0.4686(5) 0.2222(6) 0.089(4) Uiso 0.316(7) 1 d PD A 2 O22' O 1.0956(14) 0.5859(6) 0.2476(7) 0.116(6) Uiso 0.316(7) 1 d PD A 2 O23' O 0.9741(10) 0.5427(5) 0.1570(4) 0.058(3) Uiso 0.316(7) 1 d PD A 2 O24' O 0.9150(11) 0.5164(6) 0.2469(6) 0.095(4) Uiso 0.316(7) 1 d PD A 2 C60 C 0.3827(14) 0.4891(6) 0.3488(9) 0.084(6) Uani 0.67(3) 1 d PD B 1 H60A H 0.3577 0.4650 0.3856 0.101 Uiso 0.67(3) 1 calc PR B 1 H60B H 0.3044 0.4865 0.3144 0.101 Uiso 0.67(3) 1 calc PR B 1 Cl3 Cl 0.4201(8) 0.5732(3) 0.3682(3) 0.0765(18) Uani 0.67(3) 1 d PD B 1 Cl4 Cl 0.5264(4) 0.4525(2) 0.32529(16) 0.0664(12) Uani 0.67(3) 1 d PD B 1 C60' C 0.3755(18) 0.4891(7) 0.3513(9) 0.037(6) Uiso 0.33(3) 1 d PD B 2 H60C H 0.3796 0.4644 0.3914 0.044 Uiso 0.33(3) 1 calc PR B 2 H60D H 0.2811 0.4849 0.3288 0.044 Uiso 0.33(3) 1 calc PR B 2 Cl3' Cl 0.4078(12) 0.5735(4) 0.3684(6) 0.051(3) Uani 0.33(3) 1 d PD B 2 Cl4' Cl 0.485(4) 0.4510(5) 0.3072(16) 0.149(6) Uani 0.33(3) 1 d PD B 2 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 Pd 0.02639(11) 0.02209(11) 0.01841(11) -0.00035(7) 0.00025(7) 0.00176(7) P1 0.0277(3) 0.0238(3) 0.0224(3) -0.0024(3) 0.0009(3) 0.0009(3) C1 0.0287(14) 0.0334(15) 0.0299(14) -0.0026(12) -0.0018(11) -0.0006(12) N2 0.0306(13) 0.0440(15) 0.0281(13) 0.0035(11) -0.0070(10) 0.0031(11) C3 0.0323(15) 0.0319(14) 0.0214(13) -0.0027(11) 0.0010(11) 0.0081(12) N4 0.0318(12) 0.0266(12) 0.0201(11) 0.0000(9) 0.0013(9) 0.0054(9) C5 0.0356(16) 0.0323(15) 0.0299(15) 0.0001(12) 0.0040(12) 0.0023(12) C6 0.0473(18) 0.0372(17) 0.0333(16) 0.0027(13) 0.0116(14) 0.0008(14) C7 0.058(2) 0.0430(18) 0.0257(15) 0.0091(13) 0.0091(14) 0.0075(16) C8 0.0448(18) 0.0426(17) 0.0231(14) 0.0019(13) -0.0019(13) 0.0089(14) C9 0.0356(17) 0.058(2) 0.0333(16) 0.0004(15) -0.0128(13) 0.0035(15) C10 0.0344(15) 0.0284(14) 0.0254(14) -0.0025(11) -0.0003(11) -0.0023(11) C11 0.0413(17) 0.0327(16) 0.0337(16) -0.0007(12) 0.0061(13) 0.0028(13) C12 0.058(2) 0.0290(16) 0.0422(18) 0.0030(14) 0.0051(16) 0.0026(15) C13 0.056(2) 0.0383(18) 0.0384(18) 0.0064(14) 0.0010(15) -0.0132(15) C14 0.0443(19) 0.0473(19) 0.0369(17) -0.0003(14) 0.0079(14) -0.0115(15) C15 0.0356(16) 0.0353(16) 0.0330(15) -0.0038(12) 0.0029(13) -0.0022(13) C16 0.0371(15) 0.0242(14) 0.0262(14) 0.0013(11) 0.0060(12) 0.0055(11) C17 0.0468(18) 0.0340(16) 0.0329(16) -0.0055(13) 0.0051(14) 0.0040(13) C18 0.074(3) 0.0419(19) 0.0297(17) -0.0070(14) 0.0131(17) 0.0098(17) C19 0.069(3) 0.0405(19) 0.048(2) 0.0061(16) 0.0318(19) 0.0115(17) C20 0.0452(19) 0.0424(19) 0.057(2) 0.0053(16) 0.0221(17) 0.0028(15) C21 0.0403(17) 0.0340(16) 0.0420(18) -0.0022(14) 0.0087(14) 0.0005(13) P31 0.0280(3) 0.0261(3) 0.0193(3) 0.0012(2) 0.0006(3) 0.0008(3) C31 0.0362(15) 0.0304(15) 0.0201(13) -0.0020(11) -0.0012(11) -0.0014(12) N32 0.0274(12) 0.0318(12) 0.0282(12) -0.0031(10) 0.0020(10) -0.0021(10) C33 0.0292(14) 0.0280(14) 0.0265(13) -0.0033(11) 0.0084(11) -0.0030(11) N34 0.0323(12) 0.0210(11) 0.0261(12) -0.0002(9) 0.0046(9) 0.0016(9) C35 0.0363(16) 0.0327(15) 0.0308(15) 0.0026(12) 0.0044(12) 0.0055(12) C36 0.0453(18) 0.0311(16) 0.0445(18) 0.0091(14) 0.0101(15) 0.0075(13) C37 0.053(2) 0.0240(15) 0.057(2) 0.0010(14) 0.0121(17) 0.0003(14) C38 0.0398(17) 0.0308(16) 0.0448(18) -0.0061(13) 0.0084(14) -0.0054(13) C39 0.0287(15) 0.0466(19) 0.0423(18) -0.0066(14) 0.0012(13) -0.0037(13) C40 0.0367(16) 0.0299(15) 0.0259(14) -0.0026(11) -0.0084(12) 0.0060(12) C41 0.061(2) 0.0324(17) 0.0405(18) 0.0037(14) -0.0156(16) -0.0016(15) C42 0.096(3) 0.0324(19) 0.057(2) 0.0012(17) -0.039(2) 0.010(2) C43 0.086(3) 0.045(2) 0.061(2) -0.0227(19) -0.042(2) 0.033(2) C44 0.051(2) 0.067(3) 0.058(2) -0.026(2) -0.0131(18) 0.0237(19) C45 0.0423(19) 0.047(2) 0.0408(18) -0.0072(15) -0.0024(14) 0.0112(15) C46 0.0355(15) 0.0335(15) 0.0261(14) -0.0042(12) 0.0061(12) -0.0056(12) C47 0.0363(17) 0.0396(17) 0.0408(17) 0.0016(14) 0.0073(14) 0.0033(13) C48 0.0409(19) 0.050(2) 0.068(3) 0.0028(18) 0.0195(18) 0.0031(16) C49 0.051(2) 0.066(3) 0.068(3) -0.009(2) 0.031(2) -0.0126(19) C50 0.068(3) 0.083(3) 0.0342(18) -0.0037(18) 0.0196(18) -0.028(2) C51 0.0418(18) 0.071(2) 0.0277(16) 0.0032(15) 0.0022(13) -0.0157(17) Cl1 0.0355(4) 0.0456(4) 0.0463(4) -0.0012(3) 0.0064(3) 0.0057(3) O11 0.0586(17) 0.0522(16) 0.078(2) -0.0097(15) 0.0066(15) 0.0179(13) O12 0.064(2) 0.081(2) 0.103(3) 0.019(2) -0.0229(18) -0.0269(17) O13 0.0646(18) 0.0621(17) 0.0522(15) 0.0086(13) 0.0235(14) 0.0234(13) O14 0.0543(16) 0.091(2) 0.0440(15) 0.0050(14) 0.0045(12) 0.0166(15) Cl2 0.0840(7) 0.0467(5) 0.0425(5) 0.0006(4) 0.0146(5) -0.0045(5) O21 0.062(3) 0.142(5) 0.062(3) -0.021(3) 0.009(2) 0.031(3) O22 0.145(6) 0.148(6) 0.060(3) 0.032(3) 0.056(4) 0.071(5) O23 0.162(7) 0.079(4) 0.173(8) 0.081(5) -0.040(6) -0.036(4) O24 0.049(3) 0.160(7) 0.213(9) -0.092(7) 0.012(4) -0.034(4) C60 0.078(7) 0.071(7) 0.110(10) -0.012(4) 0.037(5) 0.022(4) Cl3 0.093(3) 0.071(3) 0.067(3) -0.008(2) 0.016(2) -0.004(2) Cl4 0.0765(19) 0.0656(14) 0.061(2) 0.0046(9) 0.0238(18) 0.0344(11) Cl3' 0.061(4) 0.028(3) 0.074(6) -0.003(3) 0.042(4) 0.013(2) Cl4' 0.207(13) 0.059(4) 0.222(13) 0.017(6) 0.171(11) 0.027(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 Pd N4 2.100(2) . ? Pd N34 2.112(2) . ? Pd P1 2.2319(7) . ? Pd P31 2.2411(7) . ? P1 C10 1.803(3) . ? P1 C16 1.805(3) . ? P1 C1 1.825(3) . ? C1 N2 1.455(4) . ? N2 C3 1.355(4) . ? N2 C9 1.463(4) . ? C3 N4 1.356(4) . ? C3 C8 1.416(4) . ? N4 C5 1.358(4) . ? C5 C6 1.354(4) . ? C6 C7 1.390(5) . ? C7 C8 1.363(5) . ? C10 C15 1.393(4) . ? C10 C11 1.402(4) . ? C11 C12 1.379(4) . ? C12 C13 1.377(5) . ? C13 C14 1.387(5) . ? C14 C15 1.383(4) . ? C16 C21 1.394(4) . ? C16 C17 1.396(4) . ? C17 C18 1.387(5) . ? C18 C19 1.380(5) . ? C19 C20 1.382(5) . ? C20 C21 1.394(5) . ? P31 C46 1.801(3) . ? P31 C40 1.810(3) . ? P31 C31 1.847(3) . ? C31 N32 1.467(4) . ? N32 C33 1.389(4) . ? N32 C39 1.465(4) . ? C33 N34 1.345(4) . ? C33 C38 1.398(4) . ? N34 C35 1.360(4) . ? C35 C36 1.372(4) . ? C36 C37 1.383(5) . ? C37 C38 1.374(5) . ? C40 C45 1.390(5) . ? C40 C41 1.394(5) . ? C41 C42 1.389(5) . ? C42 C43 1.360(7) . ? C43 C44 1.384(7) . ? C44 C45 1.382(5) . ? C46 C51 1.386(4) . ? C46 C47 1.396(4) . ? C47 C48 1.386(5) . ? C48 C49 1.372(6) . ? C49 C50 1.372(6) . ? C50 C51 1.400(5) . ? Cl1 O12 1.416(3) . ? Cl1 O11 1.426(3) . ? Cl1 O13 1.438(3) . ? Cl1 O14 1.438(3) . ? Cl2 O22' 1.279(10) . ? Cl2 O24 1.321(5) . ? Cl2 O21' 1.336(9) . ? Cl2 O23 1.381(5) . ? Cl2 O22 1.404(5) . ? Cl2 O21 1.491(5) . ? Cl2 O23' 1.513(8) . ? Cl2 O24' 1.553(9) . ? C60 Cl4 1.738(10) . ? C60 Cl3 1.757(10) . ? C60' Cl4' 1.719(14) . ? C60' Cl3' 1.746(12) . ? 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 N4 Pd N34 90.76(9) . . ? N4 Pd P1 81.06(7) . . ? N34 Pd P1 168.09(7) . . ? N4 Pd P31 172.93(7) . . ? N34 Pd P31 89.46(6) . . ? P1 Pd P31 99.73(3) . . ? C10 P1 C16 108.46(13) . . ? C10 P1 C1 102.93(14) . . ? C16 P1 C1 107.35(14) . . ? C10 P1 Pd 122.29(9) . . ? C16 P1 Pd 114.22(10) . . ? C1 P1 Pd 99.50(10) . . ? N2 C1 P1 117.1(2) . . ? C3 N2 C1 126.7(2) . . ? C3 N2 C9 119.4(3) . . ? C1 N2 C9 112.1(3) . . ? N2 C3 N4 119.3(3) . . ? N2 C3 C8 122.1(3) . . ? N4 C3 C8 118.5(3) . . ? C3 N4 C5 119.5(2) . . ? C3 N4 Pd 127.74(19) . . ? C5 N4 Pd 112.60(19) . . ? C6 C5 N4 123.6(3) . . ? C5 C6 C7 117.6(3) . . ? C8 C7 C6 120.3(3) . . ? C7 C8 C3 120.3(3) . . ? C15 C10 C11 119.5(3) . . ? C15 C10 P1 119.9(2) . . ? C11 C10 P1 120.6(2) . . ? C12 C11 C10 119.5(3) . . ? C13 C12 C11 120.8(3) . . ? C12 C13 C14 120.1(3) . . ? C15 C14 C13 119.9(3) . . ? C14 C15 C10 120.1(3) . . ? C21 C16 C17 120.1(3) . . ? C21 C16 P1 119.6(2) . . ? C17 C16 P1 120.3(2) . . ? C18 C17 C16 119.5(3) . . ? C19 C18 C17 120.5(3) . . ? C18 C19 C20 120.2(3) . . ? C19 C20 C21 120.2(3) . . ? C20 C21 C16 119.5(3) . . ? C46 P31 C40 111.37(15) . . ? C46 P31 C31 102.32(13) . . ? C40 P31 C31 104.33(13) . . ? C46 P31 Pd 116.31(10) . . ? C40 P31 Pd 114.98(10) . . ? C31 P31 Pd 105.72(9) . . ? N32 C31 P31 113.85(18) . . ? C33 N32 C39 117.4(2) . . ? C33 N32 C31 113.4(2) . . ? C39 N32 C31 113.7(2) . . ? N34 C33 N32 116.5(2) . . ? N34 C33 C38 120.1(3) . . ? N32 C33 C38 123.3(3) . . ? C33 N34 C35 119.7(2) . . ? C33 N34 Pd 124.31(19) . . ? C35 N34 Pd 115.23(19) . . ? N34 C35 C36 122.2(3) . . ? C35 C36 C37 118.1(3) . . ? C38 C37 C36 120.3(3) . . ? C37 C38 C33 119.4(3) . . ? C45 C40 C41 120.5(3) . . ? C45 C40 P31 116.5(2) . . ? C41 C40 P31 123.0(3) . . ? C42 C41 C40 118.2(4) . . ? C43 C42 C41 121.7(4) . . ? C42 C43 C44 119.9(4) . . ? C45 C44 C43 120.2(4) . . ? C44 C45 C40 119.6(4) . . ? C51 C46 C47 119.6(3) . . ? C51 C46 P31 122.0(3) . . ? C47 C46 P31 117.8(2) . . ? C48 C47 C46 119.9(3) . . ? C49 C48 C47 120.1(4) . . ? C48 C49 C50 120.7(3) . . ? C49 C50 C51 120.0(4) . . ? C46 C51 C50 119.6(4) . . ? O12 Cl1 O11 110.2(2) . . ? O12 Cl1 O13 109.6(2) . . ? O11 Cl1 O13 107.94(17) . . ? O12 Cl1 O14 109.6(2) . . ? O11 Cl1 O14 111.16(18) . . ? O13 Cl1 O14 108.20(16) . . ? O22' Cl2 O24 140.1(7) . . ? O22' Cl2 O21' 134.1(8) . . ? O24 Cl2 O21' 85.9(6) . . ? O22' Cl2 O23 38.3(6) . . ? O24 Cl2 O23 112.5(5) . . ? O21' Cl2 O23 142.2(7) . . ? O22' Cl2 O22 69.9(7) . . ? O24 Cl2 O22 119.5(5) . . ? O21' Cl2 O22 89.1(6) . . ? O23 Cl2 O22 107.5(4) . . ? O22' Cl2 O21 104.7(7) . . ? O24 Cl2 O21 109.7(4) . . ? O21' Cl2 O21 39.5(5) . . ? O23 Cl2 O21 102.8(5) . . ? O22 Cl2 O21 103.1(3) . . ? O22' Cl2 O23' 110.9(7) . . ? O24 Cl2 O23' 41.1(4) . . ? O21' Cl2 O23' 106.7(6) . . ? O23 Cl2 O23' 74.7(5) . . ? O22 Cl2 O23' 151.2(4) . . ? O21 Cl2 O23' 104.3(4) . . ? O22' Cl2 O24' 105.4(7) . . ? O24 Cl2 O24' 58.7(5) . . ? O21' Cl2 O24' 99.7(6) . . ? O23 Cl2 O24' 118.1(6) . . ? O22 Cl2 O24' 63.0(5) . . ? O21 Cl2 O24' 139.0(5) . . ? O23' Cl2 O24' 90.2(5) . . ? Cl4 C60 Cl3 108.6(7) . . ? Cl4' C60' Cl3' 115.8(11) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 71.47 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.610 _refine_diff_density_min -0.608 _refine_diff_density_rms 0.066 #===END