# Electronic Supplementary Material for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Manu Lahtinen' _publ_contact_author_email MANU.LAHTINEN@JYU.FI _publ_section_title ; The conformational polymorphism and weak interactions in solid state structures of ten new monomeric and dimeric substituted dibenzyldimethylammonium chloridopalladate salts ; loop_ _publ_author_name 'Manu Lahtinen' 'Anssi Peuronen' 'Jussi Valkonen' # Attachment 'CIFs_revised.cif' data_1a _database_code_depnum_ccdc_archive 'CCDC 692351' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C16 H20 N), Cl4 Pd' _chemical_formula_sum 'C32 H40 Cl4 N2 Pd' _chemical_formula_weight 700.86 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' 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 'P 1 21/n 1' 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 12.116(2) _cell_length_b 9.3247(19) _cell_length_c 13.730(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.52(3) _cell_angle_gamma 90.00 _cell_volume 1548.2(5) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.503 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 720 _exptl_absorpt_coefficient_mu 0.969 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8762 _exptl_absorpt_correction_T_max 0.9093 _exptl_absorpt_process_details 'Denzo (Z. Otwinowski, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 'Kappa APEX II' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9789 _diffrn_reflns_av_R_equivalents 0.0650 _diffrn_reflns_av_sigmaI/netI 0.1066 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 28.82 _reflns_number_total 4031 _reflns_number_gt 2735 _reflns_threshold_expression >2\s(I) _computing_data_collection Collect _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution SHELXS-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 3.0' _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^ > 2\s(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^)+(0.0439P)^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 4031 _refine_ls_number_parameters 180 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0927 _refine_ls_R_factor_gt 0.0556 _refine_ls_wR_factor_ref 0.1200 _refine_ls_wR_factor_gt 0.1072 _refine_ls_goodness_of_fit_ref 0.983 _refine_ls_restrained_S_all 0.983 _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 Pd1 Pd 0.0000 0.0000 0.5000 0.01731(13) Uani 1 2 d S . . Cl1 Cl 0.18392(7) 0.03563(11) 0.47238(7) 0.0223(2) Uani 1 1 d . . . Cl2 Cl -0.04478(8) 0.20226(12) 0.40815(7) 0.0264(3) Uani 1 1 d . . . N1 N 0.2968(2) -0.6180(4) 0.6076(2) 0.0177(7) Uani 1 1 d . . . C11 C 0.3922(3) -0.6964(5) 0.5683(3) 0.0258(10) Uani 1 1 d . . . H11A H 0.4328 -0.6318 0.5271 0.039 Uiso 1 1 calc R . . H11B H 0.3647 -0.7786 0.5296 0.039 Uiso 1 1 calc R . . H11C H 0.4417 -0.7303 0.6227 0.039 Uiso 1 1 calc R . . C12 C 0.3392(3) -0.4904(5) 0.6634(3) 0.0265(9) Uani 1 1 d . . . H12A H 0.3831 -0.5220 0.7218 0.040 Uiso 1 1 calc R . . H12B H 0.2767 -0.4324 0.6827 0.040 Uiso 1 1 calc R . . H12C H 0.3856 -0.4328 0.6223 0.040 Uiso 1 1 calc R . . C21 C 0.2138(3) -0.5744(5) 0.5245(3) 0.0195(9) Uani 1 1 d . . . H21A H 0.1776 -0.6618 0.4968 0.023 Uiso 1 1 calc R . . H21B H 0.1558 -0.5140 0.5514 0.023 Uiso 1 1 calc R . . C22 C 0.2646(3) -0.4938(4) 0.4441(2) 0.0188(8) Uani 1 1 d . . . C23 C 0.2723(3) -0.3466(5) 0.4450(3) 0.0217(9) Uani 1 1 d . . . H23 H 0.2464 -0.2939 0.4982 0.026 Uiso 1 1 calc R . . C24 C 0.3176(3) -0.2748(5) 0.3684(3) 0.0235(9) Uani 1 1 d . . . H24 H 0.3237 -0.1732 0.3702 0.028 Uiso 1 1 calc R . . C25 C 0.3538(3) -0.3493(5) 0.2903(3) 0.0261(10) Uani 1 1 d . . . H25 H 0.3847 -0.2993 0.2382 0.031 Uiso 1 1 calc R . . C26 C 0.3452(3) -0.4974(5) 0.2874(3) 0.0263(9) Uani 1 1 d . . . H26 H 0.3703 -0.5492 0.2334 0.032 Uiso 1 1 calc R . . C27 C 0.2999(3) -0.5693(5) 0.3634(3) 0.0243(9) Uani 1 1 d . . . H27 H 0.2927 -0.6707 0.3609 0.029 Uiso 1 1 calc R . . C31 C 0.2423(3) -0.7217(4) 0.6756(3) 0.0209(9) Uani 1 1 d . . . H31A H 0.2169 -0.8065 0.6370 0.025 Uiso 1 1 calc R . . H31B H 0.2992 -0.7552 0.7252 0.025 Uiso 1 1 calc R . . C32 C 0.1464(3) -0.6654(4) 0.7276(2) 0.0175(8) Uani 1 1 d . . . C33 C 0.1622(3) -0.6147(4) 0.8236(3) 0.0206(9) Uani 1 1 d . . . H33 H 0.2350 -0.6072 0.8529 0.025 Uiso 1 1 calc R . . C34 C 0.0740(3) -0.5758(5) 0.8760(3) 0.0242(9) Uani 1 1 d . . . H34 H 0.0860 -0.5429 0.9413 0.029 Uiso 1 1 calc R . . C35 C -0.0311(3) -0.5846(5) 0.8341(3) 0.0266(10) Uani 1 1 d . . . H35 H -0.0922 -0.5584 0.8704 0.032 Uiso 1 1 calc R . . C36 C -0.0486(3) -0.6312(5) 0.7394(3) 0.0291(10) Uani 1 1 d . . . H36 H -0.1216 -0.6341 0.7101 0.035 Uiso 1 1 calc R . . C37 C 0.0390(3) -0.6736(5) 0.6865(3) 0.0246(10) Uani 1 1 d . . . H37 H 0.0258 -0.7086 0.6218 0.029 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 Pd1 0.0161(2) 0.0226(3) 0.01329(19) -0.00249(19) 0.00155(14) -0.00063(19) Cl1 0.0170(5) 0.0297(6) 0.0205(4) -0.0011(4) 0.0024(3) -0.0017(4) Cl2 0.0228(5) 0.0308(6) 0.0260(5) 0.0053(5) 0.0047(4) 0.0031(5) N1 0.0180(16) 0.0183(19) 0.0171(15) -0.0021(14) 0.0028(12) 0.0001(14) C11 0.022(2) 0.031(3) 0.025(2) -0.001(2) 0.0064(16) 0.0046(19) C12 0.026(2) 0.028(3) 0.026(2) -0.001(2) 0.0025(16) -0.010(2) C21 0.0185(19) 0.023(2) 0.0167(18) 0.0033(17) -0.0019(15) -0.0004(17) C22 0.0193(18) 0.024(2) 0.0131(16) 0.0040(18) -0.0022(14) 0.0018(18) C23 0.024(2) 0.023(2) 0.0180(18) -0.0010(18) 0.0004(16) 0.0036(19) C24 0.023(2) 0.022(2) 0.025(2) 0.0007(19) -0.0023(16) -0.0021(18) C25 0.018(2) 0.036(3) 0.024(2) 0.009(2) 0.0003(16) 0.000(2) C26 0.028(2) 0.034(3) 0.0170(17) 0.004(2) 0.0015(15) 0.006(2) C27 0.029(2) 0.025(3) 0.0177(19) -0.0062(19) -0.0017(16) 0.001(2) C31 0.025(2) 0.022(2) 0.0153(18) 0.0022(17) 0.0008(15) -0.0020(18) C32 0.0210(19) 0.016(2) 0.0155(17) 0.0041(17) 0.0030(14) -0.0017(17) C33 0.021(2) 0.022(2) 0.0185(18) 0.0003(18) -0.0018(15) -0.0011(18) C34 0.033(2) 0.019(2) 0.0210(19) -0.0022(18) 0.0051(17) -0.0019(19) C35 0.023(2) 0.027(3) 0.030(2) 0.006(2) 0.0084(17) 0.0037(19) C36 0.019(2) 0.039(3) 0.029(2) 0.010(2) -0.0012(17) -0.003(2) C37 0.023(2) 0.032(3) 0.0182(18) 0.0047(19) -0.0017(16) -0.0086(19) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 Cl1 2.3072(10) 3_556 ? Pd1 Cl1 2.3072(10) . ? Pd1 Cl2 2.3147(11) . ? Pd1 Cl2 2.3147(11) 3_556 ? N1 C12 1.489(5) . ? N1 C11 1.496(5) . ? N1 C31 1.523(5) . ? N1 C21 1.529(4) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C21 C22 1.498(5) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.376(6) . ? C22 C27 1.402(5) . ? C23 C24 1.388(5) . ? C23 H23 0.9500 . ? C24 C25 1.373(5) . ? C24 H24 0.9500 . ? C25 C26 1.385(6) . ? C25 H25 0.9500 . ? C26 C27 1.382(6) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C31 C32 1.496(5) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C37 1.387(5) . ? C32 C33 1.403(5) . ? C33 C34 1.373(5) . ? C33 H33 0.9500 . ? C34 C35 1.367(5) . ? C34 H34 0.9500 . ? C35 C36 1.375(5) . ? C35 H35 0.9500 . ? C36 C37 1.380(6) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? 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 Cl1 Pd1 Cl1 180.0 3_556 . ? Cl1 Pd1 Cl2 90.60(4) 3_556 . ? Cl1 Pd1 Cl2 89.40(4) . . ? Cl1 Pd1 Cl2 89.40(4) 3_556 3_556 ? Cl1 Pd1 Cl2 90.60(4) . 3_556 ? Cl2 Pd1 Cl2 180.0 . 3_556 ? C12 N1 C11 109.1(3) . . ? C12 N1 C31 109.9(3) . . ? C11 N1 C31 106.5(3) . . ? C12 N1 C21 111.2(3) . . ? C11 N1 C21 110.4(3) . . ? C31 N1 C21 109.6(3) . . ? N1 C11 H11A 109.5 . . ? N1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N1 C12 H12A 109.5 . . ? N1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C22 C21 N1 113.7(3) . . ? C22 C21 H21A 108.8 . . ? N1 C21 H21A 108.8 . . ? C22 C21 H21B 108.8 . . ? N1 C21 H21B 108.8 . . ? H21A C21 H21B 107.7 . . ? C23 C22 C27 118.9(4) . . ? C23 C22 C21 121.6(4) . . ? C27 C22 C21 119.3(4) . . ? C22 C23 C24 120.3(4) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? C25 C24 C23 120.5(4) . . ? C25 C24 H24 119.7 . . ? C23 C24 H24 119.7 . . ? C24 C25 C26 120.0(4) . . ? C24 C25 H25 120.0 . . ? C26 C25 H25 120.0 . . ? C27 C26 C25 119.7(4) . . ? C27 C26 H26 120.2 . . ? C25 C26 H26 120.2 . . ? C26 C27 C22 120.6(4) . . ? C26 C27 H27 119.7 . . ? C22 C27 H27 119.7 . . ? C32 C31 N1 116.6(3) . . ? C32 C31 H31A 108.1 . . ? N1 C31 H31A 108.1 . . ? C32 C31 H31B 108.1 . . ? N1 C31 H31B 108.1 . . ? H31A C31 H31B 107.3 . . ? C37 C32 C33 118.1(3) . . ? C37 C32 C31 121.5(3) . . ? C33 C32 C31 120.1(3) . . ? C34 C33 C32 121.1(3) . . ? C34 C33 H33 119.5 . . ? C32 C33 H33 119.5 . . ? C35 C34 C33 119.8(4) . . ? C35 C34 H34 120.1 . . ? C33 C34 H34 120.1 . . ? C34 C35 C36 120.2(4) . . ? C34 C35 H35 119.9 . . ? C36 C35 H35 119.9 . . ? C35 C36 C37 120.6(4) . . ? C35 C36 H36 119.7 . . ? C37 C36 H36 119.7 . . ? C36 C37 C32 120.1(3) . . ? C36 C37 H37 119.9 . . ? C32 C37 H37 119.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C12 N1 C21 C22 68.6(4) . . . . ? C11 N1 C21 C22 -52.6(4) . . . . ? C31 N1 C21 C22 -169.6(3) . . . . ? N1 C21 C22 C23 -90.6(4) . . . . ? N1 C21 C22 C27 93.0(4) . . . . ? C27 C22 C23 C24 -2.1(6) . . . . ? C21 C22 C23 C24 -178.6(3) . . . . ? C22 C23 C24 C25 1.0(6) . . . . ? C23 C24 C25 C26 0.0(6) . . . . ? C24 C25 C26 C27 0.1(6) . . . . ? C25 C26 C27 C22 -1.2(6) . . . . ? C23 C22 C27 C26 2.2(6) . . . . ? C21 C22 C27 C26 178.8(3) . . . . ? C12 N1 C31 C32 59.5(4) . . . . ? C11 N1 C31 C32 177.6(3) . . . . ? C21 N1 C31 C32 -63.0(4) . . . . ? N1 C31 C32 C37 88.7(4) . . . . ? N1 C31 C32 C33 -97.3(4) . . . . ? C37 C32 C33 C34 0.7(6) . . . . ? C31 C32 C33 C34 -173.5(4) . . . . ? C32 C33 C34 C35 -0.8(6) . . . . ? C33 C34 C35 C36 -0.5(7) . . . . ? C34 C35 C36 C37 1.9(7) . . . . ? C35 C36 C37 C32 -2.1(7) . . . . ? C33 C32 C37 C36 0.7(6) . . . . ? C31 C32 C37 C36 174.8(4) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 28.82 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.545 _refine_diff_density_min -0.595 _refine_diff_density_rms 0.137 data_9 _database_code_depnum_ccdc_archive 'CCDC 692352' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C18 H24 N1), (Cl6 Pd2)' _chemical_formula_sum 'C36 H48 Cl6 N2 Pd2' _chemical_formula_weight 934.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' 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 'P 1 21/n 1' 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 9.4940(19) _cell_length_b 15.260(3) _cell_length_c 13.493(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.13(3) _cell_angle_gamma 90.00 _cell_volume 1930.1(7) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Rectangle _exptl_crystal_colour 'Dark orange' _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.608 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 944 _exptl_absorpt_coefficient_mu 1.375 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6373 _exptl_absorpt_correction_T_max 0.7518 _exptl_absorpt_process_details 'Denzo (Z. Otwinowski, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 'Kappa APEX II' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12262 _diffrn_reflns_av_R_equivalents 0.0358 _diffrn_reflns_av_sigmaI/netI 0.0548 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 28.69 _reflns_number_total 4971 _reflns_number_gt 4115 _reflns_threshold_expression >2\s(I) _computing_data_collection Collect _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution SHELXS-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 3.0' _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^ > 2\s(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^)+(0.0063P)^2^+1.5687P] 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 4971 _refine_ls_number_parameters 212 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0457 _refine_ls_R_factor_gt 0.0341 _refine_ls_wR_factor_ref 0.0728 _refine_ls_wR_factor_gt 0.0686 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.91275(2) 0.411769(12) 0.537873(15) 0.01737(6) Uani 1 1 d . . . Cl1 Cl 0.74509(8) 0.39722(5) 0.63881(5) 0.02996(16) Uani 1 1 d . . . Cl2 Cl 0.91744(7) 0.26463(4) 0.50649(5) 0.02642(15) Uani 1 1 d . . . Cl3 Cl 1.07723(7) 0.43785(4) 0.42996(5) 0.02254(14) Uani 1 1 d . . . N1 N 0.6521(2) 0.71934(14) 0.30882(16) 0.0198(5) Uani 1 1 d . . . C11 C 0.5075(3) 0.74009(17) 0.2515(2) 0.0222(6) Uani 1 1 d . . . H11A H 0.4730 0.7951 0.2763 0.033 Uiso 1 1 calc R . . H11B H 0.4412 0.6927 0.2606 0.033 Uiso 1 1 calc R . . H11C H 0.5139 0.7460 0.1800 0.033 Uiso 1 1 calc R . . C12 C 0.7508(3) 0.79389(18) 0.2971(2) 0.0290(6) Uani 1 1 d . . . H12A H 0.7570 0.8018 0.2258 0.044 Uiso 1 1 calc R . . H12B H 0.8457 0.7810 0.3343 0.044 Uiso 1 1 calc R . . H12C H 0.7140 0.8477 0.3234 0.044 Uiso 1 1 calc R . . C21 C 0.6433(3) 0.70284(17) 0.41938(19) 0.0224(6) Uani 1 1 d . . . H21A H 0.5753 0.6543 0.4235 0.027 Uiso 1 1 calc R . . H21B H 0.7382 0.6831 0.4534 0.027 Uiso 1 1 calc R . . C22 C 0.5981(3) 0.77998(16) 0.47585(19) 0.0194(5) Uani 1 1 d . . . C23 C 0.6999(3) 0.83354(18) 0.5319(2) 0.0246(6) Uani 1 1 d . . . H23 H 0.7983 0.8235 0.5307 0.030 Uiso 1 1 calc R . . C24 C 0.6591(3) 0.90107(18) 0.5892(2) 0.0258(6) Uani 1 1 d . . . H24 H 0.7300 0.9369 0.6269 0.031 Uiso 1 1 calc R . . C25 C 0.5150(3) 0.91767(17) 0.5928(2) 0.0229(6) Uani 1 1 d . . . C26 C 0.4139(3) 0.86362(17) 0.5375(2) 0.0226(6) Uani 1 1 d . . . H26 H 0.3155 0.8739 0.5385 0.027 Uiso 1 1 calc R . . C27 C 0.4545(3) 0.79475(17) 0.4807(2) 0.0208(5) Uani 1 1 d . . . H27 H 0.3838 0.7575 0.4449 0.025 Uiso 1 1 calc R . . C28 C 0.4726(4) 0.99170(18) 0.6561(2) 0.0310(7) Uani 1 1 d . . . H28A H 0.3683 0.9944 0.6491 0.046 Uiso 1 1 calc R . . H28B H 0.5089 1.0472 0.6337 0.046 Uiso 1 1 calc R . . H28C H 0.5129 0.9816 0.7266 0.046 Uiso 1 1 calc R . . C31 C 0.7153(3) 0.63796(17) 0.2653(2) 0.0246(6) Uani 1 1 d . . . H31A H 0.7286 0.6511 0.1956 0.030 Uiso 1 1 calc R . . H31B H 0.8108 0.6266 0.3046 0.030 Uiso 1 1 calc R . . C32 C 0.6277(3) 0.55579(18) 0.2647(2) 0.0227(6) Uani 1 1 d . . . C33 C 0.6357(3) 0.50288(18) 0.3491(2) 0.0260(6) Uani 1 1 d . . . H33 H 0.6988 0.5183 0.4084 0.031 Uiso 1 1 calc R . . C34 C 0.5531(3) 0.42815(18) 0.3483(2) 0.0264(6) Uani 1 1 d . . . H34 H 0.5586 0.3940 0.4076 0.032 Uiso 1 1 calc R . . C35 C 0.4619(3) 0.40202(17) 0.2619(2) 0.0254(6) Uani 1 1 d . . . C36 C 0.4591(3) 0.45289(19) 0.1764(2) 0.0270(6) Uani 1 1 d . . . H36 H 0.4002 0.4354 0.1161 0.032 Uiso 1 1 calc R . . C37 C 0.5402(3) 0.52897(18) 0.1766(2) 0.0256(6) Uani 1 1 d . . . H37 H 0.5361 0.5626 0.1170 0.031 Uiso 1 1 calc R . . C38 C 0.3682(3) 0.3225(2) 0.2631(2) 0.0367(8) Uani 1 1 d . . . H38A H 0.2889 0.3363 0.2989 0.055 Uiso 1 1 calc R . . H38B H 0.4242 0.2742 0.2971 0.055 Uiso 1 1 calc R . . H38C H 0.3304 0.3053 0.1940 0.055 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 Pd1 0.01627(10) 0.01864(11) 0.01743(11) 0.00125(8) 0.00341(7) -0.00177(7) Cl1 0.0315(4) 0.0297(4) 0.0331(4) -0.0051(3) 0.0183(3) -0.0101(3) Cl2 0.0293(4) 0.0207(3) 0.0312(4) -0.0020(3) 0.0110(3) -0.0029(3) Cl3 0.0252(3) 0.0201(3) 0.0242(3) 0.0001(3) 0.0099(3) -0.0019(2) N1 0.0189(11) 0.0186(11) 0.0226(12) -0.0010(9) 0.0054(9) -0.0003(8) C11 0.0220(13) 0.0243(14) 0.0205(13) 0.0012(11) 0.0040(11) 0.0003(11) C12 0.0265(15) 0.0265(15) 0.0354(17) -0.0036(13) 0.0092(13) -0.0089(12) C21 0.0274(14) 0.0206(13) 0.0193(13) 0.0032(11) 0.0038(11) 0.0034(11) C22 0.0248(14) 0.0166(12) 0.0162(13) 0.0019(10) 0.0019(11) -0.0016(10) C23 0.0184(13) 0.0316(15) 0.0233(14) -0.0013(12) 0.0016(11) -0.0006(11) C24 0.0272(15) 0.0255(14) 0.0248(14) -0.0040(12) 0.0046(12) -0.0076(11) C25 0.0313(15) 0.0191(13) 0.0198(13) 0.0018(11) 0.0090(11) -0.0016(11) C26 0.0217(13) 0.0241(14) 0.0230(14) -0.0002(11) 0.0069(11) -0.0010(11) C27 0.0200(13) 0.0200(13) 0.0223(14) -0.0017(11) 0.0032(11) -0.0045(10) C28 0.0430(19) 0.0243(15) 0.0274(16) -0.0039(12) 0.0110(14) 0.0010(13) C31 0.0217(13) 0.0245(14) 0.0288(15) -0.0058(12) 0.0078(12) 0.0014(11) C32 0.0183(13) 0.0219(13) 0.0279(15) -0.0050(12) 0.0037(11) 0.0049(10) C33 0.0265(15) 0.0225(14) 0.0263(15) -0.0044(12) -0.0039(12) 0.0055(11) C34 0.0317(16) 0.0228(14) 0.0245(15) -0.0003(12) 0.0041(12) 0.0029(12) C35 0.0229(14) 0.0200(13) 0.0342(16) -0.0050(12) 0.0071(12) 0.0044(11) C36 0.0232(14) 0.0280(15) 0.0281(15) -0.0066(12) -0.0011(12) 0.0027(11) C37 0.0286(15) 0.0263(15) 0.0221(14) -0.0020(12) 0.0043(12) 0.0035(12) C38 0.0381(18) 0.0321(17) 0.0408(19) -0.0068(14) 0.0084(15) -0.0087(14) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 Cl1 2.2642(9) . ? Pd1 Cl2 2.2867(8) . ? Pd1 Cl3 2.3321(9) . ? Pd1 Cl3 2.3346(8) 3_766 ? Cl3 Pd1 2.3346(8) 3_766 ? N1 C12 1.498(3) . ? N1 C11 1.499(3) . ? N1 C21 1.528(3) . ? N1 C31 1.536(3) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C21 C22 1.502(4) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C27 1.393(4) . ? C22 C23 1.394(4) . ? C23 C24 1.380(4) . ? C23 H23 0.9500 . ? C24 C25 1.399(4) . ? C24 H24 0.9500 . ? C25 C26 1.390(4) . ? C25 C28 1.509(4) . ? C26 C27 1.391(4) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C31 C32 1.504(4) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.389(4) . ? C32 C37 1.398(4) . ? C33 C34 1.383(4) . ? C33 H33 0.9500 . ? C34 C35 1.396(4) . ? C34 H34 0.9500 . ? C35 C36 1.387(4) . ? C35 C38 1.506(4) . ? C36 C37 1.393(4) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? 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 Cl1 Pd1 Cl2 92.94(3) . . ? Cl1 Pd1 Cl3 175.32(3) . . ? Cl2 Pd1 Cl3 90.99(3) . . ? Cl1 Pd1 Cl3 89.79(3) . 3_766 ? Cl2 Pd1 Cl3 176.55(3) . 3_766 ? Cl3 Pd1 Cl3 86.37(3) . 3_766 ? Pd1 Cl3 Pd1 93.63(3) . 3_766 ? C12 N1 C11 108.8(2) . . ? C12 N1 C21 111.1(2) . . ? C11 N1 C21 110.6(2) . . ? C12 N1 C31 106.6(2) . . ? C11 N1 C31 110.8(2) . . ? C21 N1 C31 109.0(2) . . ? N1 C11 H11A 109.5 . . ? N1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N1 C12 H12A 109.5 . . ? N1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C22 C21 N1 115.5(2) . . ? C22 C21 H21A 108.4 . . ? N1 C21 H21A 108.4 . . ? C22 C21 H21B 108.4 . . ? N1 C21 H21B 108.4 . . ? H21A C21 H21B 107.5 . . ? C27 C22 C23 118.6(3) . . ? C27 C22 C21 120.8(2) . . ? C23 C22 C21 120.4(2) . . ? C24 C23 C22 120.7(3) . . ? C24 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? C23 C24 C25 121.2(3) . . ? C23 C24 H24 119.4 . . ? C25 C24 H24 119.4 . . ? C26 C25 C24 118.0(3) . . ? C26 C25 C28 121.6(3) . . ? C24 C25 C28 120.4(3) . . ? C25 C26 C27 121.1(3) . . ? C25 C26 H26 119.5 . . ? C27 C26 H26 119.5 . . ? C26 C27 C22 120.4(2) . . ? C26 C27 H27 119.8 . . ? C22 C27 H27 119.8 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C32 C31 N1 115.3(2) . . ? C32 C31 H31A 108.5 . . ? N1 C31 H31A 108.5 . . ? C32 C31 H31B 108.5 . . ? N1 C31 H31B 108.5 . . ? H31A C31 H31B 107.5 . . ? C33 C32 C37 118.3(3) . . ? C33 C32 C31 121.4(2) . . ? C37 C32 C31 120.2(3) . . ? C34 C33 C32 121.0(3) . . ? C34 C33 H33 119.5 . . ? C32 C33 H33 119.5 . . ? C33 C34 C35 121.2(3) . . ? C33 C34 H34 119.4 . . ? C35 C34 H34 119.4 . . ? C36 C35 C34 117.5(3) . . ? C36 C35 C38 121.8(3) . . ? C34 C35 C38 120.7(3) . . ? C35 C36 C37 121.8(3) . . ? C35 C36 H36 119.1 . . ? C37 C36 H36 119.1 . . ? C36 C37 C32 120.0(3) . . ? C36 C37 H37 120.0 . . ? C32 C37 H37 120.0 . . ? C35 C38 H38A 109.5 . . ? C35 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C35 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? 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 Cl1 Pd1 Cl3 Pd1 35.0(3) . . . 3_766 ? Cl2 Pd1 Cl3 Pd1 -177.78(3) . . . 3_766 ? Cl3 Pd1 Cl3 Pd1 0.0 3_766 . . 3_766 ? C12 N1 C21 C22 56.6(3) . . . . ? C11 N1 C21 C22 -64.2(3) . . . . ? C31 N1 C21 C22 173.8(2) . . . . ? N1 C21 C22 C27 90.3(3) . . . . ? N1 C21 C22 C23 -95.5(3) . . . . ? C27 C22 C23 C24 -1.5(4) . . . . ? C21 C22 C23 C24 -175.8(3) . . . . ? C22 C23 C24 C25 0.1(4) . . . . ? C23 C24 C25 C26 0.5(4) . . . . ? C23 C24 C25 C28 179.8(3) . . . . ? C24 C25 C26 C27 0.3(4) . . . . ? C28 C25 C26 C27 -179.0(3) . . . . ? C25 C26 C27 C22 -1.8(4) . . . . ? C23 C22 C27 C26 2.3(4) . . . . ? C21 C22 C27 C26 176.6(2) . . . . ? C12 N1 C31 C32 -176.9(2) . . . . ? C11 N1 C31 C32 -58.7(3) . . . . ? C21 N1 C31 C32 63.2(3) . . . . ? N1 C31 C32 C33 -83.1(3) . . . . ? N1 C31 C32 C37 99.7(3) . . . . ? C37 C32 C33 C34 -3.7(4) . . . . ? C31 C32 C33 C34 179.0(3) . . . . ? C32 C33 C34 C35 1.7(4) . . . . ? C33 C34 C35 C36 1.2(4) . . . . ? C33 C34 C35 C38 -177.5(3) . . . . ? C34 C35 C36 C37 -2.1(4) . . . . ? C38 C35 C36 C37 176.6(3) . . . . ? C35 C36 C37 C32 0.1(4) . . . . ? C33 C32 C37 C36 2.8(4) . . . . ? C31 C32 C37 C36 -179.9(3) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.69 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.441 _refine_diff_density_min -0.829 _refine_diff_density_rms 0.099 data_8a _database_code_depnum_ccdc_archive 'CCDC 692353' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C18 H24 N1), (Cl6 Pd2)' _chemical_formula_sum 'C36 H48 Cl6 N2 Pd2' _chemical_formula_weight 934.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' 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 triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.5640(19) _cell_length_b 10.679(2) _cell_length_c 11.417(2) _cell_angle_alpha 97.17(3) _cell_angle_beta 107.55(3) _cell_angle_gamma 114.80(3) _cell_volume 965.7(3) _cell_formula_units_Z 1 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Plate _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.606 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 472 _exptl_absorpt_coefficient_mu 1.374 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8748 _exptl_absorpt_correction_T_max 0.9345 _exptl_absorpt_process_details 'Denzo (Z. Otwinowski, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 'Kappa APEX II' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16403 _diffrn_reflns_av_R_equivalents 0.1110 _diffrn_reflns_av_sigmaI/netI 0.1527 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 28.71 _reflns_number_total 4979 _reflns_number_gt 2941 _reflns_threshold_expression >2\s(I) _computing_data_collection Collect _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution SHELXS-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 3.0' _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^ > 2\s(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^)+(0.0190P)^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 4979 _refine_ls_number_parameters 212 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1326 _refine_ls_R_factor_gt 0.0694 _refine_ls_wR_factor_ref 0.1246 _refine_ls_wR_factor_gt 0.1075 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _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 Pd1 Pd 1.04883(5) 0.16310(5) -0.02925(4) 0.02145(15) Uani 1 1 d . . . Cl1 Cl 1.07731(17) 0.24736(19) -0.19858(14) 0.0342(4) Uani 1 1 d . . . Cl2 Cl 1.12449(17) 0.38491(18) 0.08981(15) 0.0341(4) Uani 1 1 d . . . Cl3 Cl 1.02083(16) 0.06755(16) 0.13983(13) 0.0282(4) Uani 1 1 d . . . N1 N 0.5774(5) 0.2910(5) 0.0803(4) 0.0184(10) Uani 1 1 d . . . C11 C 0.7481(6) 0.3040(7) 0.1290(5) 0.0306(16) Uani 1 1 d . . . H11A H 0.7803 0.3028 0.2187 0.046 Uiso 1 1 calc R . . H11B H 0.8290 0.3948 0.1232 0.046 Uiso 1 1 calc R . . H11C H 0.7469 0.2230 0.0770 0.046 Uiso 1 1 calc R . . C12 C 0.4485(6) 0.1469(6) 0.0769(5) 0.0221(13) Uani 1 1 d . . . H12A H 0.4453 0.0704 0.0172 0.033 Uiso 1 1 calc R . . H12B H 0.3383 0.1418 0.0483 0.033 Uiso 1 1 calc R . . H12C H 0.4778 0.1344 0.1630 0.033 Uiso 1 1 calc R . . C21 C 0.5371(7) 0.3125(7) -0.0524(5) 0.0230(13) Uani 1 1 d . . . H21A H 0.4338 0.3213 -0.0766 0.028 Uiso 1 1 calc R . . H21B H 0.6290 0.4049 -0.0478 0.028 Uiso 1 1 calc R . . C22 C 0.5125(6) 0.1947(6) -0.1572(5) 0.0213(13) Uani 1 1 d . . . C23 C 0.6491(7) 0.2006(7) -0.1830(5) 0.0287(15) Uani 1 1 d . . . H23 H 0.7593 0.2770 -0.1328 0.034 Uiso 1 1 calc R . . C24 C 0.6207(7) 0.0937(7) -0.2828(5) 0.0283(15) Uani 1 1 d . . . H24 H 0.7130 0.0963 -0.2999 0.034 Uiso 1 1 calc R . . C25 C 0.4598(7) -0.0181(7) -0.3591(5) 0.0294(15) Uani 1 1 d . . . H25 H 0.4441 -0.0909 -0.4265 0.035 Uiso 1 1 calc R . . C26 C 0.3209(7) -0.0241(7) -0.3371(5) 0.0234(13) Uani 1 1 d . . . C27 C 0.3521(7) 0.0843(6) -0.2349(5) 0.0232(13) Uani 1 1 d . . . H27 H 0.2601 0.0825 -0.2179 0.028 Uiso 1 1 calc R . . C28 C 0.1470(7) -0.1376(7) -0.4217(5) 0.0366(17) Uani 1 1 d . . . H28A H 0.0786 -0.1623 -0.3707 0.055 Uiso 1 1 calc R . . H28B H 0.1489 -0.2236 -0.4610 0.055 Uiso 1 1 calc R . . H28C H 0.0990 -0.1016 -0.4892 0.055 Uiso 1 1 calc R . . C31 C 0.5764(7) 0.4125(6) 0.1662(5) 0.0211(13) Uani 1 1 d . . . H31A H 0.6617 0.5058 0.1659 0.025 Uiso 1 1 calc R . . H31B H 0.4658 0.4075 0.1281 0.025 Uiso 1 1 calc R . . C32 C 0.6097(6) 0.4109(6) 0.3028(5) 0.0224(13) Uani 1 1 d . . . C33 C 0.7730(7) 0.4873(7) 0.3965(5) 0.0272(14) Uani 1 1 d . . . H33 H 0.8644 0.5386 0.3738 0.033 Uiso 1 1 calc R . . C34 C 0.8001(7) 0.4874(7) 0.5215(6) 0.0367(17) Uani 1 1 d . . . H34 H 0.9106 0.5414 0.5858 0.044 Uiso 1 1 calc R . . C35 C 0.6689(8) 0.4101(7) 0.5549(5) 0.0330(16) Uani 1 1 d . . . H35 H 0.6909 0.4077 0.6413 0.040 Uiso 1 1 calc R . . C36 C 0.5057(7) 0.3358(7) 0.4647(5) 0.0265(14) Uani 1 1 d . . . C37 C 0.4779(7) 0.3367(6) 0.3380(5) 0.0205(13) Uani 1 1 d . . . H37 H 0.3668 0.2856 0.2745 0.025 Uiso 1 1 calc R . . C38 C 0.3603(8) 0.2530(7) 0.4998(6) 0.0354(17) Uani 1 1 d . . . H38A H 0.2742 0.2815 0.4678 0.053 Uiso 1 1 calc R . . H38B H 0.3991 0.2741 0.5933 0.053 Uiso 1 1 calc R . . H38C H 0.3131 0.1495 0.4610 0.053 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 Pd1 0.0149(2) 0.0196(3) 0.0267(3) 0.0078(2) 0.00859(17) 0.00506(19) Cl1 0.0274(8) 0.0386(12) 0.0387(9) 0.0240(8) 0.0151(7) 0.0128(8) Cl2 0.0282(8) 0.0212(10) 0.0527(10) 0.0079(8) 0.0194(7) 0.0101(7) Cl3 0.0320(8) 0.0169(10) 0.0251(8) 0.0031(7) 0.0126(6) 0.0025(7) N1 0.020(2) 0.017(3) 0.021(2) 0.009(2) 0.0095(19) 0.010(2) C11 0.019(3) 0.035(4) 0.037(4) 0.007(3) 0.010(3) 0.015(3) C12 0.025(3) 0.011(3) 0.028(3) 0.005(3) 0.010(2) 0.007(3) C21 0.025(3) 0.022(4) 0.025(3) 0.012(3) 0.011(2) 0.011(3) C22 0.019(3) 0.026(4) 0.025(3) 0.013(3) 0.013(2) 0.013(3) C23 0.020(3) 0.030(4) 0.032(3) 0.014(3) 0.013(3) 0.005(3) C24 0.034(3) 0.038(5) 0.031(3) 0.018(3) 0.021(3) 0.025(3) C25 0.039(4) 0.027(4) 0.024(3) 0.008(3) 0.013(3) 0.017(3) C26 0.028(3) 0.027(4) 0.017(3) 0.011(3) 0.008(2) 0.014(3) C27 0.028(3) 0.022(4) 0.028(3) 0.016(3) 0.013(3) 0.015(3) C28 0.033(3) 0.038(5) 0.030(4) 0.003(3) 0.009(3) 0.013(3) C31 0.026(3) 0.012(3) 0.025(3) 0.008(3) 0.010(2) 0.008(3) C32 0.024(3) 0.016(4) 0.029(3) 0.004(3) 0.007(3) 0.014(3) C33 0.024(3) 0.022(4) 0.023(3) -0.003(3) 0.004(2) 0.007(3) C34 0.032(3) 0.035(5) 0.030(4) -0.006(3) -0.002(3) 0.019(3) C35 0.048(4) 0.039(5) 0.018(3) 0.006(3) 0.009(3) 0.029(4) C36 0.044(4) 0.020(4) 0.027(3) 0.012(3) 0.018(3) 0.020(3) C37 0.029(3) 0.018(4) 0.021(3) 0.007(3) 0.011(2) 0.015(3) C38 0.054(4) 0.041(5) 0.031(4) 0.019(3) 0.025(3) 0.031(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 Cl2 2.2687(19) . ? Pd1 Cl1 2.2733(17) . ? Pd1 Cl3 2.3267(16) . ? Pd1 Cl3 2.3333(18) 2_755 ? Cl3 Pd1 2.3333(18) 2_755 ? N1 C11 1.495(6) . ? N1 C12 1.501(7) . ? N1 C21 1.518(6) . ? N1 C31 1.531(6) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C21 C22 1.509(7) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C27 1.390(7) . ? C22 C23 1.402(7) . ? C23 C24 1.379(8) . ? C23 H23 0.9500 . ? C24 C25 1.394(8) . ? C24 H24 0.9500 . ? C25 C26 1.402(7) . ? C25 H25 0.9500 . ? C26 C27 1.398(7) . ? C26 C28 1.489(8) . ? C27 H27 0.9500 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C31 C32 1.498(7) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C37 1.388(7) . ? C32 C33 1.398(7) . ? C33 C34 1.370(8) . ? C33 H33 0.9500 . ? C34 C35 1.379(8) . ? C34 H34 0.9500 . ? C35 C36 1.384(8) . ? C35 H35 0.9500 . ? C36 C37 1.392(7) . ? C36 C38 1.506(8) . ? C37 H37 0.9500 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? 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 Cl2 Pd1 Cl1 91.26(7) . . ? Cl2 Pd1 Cl3 91.31(6) . . ? Cl1 Pd1 Cl3 177.26(6) . . ? Cl2 Pd1 Cl3 176.40(6) . 2_755 ? Cl1 Pd1 Cl3 91.75(6) . 2_755 ? Cl3 Pd1 Cl3 85.65(6) . 2_755 ? Pd1 Cl3 Pd1 94.35(6) . 2_755 ? C11 N1 C12 110.6(4) . . ? C11 N1 C21 109.4(4) . . ? C12 N1 C21 110.7(4) . . ? C11 N1 C31 109.6(4) . . ? C12 N1 C31 110.3(4) . . ? C21 N1 C31 106.1(4) . . ? N1 C11 H11A 109.5 . . ? N1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N1 C12 H12A 109.5 . . ? N1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C22 C21 N1 115.4(5) . . ? C22 C21 H21A 108.4 . . ? N1 C21 H21A 108.4 . . ? C22 C21 H21B 108.4 . . ? N1 C21 H21B 108.4 . . ? H21A C21 H21B 107.5 . . ? C27 C22 C23 119.3(5) . . ? C27 C22 C21 120.0(4) . . ? C23 C22 C21 120.6(5) . . ? C24 C23 C22 118.9(5) . . ? C24 C23 H23 120.6 . . ? C22 C23 H23 120.6 . . ? C23 C24 C25 121.5(5) . . ? C23 C24 H24 119.2 . . ? C25 C24 H24 119.2 . . ? C24 C25 C26 120.6(5) . . ? C24 C25 H25 119.7 . . ? C26 C25 H25 119.7 . . ? C27 C26 C25 117.1(5) . . ? C27 C26 C28 121.2(5) . . ? C25 C26 C28 121.6(5) . . ? C22 C27 C26 122.5(5) . . ? C22 C27 H27 118.7 . . ? C26 C27 H27 118.7 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C32 C31 N1 115.6(4) . . ? C32 C31 H31A 108.4 . . ? N1 C31 H31A 108.4 . . ? C32 C31 H31B 108.4 . . ? N1 C31 H31B 108.4 . . ? H31A C31 H31B 107.4 . . ? C37 C32 C33 119.4(5) . . ? C37 C32 C31 120.1(5) . . ? C33 C32 C31 120.5(5) . . ? C34 C33 C32 119.5(6) . . ? C34 C33 H33 120.3 . . ? C32 C33 H33 120.3 . . ? C33 C34 C35 120.7(5) . . ? C33 C34 H34 119.6 . . ? C35 C34 H34 119.6 . . ? C34 C35 C36 121.0(5) . . ? C34 C35 H35 119.5 . . ? C36 C35 H35 119.5 . . ? C35 C36 C37 118.2(5) . . ? C35 C36 C38 121.9(5) . . ? C37 C36 C38 119.9(5) . . ? C32 C37 C36 121.1(5) . . ? C32 C37 H37 119.4 . . ? C36 C37 H37 119.4 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? 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 Cl2 Pd1 Cl3 Pd1 -178.07(5) . . . 2_755 ? Cl1 Pd1 Cl3 Pd1 -18.3(12) . . . 2_755 ? Cl3 Pd1 Cl3 Pd1 0.0 2_755 . . 2_755 ? C11 N1 C21 C22 68.3(6) . . . . ? C12 N1 C21 C22 -53.8(5) . . . . ? C31 N1 C21 C22 -173.5(4) . . . . ? N1 C21 C22 C27 95.9(6) . . . . ? N1 C21 C22 C23 -88.6(6) . . . . ? C27 C22 C23 C24 -2.0(8) . . . . ? C21 C22 C23 C24 -177.6(5) . . . . ? C22 C23 C24 C25 1.0(9) . . . . ? C23 C24 C25 C26 0.7(9) . . . . ? C24 C25 C26 C27 -1.3(8) . . . . ? C24 C25 C26 C28 176.5(6) . . . . ? C23 C22 C27 C26 1.5(9) . . . . ? C21 C22 C27 C26 177.0(5) . . . . ? C25 C26 C27 C22 0.2(8) . . . . ? C28 C26 C27 C22 -177.6(6) . . . . ? C11 N1 C31 C32 -63.3(6) . . . . ? C12 N1 C31 C32 58.7(6) . . . . ? C21 N1 C31 C32 178.7(4) . . . . ? N1 C31 C32 C37 -90.2(6) . . . . ? N1 C31 C32 C33 91.6(6) . . . . ? C37 C32 C33 C34 0.1(9) . . . . ? C31 C32 C33 C34 178.3(6) . . . . ? C32 C33 C34 C35 1.7(9) . . . . ? C33 C34 C35 C36 -3.1(10) . . . . ? C34 C35 C36 C37 2.5(9) . . . . ? C34 C35 C36 C38 -178.9(5) . . . . ? C33 C32 C37 C36 -0.7(8) . . . . ? C31 C32 C37 C36 -178.9(5) . . . . ? C35 C36 C37 C32 -0.6(8) . . . . ? C38 C36 C37 C32 -179.3(5) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.71 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.733 _refine_diff_density_min -0.715 _refine_diff_density_rms 0.172 data_7 _database_code_depnum_ccdc_archive 'CCDC 692354' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C18 H24 N), Cl6 Pd2' _chemical_formula_sum 'C36 H48 Cl6 N2 Pd2' _chemical_formula_weight 934.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' 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 triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.332(2) _cell_length_b 10.381(2) _cell_length_c 11.125(2) _cell_angle_alpha 107.93(3) _cell_angle_beta 105.75(3) _cell_angle_gamma 109.92(3) _cell_volume 968.3(3) _cell_formula_units_Z 1 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Plate _exptl_crystal_colour Orange _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.602 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 472 _exptl_absorpt_coefficient_mu 1.371 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7002 _exptl_absorpt_correction_T_max 0.8983 _exptl_absorpt_process_details 'Denzo (Z. Otwinowski, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 'Kappa APEX II' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14631 _diffrn_reflns_av_R_equivalents 0.0409 _diffrn_reflns_av_sigmaI/netI 0.0563 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 28.72 _reflns_number_total 4975 _reflns_number_gt 4040 _reflns_threshold_expression >2\s(I) _computing_data_collection Collect _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution SHELXS-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 3.0' _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^ > 2\s(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^)+(0.0122P)^2^+0.6422P] 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 4975 _refine_ls_number_parameters 212 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0514 _refine_ls_R_factor_gt 0.0378 _refine_ls_wR_factor_ref 0.0737 _refine_ls_wR_factor_gt 0.0695 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.39412(2) 0.94042(2) 0.82873(2) 0.02389(7) Uani 1 1 d . . . Cl1 Cl 0.40821(8) 1.04738(8) 0.67937(8) 0.03131(17) Uani 1 1 d . . . Cl2 Cl 0.18977(8) 0.71868(8) 0.65857(8) 0.03579(18) Uani 1 1 d . . . Cl3 Cl 0.60345(8) 1.16089(8) 1.01149(8) 0.03599(19) Uani 1 1 d . . . N1 N 0.8007(2) 0.3749(2) 0.7284(2) 0.0198(5) Uani 1 1 d . . . C11 C 0.9492(3) 0.4872(3) 0.7456(3) 0.0259(6) Uani 1 1 d . . . H11A H 0.9590 0.5904 0.7836 0.039 Uiso 1 1 calc R . . H11B H 0.9538 0.4621 0.6549 0.039 Uiso 1 1 calc R . . H11C H 1.0323 0.4828 0.8096 0.039 Uiso 1 1 calc R . . C12 C 0.7881(3) 0.4196(3) 0.8638(3) 0.0237(6) Uani 1 1 d . . . H12A H 0.8738 0.4258 0.9346 0.036 Uiso 1 1 calc R . . H12B H 0.6929 0.3430 0.8532 0.036 Uiso 1 1 calc R . . H12C H 0.7892 0.5193 0.8926 0.036 Uiso 1 1 calc R . . C21 C 0.6698(3) 0.3684(3) 0.6175(3) 0.0236(6) Uani 1 1 d . . . H21A H 0.6786 0.3347 0.5280 0.028 Uiso 1 1 calc R . . H21B H 0.5731 0.2902 0.6053 0.028 Uiso 1 1 calc R . . C22 C 0.6622(3) 0.5176(3) 0.6494(3) 0.0237(6) Uani 1 1 d . . . C23 C 0.7482(3) 0.6208(3) 0.6110(3) 0.0307(7) Uani 1 1 d . . . H23 H 0.8103 0.5962 0.5686 0.037 Uiso 1 1 calc R . . C24 C 0.7445(4) 0.7581(4) 0.6338(4) 0.0393(8) Uani 1 1 d . . . H24 H 0.8063 0.8286 0.6103 0.047 Uiso 1 1 calc R . . C25 C 0.6504(3) 0.7913(4) 0.6906(3) 0.0387(8) Uani 1 1 d . . . H25 H 0.6455 0.8843 0.7048 0.046 Uiso 1 1 calc R . . C26 C 0.5637(3) 0.6903(3) 0.7267(3) 0.0351(7) Uani 1 1 d . . . H26 H 0.4987 0.7144 0.7652 0.042 Uiso 1 1 calc R . . C27 C 0.5682(3) 0.5531(3) 0.7087(3) 0.0279(6) Uani 1 1 d . . . C28 C 0.4687(3) 0.4508(4) 0.7525(4) 0.0410(8) Uani 1 1 d . . . H28A H 0.4369 0.3439 0.6928 0.061 Uiso 1 1 calc R . . H28B H 0.3789 0.4666 0.7436 0.061 Uiso 1 1 calc R . . H28C H 0.5254 0.4754 0.8496 0.061 Uiso 1 1 calc R . . C31 C 0.7866(3) 0.2131(3) 0.6752(3) 0.0232(6) Uani 1 1 d . . . H31A H 0.6894 0.1417 0.6683 0.028 Uiso 1 1 calc R . . H31B H 0.7826 0.1817 0.5801 0.028 Uiso 1 1 calc R . . C32 C 0.9141(3) 0.1975(3) 0.7650(3) 0.0242(6) Uani 1 1 d . . . C33 C 0.9082(3) 0.1762(3) 0.8817(3) 0.0308(7) Uani 1 1 d . . . H33 H 0.8259 0.1750 0.9048 0.037 Uiso 1 1 calc R . . C34 C 1.0198(4) 0.1567(3) 0.9646(3) 0.0410(8) Uani 1 1 d . . . H34 H 1.0155 0.1449 1.0450 0.049 Uiso 1 1 calc R . . C35 C 1.1373(4) 0.1545(4) 0.9290(4) 0.0446(9) Uani 1 1 d . . . H35 H 1.2149 0.1420 0.9856 0.053 Uiso 1 1 calc R . . C36 C 1.1422(3) 0.1702(4) 0.8125(4) 0.0399(8) Uani 1 1 d . . . H36 H 1.2230 0.1667 0.7888 0.048 Uiso 1 1 calc R . . C37 C 1.0326(3) 0.1912(3) 0.7277(3) 0.0306(7) Uani 1 1 d . . . C38 C 1.0430(4) 0.2020(4) 0.5983(4) 0.0402(8) Uani 1 1 d . . . H38A H 1.0757 0.3079 0.6123 0.060 Uiso 1 1 calc R . . H38B H 0.9432 0.1359 0.5193 0.060 Uiso 1 1 calc R . . H38C H 1.1167 0.1693 0.5793 0.060 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 Pd1 0.02572(12) 0.02248(11) 0.02332(12) 0.00959(9) 0.01476(9) 0.00805(9) Cl1 0.0323(4) 0.0288(4) 0.0292(4) 0.0155(3) 0.0129(3) 0.0080(3) Cl2 0.0300(4) 0.0307(4) 0.0314(4) 0.0130(3) 0.0101(3) 0.0008(3) Cl3 0.0447(4) 0.0259(4) 0.0235(4) 0.0102(3) 0.0148(3) 0.0020(3) N1 0.0167(10) 0.0188(11) 0.0188(12) 0.0067(9) 0.0052(9) 0.0062(8) C11 0.0218(13) 0.0219(13) 0.0305(17) 0.0115(12) 0.0108(12) 0.0067(11) C12 0.0269(14) 0.0229(13) 0.0192(14) 0.0088(12) 0.0093(12) 0.0101(11) C21 0.0192(13) 0.0238(14) 0.0213(15) 0.0087(12) 0.0032(11) 0.0082(11) C22 0.0212(13) 0.0222(13) 0.0223(15) 0.0090(12) 0.0038(11) 0.0096(11) C23 0.0297(15) 0.0326(16) 0.0289(17) 0.0155(14) 0.0099(13) 0.0136(13) C24 0.0422(18) 0.0295(16) 0.041(2) 0.0200(15) 0.0122(16) 0.0116(14) C25 0.0401(18) 0.0275(16) 0.0347(19) 0.0091(14) 0.0025(15) 0.0156(14) C26 0.0335(16) 0.0355(17) 0.0332(18) 0.0121(15) 0.0072(14) 0.0207(14) C27 0.0233(14) 0.0291(15) 0.0268(16) 0.0114(13) 0.0053(12) 0.0123(12) C28 0.0329(17) 0.048(2) 0.056(2) 0.0289(18) 0.0233(16) 0.0244(15) C31 0.0216(13) 0.0174(13) 0.0242(15) 0.0058(11) 0.0064(11) 0.0079(10) C32 0.0234(14) 0.0170(13) 0.0265(16) 0.0066(12) 0.0091(12) 0.0073(11) C33 0.0423(17) 0.0186(14) 0.0328(18) 0.0121(13) 0.0171(14) 0.0138(12) C34 0.066(2) 0.0237(16) 0.0300(19) 0.0126(14) 0.0151(17) 0.0207(15) C35 0.0439(19) 0.0297(17) 0.045(2) 0.0131(16) -0.0011(16) 0.0193(15) C36 0.0305(16) 0.0362(18) 0.053(2) 0.0192(17) 0.0126(16) 0.0192(14) C37 0.0274(15) 0.0282(15) 0.0371(19) 0.0145(14) 0.0133(14) 0.0141(12) C38 0.0405(18) 0.053(2) 0.045(2) 0.0250(18) 0.0280(17) 0.0299(16) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 Cl1 2.2743(9) . ? Pd1 Cl2 2.2750(18) . ? Pd1 Cl3 2.3261(9) 2_677 ? Pd1 Cl3 2.3291(19) . ? Cl3 Pd1 2.3261(9) 2_677 ? N1 C12 1.490(3) . ? N1 C11 1.495(3) . ? N1 C21 1.529(3) . ? N1 C31 1.538(3) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C21 C22 1.513(4) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C27 1.399(4) . ? C22 C23 1.399(4) . ? C23 C24 1.385(4) . ? C23 H23 0.9500 . ? C24 C25 1.375(4) . ? C24 H24 0.9500 . ? C25 C26 1.371(4) . ? C25 H25 0.9500 . ? C26 C27 1.395(4) . ? C26 H26 0.9500 . ? C27 C28 1.506(4) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C31 C32 1.513(4) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.396(4) . ? C32 C37 1.411(4) . ? C33 C34 1.384(4) . ? C33 H33 0.9500 . ? C34 C35 1.381(5) . ? C34 H34 0.9500 . ? C35 C36 1.367(5) . ? C35 H35 0.9500 . ? C36 C37 1.391(4) . ? C36 H36 0.9500 . ? C37 C38 1.506(4) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? 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 Cl1 Pd1 Cl2 92.36(4) . . ? Cl1 Pd1 Cl3 176.34(3) . 2_677 ? Cl2 Pd1 Cl3 90.60(4) . 2_677 ? Cl1 Pd1 Cl3 90.89(4) . . ? Cl2 Pd1 Cl3 176.74(3) . . ? Cl3 Pd1 Cl3 86.14(4) 2_677 . ? Pd1 Cl3 Pd1 93.86(4) 2_677 . ? C12 N1 C11 109.7(2) . . ? C12 N1 C21 110.1(2) . . ? C11 N1 C21 110.1(2) . . ? C12 N1 C31 110.5(2) . . ? C11 N1 C31 110.20(19) . . ? C21 N1 C31 106.14(19) . . ? N1 C11 H11A 109.5 . . ? N1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N1 C12 H12A 109.5 . . ? N1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C22 C21 N1 115.0(2) . . ? C22 C21 H21A 108.5 . . ? N1 C21 H21A 108.5 . . ? C22 C21 H21B 108.5 . . ? N1 C21 H21B 108.5 . . ? H21A C21 H21B 107.5 . . ? C27 C22 C23 119.0(3) . . ? C27 C22 C21 123.0(2) . . ? C23 C22 C21 117.9(2) . . ? C24 C23 C22 121.3(3) . . ? C24 C23 H23 119.4 . . ? C22 C23 H23 119.4 . . ? C25 C24 C23 119.4(3) . . ? C25 C24 H24 120.3 . . ? C23 C24 H24 120.3 . . ? C26 C25 C24 120.0(3) . . ? C26 C25 H25 120.0 . . ? C24 C25 H25 120.0 . . ? C25 C26 C27 122.0(3) . . ? C25 C26 H26 119.0 . . ? C27 C26 H26 119.0 . . ? C26 C27 C22 118.4(3) . . ? C26 C27 C28 117.5(3) . . ? C22 C27 C28 124.1(3) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C32 C31 N1 114.7(2) . . ? C32 C31 H31A 108.6 . . ? N1 C31 H31A 108.6 . . ? C32 C31 H31B 108.6 . . ? N1 C31 H31B 108.6 . . ? H31A C31 H31B 107.6 . . ? C33 C32 C37 118.8(3) . . ? C33 C32 C31 119.3(2) . . ? C37 C32 C31 121.6(3) . . ? C34 C33 C32 121.4(3) . . ? C34 C33 H33 119.3 . . ? C32 C33 H33 119.3 . . ? C35 C34 C33 119.3(3) . . ? C35 C34 H34 120.4 . . ? C33 C34 H34 120.4 . . ? C36 C35 C34 120.1(3) . . ? C36 C35 H35 120.0 . . ? C34 C35 H35 120.0 . . ? C35 C36 C37 122.1(3) . . ? C35 C36 H36 118.9 . . ? C37 C36 H36 118.9 . . ? C36 C37 C32 118.3(3) . . ? C36 C37 C38 118.9(3) . . ? C32 C37 C38 122.9(3) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? 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 Cl1 Pd1 Cl3 Pd1 -177.86(3) . . . 2_677 ? Cl2 Pd1 Cl3 Pd1 -2.8(5) . . . 2_677 ? Cl3 Pd1 Cl3 Pd1 0.0 2_677 . . 2_677 ? C12 N1 C21 C22 60.4(3) . . . . ? C11 N1 C21 C22 -60.7(3) . . . . ? C31 N1 C21 C22 -180.0(2) . . . . ? N1 C21 C22 C27 -97.1(3) . . . . ? N1 C21 C22 C23 86.1(3) . . . . ? C27 C22 C23 C24 1.5(4) . . . . ? C21 C22 C23 C24 178.5(3) . . . . ? C22 C23 C24 C25 -2.3(5) . . . . ? C23 C24 C25 C26 1.3(5) . . . . ? C24 C25 C26 C27 0.5(5) . . . . ? C25 C26 C27 C22 -1.3(5) . . . . ? C25 C26 C27 C28 179.8(3) . . . . ? C23 C22 C27 C26 0.3(4) . . . . ? C21 C22 C27 C26 -176.5(3) . . . . ? C23 C22 C27 C28 179.1(3) . . . . ? C21 C22 C27 C28 2.3(4) . . . . ? C12 N1 C31 C32 -65.3(3) . . . . ? C11 N1 C31 C32 56.1(3) . . . . ? C21 N1 C31 C32 175.3(2) . . . . ? N1 C31 C32 C33 83.2(3) . . . . ? N1 C31 C32 C37 -102.1(3) . . . . ? C37 C32 C33 C34 3.2(4) . . . . ? C31 C32 C33 C34 178.0(3) . . . . ? C32 C33 C34 C35 -1.6(4) . . . . ? C33 C34 C35 C36 -0.5(5) . . . . ? C34 C35 C36 C37 1.1(5) . . . . ? C35 C36 C37 C32 0.5(5) . . . . ? C35 C36 C37 C38 -177.8(3) . . . . ? C33 C32 C37 C36 -2.6(4) . . . . ? C31 C32 C37 C36 -177.3(3) . . . . ? C33 C32 C37 C38 175.7(3) . . . . ? C31 C32 C37 C38 1.0(4) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.72 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.410 _refine_diff_density_min -0.592 _refine_diff_density_rms 0.096 data_5 _database_code_depnum_ccdc_archive 'CCDC 692355' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C18 H24 N), Cl4 Pd' _chemical_formula_sum 'C36 H48 Cl4 N2 Pd' _chemical_formula_weight 756.96 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' 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 triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.5340(17) _cell_length_b 10.496(2) _cell_length_c 10.809(2) _cell_angle_alpha 67.60(3) _cell_angle_beta 75.21(3) _cell_angle_gamma 79.37(3) _cell_volume 861.4(3) _cell_formula_units_Z 1 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour 'Dark Orange' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.459 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 392 _exptl_absorpt_coefficient_mu 0.877 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7788 _exptl_absorpt_correction_T_max 0.8441 _exptl_absorpt_process_details 'Denzo (Z. Otwinowski, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Kappa APEX II' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14759 _diffrn_reflns_av_R_equivalents 0.0412 _diffrn_reflns_av_sigmaI/netI 0.0497 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 28.81 _reflns_number_total 4477 _reflns_number_gt 4038 _reflns_threshold_expression >2\s(I) _computing_data_collection Collect _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution SHELXS-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 3.0' _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^)+(0.0218P)^2^+0.5530P] 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 4477 _refine_ls_number_parameters 198 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0389 _refine_ls_R_factor_gt 0.0340 _refine_ls_wR_factor_ref 0.0749 _refine_ls_wR_factor_gt 0.0730 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _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 Pd1 Pd 1.0000 0.0000 1.0000 0.01569(7) Uani 1 2 d S . . Cl2 Cl 1.15540(7) 0.11569(6) 1.05919(6) 0.02972(13) Uani 1 1 d . . . Cl1 Cl 1.10838(6) 0.11108(6) 0.77346(5) 0.02432(12) Uani 1 1 d . . . N1 N 0.5684(2) 0.30834(17) 0.79011(18) 0.0174(3) Uani 1 1 d . . . C35 C 0.9158(3) 0.6909(2) 0.7228(3) 0.0267(5) Uani 1 1 d . . . H35 H 0.9491 0.7749 0.7168 0.032 Uiso 1 1 calc R . . C21 C 0.5016(3) 0.3076(2) 0.9336(2) 0.0219(4) Uani 1 1 d . . . H21A H 0.3824 0.3027 0.9542 0.026 Uiso 1 1 calc R . . H21B H 0.5194 0.3968 0.9367 0.026 Uiso 1 1 calc R . . C43 C 0.4776(3) 0.2069(2) 0.5534(2) 0.0213(4) Uani 1 1 d . . . H43 H 0.3733 0.2511 0.5787 0.026 Uiso 1 1 calc R . . C32 C 0.8093(2) 0.4468(2) 0.7431(2) 0.0206(4) Uani 1 1 d . . . C11 C 0.4867(2) 0.4336(2) 0.6929(2) 0.0209(4) Uani 1 1 d . . . H11A H 0.5237 0.4295 0.5998 0.025 Uiso 1 1 calc R . . H11B H 0.5249 0.5178 0.6913 0.025 Uiso 1 1 calc R . . C47 C 0.7356(3) 0.0927(2) 0.6048(2) 0.0222(4) Uani 1 1 d . . . H47 H 0.8095 0.0587 0.6653 0.027 Uiso 1 1 calc R . . C42 C 0.5852(2) 0.1610(2) 0.6426(2) 0.0196(4) Uani 1 1 d . . . C44 C 0.5210(3) 0.1890(2) 0.4283(2) 0.0242(5) Uani 1 1 d . . . H44 H 0.4473 0.2222 0.3677 0.029 Uiso 1 1 calc R . . C31 C 0.7530(2) 0.3163(2) 0.7490(2) 0.0209(4) Uani 1 1 d . . . H31A H 0.8053 0.2362 0.8149 0.025 Uiso 1 1 calc R . . H31B H 0.7918 0.3072 0.6580 0.025 Uiso 1 1 calc R . . C45 C 0.6716(3) 0.1226(2) 0.3915(2) 0.0244(5) Uani 1 1 d . . . H45 H 0.7018 0.1104 0.3056 0.029 Uiso 1 1 calc R . . C36 C 0.8858(3) 0.5848(2) 0.8475(3) 0.0272(5) Uani 1 1 d . . . H36 H 0.9004 0.5956 0.9270 0.033 Uiso 1 1 calc R . . C37 C 0.8348(3) 0.4629(2) 0.8577(2) 0.0253(5) Uani 1 1 d . . . H37 H 0.8172 0.3898 0.9437 0.030 Uiso 1 1 calc R . . C41 C 0.5347(3) 0.1729(2) 0.7820(2) 0.0196(4) Uani 1 1 d . . . H41A H 0.5920 0.0944 0.8455 0.023 Uiso 1 1 calc R . . H41B H 0.4166 0.1633 0.8146 0.023 Uiso 1 1 calc R . . C46 C 0.7779(3) 0.0742(2) 0.4809(2) 0.0251(5) Uani 1 1 d . . . H46 H 0.8809 0.0277 0.4563 0.030 Uiso 1 1 calc R . . C22 C 0.5726(3) 0.1917(2) 1.0450(2) 0.0292(5) Uani 1 1 d . . . H22A H 0.5547 0.1024 1.0444 0.044 Uiso 1 1 calc R . . H22B H 0.5194 0.1998 1.1339 0.044 Uiso 1 1 calc R . . H22C H 0.6897 0.1979 1.0291 0.044 Uiso 1 1 calc R . . C34 C 0.8971(3) 0.6741(2) 0.6075(3) 0.0270(5) Uani 1 1 d . . . H34 H 0.9205 0.7457 0.5210 0.032 Uiso 1 1 calc R . . C33 C 0.8441(2) 0.5528(2) 0.6172(2) 0.0219(4) Uani 1 1 d . . . H33 H 0.8313 0.5419 0.5371 0.026 Uiso 1 1 calc R . . C12 C 0.3018(3) 0.4490(2) 0.7254(3) 0.0282(5) Uani 1 1 d . . . H12A H 0.2617 0.3616 0.7399 0.042 Uiso 1 1 calc R . . H12B H 0.2615 0.5228 0.6490 0.042 Uiso 1 1 calc R . . H12C H 0.2627 0.4724 0.8084 0.042 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 Pd1 0.01518(11) 0.01676(12) 0.01547(12) -0.00669(8) -0.00246(8) -0.00104(8) Cl2 0.0354(3) 0.0338(3) 0.0260(3) -0.0115(2) -0.0070(2) -0.0146(2) Cl1 0.0221(3) 0.0299(3) 0.0174(3) -0.0062(2) -0.0008(2) -0.0033(2) N1 0.0172(8) 0.0182(8) 0.0169(9) -0.0066(7) -0.0023(7) -0.0026(6) C35 0.0246(11) 0.0232(11) 0.0343(13) -0.0132(10) -0.0020(9) -0.0059(9) C21 0.0236(10) 0.0253(11) 0.0185(11) -0.0113(9) -0.0003(8) -0.0040(8) C43 0.0198(10) 0.0200(10) 0.0233(11) -0.0071(9) -0.0024(8) -0.0036(8) C32 0.0163(9) 0.0208(10) 0.0250(11) -0.0102(9) -0.0021(8) -0.0010(8) C11 0.0214(10) 0.0175(10) 0.0218(11) -0.0050(8) -0.0054(8) -0.0003(8) C47 0.0237(10) 0.0194(10) 0.0245(12) -0.0077(9) -0.0075(9) -0.0005(8) C42 0.0225(10) 0.0159(10) 0.0195(11) -0.0054(8) -0.0026(8) -0.0042(8) C44 0.0263(11) 0.0241(11) 0.0240(12) -0.0085(9) -0.0073(9) -0.0034(8) C31 0.0175(9) 0.0195(10) 0.0251(11) -0.0085(9) -0.0029(8) -0.0011(8) C45 0.0302(11) 0.0231(11) 0.0206(11) -0.0101(9) -0.0026(9) -0.0027(9) C36 0.0250(11) 0.0345(13) 0.0280(13) -0.0162(10) -0.0061(9) -0.0045(9) C37 0.0247(11) 0.0262(12) 0.0239(12) -0.0056(9) -0.0058(9) -0.0057(9) C41 0.0230(10) 0.0165(10) 0.0187(10) -0.0053(8) -0.0023(8) -0.0052(8) C46 0.0232(11) 0.0243(11) 0.0288(12) -0.0129(10) -0.0031(9) 0.0002(8) C22 0.0391(13) 0.0288(12) 0.0189(11) -0.0052(9) -0.0071(10) -0.0069(10) C34 0.0258(11) 0.0230(11) 0.0281(12) -0.0050(9) -0.0029(9) -0.0052(9) C33 0.0189(10) 0.0249(11) 0.0227(11) -0.0091(9) -0.0046(8) -0.0022(8) C12 0.0210(11) 0.0309(12) 0.0323(13) -0.0120(10) -0.0076(9) 0.0032(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 Cl2 2.2939(8) 2_757 ? Pd1 Cl2 2.2939(8) . ? Pd1 Cl1 2.2971(10) . ? Pd1 Cl1 2.2971(10) 2_757 ? N1 C21 1.507(3) . ? N1 C11 1.517(3) . ? N1 C31 1.533(3) . ? N1 C41 1.539(3) . ? C35 C34 1.374(3) . ? C35 C36 1.381(3) . ? C35 H35 0.9500 . ? C21 C22 1.510(3) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C43 C44 1.383(3) . ? C43 C42 1.392(3) . ? C43 H43 0.9500 . ? C32 C37 1.386(3) . ? C32 C33 1.393(3) . ? C32 C31 1.507(3) . ? C11 C12 1.519(3) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C47 C46 1.374(3) . ? C47 C42 1.395(3) . ? C47 H47 0.9500 . ? C42 C41 1.505(3) . ? C44 C45 1.384(3) . ? C44 H44 0.9500 . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C45 C46 1.385(3) . ? C45 H45 0.9500 . ? C36 C37 1.382(3) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C46 H46 0.9500 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C34 C33 1.388(3) . ? C34 H34 0.9500 . ? C33 H33 0.9500 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? 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 Cl2 Pd1 Cl2 180.00(2) 2_757 . ? Cl2 Pd1 Cl1 90.45(3) 2_757 . ? Cl2 Pd1 Cl1 89.55(3) . . ? Cl2 Pd1 Cl1 89.55(3) 2_757 2_757 ? Cl2 Pd1 Cl1 90.45(3) . 2_757 ? Cl1 Pd1 Cl1 180.0 . 2_757 ? C21 N1 C11 108.44(16) . . ? C21 N1 C31 111.89(17) . . ? C11 N1 C31 108.82(16) . . ? C21 N1 C41 108.87(16) . . ? C11 N1 C41 111.21(16) . . ? C31 N1 C41 107.63(15) . . ? C34 C35 C36 119.6(2) . . ? C34 C35 H35 120.2 . . ? C36 C35 H35 120.2 . . ? N1 C21 C22 116.10(18) . . ? N1 C21 H21A 108.3 . . ? C22 C21 H21A 108.3 . . ? N1 C21 H21B 108.3 . . ? C22 C21 H21B 108.3 . . ? H21A C21 H21B 107.4 . . ? C44 C43 C42 120.7(2) . . ? C44 C43 H43 119.6 . . ? C42 C43 H43 119.6 . . ? C37 C32 C33 118.6(2) . . ? C37 C32 C31 122.4(2) . . ? C33 C32 C31 119.0(2) . . ? N1 C11 C12 116.06(18) . . ? N1 C11 H11A 108.3 . . ? C12 C11 H11A 108.3 . . ? N1 C11 H11B 108.3 . . ? C12 C11 H11B 108.3 . . ? H11A C11 H11B 107.4 . . ? C46 C47 C42 120.6(2) . . ? C46 C47 H47 119.7 . . ? C42 C47 H47 119.7 . . ? C43 C42 C47 118.5(2) . . ? C43 C42 C41 120.81(19) . . ? C47 C42 C41 120.4(2) . . ? C43 C44 C45 120.1(2) . . ? C43 C44 H44 120.0 . . ? C45 C44 H44 120.0 . . ? C32 C31 N1 115.40(17) . . ? C32 C31 H31A 108.4 . . ? N1 C31 H31A 108.4 . . ? C32 C31 H31B 108.4 . . ? N1 C31 H31B 108.4 . . ? H31A C31 H31B 107.5 . . ? C44 C45 C46 119.5(2) . . ? C44 C45 H45 120.2 . . ? C46 C45 H45 120.2 . . ? C35 C36 C37 120.7(2) . . ? C35 C36 H36 119.7 . . ? C37 C36 H36 119.7 . . ? C36 C37 C32 120.3(2) . . ? C36 C37 H37 119.8 . . ? C32 C37 H37 119.8 . . ? C42 C41 N1 115.59(16) . . ? C42 C41 H41A 108.4 . . ? N1 C41 H41A 108.4 . . ? C42 C41 H41B 108.4 . . ? N1 C41 H41B 108.4 . . ? H41A C41 H41B 107.4 . . ? C47 C46 C45 120.6(2) . . ? C47 C46 H46 119.7 . . ? C45 C46 H46 119.7 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C35 C34 C33 120.1(2) . . ? C35 C34 H34 120.0 . . ? C33 C34 H34 120.0 . . ? C34 C33 C32 120.7(2) . . ? C34 C33 H33 119.7 . . ? C32 C33 H33 119.7 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? 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 C11 N1 C21 C22 -178.32(18) . . . . ? C31 N1 C21 C22 -58.3(2) . . . . ? C41 N1 C21 C22 60.5(2) . . . . ? C21 N1 C11 C12 -53.3(2) . . . . ? C31 N1 C11 C12 -175.19(19) . . . . ? C41 N1 C11 C12 66.4(2) . . . . ? C44 C43 C42 C47 -1.9(3) . . . . ? C44 C43 C42 C41 -176.39(19) . . . . ? C46 C47 C42 C43 1.5(3) . . . . ? C46 C47 C42 C41 175.96(19) . . . . ? C42 C43 C44 C45 1.1(3) . . . . ? C37 C32 C31 N1 84.9(3) . . . . ? C33 C32 C31 N1 -98.0(2) . . . . ? C21 N1 C31 C32 -63.7(2) . . . . ? C11 N1 C31 C32 56.1(2) . . . . ? C41 N1 C31 C32 176.72(18) . . . . ? C43 C44 C45 C46 0.2(3) . . . . ? C34 C35 C36 C37 -1.0(3) . . . . ? C35 C36 C37 C32 -1.5(3) . . . . ? C33 C32 C37 C36 3.2(3) . . . . ? C31 C32 C37 C36 -179.7(2) . . . . ? C43 C42 C41 N1 -90.0(2) . . . . ? C47 C42 C41 N1 95.6(2) . . . . ? C21 N1 C41 C42 176.44(17) . . . . ? C11 N1 C41 C42 57.0(2) . . . . ? C31 N1 C41 C42 -62.1(2) . . . . ? C42 C47 C46 C45 -0.2(3) . . . . ? C44 C45 C46 C47 -0.7(3) . . . . ? C36 C35 C34 C33 1.8(3) . . . . ? C35 C34 C33 C32 0.0(3) . . . . ? C37 C32 C33 C34 -2.4(3) . . . . ? C31 C32 C33 C34 -179.63(19) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.81 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.374 _refine_diff_density_min -0.544 _refine_diff_density_rms 0.084 data_4 _database_code_depnum_ccdc_archive 'CCDC 692356' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C18 H24 N), Cl4 Pd' _chemical_formula_sum 'C36 H48 Cl4 N2 Pd' _chemical_formula_weight 756.96 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' 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 'P 1 21/c1' 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 15.791(3) _cell_length_b 11.540(2) _cell_length_c 18.860(4) _cell_angle_alpha 90.00 _cell_angle_beta 93.92(3) _cell_angle_gamma 90.00 _cell_volume 3429.0(12) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Prism _exptl_crystal_colour 'Dark yellow' _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.466 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1568 _exptl_absorpt_coefficient_mu 0.881 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8163 _exptl_absorpt_correction_T_max 0.9016 _exptl_absorpt_process_details 'Denzo (Z. Otwinowski, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30075 _diffrn_reflns_av_R_equivalents 0.0767 _diffrn_reflns_av_sigmaI/netI 0.1024 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 29.42 _reflns_number_total 9218 _reflns_number_gt 6177 _reflns_threshold_expression >2\s(I) _computing_data_collection Collect _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution SHELXS-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 3.0' _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^)+(0.0207P)^2^+1.7617P] 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 9218 _refine_ls_number_parameters 396 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0945 _refine_ls_R_factor_gt 0.0563 _refine_ls_wR_factor_ref 0.1118 _refine_ls_wR_factor_gt 0.1004 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _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 C62 C 0.3401(2) 0.0161(3) 0.09821(18) 0.0201(8) Uani 1 1 d . . . Pd1 Pd 0.249762(19) 0.45271(2) 0.245477(13) 0.01630(8) Uani 1 1 d . . . Cl2 Cl 0.16466(7) 0.53859(7) 0.15753(4) 0.0243(2) Uani 1 1 d . . . Cl3 Cl 0.20213(6) 0.27546(7) 0.20502(4) 0.0233(2) Uani 1 1 d . . . Cl4 Cl 0.33585(7) 0.36466(8) 0.33235(5) 0.0284(2) Uani 1 1 d . . . Cl1 Cl 0.29611(6) 0.63261(7) 0.28407(5) 0.0268(2) Uani 1 1 d . . . N2 N 0.4630(2) 0.1215(2) 0.16087(13) 0.0158(6) Uani 1 1 d . . . N1 N 0.0640(2) 0.8048(2) 0.25812(14) 0.0168(6) Uani 1 1 d . . . C52 C 0.4906(2) 0.3411(3) 0.15623(17) 0.0180(8) Uani 1 1 d . . . C32 C 0.0813(2) 0.9781(3) 0.33999(17) 0.0174(8) Uani 1 1 d . . . C33 C 0.0659(3) 0.9663(3) 0.41110(17) 0.0205(8) Uani 1 1 d . . . H33 H 0.0208 0.9180 0.4242 0.025 Uiso 1 1 calc R . . C55 C 0.5061(3) 0.5550(3) 0.08852(16) 0.0205(8) Uani 1 1 d . . . C41 C 0.5164(2) 0.1062(3) 0.09968(17) 0.0199(8) Uani 1 1 d . . . H41A H 0.5764 0.1127 0.1161 0.030 Uiso 1 1 calc R . . H41B H 0.5022 0.1663 0.0641 0.030 Uiso 1 1 calc R . . H41C H 0.5057 0.0296 0.0785 0.030 Uiso 1 1 calc R . . C34 C 0.1149(3) 1.0235(3) 0.46276(18) 0.0230(9) Uani 1 1 d . . . H34 H 0.1040 1.0136 0.5113 0.028 Uiso 1 1 calc R . . C53 C 0.5679(3) 0.3794(3) 0.13681(17) 0.0218(8) Uani 1 1 d . . . H53 H 0.6169 0.3329 0.1468 0.026 Uiso 1 1 calc R . . C54 C 0.5756(3) 0.4847(3) 0.10287(17) 0.0226(8) Uani 1 1 d . . . H54 H 0.6297 0.5088 0.0893 0.027 Uiso 1 1 calc R . . C56 C 0.4285(3) 0.5152(3) 0.10673(17) 0.0221(8) Uani 1 1 d . . . H56 H 0.3792 0.5609 0.0960 0.026 Uiso 1 1 calc R . . C61 C 0.3709(2) 0.1233(3) 0.13680(18) 0.0213(8) Uani 1 1 d . . . H61A H 0.3599 0.1909 0.1051 0.026 Uiso 1 1 calc R . . H61B H 0.3374 0.1342 0.1788 0.026 Uiso 1 1 calc R . . C27 C 0.0198(3) 0.7706(3) 0.07824(17) 0.0207(8) Uani 1 1 d . . . H27 H 0.0657 0.7173 0.0827 0.025 Uiso 1 1 calc R . . C12 C 0.0831(3) 0.7231(3) 0.31843(17) 0.0231(9) Uani 1 1 d . . . H12A H 0.1070 0.6514 0.3005 0.035 Uiso 1 1 calc R . . H12B H 0.0307 0.7055 0.3413 0.035 Uiso 1 1 calc R . . H12C H 0.1242 0.7589 0.3531 0.035 Uiso 1 1 calc R . . C22 C -0.0213(2) 0.8018(3) 0.13790(17) 0.0158(7) Uani 1 1 d . . . C31 C 0.0260(2) 0.9164(3) 0.28437(17) 0.0199(8) Uani 1 1 d . . . H31A H 0.0145 0.9691 0.2434 0.024 Uiso 1 1 calc R . . H31B H -0.0291 0.8985 0.3041 0.024 Uiso 1 1 calc R . . C35 C 0.1798(3) 1.0951(3) 0.44499(18) 0.0209(8) Uani 1 1 d . . . C51 C 0.4861(3) 0.2335(3) 0.20056(17) 0.0204(8) Uani 1 1 d . . . H51A H 0.4437 0.2466 0.2361 0.025 Uiso 1 1 calc R . . H51B H 0.5418 0.2225 0.2270 0.025 Uiso 1 1 calc R . . C28 C -0.1026(3) 0.9338(3) -0.06893(18) 0.0293(10) Uani 1 1 d . . . H28A H -0.1262 0.8691 -0.0976 0.044 Uiso 1 1 calc R . . H28B H -0.0547 0.9676 -0.0921 0.044 Uiso 1 1 calc R . . H28C H -0.1465 0.9929 -0.0644 0.044 Uiso 1 1 calc R . . C21 C 0.0004(2) 0.7434(3) 0.20758(17) 0.0183(8) Uani 1 1 d . . . H21A H 0.0229 0.6653 0.1979 0.022 Uiso 1 1 calc R . . H21B H -0.0526 0.7328 0.2319 0.022 Uiso 1 1 calc R . . C11 C 0.1428(2) 0.8272(3) 0.22225(17) 0.0181(8) Uani 1 1 d . . . H11A H 0.1867 0.8564 0.2570 0.027 Uiso 1 1 calc R . . H11B H 0.1316 0.8850 0.1847 0.027 Uiso 1 1 calc R . . H11C H 0.1623 0.7551 0.2013 0.027 Uiso 1 1 calc R . . C23 C -0.0886(3) 0.8768(3) 0.12908(18) 0.0239(9) Uani 1 1 d . . . H23 H -0.1186 0.8981 0.1691 0.029 Uiso 1 1 calc R . . C25 C -0.0725(3) 0.8903(3) 0.00400(18) 0.0226(8) Uani 1 1 d . . . C38 C 0.2341(3) 1.1572(3) 0.5017(2) 0.0332(10) Uani 1 1 d . . . H38A H 0.2903 1.1210 0.5067 0.050 Uiso 1 1 calc R . . H38B H 0.2073 1.1524 0.5470 0.050 Uiso 1 1 calc R . . H38C H 0.2399 1.2388 0.4883 0.050 Uiso 1 1 calc R . . C37 C 0.1458(3) 1.0509(3) 0.32259(17) 0.0211(8) Uani 1 1 d . . . H37 H 0.1570 1.0611 0.2741 0.025 Uiso 1 1 calc R . . C24 C -0.1134(3) 0.9216(3) 0.06334(19) 0.0252(9) Uani 1 1 d . . . H24 H -0.1593 0.9749 0.0588 0.030 Uiso 1 1 calc R . . C26 C -0.0052(3) 0.8157(3) 0.01254(18) 0.0236(9) Uani 1 1 d . . . H26 H 0.0248 0.7948 -0.0275 0.028 Uiso 1 1 calc R . . C64 C 0.3053(2) -0.0856(3) -0.01096(19) 0.0238(8) Uani 1 1 d . . . H64 H 0.3010 -0.0860 -0.0615 0.029 Uiso 1 1 calc R . . C63 C 0.3334(3) 0.0124(3) 0.02464(19) 0.0249(9) Uani 1 1 d . . . H63 H 0.3484 0.0787 -0.0016 0.030 Uiso 1 1 calc R . . C36 C 0.1941(3) 1.1090(3) 0.37447(18) 0.0209(8) Uani 1 1 d . . . H36 H 0.2380 1.1594 0.3614 0.025 Uiso 1 1 calc R . . C67 C 0.3168(2) -0.0819(3) 0.13459(19) 0.0227(8) Uani 1 1 d . . . H67 H 0.3192 -0.0805 0.1851 0.027 Uiso 1 1 calc R . . C65 C 0.2832(3) -0.1837(3) 0.0255(2) 0.0261(9) Uani 1 1 d . . . C57 C 0.4210(2) 0.4094(3) 0.14039(17) 0.0191(8) Uani 1 1 d . . . H57 H 0.3668 0.3839 0.1527 0.023 Uiso 1 1 calc R . . C66 C 0.2903(3) -0.1809(3) 0.0994(2) 0.0264(9) Uani 1 1 d . . . H66 H 0.2767 -0.2479 0.1256 0.032 Uiso 1 1 calc R . . C58 C 0.5151(3) 0.6713(3) 0.05373(19) 0.0310(10) Uani 1 1 d . . . H58A H 0.4601 0.7109 0.0505 0.047 Uiso 1 1 calc R . . H58B H 0.5345 0.6606 0.0059 0.047 Uiso 1 1 calc R . . H58C H 0.5566 0.7181 0.0821 0.047 Uiso 1 1 calc R . . C68 C 0.2524(3) -0.2898(3) -0.0130(2) 0.0416(12) Uani 1 1 d . . . H68A H 0.2420 -0.2723 -0.0637 0.062 Uiso 1 1 calc R . . H68B H 0.1995 -0.3161 0.0061 0.062 Uiso 1 1 calc R . . H68C H 0.2953 -0.3510 -0.0068 0.062 Uiso 1 1 calc R . . C42 C 0.4825(3) 0.0260(3) 0.21208(18) 0.0247(9) Uani 1 1 d . . . H42A H 0.4689 -0.0484 0.1891 0.037 Uiso 1 1 calc R . . H42B H 0.4485 0.0355 0.2533 0.037 Uiso 1 1 calc R . . H42C H 0.5430 0.0280 0.2278 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 C62 0.012(2) 0.0219(18) 0.0258(18) -0.0015(14) -0.0001(15) -0.0021(16) Pd1 0.01467(16) 0.01716(13) 0.01720(13) 0.00059(10) 0.00205(10) 0.00092(12) Cl2 0.0273(6) 0.0221(4) 0.0225(4) -0.0012(3) -0.0055(4) 0.0031(4) Cl3 0.0257(6) 0.0179(4) 0.0269(4) -0.0023(3) 0.0055(4) -0.0012(4) Cl4 0.0262(6) 0.0290(5) 0.0292(5) 0.0094(4) -0.0050(4) 0.0005(4) Cl1 0.0228(6) 0.0209(4) 0.0351(5) -0.0035(4) -0.0090(4) 0.0010(4) N2 0.0178(18) 0.0144(14) 0.0155(13) 0.0004(10) 0.0020(12) -0.0001(13) N1 0.0184(19) 0.0145(14) 0.0177(14) -0.0005(11) 0.0036(13) -0.0008(13) C52 0.021(2) 0.0180(17) 0.0152(16) -0.0043(13) 0.0011(15) 0.0018(16) C32 0.017(2) 0.0156(17) 0.0195(16) -0.0002(13) 0.0022(15) 0.0065(15) C33 0.025(2) 0.0170(17) 0.0202(17) 0.0012(13) 0.0037(16) 0.0002(16) C55 0.031(3) 0.0181(17) 0.0125(15) -0.0033(13) -0.0013(15) -0.0049(17) C41 0.017(2) 0.0234(18) 0.0202(17) 0.0003(14) 0.0053(15) 0.0014(16) C34 0.029(3) 0.0238(19) 0.0163(17) 0.0038(14) 0.0026(16) 0.0079(18) C53 0.022(2) 0.0212(18) 0.0219(18) -0.0017(14) 0.0002(16) -0.0003(17) C54 0.021(2) 0.0244(19) 0.0230(18) -0.0022(14) 0.0035(16) -0.0064(17) C56 0.025(2) 0.0186(17) 0.0225(18) -0.0021(14) -0.0016(17) 0.0041(17) C61 0.015(2) 0.0245(19) 0.0246(18) -0.0024(14) 0.0042(16) 0.0020(17) C27 0.021(2) 0.0164(17) 0.0239(18) -0.0036(14) -0.0003(16) 0.0047(16) C12 0.029(3) 0.0202(18) 0.0196(18) 0.0085(14) -0.0022(16) -0.0005(17) C22 0.015(2) 0.0147(16) 0.0174(16) -0.0021(12) -0.0005(14) -0.0050(15) C31 0.022(2) 0.0202(17) 0.0175(17) -0.0014(13) 0.0028(16) 0.0056(16) C35 0.021(2) 0.0153(16) 0.0256(19) -0.0033(14) -0.0036(16) 0.0093(16) C51 0.026(2) 0.0209(17) 0.0139(16) -0.0026(13) -0.0020(15) 0.0013(17) C28 0.035(3) 0.028(2) 0.0234(19) 0.0038(15) -0.0041(18) -0.0042(19) C21 0.018(2) 0.0174(16) 0.0192(17) -0.0001(13) 0.0006(15) -0.0022(16) C11 0.012(2) 0.0218(18) 0.0203(17) 0.0001(13) 0.0036(15) -0.0003(15) C23 0.019(2) 0.033(2) 0.0201(18) -0.0019(15) 0.0031(16) 0.0007(18) C25 0.023(2) 0.0222(18) 0.0221(18) 0.0026(14) -0.0041(16) -0.0072(17) C38 0.037(3) 0.032(2) 0.030(2) -0.0085(17) -0.007(2) 0.001(2) C37 0.029(2) 0.0151(16) 0.0195(17) 0.0011(13) 0.0058(16) 0.0056(17) C24 0.016(2) 0.030(2) 0.029(2) 0.0006(15) -0.0007(17) 0.0021(17) C26 0.029(3) 0.0237(18) 0.0181(18) -0.0052(14) 0.0031(17) -0.0010(18) C64 0.014(2) 0.034(2) 0.0236(18) -0.0029(15) 0.0013(16) 0.0032(18) C63 0.017(2) 0.030(2) 0.029(2) 0.0068(16) 0.0045(17) 0.0019(18) C36 0.020(2) 0.0160(17) 0.0269(19) 0.0011(14) 0.0020(16) 0.0000(16) C67 0.017(2) 0.029(2) 0.0230(18) -0.0008(15) 0.0058(16) -0.0030(17) C65 0.013(2) 0.026(2) 0.039(2) -0.0052(16) -0.0003(18) 0.0039(17) C57 0.017(2) 0.0220(17) 0.0184(17) -0.0032(13) 0.0026(15) -0.0010(16) C66 0.021(2) 0.0233(19) 0.035(2) 0.0045(16) 0.0055(18) 0.0022(18) C58 0.044(3) 0.0210(19) 0.027(2) 0.0026(15) -0.002(2) -0.0028(19) C68 0.036(3) 0.032(2) 0.056(3) -0.018(2) 0.000(2) -0.007(2) C42 0.032(3) 0.0194(18) 0.0227(18) 0.0060(14) 0.0000(17) 0.0003(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C62 C63 1.385(5) . ? C62 C67 1.386(5) . ? C62 C61 1.500(5) . ? Pd1 Cl2 2.2880(11) . ? Pd1 Cl3 2.2921(9) . ? Pd1 Cl4 2.2936(11) . ? Pd1 Cl1 2.3029(10) . ? N2 C42 1.483(4) . ? N2 C41 1.485(4) . ? N2 C61 1.495(5) . ? N2 C51 1.526(4) . ? N1 C11 1.479(4) . ? N1 C12 1.492(4) . ? N1 C21 1.512(4) . ? N1 C31 1.518(4) . ? C52 C57 1.369(5) . ? C52 C53 1.371(5) . ? C52 C51 1.501(4) . ? C32 C37 1.378(5) . ? C32 C33 1.386(4) . ? C32 C31 1.498(5) . ? C33 C34 1.372(5) . ? C55 C56 1.375(5) . ? C55 C54 1.377(5) . ? C55 C58 1.505(5) . ? C34 C35 1.375(5) . ? C53 C54 1.383(5) . ? C56 C57 1.384(5) . ? C27 C26 1.377(5) . ? C27 C22 1.384(5) . ? C22 C23 1.372(5) . ? C22 C21 1.496(4) . ? C35 C36 1.373(5) . ? C35 C38 1.506(5) . ? C28 C25 1.510(5) . ? C23 C24 1.375(5) . ? C25 C26 1.368(5) . ? C25 C24 1.378(5) . ? C37 C36 1.373(5) . ? C64 C63 1.373(5) . ? C64 C65 1.382(5) . ? C67 C66 1.373(5) . ? C65 C66 1.390(5) . ? C65 C68 1.489(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C63 C62 C67 117.8(3) . . ? C63 C62 C61 120.8(3) . . ? C67 C62 C61 121.4(3) . . ? Cl2 Pd1 Cl3 88.98(4) . . ? Cl2 Pd1 Cl4 179.10(4) . . ? Cl3 Pd1 Cl4 90.42(4) . . ? Cl2 Pd1 Cl1 89.82(4) . . ? Cl3 Pd1 Cl1 178.79(4) . . ? Cl4 Pd1 Cl1 90.78(4) . . ? C42 N2 C41 108.3(3) . . ? C42 N2 C61 111.3(3) . . ? C41 N2 C61 111.0(3) . . ? C42 N2 C51 106.1(2) . . ? C41 N2 C51 110.7(3) . . ? C61 N2 C51 109.4(3) . . ? C11 N1 C12 109.0(3) . . ? C11 N1 C21 109.6(3) . . ? C12 N1 C21 106.0(2) . . ? C11 N1 C31 111.4(3) . . ? C12 N1 C31 110.6(2) . . ? C21 N1 C31 110.1(3) . . ? C57 C52 C53 118.1(3) . . ? C57 C52 C51 122.0(3) . . ? C53 C52 C51 119.5(3) . . ? C37 C32 C33 118.1(3) . . ? C37 C32 C31 121.9(3) . . ? C33 C32 C31 119.9(3) . . ? C34 C33 C32 120.8(4) . . ? C56 C55 C54 117.8(3) . . ? C56 C55 C58 121.3(4) . . ? C54 C55 C58 120.9(4) . . ? C33 C34 C35 120.7(3) . . ? C52 C53 C54 121.0(4) . . ? C55 C54 C53 121.0(4) . . ? C55 C56 C57 120.9(4) . . ? N2 C61 C62 114.3(3) . . ? C26 C27 C22 120.8(3) . . ? C23 C22 C27 117.9(3) . . ? C23 C22 C21 121.3(3) . . ? C27 C22 C21 120.3(3) . . ? C32 C31 N1 114.0(3) . . ? C36 C35 C34 118.7(3) . . ? C36 C35 C38 120.6(4) . . ? C34 C35 C38 120.7(3) . . ? C52 C51 N2 116.5(3) . . ? C22 C21 N1 116.4(3) . . ? C22 C23 C24 121.1(3) . . ? C26 C25 C24 118.2(3) . . ? C26 C25 C28 120.7(3) . . ? C24 C25 C28 121.1(4) . . ? C36 C37 C32 120.8(3) . . ? C23 C24 C25 120.9(4) . . ? C25 C26 C27 121.1(3) . . ? C63 C64 C65 121.0(3) . . ? C64 C63 C62 121.0(3) . . ? C37 C36 C35 120.9(4) . . ? C66 C67 C62 121.5(3) . . ? C64 C65 C66 118.3(3) . . ? C64 C65 C68 121.1(4) . . ? C66 C65 C68 120.6(4) . . ? C52 C57 C56 121.1(4) . . ? C67 C66 C65 120.3(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 C37 C32 C33 C34 -1.5(5) . . . . ? C31 C32 C33 C34 -178.9(3) . . . . ? C32 C33 C34 C35 0.8(5) . . . . ? C57 C52 C53 C54 0.7(5) . . . . ? C51 C52 C53 C54 -172.7(3) . . . . ? C56 C55 C54 C53 -2.3(5) . . . . ? C58 C55 C54 C53 178.0(3) . . . . ? C52 C53 C54 C55 1.0(5) . . . . ? C54 C55 C56 C57 2.0(5) . . . . ? C58 C55 C56 C57 -178.3(3) . . . . ? C42 N2 C61 C62 -61.9(4) . . . . ? C41 N2 C61 C62 58.8(4) . . . . ? C51 N2 C61 C62 -178.8(3) . . . . ? C63 C62 C61 N2 -97.3(4) . . . . ? C67 C62 C61 N2 83.3(4) . . . . ? C26 C27 C22 C23 1.5(5) . . . . ? C26 C27 C22 C21 173.8(3) . . . . ? C37 C32 C31 N1 83.3(4) . . . . ? C33 C32 C31 N1 -99.3(4) . . . . ? C11 N1 C31 C32 -63.5(4) . . . . ? C12 N1 C31 C32 57.9(4) . . . . ? C21 N1 C31 C32 174.7(3) . . . . ? C33 C34 C35 C36 0.6(5) . . . . ? C33 C34 C35 C38 -179.6(3) . . . . ? C57 C52 C51 N2 88.8(4) . . . . ? C53 C52 C51 N2 -98.0(4) . . . . ? C42 N2 C51 C52 166.8(3) . . . . ? C41 N2 C51 C52 49.5(4) . . . . ? C61 N2 C51 C52 -73.1(4) . . . . ? C23 C22 C21 N1 -91.9(4) . . . . ? C27 C22 C21 N1 96.1(4) . . . . ? C11 N1 C21 C22 -55.2(4) . . . . ? C12 N1 C21 C22 -172.8(3) . . . . ? C31 N1 C21 C22 67.6(4) . . . . ? C27 C22 C23 C24 -1.5(5) . . . . ? C21 C22 C23 C24 -173.7(3) . . . . ? C33 C32 C37 C36 0.8(5) . . . . ? C31 C32 C37 C36 178.2(3) . . . . ? C22 C23 C24 C25 1.6(6) . . . . ? C26 C25 C24 C23 -1.6(6) . . . . ? C28 C25 C24 C23 176.4(3) . . . . ? C24 C25 C26 C27 1.7(6) . . . . ? C28 C25 C26 C27 -176.3(3) . . . . ? C22 C27 C26 C25 -1.7(6) . . . . ? C65 C64 C63 C62 -0.2(6) . . . . ? C67 C62 C63 C64 -0.7(6) . . . . ? C61 C62 C63 C64 179.9(4) . . . . ? C32 C37 C36 C35 0.6(5) . . . . ? C34 C35 C36 C37 -1.3(5) . . . . ? C38 C35 C36 C37 178.8(3) . . . . ? C63 C62 C67 C66 2.0(6) . . . . ? C61 C62 C67 C66 -178.7(4) . . . . ? C63 C64 C65 C66 -0.2(6) . . . . ? C63 C64 C65 C68 179.7(4) . . . . ? C53 C52 C57 C56 -1.0(5) . . . . ? C51 C52 C57 C56 172.3(3) . . . . ? C55 C56 C57 C52 -0.3(5) . . . . ? C62 C67 C66 C65 -2.4(6) . . . . ? C64 C65 C66 C67 1.5(6) . . . . ? C68 C65 C66 C67 -178.4(4) . . . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.558 _refine_diff_density_min -0.692 _refine_diff_density_rms 0.128 data_10 _database_code_depnum_ccdc_archive 'CCDC 692357' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H48 Cl6 N2 Pd2' _chemical_formula_weight 934.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' 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 'P 1 21/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.488(3) _cell_length_b 16.310(3) _cell_length_c 17.107(3) _cell_angle_alpha 90.00 _cell_angle_beta 105.13(3) _cell_angle_gamma 90.00 _cell_volume 3902.2(14) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Needle _exptl_crystal_colour Orange _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.590 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1888 _exptl_absorpt_coefficient_mu 1.360 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5859 _exptl_absorpt_correction_T_max 0.8990 _exptl_absorpt_process_details 'Denzo (Z. Otwinowski, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 'Kappa APEX II' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35183 _diffrn_reflns_av_R_equivalents 0.0801 _diffrn_reflns_av_sigmaI/netI 0.1081 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 28.70 _reflns_number_total 10043 _reflns_number_gt 5601 _reflns_threshold_expression >2\s(I) _computing_data_collection Collect _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution SHELXS-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 3.0' _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^ > 2\s(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^)+(0.0212P)^2^+1.3008P] 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 10043 _refine_ls_number_parameters 419 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1277 _refine_ls_R_factor_gt 0.0563 _refine_ls_wR_factor_ref 0.0995 _refine_ls_wR_factor_gt 0.0829 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.18228(2) 0.55900(2) 0.303116(19) 0.02974(10) Uani 1 1 d . . . Pd2 Pd 0.29347(2) 0.42675(2) 0.205329(19) 0.03077(11) Uani 1 1 d . . . Cl1 Cl 0.05964(9) 0.54571(9) 0.36231(8) 0.0516(4) Uani 1 1 d . . . Cl2 Cl 0.21750(8) 0.68696(8) 0.35425(7) 0.0406(3) Uani 1 1 d . . . Cl3 Cl 0.15211(8) 0.42915(8) 0.24642(7) 0.0400(3) Uani 1 1 d . . . Cl4 Cl 0.31048(8) 0.56350(8) 0.24494(7) 0.0422(3) Uani 1 1 d . . . Cl5 Cl 0.26724(8) 0.29401(8) 0.16405(7) 0.0405(3) Uani 1 1 d . . . Cl6 Cl 0.43354(8) 0.43204(10) 0.17008(8) 0.0514(4) Uani 1 1 d . . . N1 N -0.0879(2) 0.7175(2) 0.0938(2) 0.0261(9) Uani 1 1 d . . . N2 N 0.5796(2) 0.2770(2) 0.41744(19) 0.0252(9) Uani 1 1 d . . . C11 C -0.0389(3) 0.7936(3) 0.0748(3) 0.0372(12) Uani 1 1 d . . . H11A H 0.0274 0.7791 0.0744 0.045 Uiso 1 1 calc R . . H11B H -0.0349 0.8337 0.1190 0.045 Uiso 1 1 calc R . . C12 C -0.0869(3) 0.8352(3) -0.0055(3) 0.0470(14) Uani 1 1 d . . . H12A H -0.1054 0.7936 -0.0481 0.071 Uiso 1 1 calc R . . H12B H -0.0421 0.8740 -0.0196 0.071 Uiso 1 1 calc R . . H12C H -0.1439 0.8646 -0.0003 0.071 Uiso 1 1 calc R . . C21 C -0.0321(3) 0.6862(3) 0.1765(2) 0.0349(12) Uani 1 1 d . . . H21A H -0.0622 0.6346 0.1878 0.042 Uiso 1 1 calc R . . H21B H 0.0335 0.6726 0.1736 0.042 Uiso 1 1 calc R . . C22 C -0.0249(3) 0.7439(3) 0.2474(3) 0.0469(15) Uani 1 1 d . . . H22A H 0.0080 0.7943 0.2388 0.070 Uiso 1 1 calc R . . H22B H 0.0112 0.7174 0.2975 0.070 Uiso 1 1 calc R . . H22C H -0.0892 0.7574 0.2519 0.070 Uiso 1 1 calc R . . C31 C -0.0894(3) 0.6498(3) 0.0319(2) 0.0263(10) Uani 1 1 d . . . H31A H -0.1145 0.5995 0.0512 0.032 Uiso 1 1 calc R . . H31B H -0.1354 0.6660 -0.0195 0.032 Uiso 1 1 calc R . . C32 C 0.0030(3) 0.6287(3) 0.0135(2) 0.0223(10) Uani 1 1 d . . . C33 C 0.0224(3) 0.6582(3) -0.0551(3) 0.0478(15) Uani 1 1 d . . . H33 H -0.0199 0.6969 -0.0874 0.057 Uiso 1 1 calc R . . C34 C 0.1022(4) 0.6331(4) -0.0788(3) 0.0637(19) Uani 1 1 d . . . H34 H 0.1130 0.6532 -0.1278 0.076 Uiso 1 1 calc R . . C35 C 0.1657(3) 0.5791(3) -0.0315(3) 0.0414(13) Uani 1 1 d . . . H35 H 0.2211 0.5621 -0.0470 0.050 Uiso 1 1 calc R . . C36 C 0.1481(3) 0.5503(3) 0.0383(3) 0.0366(12) Uani 1 1 d . . . H36 H 0.1921 0.5138 0.0718 0.044 Uiso 1 1 calc R . . C37 C 0.0676(3) 0.5736(3) 0.0602(2) 0.0319(11) Uani 1 1 d . . . H37 H 0.0558 0.5517 0.1082 0.038 Uiso 1 1 calc R . . C41 C -0.1923(3) 0.7389(3) 0.0920(3) 0.0307(11) Uani 1 1 d . . . H41A H -0.1918 0.7808 0.1340 0.037 Uiso 1 1 calc R . . H41B H -0.2236 0.7635 0.0388 0.037 Uiso 1 1 calc R . . C42 C -0.2507(3) 0.6667(3) 0.1060(3) 0.0280(11) Uani 1 1 d . . . C43 C -0.3081(3) 0.6244(3) 0.0406(3) 0.0299(11) Uani 1 1 d . . . H43 H -0.3092 0.6409 -0.0129 0.036 Uiso 1 1 calc R . . C44 C -0.3635(3) 0.5588(3) 0.0519(3) 0.0353(12) Uani 1 1 d . . . H44 H -0.4015 0.5300 0.0066 0.042 Uiso 1 1 calc R . . C45 C -0.3631(3) 0.5357(3) 0.1281(3) 0.0444(13) Uani 1 1 d . . . H45 H -0.4007 0.4903 0.1359 0.053 Uiso 1 1 calc R . . C46 C -0.3088(4) 0.5774(4) 0.1948(3) 0.0489(15) Uani 1 1 d . . . H46 H -0.3094 0.5609 0.2479 0.059 Uiso 1 1 calc R . . C47 C -0.2538(3) 0.6432(3) 0.1836(3) 0.0414(13) Uani 1 1 d . . . H47 H -0.2176 0.6728 0.2292 0.050 Uiso 1 1 calc R . . C51 C 0.5338(3) 0.2086(3) 0.4531(3) 0.0360(12) Uani 1 1 d . . . H51A H 0.5283 0.1601 0.4173 0.043 Uiso 1 1 calc R . . H51B H 0.4681 0.2257 0.4527 0.043 Uiso 1 1 calc R . . C52 C 0.5852(3) 0.1829(3) 0.5384(3) 0.0501(15) Uani 1 1 d . . . H52A H 0.6424 0.1513 0.5374 0.075 Uiso 1 1 calc R . . H52B H 0.5426 0.1490 0.5610 0.075 Uiso 1 1 calc R . . H52C H 0.6039 0.2318 0.5721 0.075 Uiso 1 1 calc R . . C61 C 0.5193(3) 0.2927(3) 0.3309(2) 0.0302(11) Uani 1 1 d . . . H61A H 0.4551 0.3111 0.3336 0.036 Uiso 1 1 calc R . . H61B H 0.5488 0.3385 0.3081 0.036 Uiso 1 1 calc R . . C62 C 0.5069(3) 0.2215(3) 0.2730(3) 0.0417(13) Uani 1 1 d . . . H62A H 0.5698 0.1997 0.2725 0.063 Uiso 1 1 calc R . . H62B H 0.4735 0.2400 0.2184 0.063 Uiso 1 1 calc R . . H62C H 0.4694 0.1785 0.2903 0.063 Uiso 1 1 calc R . . C71 C 0.5836(3) 0.3573(3) 0.4647(2) 0.0247(10) Uani 1 1 d . . . H71A H 0.6371 0.3535 0.5143 0.030 Uiso 1 1 calc R . . H71B H 0.5990 0.4023 0.4313 0.030 Uiso 1 1 calc R . . C72 C 0.4954(3) 0.3807(3) 0.4893(2) 0.0239(10) Uani 1 1 d . . . C73 C 0.4169(3) 0.4168(3) 0.4383(3) 0.0413(14) Uani 1 1 d . . . H73 H 0.4162 0.4252 0.3832 0.050 Uiso 1 1 calc R . . C74 C 0.3392(3) 0.4412(3) 0.4647(3) 0.0505(16) Uani 1 1 d . . . H74 H 0.2850 0.4643 0.4275 0.061 Uiso 1 1 calc R . . C75 C 0.3398(3) 0.4323(3) 0.5446(3) 0.0411(13) Uani 1 1 d . . . H75 H 0.2857 0.4478 0.5627 0.049 Uiso 1 1 calc R . . C76 C 0.4189(4) 0.4010(4) 0.5975(3) 0.0622(18) Uani 1 1 d . . . H76 H 0.4215 0.3976 0.6535 0.075 Uiso 1 1 calc R . . C77 C 0.4954(4) 0.3740(4) 0.5701(3) 0.0495(16) Uani 1 1 d . . . H77 H 0.5491 0.3503 0.6074 0.059 Uiso 1 1 calc R . . C81 C 0.6834(3) 0.2515(3) 0.4185(3) 0.0286(11) Uani 1 1 d . . . H81A H 0.7191 0.2400 0.4752 0.034 Uiso 1 1 calc R . . H81B H 0.6808 0.2000 0.3875 0.034 Uiso 1 1 calc R . . C82 C 0.7376(3) 0.3140(3) 0.3843(3) 0.0285(11) Uani 1 1 d . . . C83 C 0.7340(3) 0.3150(3) 0.3030(3) 0.0388(12) Uani 1 1 d . . . H83 H 0.6958 0.2756 0.2681 0.047 Uiso 1 1 calc R . . C84 C 0.7848(3) 0.3723(4) 0.2710(3) 0.0505(15) Uani 1 1 d . . . H84 H 0.7802 0.3727 0.2146 0.061 Uiso 1 1 calc R . . C85 C 0.8426(3) 0.4291(3) 0.3218(3) 0.0424(13) Uani 1 1 d . . . H85 H 0.8779 0.4683 0.3004 0.051 Uiso 1 1 calc R . . C86 C 0.8483(3) 0.4280(3) 0.4037(3) 0.0339(11) Uani 1 1 d . . . H86 H 0.8877 0.4666 0.4388 0.041 Uiso 1 1 calc R . . C87 C 0.7968(3) 0.3710(3) 0.4348(3) 0.0301(11) Uani 1 1 d . . . H87 H 0.8016 0.3706 0.4912 0.036 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 Pd1 0.02653(18) 0.0321(2) 0.02766(17) 0.00404(17) 0.00188(14) -0.00620(16) Pd2 0.02751(18) 0.0373(3) 0.02525(16) 0.00428(17) 0.00289(14) -0.00653(17) Cl1 0.0374(7) 0.0615(11) 0.0613(8) -0.0105(7) 0.0228(6) -0.0124(7) Cl2 0.0406(7) 0.0353(8) 0.0403(6) -0.0020(6) 0.0007(6) -0.0043(6) Cl3 0.0376(6) 0.0350(8) 0.0508(7) -0.0035(6) 0.0177(6) -0.0144(6) Cl4 0.0451(7) 0.0408(9) 0.0454(6) -0.0046(6) 0.0203(6) -0.0197(6) Cl5 0.0395(7) 0.0344(8) 0.0435(6) 0.0032(6) 0.0034(6) 0.0002(6) Cl6 0.0333(6) 0.0718(11) 0.0525(7) 0.0005(8) 0.0176(6) -0.0071(7) N1 0.0236(18) 0.021(2) 0.0328(19) 0.0001(17) 0.0059(16) 0.0007(16) N2 0.0196(17) 0.030(2) 0.0270(18) -0.0014(17) 0.0078(15) -0.0011(16) C11 0.029(2) 0.025(3) 0.055(3) -0.004(2) 0.008(2) -0.007(2) C12 0.040(3) 0.037(4) 0.063(3) 0.017(3) 0.011(3) -0.007(2) C21 0.029(2) 0.042(3) 0.030(2) -0.003(2) 0.000(2) 0.010(2) C22 0.039(3) 0.062(4) 0.034(3) -0.014(3) -0.001(2) 0.012(3) C31 0.026(2) 0.024(3) 0.029(2) 0.001(2) 0.0066(19) -0.0026(19) C32 0.019(2) 0.018(3) 0.029(2) -0.0012(19) 0.0045(18) -0.0014(18) C33 0.042(3) 0.057(4) 0.053(3) 0.022(3) 0.028(3) 0.027(3) C34 0.068(4) 0.071(5) 0.068(4) 0.036(3) 0.046(3) 0.030(4) C35 0.024(2) 0.033(3) 0.072(4) -0.004(3) 0.023(2) -0.002(2) C36 0.030(2) 0.031(3) 0.041(3) -0.003(2) -0.003(2) 0.011(2) C37 0.040(3) 0.025(3) 0.030(2) 0.003(2) 0.006(2) 0.010(2) C41 0.020(2) 0.032(3) 0.039(2) -0.003(2) 0.006(2) 0.002(2) C42 0.024(2) 0.025(3) 0.038(2) 0.000(2) 0.011(2) 0.007(2) C43 0.021(2) 0.030(3) 0.040(2) -0.001(2) 0.011(2) 0.003(2) C44 0.022(2) 0.030(3) 0.058(3) -0.001(3) 0.017(2) 0.001(2) C45 0.037(3) 0.030(3) 0.075(4) 0.008(3) 0.031(3) 0.003(2) C46 0.054(3) 0.053(4) 0.052(3) 0.019(3) 0.038(3) 0.012(3) C47 0.043(3) 0.045(4) 0.039(3) 0.006(3) 0.017(2) 0.008(3) C51 0.027(2) 0.033(3) 0.052(3) 0.000(2) 0.016(2) -0.010(2) C52 0.043(3) 0.051(4) 0.056(3) 0.027(3) 0.014(3) -0.011(3) C61 0.027(2) 0.032(3) 0.029(2) -0.001(2) 0.002(2) 0.005(2) C62 0.031(3) 0.054(4) 0.039(3) -0.015(3) 0.005(2) -0.001(2) C71 0.026(2) 0.023(3) 0.026(2) -0.0040(19) 0.0076(19) -0.0072(19) C72 0.021(2) 0.025(3) 0.026(2) 0.000(2) 0.0076(19) -0.0031(19) C73 0.052(3) 0.041(4) 0.023(2) -0.002(2) -0.004(2) 0.023(3) C74 0.036(3) 0.050(4) 0.052(3) -0.019(3) -0.012(3) 0.020(3) C75 0.027(2) 0.033(3) 0.071(3) 0.002(3) 0.027(3) 0.004(2) C76 0.078(4) 0.070(5) 0.055(3) 0.040(3) 0.046(3) 0.043(4) C77 0.043(3) 0.075(5) 0.036(3) 0.024(3) 0.019(2) 0.036(3) C81 0.020(2) 0.030(3) 0.035(2) 0.000(2) 0.006(2) 0.003(2) C82 0.022(2) 0.027(3) 0.037(2) -0.004(2) 0.008(2) 0.005(2) C83 0.034(3) 0.041(4) 0.043(3) -0.005(2) 0.012(2) -0.007(2) C84 0.043(3) 0.065(5) 0.046(3) 0.012(3) 0.016(3) -0.001(3) C85 0.032(3) 0.037(3) 0.063(3) 0.013(3) 0.023(3) -0.001(2) C86 0.020(2) 0.026(3) 0.057(3) -0.005(2) 0.013(2) 0.001(2) C87 0.022(2) 0.034(3) 0.036(2) -0.002(2) 0.011(2) 0.004(2) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 Cl2 2.2688(14) . ? Pd1 Cl1 2.2735(14) . ? Pd1 Cl3 2.3230(14) . ? Pd1 Cl4 2.3259(14) . ? Pd2 Cl6 2.2645(14) . ? Pd2 Cl5 2.2780(14) . ? Pd2 Cl4 2.3255(15) . ? Pd2 Cl3 2.3326(13) . ? N1 C11 1.508(5) . ? N1 C21 1.523(5) . ? N1 C31 1.526(5) . ? N1 C41 1.544(5) . ? N2 C51 1.506(5) . ? N2 C61 1.531(5) . ? N2 C71 1.533(5) . ? N2 C81 1.556(5) . ? C11 C12 1.526(6) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C21 C22 1.519(6) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C31 C32 1.492(6) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.364(6) . ? C32 C37 1.391(5) . ? C33 C34 1.383(7) . ? C33 H33 0.9500 . ? C34 C35 1.375(7) . ? C34 H34 0.9500 . ? C35 C36 1.367(7) . ? C35 H35 0.9500 . ? C36 C37 1.368(6) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? C41 C42 1.506(6) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.391(6) . ? C42 C47 1.392(6) . ? C43 C44 1.380(6) . ? C43 H43 0.9500 . ? C44 C45 1.355(7) . ? C44 H44 0.9500 . ? C45 C46 1.383(7) . ? C45 H45 0.9500 . ? C46 C47 1.380(7) . ? C46 H46 0.9500 . ? C47 H47 0.9500 . ? C51 C52 1.515(6) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C61 C62 1.507(6) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C71 C72 1.496(6) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C72 C73 1.373(5) . ? C72 C77 1.386(6) . ? C73 C74 1.377(7) . ? C73 H73 0.9500 . ? C74 C75 1.372(7) . ? C74 H74 0.9500 . ? C75 C76 1.361(6) . ? C75 H75 0.9500 . ? C76 C77 1.384(7) . ? C76 H76 0.9500 . ? C77 H77 0.9500 . ? C81 C82 1.495(6) . ? C81 H81A 0.9900 . ? C81 H81B 0.9900 . ? C82 C83 1.379(6) . ? C82 C87 1.400(6) . ? C83 C84 1.387(7) . ? C83 H83 0.9500 . ? C84 C85 1.391(7) . ? C84 H84 0.9500 . ? C85 C86 1.382(7) . ? C85 H85 0.9500 . ? C86 C87 1.382(6) . ? C86 H86 0.9500 . ? C87 H87 0.9500 . ? 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 Cl2 Pd1 Cl1 92.25(5) . . ? Cl2 Pd1 Cl3 176.83(5) . . ? Cl1 Pd1 Cl3 90.87(5) . . ? Cl2 Pd1 Cl4 90.66(5) . . ? Cl1 Pd1 Cl4 176.15(6) . . ? Cl3 Pd1 Cl4 86.24(5) . . ? Cl6 Pd2 Cl5 92.42(5) . . ? Cl6 Pd2 Cl4 90.39(5) . . ? Cl5 Pd2 Cl4 176.59(4) . . ? Cl6 Pd2 Cl3 176.27(5) . . ? Cl5 Pd2 Cl3 91.19(5) . . ? Cl4 Pd2 Cl3 86.03(4) . . ? Pd1 Cl3 Pd2 93.26(4) . . ? Pd2 Cl4 Pd1 93.37(5) . . ? C11 N1 C21 108.1(3) . . ? C11 N1 C31 111.6(3) . . ? C21 N1 C31 108.1(3) . . ? C11 N1 C41 108.9(3) . . ? C21 N1 C41 111.9(3) . . ? C31 N1 C41 108.3(3) . . ? C51 N2 C61 108.3(3) . . ? C51 N2 C71 112.3(3) . . ? C61 N2 C71 107.5(3) . . ? C51 N2 C81 108.9(3) . . ? C61 N2 C81 111.2(3) . . ? C71 N2 C81 108.6(3) . . ? N1 C11 C12 115.5(3) . . ? N1 C11 H11A 108.4 . . ? C12 C11 H11A 108.4 . . ? N1 C11 H11B 108.4 . . ? C12 C11 H11B 108.4 . . ? H11A C11 H11B 107.5 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C22 C21 N1 116.3(4) . . ? C22 C21 H21A 108.2 . . ? N1 C21 H21A 108.2 . . ? C22 C21 H21B 108.2 . . ? N1 C21 H21B 108.2 . . ? H21A C21 H21B 107.4 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C32 C31 N1 117.6(3) . . ? C32 C31 H31A 107.9 . . ? N1 C31 H31A 107.9 . . ? C32 C31 H31B 107.9 . . ? N1 C31 H31B 107.9 . . ? H31A C31 H31B 107.2 . . ? C33 C32 C37 117.6(4) . . ? C33 C32 C31 119.8(4) . . ? C37 C32 C31 122.3(4) . . ? C32 C33 C34 121.6(5) . . ? C32 C33 H33 119.2 . . ? C34 C33 H33 119.2 . . ? C35 C34 C33 119.9(5) . . ? C35 C34 H34 120.0 . . ? C33 C34 H34 120.0 . . ? C36 C35 C34 119.0(5) . . ? C36 C35 H35 120.5 . . ? C34 C35 H35 120.5 . . ? C35 C36 C37 120.8(4) . . ? C35 C36 H36 119.6 . . ? C37 C36 H36 119.6 . . ? C36 C37 C32 121.0(4) . . ? C36 C37 H37 119.5 . . ? C32 C37 H37 119.5 . . ? C42 C41 N1 114.1(4) . . ? C42 C41 H41A 108.7 . . ? N1 C41 H41A 108.7 . . ? C42 C41 H41B 108.7 . . ? N1 C41 H41B 108.7 . . ? H41A C41 H41B 107.6 . . ? C43 C42 C47 118.0(5) . . ? C43 C42 C41 120.2(4) . . ? C47 C42 C41 121.7(4) . . ? C44 C43 C42 121.2(4) . . ? C44 C43 H43 119.4 . . ? C42 C43 H43 119.4 . . ? C45 C44 C43 119.6(5) . . ? C45 C44 H44 120.2 . . ? C43 C44 H44 120.2 . . ? C44 C45 C46 121.0(5) . . ? C44 C45 H45 119.5 . . ? C46 C45 H45 119.5 . . ? C47 C46 C45 119.5(5) . . ? C47 C46 H46 120.2 . . ? C45 C46 H46 120.2 . . ? C46 C47 C42 120.6(5) . . ? C46 C47 H47 119.7 . . ? C42 C47 H47 119.7 . . ? N2 C51 C52 115.9(3) . . ? N2 C51 H51A 108.3 . . ? C52 C51 H51A 108.3 . . ? N2 C51 H51B 108.3 . . ? C52 C51 H51B 108.3 . . ? H51A C51 H51B 107.4 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C62 C61 N2 116.5(4) . . ? C62 C61 H61A 108.2 . . ? N2 C61 H61A 108.2 . . ? C62 C61 H61B 108.2 . . ? N2 C61 H61B 108.2 . . ? H61A C61 H61B 107.3 . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C72 C71 N2 116.7(3) . . ? C72 C71 H71A 108.1 . . ? N2 C71 H71A 108.1 . . ? C72 C71 H71B 108.1 . . ? N2 C71 H71B 108.1 . . ? H71A C71 H71B 107.3 . . ? C73 C72 C77 116.9(4) . . ? C73 C72 C71 123.9(4) . . ? C77 C72 C71 118.8(4) . . ? C72 C73 C74 121.9(4) . . ? C72 C73 H73 119.1 . . ? C74 C73 H73 119.1 . . ? C75 C74 C73 120.2(4) . . ? C75 C74 H74 119.9 . . ? C73 C74 H74 119.9 . . ? C76 C75 C74 119.2(5) . . ? C76 C75 H75 120.4 . . ? C74 C75 H75 120.4 . . ? C75 C76 C77 120.2(5) . . ? C75 C76 H76 119.9 . . ? C77 C76 H76 119.9 . . ? C76 C77 C72 121.4(4) . . ? C76 C77 H77 119.3 . . ? C72 C77 H77 119.3 . . ? C82 C81 N2 114.7(4) . . ? C82 C81 H81A 108.6 . . ? N2 C81 H81A 108.6 . . ? C82 C81 H81B 108.6 . . ? N2 C81 H81B 108.6 . . ? H81A C81 H81B 107.6 . . ? C83 C82 C87 118.0(5) . . ? C83 C82 C81 121.2(4) . . ? C87 C82 C81 120.7(4) . . ? C82 C83 C84 121.5(5) . . ? C82 C83 H83 119.3 . . ? C84 C83 H83 119.3 . . ? C83 C84 C85 119.8(5) . . ? C83 C84 H84 120.1 . . ? C85 C84 H84 120.1 . . ? C86 C85 C84 119.5(5) . . ? C86 C85 H85 120.3 . . ? C84 C85 H85 120.3 . . ? C87 C86 C85 120.2(4) . . ? C87 C86 H86 119.9 . . ? C85 C86 H86 119.9 . . ? C86 C87 C82 121.0(4) . . ? C86 C87 H87 119.5 . . ? C82 C87 H87 119.5 . . ? 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 Cl2 Pd1 Cl3 Pd2 19.8(8) . . . . ? Cl1 Pd1 Cl3 Pd2 -169.46(5) . . . . ? Cl4 Pd1 Cl3 Pd2 7.99(4) . . . . ? Cl6 Pd2 Cl3 Pd1 8.4(8) . . . . ? Cl5 Pd2 Cl3 Pd1 173.98(4) . . . . ? Cl4 Pd2 Cl3 Pd1 -7.99(4) . . . . ? Cl6 Pd2 Cl4 Pd1 -170.97(4) . . . . ? Cl5 Pd2 Cl4 Pd1 43.3(8) . . . . ? Cl3 Pd2 Cl4 Pd1 7.98(4) . . . . ? Cl2 Pd1 Cl4 Pd2 172.63(4) . . . . ? Cl1 Pd1 Cl4 Pd2 33.4(7) . . . . ? Cl3 Pd1 Cl4 Pd2 -8.01(4) . . . . ? C21 N1 C11 C12 -178.4(4) . . . . ? C31 N1 C11 C12 62.9(5) . . . . ? C41 N1 C11 C12 -56.6(5) . . . . ? C11 N1 C21 C22 60.9(5) . . . . ? C31 N1 C21 C22 -178.2(4) . . . . ? C41 N1 C21 C22 -59.0(5) . . . . ? C11 N1 C31 C32 50.5(5) . . . . ? C21 N1 C31 C32 -68.2(5) . . . . ? C41 N1 C31 C32 170.3(4) . . . . ? N1 C31 C32 C33 -100.8(5) . . . . ? N1 C31 C32 C37 85.1(5) . . . . ? C37 C32 C33 C34 1.4(8) . . . . ? C31 C32 C33 C34 -173.0(5) . . . . ? C32 C33 C34 C35 -2.0(9) . . . . ? C33 C34 C35 C36 0.7(9) . . . . ? C34 C35 C36 C37 1.1(8) . . . . ? C35 C36 C37 C32 -1.7(7) . . . . ? C33 C32 C37 C36 0.4(7) . . . . ? C31 C32 C37 C36 174.7(4) . . . . ? C11 N1 C41 C42 177.1(3) . . . . ? C21 N1 C41 C42 -63.5(5) . . . . ? C31 N1 C41 C42 55.6(4) . . . . ? N1 C41 C42 C43 -95.4(5) . . . . ? N1 C41 C42 C47 88.4(5) . . . . ? C47 C42 C43 C44 -2.7(7) . . . . ? C41 C42 C43 C44 -179.0(4) . . . . ? C42 C43 C44 C45 0.9(7) . . . . ? C43 C44 C45 C46 0.6(7) . . . . ? C44 C45 C46 C47 -0.3(8) . . . . ? C45 C46 C47 C42 -1.5(8) . . . . ? C43 C42 C47 C46 3.0(7) . . . . ? C41 C42 C47 C46 179.2(4) . . . . ? C61 N2 C51 C52 178.5(4) . . . . ? C71 N2 C51 C52 -62.9(5) . . . . ? C81 N2 C51 C52 57.4(5) . . . . ? C51 N2 C61 C62 -59.2(5) . . . . ? C71 N2 C61 C62 179.3(4) . . . . ? C81 N2 C61 C62 60.5(5) . . . . ? C51 N2 C71 C72 -44.0(5) . . . . ? C61 N2 C71 C72 75.1(4) . . . . ? C81 N2 C71 C72 -164.5(3) . . . . ? N2 C71 C72 C73 -79.9(6) . . . . ? N2 C71 C72 C77 107.2(5) . . . . ? C77 C72 C73 C74 -3.5(8) . . . . ? C71 C72 C73 C74 -176.6(5) . . . . ? C72 C73 C74 C75 2.2(8) . . . . ? C73 C74 C75 C76 1.5(9) . . . . ? C74 C75 C76 C77 -3.8(9) . . . . ? C75 C76 C77 C72 2.4(10) . . . . ? C73 C72 C77 C76 1.2(8) . . . . ? C71 C72 C77 C76 174.6(5) . . . . ? C51 N2 C81 C82 179.7(3) . . . . ? C61 N2 C81 C82 60.4(5) . . . . ? C71 N2 C81 C82 -57.7(4) . . . . ? N2 C81 C82 C83 -89.0(5) . . . . ? N2 C81 C82 C87 93.7(5) . . . . ? C87 C82 C83 C84 -2.0(7) . . . . ? C81 C82 C83 C84 -179.3(4) . . . . ? C82 C83 C84 C85 1.4(8) . . . . ? C83 C84 C85 C86 -0.3(8) . . . . ? C84 C85 C86 C87 -0.1(7) . . . . ? C85 C86 C87 C82 -0.5(7) . . . . ? C83 C82 C87 C86 1.5(6) . . . . ? C81 C82 C87 C86 178.9(4) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.70 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.595 _refine_diff_density_min -0.632 _refine_diff_density_rms 0.119 data_8b _database_code_depnum_ccdc_archive 'CCDC 703944' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C18 H24 N), Cl6 Pd2' _chemical_formula_sum 'C36 H48 Cl6 N2 Pd2' _chemical_formula_weight 934.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' 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 'P 1 21/n 1' 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 17.3444(3) _cell_length_b 14.4107(4) _cell_length_c 17.3961(4) _cell_angle_alpha 90.00 _cell_angle_beta 118.5010(10) _cell_angle_gamma 90.00 _cell_volume 3821.12(15) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour 'Dark Orange' _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.624 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1888 _exptl_absorpt_coefficient_mu 1.389 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6970 _exptl_absorpt_correction_T_max 0.8510 _exptl_absorpt_process_details 'Denzo (Z. Otwinowski, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 62042 _diffrn_reflns_av_R_equivalents 0.0767 _diffrn_reflns_av_sigmaI/netI 0.0664 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.36 _diffrn_reflns_theta_max 28.69 _reflns_number_total 9865 _reflns_number_gt 6390 _reflns_threshold_expression >2\s(I) _computing_data_collection Collect _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution SHELXS-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 3.0' _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^ > 2\s(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^)+(0.0196P)^2^+3.4492P] 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 9865 _refine_ls_number_parameters 423 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0871 _refine_ls_R_factor_gt 0.0466 _refine_ls_wR_factor_ref 0.0939 _refine_ls_wR_factor_gt 0.0832 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.508249(16) 0.11734(2) 0.993949(17) 0.02731(8) Uani 1 1 d . . . Pd2 Pd 0.002756(16) 0.11759(2) 0.989334(17) 0.02880(8) Uani 1 1 d . . . Cl1 Cl 0.41586(6) 0.23872(7) 0.97203(7) 0.0418(3) Uani 1 1 d . . . Cl2 Cl 0.61727(6) 0.21608(7) 1.00880(6) 0.0392(2) Uani 1 1 d . . . Cl3 Cl 0.59752(6) -0.01123(7) 1.01506(7) 0.0361(2) Uani 1 1 d . . . Cl4 Cl -0.01699(6) 0.21577(8) 0.87850(6) 0.0407(2) Uani 1 1 d . . . Cl5 Cl 0.02467(6) 0.23982(7) 1.07985(6) 0.0434(3) Uani 1 1 d . . . Cl6 Cl -0.01925(7) -0.01253(7) 0.90169(6) 0.0389(2) Uani 1 1 d . . . N1 N 0.22889(16) 0.24158(18) 0.33307(16) 0.0198(6) Uani 1 1 d . . . N2 N 0.66378(16) 0.23645(18) 0.26787(17) 0.0195(6) Uani 1 1 d . . . C11 C 0.2853(2) 0.2584(3) 0.4290(2) 0.0273(8) Uani 1 1 d . . . H11A H 0.2633 0.3124 0.4467 0.041 Uiso 1 1 calc R . . H11B H 0.3458 0.2699 0.4414 0.041 Uiso 1 1 calc R . . H11C H 0.2837 0.2037 0.4618 0.041 Uiso 1 1 calc R . . C12 C 0.13716(19) 0.2223(2) 0.3166(2) 0.0252(8) Uani 1 1 d . . . H12A H 0.1373 0.1673 0.3498 0.038 Uiso 1 1 calc R . . H12B H 0.0991 0.2111 0.2540 0.038 Uiso 1 1 calc R . . H12C H 0.1152 0.2758 0.3351 0.038 Uiso 1 1 calc R . . C21 C 0.2318(2) 0.3244(2) 0.2798(2) 0.0215(7) Uani 1 1 d . . . H21A H 0.2936 0.3357 0.2945 0.026 Uiso 1 1 calc R . . H21B H 0.1991 0.3081 0.2170 0.026 Uiso 1 1 calc R . . C22 C 0.1941(2) 0.4133(2) 0.2941(2) 0.0210(7) Uani 1 1 d . . . C23 C 0.1091(2) 0.4399(2) 0.2339(2) 0.0263(8) Uani 1 1 d . . . H23 H 0.0744 0.4015 0.1851 0.032 Uiso 1 1 calc R . . C24 C 0.0757(2) 0.5227(2) 0.2456(2) 0.0291(8) Uani 1 1 d . . . H24 H 0.0181 0.5414 0.2043 0.035 Uiso 1 1 calc R . . C25 C 0.1255(2) 0.5784(3) 0.3169(2) 0.0296(8) Uani 1 1 d . . . H25 H 0.1011 0.6343 0.3249 0.036 Uiso 1 1 calc R . . C26 C 0.2111(2) 0.5537(2) 0.3774(2) 0.0248(8) Uani 1 1 d . . . C27 C 0.2440(2) 0.4719(2) 0.3638(2) 0.0236(7) Uani 1 1 d . . . H27 H 0.3028 0.4550 0.4034 0.028 Uiso 1 1 calc R . . C28 C 0.2654(2) 0.6156(3) 0.4548(3) 0.0380(10) Uani 1 1 d . . . H28A H 0.3086 0.5780 0.5031 0.057 Uiso 1 1 calc R . . H28B H 0.2269 0.6468 0.4735 0.057 Uiso 1 1 calc R . . H28C H 0.2958 0.6622 0.4380 0.057 Uiso 1 1 calc R . . C31 C 0.2638(2) 0.1591(2) 0.3033(2) 0.0267(8) Uani 1 1 d . . . H31A H 0.2217 0.1451 0.2415 0.032 Uiso 1 1 calc R . . H31B H 0.3199 0.1774 0.3056 0.032 Uiso 1 1 calc R . . C32 C 0.2790(2) 0.0718(2) 0.3562(2) 0.0256(8) Uani 1 1 d . . . C33 C 0.3617(2) 0.0532(3) 0.4256(2) 0.0334(9) Uani 1 1 d . . . H33 H 0.4072 0.0978 0.4423 0.040 Uiso 1 1 calc R . . C34 C 0.3780(3) -0.0306(3) 0.4706(3) 0.0401(10) Uani 1 1 d . . . H34 H 0.4350 -0.0440 0.5170 0.048 Uiso 1 1 calc R . . C35 C 0.3112(3) -0.0939(3) 0.4474(3) 0.0391(10) Uani 1 1 d . . . H35 H 0.3230 -0.1508 0.4786 0.047 Uiso 1 1 calc R . . C36 C 0.2274(3) -0.0774(3) 0.3803(2) 0.0326(9) Uani 1 1 d . . . C37 C 0.2125(2) 0.0068(2) 0.3343(2) 0.0277(8) Uani 1 1 d . . . H37 H 0.1558 0.0195 0.2873 0.033 Uiso 1 1 calc R . . C38 C 0.1540(3) -0.1444(3) 0.3567(3) 0.0485(11) Uani 1 1 d . . . H38A H 0.1689 -0.2037 0.3396 0.073 Uiso 1 1 calc R . . H38B H 0.1004 -0.1196 0.3078 0.073 Uiso 1 1 calc R . . H38C H 0.1444 -0.1540 0.4073 0.073 Uiso 1 1 calc R . . C41 C 0.5683(2) 0.2173(2) 0.2117(2) 0.0270(8) Uani 1 1 d . . . H41A H 0.5524 0.1605 0.2319 0.041 Uiso 1 1 calc R . . H41B H 0.5557 0.2094 0.1509 0.041 Uiso 1 1 calc R . . H41C H 0.5340 0.2695 0.2156 0.041 Uiso 1 1 calc R . . C42 C 0.6801(2) 0.2531(2) 0.3591(2) 0.0253(8) Uani 1 1 d . . . H42A H 0.6462 0.3071 0.3600 0.038 Uiso 1 1 calc R . . H42B H 0.7428 0.2648 0.3972 0.038 Uiso 1 1 calc R . . H42C H 0.6622 0.1984 0.3801 0.038 Uiso 1 1 calc R . . C51 C 0.7191(2) 0.1552(2) 0.2651(2) 0.0235(7) Uani 1 1 d . . . H51A H 0.7033 0.1431 0.2033 0.028 Uiso 1 1 calc R . . H51B H 0.7816 0.1737 0.2960 0.028 Uiso 1 1 calc R . . C52 C 0.7090(2) 0.0659(2) 0.3050(2) 0.0220(7) Uani 1 1 d . . . C53 C 0.7677(2) 0.0439(3) 0.3917(2) 0.0278(8) Uani 1 1 d . . . H53 H 0.8134 0.0860 0.4262 0.033 Uiso 1 1 calc R . . C54 C 0.7600(2) -0.0379(3) 0.4275(2) 0.0334(9) Uani 1 1 d . . . H54 H 0.7998 -0.0520 0.4868 0.040 Uiso 1 1 calc R . . C55 C 0.6938(2) -0.1002(2) 0.3771(2) 0.0305(9) Uani 1 1 d . . . H55 H 0.6889 -0.1569 0.4023 0.037 Uiso 1 1 calc R . . C56 C 0.6348(2) -0.0807(2) 0.2902(2) 0.0258(8) Uani 1 1 d . . . C57 C 0.6438(2) 0.0022(2) 0.2552(2) 0.0240(8) Uani 1 1 d . . . H57 H 0.6044 0.0160 0.1957 0.029 Uiso 1 1 calc R . . C58 C 0.5644(2) -0.1495(3) 0.2354(2) 0.0337(9) Uani 1 1 d . . . H58A H 0.5122 -0.1161 0.1927 0.051 Uiso 1 1 calc R . . H58B H 0.5492 -0.1869 0.2733 0.051 Uiso 1 1 calc R . . H58C H 0.5859 -0.1902 0.2046 0.051 Uiso 1 1 calc R . . C61 C 0.6923(2) 0.3199(2) 0.2336(2) 0.0267(8) Uani 1 1 d . . . H61A H 0.7548 0.3328 0.2744 0.032 Uiso 1 1 calc R . . H61B H 0.6879 0.3031 0.1764 0.032 Uiso 1 1 calc R . . C62 C 0.6409(2) 0.4074(2) 0.2222(2) 0.0259(8) Uani 1 1 d . . . C63 C 0.5707(2) 0.4300(3) 0.1419(3) 0.0352(9) Uani 1 1 d . . . H63 H 0.5521 0.3880 0.0942 0.042 Uiso 1 1 calc R . . C64 C 0.5275(3) 0.5140(3) 0.1308(3) 0.0434(11) Uani 1 1 d . . . H64 H 0.4802 0.5301 0.0753 0.052 Uiso 1 1 calc R . . C65 C 0.5531(2) 0.5736(3) 0.2001(3) 0.0456(11) Uani 1 1 d . . . H65 H 0.5227 0.6308 0.1916 0.055 Uiso 1 1 calc R . . C66 C 0.6217(2) 0.5533(3) 0.2821(3) 0.0339(9) Uani 1 1 d . . . C67 C 0.6662(2) 0.4700(2) 0.2917(2) 0.0263(8) Uani 1 1 d . . . H67 H 0.7148 0.4552 0.3468 0.032 Uiso 1 1 calc R . . C68 C 0.6503(3) 0.6177(3) 0.3586(3) 0.0498(12) Uani 1 1 d . . . H68A H 0.6869 0.5838 0.4128 0.075 Uiso 1 1 calc R . . H68B H 0.5986 0.6426 0.3603 0.075 Uiso 1 1 calc R . . H68C H 0.6842 0.6690 0.3526 0.075 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 Pd1 0.02167(15) 0.03724(18) 0.02178(14) -0.00213(12) 0.00937(12) 0.00279(12) Pd2 0.02154(15) 0.03792(18) 0.02505(15) -0.00219(12) 0.00957(12) 0.00232(12) Cl1 0.0305(5) 0.0403(6) 0.0442(6) -0.0028(5) 0.0095(4) 0.0096(4) Cl2 0.0358(5) 0.0486(7) 0.0368(5) -0.0047(4) 0.0201(4) -0.0082(4) Cl3 0.0235(5) 0.0403(6) 0.0467(6) -0.0028(4) 0.0186(4) 0.0045(4) Cl4 0.0336(5) 0.0527(7) 0.0391(6) 0.0082(5) 0.0200(5) 0.0039(4) Cl5 0.0461(6) 0.0403(6) 0.0328(5) -0.0102(4) 0.0098(5) -0.0081(5) Cl6 0.0512(6) 0.0397(6) 0.0263(5) -0.0017(4) 0.0190(5) 0.0095(4) N1 0.0224(14) 0.0184(16) 0.0217(14) 0.0005(11) 0.0130(12) 0.0001(11) N2 0.0172(13) 0.0204(16) 0.0227(14) -0.0017(11) 0.0109(12) -0.0030(11) C11 0.0296(19) 0.032(2) 0.0189(17) 0.0001(15) 0.0108(15) 0.0026(15) C12 0.0214(17) 0.027(2) 0.033(2) 0.0018(15) 0.0176(16) 0.0009(14) C21 0.0265(18) 0.0208(19) 0.0230(17) 0.0021(14) 0.0166(15) 0.0002(14) C22 0.0246(18) 0.0175(18) 0.0241(17) 0.0039(14) 0.0143(15) -0.0007(13) C23 0.0294(19) 0.023(2) 0.0262(18) 0.0020(15) 0.0128(16) -0.0026(15) C24 0.0246(19) 0.024(2) 0.036(2) 0.0049(16) 0.0123(17) 0.0034(14) C25 0.032(2) 0.019(2) 0.045(2) -0.0023(16) 0.0249(18) -0.0021(15) C26 0.0275(19) 0.023(2) 0.0274(19) -0.0013(14) 0.0157(16) -0.0024(14) C27 0.0218(17) 0.025(2) 0.0243(18) 0.0050(14) 0.0116(15) 0.0016(14) C28 0.036(2) 0.029(2) 0.045(2) -0.0148(18) 0.0160(19) -0.0032(17) C31 0.035(2) 0.021(2) 0.032(2) -0.0004(15) 0.0222(17) 0.0032(15) C32 0.036(2) 0.0172(19) 0.0317(19) -0.0026(15) 0.0223(17) 0.0060(15) C33 0.038(2) 0.028(2) 0.039(2) 0.0005(17) 0.0224(19) 0.0092(16) C34 0.043(2) 0.040(3) 0.037(2) 0.0025(19) 0.018(2) 0.016(2) C35 0.058(3) 0.032(2) 0.036(2) 0.0103(18) 0.030(2) 0.017(2) C36 0.054(2) 0.021(2) 0.039(2) -0.0059(16) 0.034(2) -0.0028(17) C37 0.037(2) 0.023(2) 0.030(2) -0.0039(15) 0.0217(18) 0.0019(15) C38 0.066(3) 0.035(3) 0.054(3) -0.003(2) 0.036(2) -0.010(2) C41 0.0210(18) 0.026(2) 0.0298(19) -0.0004(15) 0.0082(15) -0.0055(14) C42 0.0283(18) 0.026(2) 0.0247(18) -0.0022(15) 0.0154(15) 0.0037(15) C51 0.0284(18) 0.0190(19) 0.0296(19) -0.0041(14) 0.0191(16) -0.0008(14) C52 0.0275(18) 0.0175(19) 0.0275(18) 0.0003(14) 0.0185(15) 0.0047(14) C53 0.032(2) 0.025(2) 0.0272(19) -0.0031(15) 0.0154(16) 0.0016(15) C54 0.044(2) 0.026(2) 0.027(2) 0.0027(16) 0.0154(18) 0.0062(17) C55 0.048(2) 0.019(2) 0.031(2) 0.0030(15) 0.0245(18) 0.0032(16) C56 0.0303(19) 0.0194(19) 0.036(2) -0.0051(15) 0.0220(17) 0.0006(14) C57 0.0270(19) 0.024(2) 0.0223(18) 0.0005(14) 0.0127(15) 0.0061(14) C58 0.037(2) 0.024(2) 0.041(2) -0.0041(17) 0.0200(18) -0.0051(16) C61 0.0289(19) 0.023(2) 0.038(2) 0.0013(16) 0.0247(17) -0.0037(14) C62 0.0301(19) 0.0180(19) 0.039(2) 0.0022(15) 0.0237(17) -0.0032(14) C63 0.039(2) 0.024(2) 0.041(2) 0.0006(17) 0.0177(19) -0.0068(17) C64 0.034(2) 0.034(3) 0.053(3) 0.010(2) 0.013(2) -0.0001(18) C65 0.032(2) 0.027(2) 0.080(3) 0.007(2) 0.028(2) 0.0011(17) C66 0.036(2) 0.019(2) 0.059(3) -0.0046(18) 0.032(2) -0.0057(16) C67 0.0225(18) 0.022(2) 0.037(2) 0.0005(16) 0.0167(16) -0.0038(14) C68 0.056(3) 0.032(3) 0.074(3) -0.012(2) 0.041(3) -0.004(2) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 Cl1 2.2781(10) . ? Pd1 Cl2 2.2806(10) . ? Pd1 Cl3 2.3286(9) . ? Pd1 Cl3 2.3354(10) 3_657 ? Pd2 Cl5 2.2706(10) . ? Pd2 Cl4 2.2817(10) . ? Pd2 Cl6 2.3304(10) . ? Pd2 Cl6 2.3346(10) 3_557 ? Cl3 Pd1 2.3354(10) 3_657 ? Cl6 Pd2 2.3346(10) 3_557 ? N1 C11 1.498(4) . ? N1 C12 1.502(4) . ? N1 C21 1.526(4) . ? N1 C31 1.533(4) . ? N2 C42 1.493(4) . ? N2 C41 1.494(4) . ? N2 C61 1.526(4) . ? N2 C51 1.529(4) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C21 C22 1.511(5) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C27 1.390(5) . ? C22 C23 1.394(4) . ? C23 C24 1.384(5) . ? C23 H23 0.9500 . ? C24 C25 1.381(5) . ? C24 H24 0.9500 . ? C25 C26 1.395(5) . ? C25 H25 0.9500 . ? C26 C27 1.380(5) . ? C26 C28 1.512(5) . ? C27 H27 0.9500 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C31 C32 1.506(5) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C37 1.390(5) . ? C32 C33 1.391(5) . ? C33 C34 1.393(5) . ? C33 H33 0.9500 . ? C34 C35 1.375(6) . ? C34 H34 0.9500 . ? C35 C36 1.384(5) . ? C35 H35 0.9500 . ? C36 C37 1.407(5) . ? C36 C38 1.492(5) . ? C37 H37 0.9500 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C51 C52 1.511(5) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 C57 1.392(5) . ? C52 C53 1.395(5) . ? C53 C54 1.369(5) . ? C53 H53 0.9500 . ? C54 C55 1.390(5) . ? C54 H54 0.9500 . ? C55 C56 1.392(5) . ? C55 H55 0.9500 . ? C56 C57 1.383(5) . ? C56 C58 1.507(5) . ? C57 H57 0.9500 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C61 C62 1.501(5) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 C63 1.385(5) . ? C62 C67 1.401(5) . ? C63 C64 1.388(5) . ? C63 H63 0.9500 . ? C64 C65 1.371(6) . ? C64 H64 0.9500 . ? C65 C66 1.385(5) . ? C65 H65 0.9500 . ? C66 C67 1.394(5) . ? C66 C68 1.499(5) . ? C67 H67 0.9500 . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? 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 Cl1 Pd1 Cl2 91.08(4) . . ? Cl1 Pd1 Cl3 177.44(4) . . ? Cl2 Pd1 Cl3 91.47(4) . . ? Cl1 Pd1 Cl3 91.39(4) . 3_657 ? Cl2 Pd1 Cl3 176.83(4) . 3_657 ? Cl3 Pd1 Cl3 86.07(3) . 3_657 ? Cl5 Pd2 Cl4 90.74(4) . . ? Cl5 Pd2 Cl6 177.28(4) . . ? Cl4 Pd2 Cl6 91.97(4) . . ? Cl5 Pd2 Cl6 91.42(4) . 3_557 ? Cl4 Pd2 Cl6 177.58(4) . 3_557 ? Cl6 Pd2 Cl6 85.86(4) . 3_557 ? Pd1 Cl3 Pd1 93.93(3) . 3_657 ? Pd2 Cl6 Pd2 94.14(4) . 3_557 ? C11 N1 C12 108.2(3) . . ? C11 N1 C21 110.9(2) . . ? C12 N1 C21 111.6(2) . . ? C11 N1 C31 110.4(2) . . ? C12 N1 C31 110.2(3) . . ? C21 N1 C31 105.6(2) . . ? C42 N2 C41 108.3(2) . . ? C42 N2 C61 110.9(3) . . ? C41 N2 C61 110.8(2) . . ? C42 N2 C51 110.7(2) . . ? C41 N2 C51 110.8(2) . . ? C61 N2 C51 105.4(2) . . ? N1 C11 H11A 109.5 . . ? N1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N1 C12 H12A 109.5 . . ? N1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C22 C21 N1 114.9(3) . . ? C22 C21 H21A 108.5 . . ? N1 C21 H21A 108.5 . . ? C22 C21 H21B 108.5 . . ? N1 C21 H21B 108.5 . . ? H21A C21 H21B 107.5 . . ? C27 C22 C23 118.9(3) . . ? C27 C22 C21 121.3(3) . . ? C23 C22 C21 119.7(3) . . ? C24 C23 C22 119.6(3) . . ? C24 C23 H23 120.2 . . ? C22 C23 H23 120.2 . . ? C25 C24 C23 120.5(3) . . ? C25 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C24 C25 C26 120.9(3) . . ? C24 C25 H25 119.6 . . ? C26 C25 H25 119.6 . . ? C27 C26 C25 117.9(3) . . ? C27 C26 C28 121.6(3) . . ? C25 C26 C28 120.5(3) . . ? C26 C27 C22 122.2(3) . . ? C26 C27 H27 118.9 . . ? C22 C27 H27 118.9 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C32 C31 N1 115.0(3) . . ? C32 C31 H31A 108.5 . . ? N1 C31 H31A 108.5 . . ? C32 C31 H31B 108.5 . . ? N1 C31 H31B 108.5 . . ? H31A C31 H31B 107.5 . . ? C37 C32 C33 119.0(3) . . ? C37 C32 C31 121.0(3) . . ? C33 C32 C31 119.9(3) . . ? C32 C33 C34 120.3(4) . . ? C32 C33 H33 119.9 . . ? C34 C33 H33 119.9 . . ? C35 C34 C33 119.5(4) . . ? C35 C34 H34 120.2 . . ? C33 C34 H34 120.2 . . ? C34 C35 C36 122.2(4) . . ? C34 C35 H35 118.9 . . ? C36 C35 H35 118.9 . . ? C35 C36 C37 117.5(3) . . ? C35 C36 C38 122.4(4) . . ? C37 C36 C38 120.1(4) . . ? C32 C37 C36 121.4(3) . . ? C32 C37 H37 119.3 . . ? C36 C37 H37 119.3 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N2 C41 H41A 109.5 . . ? N2 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? N2 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? N2 C42 H42A 109.5 . . ? N2 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? N2 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C52 C51 N2 115.2(3) . . ? C52 C51 H51A 108.5 . . ? N2 C51 H51A 108.5 . . ? C52 C51 H51B 108.5 . . ? N2 C51 H51B 108.5 . . ? H51A C51 H51B 107.5 . . ? C57 C52 C53 118.7(3) . . ? C57 C52 C51 120.9(3) . . ? C53 C52 C51 120.4(3) . . ? C54 C53 C52 120.5(3) . . ? C54 C53 H53 119.7 . . ? C52 C53 H53 119.7 . . ? C53 C54 C55 120.0(3) . . ? C53 C54 H54 120.0 . . ? C55 C54 H54 120.0 . . ? C54 C55 C56 120.9(3) . . ? C54 C55 H55 119.6 . . ? C56 C55 H55 119.6 . . ? C57 C56 C55 118.2(3) . . ? C57 C56 C58 121.2(3) . . ? C55 C56 C58 120.6(3) . . ? C56 C57 C52 121.7(3) . . ? C56 C57 H57 119.2 . . ? C52 C57 H57 119.2 . . ? C56 C58 H58A 109.5 . . ? C56 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C56 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C62 C61 N2 115.5(3) . . ? C62 C61 H61A 108.4 . . ? N2 C61 H61A 108.4 . . ? C62 C61 H61B 108.4 . . ? N2 C61 H61B 108.4 . . ? H61A C61 H61B 107.5 . . ? C63 C62 C67 118.8(3) . . ? C63 C62 C61 120.8(3) . . ? C67 C62 C61 120.3(3) . . ? C62 C63 C64 120.1(4) . . ? C62 C63 H63 119.9 . . ? C64 C63 H63 119.9 . . ? C65 C64 C63 119.9(4) . . ? C65 C64 H64 120.1 . . ? C63 C64 H64 120.1 . . ? C64 C65 C66 122.1(4) . . ? C64 C65 H65 118.9 . . ? C66 C65 H65 118.9 . . ? C65 C66 C67 117.4(4) . . ? C65 C66 C68 122.8(4) . . ? C67 C66 C68 119.8(4) . . ? C66 C67 C62 121.6(3) . . ? C66 C67 H67 119.2 . . ? C62 C67 H67 119.2 . . ? C66 C68 H68A 109.5 . . ? C66 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C66 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? 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 Cl1 Pd1 Cl3 Pd1 -7.2(9) . . . 3_657 ? Cl2 Pd1 Cl3 Pd1 178.00(4) . . . 3_657 ? Cl3 Pd1 Cl3 Pd1 0.0 3_657 . . 3_657 ? Cl5 Pd2 Cl6 Pd2 -2.8(8) . . . 3_557 ? Cl4 Pd2 Cl6 Pd2 -178.92(4) . . . 3_557 ? Cl6 Pd2 Cl6 Pd2 0.0 3_557 . . 3_557 ? C11 N1 C21 C22 -64.4(3) . . . . ? C12 N1 C21 C22 56.3(3) . . . . ? C31 N1 C21 C22 176.0(3) . . . . ? N1 C21 C22 C27 83.6(4) . . . . ? N1 C21 C22 C23 -99.8(4) . . . . ? C27 C22 C23 C24 -1.3(5) . . . . ? C21 C22 C23 C24 -178.0(3) . . . . ? C22 C23 C24 C25 -0.8(5) . . . . ? C23 C24 C25 C26 1.6(6) . . . . ? C24 C25 C26 C27 -0.3(5) . . . . ? C24 C25 C26 C28 179.4(4) . . . . ? C25 C26 C27 C22 -1.8(5) . . . . ? C28 C26 C27 C22 178.4(3) . . . . ? C23 C22 C27 C26 2.7(5) . . . . ? C21 C22 C27 C26 179.3(3) . . . . ? C11 N1 C31 C32 51.9(4) . . . . ? C12 N1 C31 C32 -67.6(4) . . . . ? C21 N1 C31 C32 171.8(3) . . . . ? N1 C31 C32 C37 89.1(4) . . . . ? N1 C31 C32 C33 -94.1(4) . . . . ? C37 C32 C33 C34 1.9(5) . . . . ? C31 C32 C33 C34 -175.0(3) . . . . ? C32 C33 C34 C35 -1.6(6) . . . . ? C33 C34 C35 C36 0.1(6) . . . . ? C34 C35 C36 C37 1.2(6) . . . . ? C34 C35 C36 C38 -178.0(4) . . . . ? C33 C32 C37 C36 -0.5(5) . . . . ? C31 C32 C37 C36 176.3(3) . . . . ? C35 C36 C37 C32 -1.0(5) . . . . ? C38 C36 C37 C32 178.3(3) . . . . ? C42 N2 C51 C52 54.0(3) . . . . ? C41 N2 C51 C52 -66.1(4) . . . . ? C61 N2 C51 C52 174.0(3) . . . . ? N2 C51 C52 C57 87.8(4) . . . . ? N2 C51 C52 C53 -95.1(4) . . . . ? C57 C52 C53 C54 -1.4(5) . . . . ? C51 C52 C53 C54 -178.6(3) . . . . ? C52 C53 C54 C55 0.8(5) . . . . ? C53 C54 C55 C56 -0.1(6) . . . . ? C54 C55 C56 C57 0.2(5) . . . . ? C54 C55 C56 C58 178.8(3) . . . . ? C55 C56 C57 C52 -0.8(5) . . . . ? C58 C56 C57 C52 -179.5(3) . . . . ? C53 C52 C57 C56 1.4(5) . . . . ? C51 C52 C57 C56 178.6(3) . . . . ? C42 N2 C61 C62 -65.6(4) . . . . ? C41 N2 C61 C62 54.7(4) . . . . ? C51 N2 C61 C62 174.6(3) . . . . ? N2 C61 C62 C63 -95.0(4) . . . . ? N2 C61 C62 C67 88.4(4) . . . . ? C67 C62 C63 C64 0.9(5) . . . . ? C61 C62 C63 C64 -175.7(3) . . . . ? C62 C63 C64 C65 -1.5(6) . . . . ? C63 C64 C65 C66 0.2(6) . . . . ? C64 C65 C66 C67 1.6(6) . . . . ? C64 C65 C66 C68 -179.9(4) . . . . ? C65 C66 C67 C62 -2.1(5) . . . . ? C68 C66 C67 C62 179.3(3) . . . . ? C63 C62 C67 C66 0.9(5) . . . . ? C61 C62 C67 C66 177.6(3) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.69 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.456 _refine_diff_density_min -0.508 _refine_diff_density_rms 0.100 data_6 _database_code_depnum_ccdc_archive 'CCDC 703945' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C16 H20 N1), (Cl6 Pd2)' _chemical_formula_sum 'C32 H40 Cl6 N2 Pd2' _chemical_formula_weight 878.16 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' 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 'P 1 21/n 1' 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 9.2280(18) _cell_length_b 13.467(3) _cell_length_c 13.912(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.45(3) _cell_angle_gamma 90.00 _cell_volume 1710.1(6) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Plate _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.705 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 880 _exptl_absorpt_coefficient_mu 1.546 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8362 _exptl_absorpt_correction_T_max 0.9407 _exptl_absorpt_process_details 'Denzo (Z. Otwinowski, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 'Kappa APEX II' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9948 _diffrn_reflns_av_R_equivalents 0.0951 _diffrn_reflns_av_sigmaI/netI 0.1935 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.70 _diffrn_reflns_theta_max 28.70 _reflns_number_total 4388 _reflns_number_gt 2151 _reflns_threshold_expression >2\s(I) _computing_data_collection Collect _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution SHELXS-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 3.0' _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^ > 2\s(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^)+(0.0555P)^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 4388 _refine_ls_number_parameters 192 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1829 _refine_ls_R_factor_gt 0.0812 _refine_ls_wR_factor_ref 0.1696 _refine_ls_wR_factor_gt 0.1375 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _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 Pd1 Pd 0.92247(7) 0.05600(5) 0.58767(4) 0.0236(2) Uani 1 1 d . . . Cl1 Cl 0.9479(3) 0.03845(16) 0.75169(13) 0.0361(6) Uani 1 1 d . . . Cl2 Cl 0.7454(2) 0.17249(15) 0.58979(14) 0.0300(5) Uani 1 1 d . . . Cl3 Cl 0.9026(2) 0.06697(16) 0.41948(13) 0.0311(5) Uani 1 1 d . . . N1 N 0.4493(7) 0.1312(4) 0.3060(4) 0.0203(15) Uani 1 1 d . . . C11 C 0.4864(9) 0.0437(6) 0.3735(5) 0.029(2) Uani 1 1 d . . . H11A H 0.5585 0.0014 0.3482 0.043 Uiso 1 1 calc R . . H11B H 0.3974 0.0053 0.3778 0.043 Uiso 1 1 calc R . . H11C H 0.5274 0.0679 0.4383 0.043 Uiso 1 1 calc R . . C12 C 0.5819(9) 0.1913(6) 0.3045(5) 0.029(2) Uani 1 1 d . . . H12A H 0.6198 0.2129 0.3707 0.043 Uiso 1 1 calc R . . H12B H 0.5580 0.2496 0.2631 0.043 Uiso 1 1 calc R . . H12C H 0.6564 0.1515 0.2788 0.043 Uiso 1 1 calc R . . C21 C 0.3884(9) 0.0919(6) 0.2032(5) 0.025(2) Uani 1 1 d . . . H21A H 0.2900 0.0633 0.2051 0.030 Uiso 1 1 calc R . . H21B H 0.3764 0.1488 0.1576 0.030 Uiso 1 1 calc R . . C22 C 0.4815(9) 0.0150(6) 0.1640(5) 0.0234(19) Uani 1 1 d . . . C23 C 0.5974(9) 0.0391(6) 0.1171(5) 0.029(2) Uani 1 1 d . . . H23 H 0.6242 0.1068 0.1119 0.035 Uiso 1 1 calc R . . C24 C 0.6774(10) -0.0352(7) 0.0765(6) 0.039(2) Uani 1 1 d . . . H24 H 0.7596 -0.0180 0.0460 0.047 Uiso 1 1 calc R . . C25 C 0.6353(10) -0.1323(7) 0.0814(6) 0.034(2) Uani 1 1 d . . . H25 H 0.6877 -0.1829 0.0535 0.041 Uiso 1 1 calc R . . C26 C 0.5171(10) -0.1568(6) 0.1269(5) 0.031(2) Uani 1 1 d . . . H26 H 0.4875 -0.2242 0.1297 0.037 Uiso 1 1 calc R . . C27 C 0.4410(10) -0.0829(6) 0.1688(5) 0.030(2) Uani 1 1 d . . . H27 H 0.3606 -0.1003 0.2009 0.036 Uiso 1 1 calc R . . C31 C 0.3274(9) 0.1934(6) 0.3386(5) 0.029(2) Uani 1 1 d . . . H31A H 0.3094 0.2520 0.2955 0.035 Uiso 1 1 calc R . . H31B H 0.2363 0.1535 0.3310 0.035 Uiso 1 1 calc R . . C32 C 0.3608(9) 0.2288(6) 0.4431(5) 0.0221(18) Uani 1 1 d . . . C33 C 0.3062(9) 0.1761(7) 0.5164(6) 0.030(2) Uani 1 1 d . . . H33 H 0.2514 0.1170 0.5013 0.036 Uiso 1 1 calc R . . C34 C 0.3321(10) 0.2104(7) 0.6111(6) 0.033(2) Uani 1 1 d . . . H34 H 0.2946 0.1742 0.6607 0.039 Uiso 1 1 calc R . . C35 C 0.4107(9) 0.2952(7) 0.6349(5) 0.028(2) Uani 1 1 d . . . H35 H 0.4288 0.3173 0.7004 0.033 Uiso 1 1 calc R . . C36 C 0.4633(10) 0.3482(6) 0.5625(6) 0.032(2) Uani 1 1 d . . . H36 H 0.5185 0.4070 0.5783 0.039 Uiso 1 1 calc R . . C37 C 0.4363(9) 0.3164(6) 0.4675(6) 0.028(2) Uani 1 1 d . . . H37 H 0.4698 0.3550 0.4181 0.033 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 Pd1 0.0255(4) 0.0195(3) 0.0246(3) 0.0020(3) -0.0003(2) 0.0005(3) Cl1 0.0481(16) 0.0357(14) 0.0236(10) 0.0021(10) 0.0026(9) 0.0019(12) Cl2 0.0357(14) 0.0213(11) 0.0332(11) -0.0007(9) 0.0052(9) 0.0051(10) Cl3 0.0335(13) 0.0317(12) 0.0266(10) 0.0046(10) -0.0005(8) 0.0122(11) N1 0.025(4) 0.011(3) 0.023(3) 0.004(3) -0.002(3) 0.004(3) C11 0.033(5) 0.020(5) 0.029(4) 0.001(4) -0.007(4) 0.003(4) C12 0.027(5) 0.031(5) 0.028(4) -0.004(4) 0.001(4) 0.004(4) C21 0.032(5) 0.019(4) 0.019(4) -0.004(4) -0.013(3) -0.007(4) C22 0.019(5) 0.025(5) 0.022(4) -0.002(4) -0.007(3) -0.002(4) C23 0.028(5) 0.028(5) 0.028(4) -0.006(4) -0.010(4) -0.010(4) C24 0.020(5) 0.061(7) 0.034(5) -0.007(5) -0.002(4) -0.003(5) C25 0.040(6) 0.036(6) 0.022(4) -0.009(4) -0.010(4) 0.012(5) C26 0.044(6) 0.016(4) 0.028(5) 0.001(4) -0.006(4) -0.001(4) C27 0.047(6) 0.019(5) 0.026(4) -0.006(4) 0.007(4) -0.004(4) C31 0.028(5) 0.024(5) 0.033(5) -0.005(4) -0.006(4) 0.004(4) C32 0.021(5) 0.019(4) 0.026(4) 0.001(4) 0.000(3) 0.009(4) C33 0.019(5) 0.030(5) 0.039(5) 0.002(4) -0.001(4) 0.010(4) C34 0.036(6) 0.036(6) 0.026(4) 0.005(4) 0.004(4) 0.008(5) C35 0.031(5) 0.035(5) 0.017(4) -0.003(4) 0.003(3) 0.009(4) C36 0.035(6) 0.023(5) 0.035(5) -0.020(4) -0.004(4) 0.001(4) C37 0.039(6) 0.010(4) 0.034(5) -0.003(4) 0.005(4) 0.002(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 Cl2 2.268(2) . ? Pd1 Cl1 2.272(2) . ? Pd1 Cl3 2.325(2) . ? Pd1 Cl3 2.325(2) 3_756 ? Cl3 Pd1 2.325(2) 3_756 ? N1 C12 1.470(10) . ? N1 C11 1.514(9) . ? N1 C31 1.525(10) . ? N1 C21 1.551(8) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C21 C22 1.499(11) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.372(11) . ? C22 C27 1.375(11) . ? C23 C24 1.409(12) . ? C23 H23 0.9500 . ? C24 C25 1.369(12) . ? C24 H24 0.9500 . ? C25 C26 1.379(12) . ? C25 H25 0.9500 . ? C26 C27 1.394(11) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C31 C32 1.517(10) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C37 1.387(11) . ? C32 C33 1.395(11) . ? C33 C34 1.383(11) . ? C33 H33 0.9500 . ? C34 C35 1.367(12) . ? C34 H34 0.9500 . ? C35 C36 1.380(12) . ? C35 H35 0.9500 . ? C36 C37 1.376(10) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? 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 Cl2 Pd1 Cl1 91.56(8) . . ? Cl2 Pd1 Cl3 91.07(8) . . ? Cl1 Pd1 Cl3 177.28(8) . . ? Cl2 Pd1 Cl3 177.59(8) . 3_756 ? Cl1 Pd1 Cl3 89.95(8) . 3_756 ? Cl3 Pd1 Cl3 87.40(7) . 3_756 ? Pd1 Cl3 Pd1 92.60(7) . 3_756 ? C12 N1 C11 108.9(6) . . ? C12 N1 C31 110.7(6) . . ? C11 N1 C31 110.6(6) . . ? C12 N1 C21 111.4(6) . . ? C11 N1 C21 109.0(6) . . ? C31 N1 C21 106.2(6) . . ? N1 C11 H11A 109.5 . . ? N1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N1 C12 H12A 109.5 . . ? N1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C22 C21 N1 115.0(6) . . ? C22 C21 H21A 108.5 . . ? N1 C21 H21A 108.5 . . ? C22 C21 H21B 108.5 . . ? N1 C21 H21B 108.5 . . ? H21A C21 H21B 107.5 . . ? C23 C22 C27 119.2(8) . . ? C23 C22 C21 122.6(8) . . ? C27 C22 C21 118.1(8) . . ? C22 C23 C24 120.9(8) . . ? C22 C23 H23 119.6 . . ? C24 C23 H23 119.6 . . ? C25 C24 C23 119.3(9) . . ? C25 C24 H24 120.4 . . ? C23 C24 H24 120.4 . . ? C24 C25 C26 120.0(9) . . ? C24 C25 H25 120.0 . . ? C26 C25 H25 120.0 . . ? C25 C26 C27 120.2(8) . . ? C25 C26 H26 119.9 . . ? C27 C26 H26 119.9 . . ? C22 C27 C26 120.4(8) . . ? C22 C27 H27 119.8 . . ? C26 C27 H27 119.8 . . ? C32 C31 N1 113.8(6) . . ? C32 C31 H31A 108.8 . . ? N1 C31 H31A 108.8 . . ? C32 C31 H31B 108.8 . . ? N1 C31 H31B 108.8 . . ? H31A C31 H31B 107.7 . . ? C37 C32 C33 118.4(7) . . ? C37 C32 C31 121.7(7) . . ? C33 C32 C31 119.7(8) . . ? C34 C33 C32 119.7(8) . . ? C34 C33 H33 120.1 . . ? C32 C33 H33 120.1 . . ? C35 C34 C33 121.3(8) . . ? C35 C34 H34 119.3 . . ? C33 C34 H34 119.3 . . ? C34 C35 C36 119.1(7) . . ? C34 C35 H35 120.4 . . ? C36 C35 H35 120.4 . . ? C37 C36 C35 120.4(8) . . ? C37 C36 H36 119.8 . . ? C35 C36 H36 119.8 . . ? C36 C37 C32 120.9(8) . . ? C36 C37 H37 119.5 . . ? C32 C37 H37 119.5 . . ? 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 Cl2 Pd1 Cl3 Pd1 -178.14(8) . . . 3_756 ? Cl1 Pd1 Cl3 Pd1 -13.2(19) . . . 3_756 ? Cl3 Pd1 Cl3 Pd1 0.0 3_756 . . 3_756 ? C12 N1 C21 C22 69.1(8) . . . . ? C11 N1 C21 C22 -51.1(9) . . . . ? C31 N1 C21 C22 -170.3(7) . . . . ? N1 C21 C22 C23 -84.6(9) . . . . ? N1 C21 C22 C27 100.7(9) . . . . ? C27 C22 C23 C24 -1.8(12) . . . . ? C21 C22 C23 C24 -176.5(7) . . . . ? C22 C23 C24 C25 2.1(12) . . . . ? C23 C24 C25 C26 -0.8(12) . . . . ? C24 C25 C26 C27 -0.7(12) . . . . ? C23 C22 C27 C26 0.3(12) . . . . ? C21 C22 C27 C26 175.2(7) . . . . ? C25 C26 C27 C22 1.0(12) . . . . ? C12 N1 C31 C32 -65.5(8) . . . . ? C11 N1 C31 C32 55.3(9) . . . . ? C21 N1 C31 C32 173.4(7) . . . . ? N1 C31 C32 C37 87.2(9) . . . . ? N1 C31 C32 C33 -97.3(9) . . . . ? C37 C32 C33 C34 -2.0(11) . . . . ? C31 C32 C33 C34 -177.7(7) . . . . ? C32 C33 C34 C35 0.0(12) . . . . ? C33 C34 C35 C36 0.9(13) . . . . ? C34 C35 C36 C37 0.4(13) . . . . ? C35 C36 C37 C32 -2.5(12) . . . . ? C33 C32 C37 C36 3.3(12) . . . . ? C31 C32 C37 C36 178.8(7) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 28.70 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 2.166 _refine_diff_density_min -0.912 _refine_diff_density_rms 0.195 data_3 _database_code_depnum_ccdc_archive 'CCDC 703946' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C18 H24 N), Cl4 Pd' _chemical_formula_sum 'C36 H48 Cl4 N2 Pd' _chemical_formula_weight 756.96 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' 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 'P 1 21/c 1' 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 11.223(2) _cell_length_b 10.657(2) _cell_length_c 15.065(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.66(3) _cell_angle_gamma 90.00 _cell_volume 1798.2(6) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Orange _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.398 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 784 _exptl_absorpt_coefficient_mu 0.840 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8635 _exptl_absorpt_correction_T_max 0.9059 _exptl_absorpt_process_details 'Denzo (Z. Otwinowski, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 'Kappa APEX II' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13994 _diffrn_reflns_av_R_equivalents 0.0761 _diffrn_reflns_av_sigmaI/netI 0.1234 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 28.74 _reflns_number_total 4648 _reflns_number_gt 2293 _reflns_threshold_expression >2\s(I) _computing_data_collection Collect _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution SHELXS-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 3.0' _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^)+(0.0685P)^2^+0.5191P] 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 4648 _refine_ls_number_parameters 205 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1612 _refine_ls_R_factor_gt 0.0671 _refine_ls_wR_factor_ref 0.1719 _refine_ls_wR_factor_gt 0.1406 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _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 Pd1 Pd 0.5000 0.0000 0.0000 0.0446(2) Uani 1 2 d S . . Cl1 Cl 0.32803(14) 0.01574(14) 0.07425(8) 0.0540(4) Uani 1 1 d . . . Cl2 Cl 0.60500(14) 0.08951(14) 0.11983(8) 0.0535(4) Uani 1 1 d . . . N1 N 0.5510(3) -0.3400(4) 0.1470(2) 0.0304(9) Uani 1 1 d . . . C33 C 0.2833(5) -0.4869(5) 0.1442(3) 0.0379(12) Uani 1 1 d . . . H33 H 0.3114 -0.5151 0.2016 0.045 Uiso 1 1 calc R . . C37 C 0.2826(4) -0.3356(5) 0.0267(3) 0.0316(11) Uani 1 1 d . . . H37 H 0.3120 -0.2600 0.0027 0.038 Uiso 1 1 calc R . . C31 C 0.4235(4) -0.3014(5) 0.1604(3) 0.0327(11) Uani 1 1 d . . . H31A H 0.4098 -0.3080 0.2245 0.039 Uiso 1 1 calc R . . H31B H 0.4137 -0.2121 0.1433 0.039 Uiso 1 1 calc R . . C36 C 0.1943(5) -0.4015(5) -0.0220(3) 0.0369(12) Uani 1 1 d . . . C32 C 0.3297(4) -0.3763(5) 0.1094(3) 0.0303(11) Uani 1 1 d . . . C21 C 0.6308(4) -0.2500(5) 0.2033(3) 0.0385(13) Uani 1 1 d . . . H21A H 0.6064 -0.1629 0.1881 0.046 Uiso 1 1 calc R . . H21B H 0.6162 -0.2636 0.2667 0.046 Uiso 1 1 calc R . . C35 C 0.1550(5) -0.5124(5) 0.0129(4) 0.0415(13) Uani 1 1 d . . . H35 H 0.0974 -0.5609 -0.0210 0.050 Uiso 1 1 calc R . . C23 C 0.8322(5) -0.3414(6) 0.2468(4) 0.0495(15) Uani 1 1 d . A . H23 H 0.7975 -0.3904 0.2911 0.059 Uiso 1 1 calc R . . C34 C 0.1969(5) -0.5552(5) 0.0955(4) 0.0422(13) Uani 1 1 d . . . H34 H 0.1667 -0.6308 0.1188 0.051 Uiso 1 1 calc R . . C11 C 0.5757(4) -0.3279(5) 0.0511(3) 0.0359(12) Uani 1 1 d . . . H11A H 0.6579 -0.3541 0.0428 0.054 Uiso 1 1 calc R . . H11B H 0.5650 -0.2404 0.0324 0.054 Uiso 1 1 calc R . . H11C H 0.5203 -0.3814 0.0152 0.054 Uiso 1 1 calc R . . C12 C 0.5741(5) -0.4710(5) 0.1767(3) 0.0370(13) Uani 1 1 d . . . H12A H 0.5210 -0.5280 0.1418 0.056 Uiso 1 1 calc R . . H12B H 0.5591 -0.4787 0.2399 0.056 Uiso 1 1 calc R . . H12C H 0.6573 -0.4929 0.1680 0.056 Uiso 1 1 calc R . . C22 C 0.7627(5) -0.2621(5) 0.1926(4) 0.0445(14) Uani 1 1 d . . . C27 C 0.8167(5) -0.1900(6) 0.1307(4) 0.0520(15) Uani 1 1 d . A . H27 H 0.7692 -0.1340 0.0944 0.062 Uiso 1 1 calc R . . C38 C 0.1421(5) -0.3504(6) -0.1091(3) 0.0516(15) Uani 1 1 d . . . H38A H 0.0708 -0.3007 -0.0988 0.077 Uiso 1 1 calc R . . H38B H 0.1202 -0.4201 -0.1494 0.077 Uiso 1 1 calc R . . H38C H 0.2012 -0.2972 -0.1360 0.077 Uiso 1 1 calc R . . C25 C 1.0061(5) -0.2763(6) 0.1723(4) 0.0578(17) Uani 1 1 d . A . H25 H 1.0894 -0.2823 0.1652 0.069 Uiso 1 1 calc R . . C24 C 0.9553(6) -0.3479(6) 0.2351(4) 0.0610(18) Uani 1 1 d . . . H24 H 1.0040 -0.4030 0.2713 0.073 Uiso 0.670(10) 1 calc PR A 1 C26 C 0.9382(6) -0.1968(7) 0.1200(4) 0.0627(17) Uani 1 1 d . . . H26 H 0.9735 -0.1466 0.0766 0.075 Uiso 0.330(10) 1 calc PR A 2 C28A C 0.9950(9) -0.1223(10) 0.0587(7) 0.075(3) Uani 0.670(10) 1 d P A 1 H28A H 1.0810 -0.1202 0.0746 0.112 Uiso 0.670(10) 1 calc PR A 1 H28B H 0.9628 -0.0369 0.0596 0.112 Uiso 0.670(10) 1 calc PR A 1 H28C H 0.9808 -0.1578 -0.0011 0.112 Uiso 0.670(10) 1 calc PR A 1 C28B C 1.0263(18) -0.428(2) 0.2854(14) 0.075(3) Uani 0.330(10) 1 d P A 2 H28D H 1.0194 -0.5125 0.2605 0.112 Uiso 0.330(10) 1 calc PR A 2 H28E H 1.0012 -0.4283 0.3465 0.112 Uiso 0.330(10) 1 calc PR A 2 H28F H 1.1095 -0.3997 0.2854 0.112 Uiso 0.330(10) 1 calc PR A 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 Pd1 0.0644(5) 0.0429(4) 0.0261(3) 0.0028(3) 0.0012(2) -0.0067(3) Cl1 0.0625(10) 0.0645(10) 0.0355(6) 0.0012(7) 0.0067(6) -0.0023(8) Cl2 0.0731(11) 0.0605(9) 0.0265(6) -0.0020(6) -0.0009(6) -0.0178(8) N1 0.030(2) 0.036(2) 0.0248(18) -0.0060(18) -0.0004(16) -0.0012(19) C33 0.037(3) 0.038(3) 0.038(2) 0.005(2) 0.000(2) 0.008(3) C37 0.030(3) 0.032(3) 0.032(2) 0.004(2) -0.002(2) 0.003(2) C31 0.031(3) 0.041(3) 0.026(2) -0.003(2) 0.000(2) 0.002(2) C36 0.030(3) 0.044(3) 0.036(2) -0.003(2) -0.005(2) 0.006(3) C32 0.022(3) 0.037(3) 0.032(2) -0.005(2) 0.000(2) 0.005(2) C21 0.030(3) 0.045(3) 0.040(3) -0.017(2) -0.005(2) -0.006(3) C35 0.026(3) 0.041(3) 0.057(3) -0.008(3) -0.003(2) -0.004(3) C23 0.036(4) 0.061(4) 0.051(3) -0.017(3) -0.007(3) -0.007(3) C34 0.030(3) 0.037(3) 0.059(3) 0.008(3) 0.003(3) -0.002(3) C11 0.038(3) 0.040(3) 0.030(2) -0.006(2) 0.002(2) -0.006(3) C12 0.035(3) 0.044(3) 0.032(2) -0.007(2) -0.005(2) 0.001(2) C22 0.032(3) 0.048(3) 0.052(3) -0.023(3) -0.007(3) -0.004(3) C27 0.040(4) 0.054(4) 0.062(3) -0.012(3) 0.000(3) 0.000(3) C38 0.052(4) 0.055(4) 0.046(3) 0.002(3) -0.015(3) 0.003(3) C25 0.029(4) 0.073(4) 0.072(4) -0.023(4) 0.006(3) -0.019(3) C24 0.043(4) 0.069(4) 0.067(4) -0.034(4) -0.025(3) 0.012(4) C26 0.041(4) 0.075(5) 0.072(4) -0.003(4) 0.004(3) -0.004(4) C28A 0.042(6) 0.091(7) 0.093(7) 0.006(6) 0.018(5) -0.019(5) C28B 0.042(6) 0.091(7) 0.093(7) 0.006(6) 0.018(5) -0.019(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 Pd1 Cl1 2.2978(15) . ? Pd1 Cl1 2.2978(16) 3_655 ? Pd1 Cl2 2.2991(14) . ? Pd1 Cl2 2.2991(14) 3_655 ? N1 C12 1.484(6) . ? N1 C11 1.495(5) . ? N1 C31 1.515(6) . ? N1 C21 1.532(6) . ? C33 C34 1.385(7) . ? C33 C32 1.404(7) . ? C33 H33 0.9500 . ? C37 C36 1.386(7) . ? C37 C32 1.391(6) . ? C37 H37 0.9500 . ? C31 C32 1.494(6) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C36 C35 1.377(7) . ? C36 C38 1.505(7) . ? C21 C22 1.505(7) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C35 C34 1.380(7) . ? C35 H35 0.9500 . ? C23 C22 1.380(8) . ? C23 C24 1.407(8) . ? C23 H23 0.9500 . ? C34 H34 0.9500 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C22 C27 1.378(8) . ? C27 C26 1.385(8) . ? C27 H27 0.9500 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C25 C26 1.358(9) . ? C25 C24 1.367(8) . ? C25 H25 0.9500 . ? C24 C28B 1.36(2) . ? C24 H24 0.9500 . ? C26 C28A 1.401(11) . ? C26 H26 0.9500 . ? C28A H28A 0.9800 . ? C28A H28B 0.9800 . ? C28A H28C 0.9800 . ? C28B H28D 0.9800 . ? C28B H28E 0.9800 . ? C28B H28F 0.9800 . ? 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 Cl1 Pd1 Cl1 180.00(5) . 3_655 ? Cl1 Pd1 Cl2 89.53(5) . . ? Cl1 Pd1 Cl2 90.47(5) 3_655 . ? Cl1 Pd1 Cl2 90.47(5) . 3_655 ? Cl1 Pd1 Cl2 89.53(5) 3_655 3_655 ? Cl2 Pd1 Cl2 180.00(4) . 3_655 ? C12 N1 C11 109.5(4) . . ? C12 N1 C31 111.3(4) . . ? C11 N1 C31 109.9(3) . . ? C12 N1 C21 109.7(4) . . ? C11 N1 C21 110.1(4) . . ? C31 N1 C21 106.3(3) . . ? C34 C33 C32 120.4(5) . . ? C34 C33 H33 119.8 . . ? C32 C33 H33 119.8 . . ? C36 C37 C32 122.2(4) . . ? C36 C37 H37 118.9 . . ? C32 C37 H37 118.9 . . ? C32 C31 N1 115.2(4) . . ? C32 C31 H31A 108.5 . . ? N1 C31 H31A 108.5 . . ? C32 C31 H31B 108.5 . . ? N1 C31 H31B 108.5 . . ? H31A C31 H31B 107.5 . . ? C35 C36 C37 118.0(4) . . ? C35 C36 C38 121.8(5) . . ? C37 C36 C38 120.2(5) . . ? C37 C32 C33 117.9(4) . . ? C37 C32 C31 120.6(4) . . ? C33 C32 C31 121.5(4) . . ? C22 C21 N1 115.6(4) . . ? C22 C21 H21A 108.4 . . ? N1 C21 H21A 108.4 . . ? C22 C21 H21B 108.4 . . ? N1 C21 H21B 108.4 . . ? H21A C21 H21B 107.5 . . ? C36 C35 C34 121.9(5) . . ? C36 C35 H35 119.1 . . ? C34 C35 H35 119.1 . . ? C22 C23 C24 118.6(6) . . ? C22 C23 H23 120.7 . . ? C24 C23 H23 120.7 . . ? C35 C34 C33 119.5(5) . . ? C35 C34 H34 120.3 . . ? C33 C34 H34 120.3 . . ? N1 C11 H11A 109.5 . . ? N1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N1 C12 H12A 109.5 . . ? N1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C27 C22 C23 119.1(5) . . ? C27 C22 C21 120.2(5) . . ? C23 C22 C21 120.7(5) . . ? C22 C27 C26 121.9(6) . . ? C22 C27 H27 119.0 . . ? C26 C27 H27 119.0 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C26 C25 C24 120.5(6) . . ? C26 C25 H25 119.8 . . ? C24 C25 H25 119.8 . . ? C28B C24 C25 118.6(10) . . ? C28B C24 C23 120.4(11) . . ? C25 C24 C23 121.0(6) . . ? C28B C24 H24 1.3 . . ? C25 C24 H24 119.5 . . ? C23 C24 H24 119.5 . . ? C25 C26 C27 119.0(6) . . ? C25 C26 C28A 118.3(7) . . ? C27 C26 C28A 122.7(8) . . ? C25 C26 H26 120.5 . . ? C27 C26 H26 120.5 . . ? C28A C26 H26 2.6 . . ? C26 C28A H28A 109.5 . . ? C26 C28A H28B 109.5 . . ? C26 C28A H28C 109.5 . . ? C24 C28B H28D 109.5 . . ? C24 C28B H28E 109.5 . . ? H28D C28B H28E 109.5 . . ? C24 C28B H28F 109.5 . . ? H28D C28B H28F 109.5 . . ? H28E C28B H28F 109.5 . . ? 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 C12 N1 C31 C32 -61.7(5) . . . . ? C11 N1 C31 C32 59.7(5) . . . . ? C21 N1 C31 C32 178.8(4) . . . . ? C32 C37 C36 C35 -1.6(7) . . . . ? C32 C37 C36 C38 177.1(4) . . . . ? C36 C37 C32 C33 -1.2(7) . . . . ? C36 C37 C32 C31 -179.0(4) . . . . ? C34 C33 C32 C37 2.6(7) . . . . ? C34 C33 C32 C31 -179.7(4) . . . . ? N1 C31 C32 C37 -94.2(5) . . . . ? N1 C31 C32 C33 88.2(5) . . . . ? C12 N1 C21 C22 65.8(5) . . . . ? C11 N1 C21 C22 -54.8(6) . . . . ? C31 N1 C21 C22 -173.7(4) . . . . ? C37 C36 C35 C34 3.2(8) . . . . ? C38 C36 C35 C34 -175.5(5) . . . . ? C36 C35 C34 C33 -1.8(8) . . . . ? C32 C33 C34 C35 -1.2(8) . . . . ? C24 C23 C22 C27 -1.7(8) . . . . ? C24 C23 C22 C21 -179.0(5) . . . . ? N1 C21 C22 C27 91.8(6) . . . . ? N1 C21 C22 C23 -90.9(6) . . . . ? C23 C22 C27 C26 1.5(8) . . . . ? C21 C22 C27 C26 178.8(5) . . . . ? C26 C25 C24 C28B 179.1(12) . . . . ? C26 C25 C24 C23 0.2(9) . . . . ? C22 C23 C24 C28B -178.0(12) . . . . ? C22 C23 C24 C25 0.9(8) . . . . ? C24 C25 C26 C27 -0.5(9) . . . . ? C24 C25 C26 C28A 177.9(7) . . . . ? C22 C27 C26 C25 -0.4(9) . . . . ? C22 C27 C26 C28A -178.7(7) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.74 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.466 _refine_diff_density_min -0.537 _refine_diff_density_rms 0.098 data_1b _database_code_depnum_ccdc_archive 'CCDC 703947' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C16 H20 N), Cl4 Pd' _chemical_formula_sum 'C32 H40 Cl4 N2 Pd' _chemical_formula_weight 700.86 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' 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 triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.6420(17) _cell_length_b 10.201(2) _cell_length_c 10.998(2) _cell_angle_alpha 63.85(3) _cell_angle_beta 82.50(3) _cell_angle_gamma 65.19(3) _cell_volume 788.3(3) _cell_formula_units_Z 1 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.476 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 360 _exptl_absorpt_coefficient_mu 0.952 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7504 _exptl_absorpt_correction_T_max 0.8037 _exptl_absorpt_process_details 'Denzo (Z. Otwinowski, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 'Kappa APEX II' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11388 _diffrn_reflns_av_R_equivalents 0.0415 _diffrn_reflns_av_sigmaI/netI 0.0581 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 28.78 _reflns_number_total 4087 _reflns_number_gt 3483 _reflns_threshold_expression >2\s(I) _computing_data_collection Collect _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution SHELXS-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 3.0' _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^)+(0.0218P)^2^+0.4361P] 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 4087 _refine_ls_number_parameters 180 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0481 _refine_ls_R_factor_gt 0.0380 _refine_ls_wR_factor_ref 0.0816 _refine_ls_wR_factor_gt 0.0778 _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 Pd1 Pd 1.0000 0.5000 0.5000 0.02042(8) Uani 1 2 d S . . Cl2 Cl 1.19423(8) 0.23638(7) 0.57795(7) 0.02873(15) Uani 1 1 d . . . Cl1 Cl 0.83225(8) 0.43826(8) 0.68070(7) 0.02923(15) Uani 1 1 d . . . N1 N 0.6948(3) 0.1624(2) 0.5834(2) 0.0223(4) Uani 1 1 d . . . C31 C 0.5944(3) 0.1849(3) 0.7039(3) 0.0252(5) Uani 1 1 d . . . H31A H 0.5987 0.2773 0.7100 0.030 Uiso 1 1 calc R . . H31B H 0.4732 0.2108 0.6862 0.030 Uiso 1 1 calc R . . C12 C 0.8813(3) 0.1059(3) 0.6141(3) 0.0255(5) Uani 1 1 d . . . H12A H 0.9237 -0.0015 0.6891 0.038 Uiso 1 1 calc R . . H12B H 0.8993 0.1792 0.6398 0.038 Uiso 1 1 calc R . . H12C H 0.9432 0.1028 0.5334 0.038 Uiso 1 1 calc R . . C21 C 0.6283(3) 0.3265(3) 0.4622(3) 0.0258(5) Uani 1 1 d . . . H21A H 0.5025 0.3671 0.4517 0.031 Uiso 1 1 calc R . . H21B H 0.6541 0.4008 0.4827 0.031 Uiso 1 1 calc R . . C22 C 0.7005(3) 0.3298(3) 0.3291(3) 0.0271(6) Uani 1 1 d . . . C32 C 0.6595(3) 0.0418(3) 0.8377(3) 0.0255(5) Uani 1 1 d . . . C11 C 0.6653(4) 0.0439(3) 0.5552(3) 0.0299(6) Uani 1 1 d . . . H11A H 0.7236 0.0362 0.4744 0.045 Uiso 1 1 calc R . . H11B H 0.5425 0.0788 0.5393 0.045 Uiso 1 1 calc R . . H11C H 0.7104 -0.0609 0.6332 0.045 Uiso 1 1 calc R . . C34 C 0.6704(4) -0.2145(3) 1.0044(3) 0.0332(6) Uani 1 1 d . . . H34 H 0.6385 -0.3014 1.0310 0.040 Uiso 1 1 calc R . . C37 C 0.7674(3) 0.0364(3) 0.9260(3) 0.0296(6) Uani 1 1 d . . . H37 H 0.8011 0.1221 0.8995 0.036 Uiso 1 1 calc R . . C36 C 0.8252(4) -0.0924(4) 1.0510(3) 0.0340(6) Uani 1 1 d . . . H36 H 0.8973 -0.0943 1.1106 0.041 Uiso 1 1 calc R . . C25 C 0.8274(4) 0.3415(3) 0.0795(3) 0.0407(7) Uani 1 1 d . . . H25 H 0.8717 0.3440 -0.0049 0.049 Uiso 1 1 calc R . . C35 C 0.7782(3) -0.2192(4) 1.0899(3) 0.0333(6) Uani 1 1 d . . . H35 H 0.8200 -0.3089 1.1752 0.040 Uiso 1 1 calc R . . C23 C 0.8512(4) 0.3510(3) 0.2897(3) 0.0306(6) Uani 1 1 d . . . H23 H 0.9116 0.3618 0.3485 0.037 Uiso 1 1 calc R . . C33 C 0.6083(3) -0.0839(3) 0.8799(3) 0.0294(6) Uani 1 1 d . . . H33 H 0.5308 -0.0799 0.8232 0.035 Uiso 1 1 calc R . . C24 C 0.9141(4) 0.3564(3) 0.1664(3) 0.0366(7) Uani 1 1 d . . . H24 H 1.0174 0.3705 0.1412 0.044 Uiso 1 1 calc R . . C27 C 0.6117(4) 0.3174(4) 0.2393(3) 0.0367(7) Uani 1 1 d . . . H27 H 0.5073 0.3052 0.2633 0.044 Uiso 1 1 calc R . . C26 C 0.6760(4) 0.3228(4) 0.1157(3) 0.0422(8) Uani 1 1 d . . . H26 H 0.6158 0.3137 0.0556 0.051 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 Pd1 0.01427(13) 0.02465(15) 0.02754(16) -0.01636(12) 0.00053(10) -0.00678(11) Cl2 0.0184(3) 0.0266(3) 0.0420(4) -0.0182(3) 0.0004(3) -0.0057(3) Cl1 0.0230(3) 0.0333(3) 0.0322(4) -0.0168(3) 0.0054(3) -0.0103(3) N1 0.0161(10) 0.0249(11) 0.0309(12) -0.0188(10) 0.0028(8) -0.0058(8) C31 0.0162(12) 0.0330(14) 0.0346(15) -0.0239(12) 0.0065(10) -0.0085(11) C12 0.0150(12) 0.0294(13) 0.0318(14) -0.0156(12) 0.0034(10) -0.0068(10) C21 0.0214(13) 0.0245(13) 0.0301(14) -0.0161(11) -0.0013(10) -0.0025(10) C22 0.0247(13) 0.0234(13) 0.0290(14) -0.0145(11) -0.0039(11) -0.0009(11) C32 0.0171(12) 0.0320(14) 0.0313(14) -0.0197(12) 0.0053(10) -0.0080(10) C11 0.0289(14) 0.0360(15) 0.0407(16) -0.0290(14) 0.0064(12) -0.0152(12) C34 0.0261(14) 0.0366(15) 0.0408(17) -0.0204(14) 0.0079(12) -0.0139(12) C37 0.0212(13) 0.0399(16) 0.0365(16) -0.0231(13) 0.0062(11) -0.0142(12) C36 0.0230(14) 0.0502(18) 0.0317(15) -0.0213(14) 0.0014(11) -0.0134(13) C25 0.0466(19) 0.0364(16) 0.0329(16) -0.0199(14) 0.0061(14) -0.0071(14) C35 0.0239(14) 0.0397(16) 0.0332(15) -0.0167(13) 0.0046(12) -0.0099(12) C23 0.0293(15) 0.0286(14) 0.0353(16) -0.0151(13) -0.0023(12) -0.0102(12) C33 0.0218(13) 0.0402(16) 0.0356(15) -0.0244(13) 0.0055(11) -0.0131(12) C24 0.0300(15) 0.0317(15) 0.0373(17) -0.0098(13) 0.0039(13) -0.0088(12) C27 0.0301(15) 0.0482(18) 0.0373(16) -0.0237(15) 0.0006(12) -0.0146(14) C26 0.0449(19) 0.0541(19) 0.0369(17) -0.0296(16) -0.0010(14) -0.0166(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 Cl2 2.3108(13) 2_766 ? Pd1 Cl2 2.3108(13) . ? Pd1 Cl1 2.3150(10) . ? Pd1 Cl1 2.3150(10) 2_766 ? N1 C11 1.494(3) . ? N1 C12 1.494(3) . ? N1 C21 1.528(3) . ? N1 C31 1.537(3) . ? C31 C32 1.499(4) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C21 C22 1.507(3) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.391(4) . ? C22 C27 1.404(4) . ? C32 C33 1.398(4) . ? C32 C37 1.400(4) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C34 C35 1.381(4) . ? C34 C33 1.386(4) . ? C34 H34 0.9500 . ? C37 C36 1.379(4) . ? C37 H37 0.9500 . ? C36 C35 1.389(4) . ? C36 H36 0.9500 . ? C25 C24 1.381(4) . ? C25 C26 1.383(4) . ? C25 H25 0.9500 . ? C35 H35 0.9500 . ? C23 C24 1.380(4) . ? C23 H23 0.9500 . ? C33 H33 0.9500 . ? C24 H24 0.9500 . ? C27 C26 1.386(4) . ? C27 H27 0.9500 . ? C26 H26 0.9500 . ? 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 Cl2 Pd1 Cl2 180.0 2_766 . ? Cl2 Pd1 Cl1 88.24(4) 2_766 . ? Cl2 Pd1 Cl1 91.76(4) . . ? Cl2 Pd1 Cl1 91.76(4) 2_766 2_766 ? Cl2 Pd1 Cl1 88.24(4) . 2_766 ? Cl1 Pd1 Cl1 180.000(1) . 2_766 ? C11 N1 C12 109.67(19) . . ? C11 N1 C21 110.54(19) . . ? C12 N1 C21 110.2(2) . . ? C11 N1 C31 110.35(19) . . ? C12 N1 C31 109.90(19) . . ? C21 N1 C31 106.15(18) . . ? C32 C31 N1 114.1(2) . . ? C32 C31 H31A 108.7 . . ? N1 C31 H31A 108.7 . . ? C32 C31 H31B 108.7 . . ? N1 C31 H31B 108.7 . . ? H31A C31 H31B 107.6 . . ? N1 C12 H12A 109.5 . . ? N1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C22 C21 N1 115.22(19) . . ? C22 C21 H21A 108.5 . . ? N1 C21 H21A 108.5 . . ? C22 C21 H21B 108.5 . . ? N1 C21 H21B 108.5 . . ? H21A C21 H21B 107.5 . . ? C23 C22 C27 118.5(3) . . ? C23 C22 C21 121.7(2) . . ? C27 C22 C21 119.8(3) . . ? C33 C32 C37 118.8(3) . . ? C33 C32 C31 121.4(2) . . ? C37 C32 C31 119.7(2) . . ? N1 C11 H11A 109.5 . . ? N1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C35 C34 C33 120.5(3) . . ? C35 C34 H34 119.7 . . ? C33 C34 H34 119.7 . . ? C36 C37 C32 120.6(3) . . ? C36 C37 H37 119.7 . . ? C32 C37 H37 119.7 . . ? C37 C36 C35 120.1(3) . . ? C37 C36 H36 120.0 . . ? C35 C36 H36 120.0 . . ? C24 C25 C26 119.8(3) . . ? C24 C25 H25 120.1 . . ? C26 C25 H25 120.1 . . ? C34 C35 C36 119.8(3) . . ? C34 C35 H35 120.1 . . ? C36 C35 H35 120.1 . . ? C24 C23 C22 120.9(3) . . ? C24 C23 H23 119.5 . . ? C22 C23 H23 119.5 . . ? C34 C33 C32 120.1(3) . . ? C34 C33 H33 120.0 . . ? C32 C33 H33 120.0 . . ? C23 C24 C25 120.3(3) . . ? C23 C24 H24 119.9 . . ? C25 C24 H24 119.9 . . ? C26 C27 C22 120.1(3) . . ? C26 C27 H27 119.9 . . ? C22 C27 H27 119.9 . . ? C25 C26 C27 120.4(3) . . ? C25 C26 H26 119.8 . . ? C27 C26 H26 119.8 . . ? 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 C11 N1 C31 C32 68.7(3) . . . . ? C12 N1 C31 C32 -52.3(3) . . . . ? C21 N1 C31 C32 -171.5(2) . . . . ? C11 N1 C21 C22 -55.9(3) . . . . ? C12 N1 C21 C22 65.5(3) . . . . ? C31 N1 C21 C22 -175.6(2) . . . . ? N1 C21 C22 C23 -87.8(3) . . . . ? N1 C21 C22 C27 94.6(3) . . . . ? N1 C31 C32 C33 -84.5(3) . . . . ? N1 C31 C32 C37 98.7(3) . . . . ? C33 C32 C37 C36 1.5(4) . . . . ? C31 C32 C37 C36 178.3(2) . . . . ? C32 C37 C36 C35 0.7(4) . . . . ? C33 C34 C35 C36 -0.2(4) . . . . ? C37 C36 C35 C34 -1.4(4) . . . . ? C27 C22 C23 C24 -1.3(4) . . . . ? C21 C22 C23 C24 -178.9(2) . . . . ? C35 C34 C33 C32 2.4(4) . . . . ? C37 C32 C33 C34 -3.0(4) . . . . ? C31 C32 C33 C34 -179.8(2) . . . . ? C22 C23 C24 C25 0.3(4) . . . . ? C26 C25 C24 C23 0.7(5) . . . . ? C23 C22 C27 C26 1.3(4) . . . . ? C21 C22 C27 C26 179.0(3) . . . . ? C24 C25 C26 C27 -0.7(5) . . . . ? C22 C27 C26 C25 -0.4(5) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.78 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.373 _refine_diff_density_min -0.550 _refine_diff_density_rms 0.091 data_2 _database_code_depnum_ccdc_archive 'CCDC 703948' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C18 H24 N), Cl4 Pd' _chemical_formula_sum 'C36 H48 Cl4 N2 Pd' _chemical_formula_weight 756.96 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' 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 triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.2770(17) _cell_length_b 10.612(2) _cell_length_c 11.527(2) _cell_angle_alpha 107.25(3) _cell_angle_beta 105.75(3) _cell_angle_gamma 103.75(3) _cell_volume 873.1(3) _cell_formula_units_Z 1 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Orange _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.440 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 392 _exptl_absorpt_coefficient_mu 0.865 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8598 _exptl_absorpt_correction_T_max 0.9033 _exptl_absorpt_process_details 'Denzo (Z. Otwinowski, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 'Kappa APEX II' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13580 _diffrn_reflns_av_R_equivalents 0.0331 _diffrn_reflns_av_sigmaI/netI 0.0422 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 28.72 _reflns_number_total 4511 _reflns_number_gt 4042 _reflns_threshold_expression >2sigma(I) _computing_data_collection Collect _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution SHELXS-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 3.0' _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^)+(0.0200P)^2^+0.5521P] 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 4511 _refine_ls_number_parameters 243 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0379 _refine_ls_R_factor_gt 0.0323 _refine_ls_wR_factor_ref 0.0719 _refine_ls_wR_factor_gt 0.0695 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _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 Pd1 Pd 0.0000 0.5000 0.0000 0.02577(7) Uani 1 2 d S . . Cl2 Cl 0.00368(7) 0.44485(6) 0.18000(5) 0.03519(13) Uani 1 1 d . . . Cl1 Cl 0.16368(8) 0.35675(6) -0.04777(6) 0.03823(13) Uani 1 1 d . . . N1 N -0.4325(2) 0.39349(16) 0.26967(15) 0.0214(3) Uani 1 1 d . B . C11 C -0.5976(3) 0.3645(2) 0.3019(2) 0.0277(4) Uani 1 1 d . . . H11A H -0.6190 0.2775 0.3181 0.042 Uiso 1 1 calc R . . H11B H -0.7003 0.3542 0.2286 0.042 Uiso 1 1 calc R . . H11C H -0.5815 0.4428 0.3803 0.042 Uiso 1 1 calc R . . C12 C -0.2772(3) 0.4095(2) 0.38164(19) 0.0252(4) Uani 1 1 d . . . H12A H -0.2576 0.4910 0.4585 0.038 Uiso 1 1 calc R . . H12B H -0.1700 0.4234 0.3592 0.038 Uiso 1 1 calc R . . H12C H -0.3015 0.3245 0.4010 0.038 Uiso 1 1 calc R . . C21 C -0.3980(3) 0.52675(19) 0.2390(2) 0.0253(4) Uani 1 1 d . . . H21A H -0.2897 0.5413 0.2164 0.030 Uiso 1 1 calc R . . H21B H -0.5000 0.5113 0.1611 0.030 Uiso 1 1 calc R . . C22 C -0.3730(3) 0.6586(2) 0.3487(2) 0.0246(4) Uani 1 1 d . . . C28 C -0.0327(3) 0.7430(2) 0.4164(3) 0.0403(5) Uani 1 1 d . . . H28A H -0.0153 0.6612 0.4337 0.060 Uiso 1 1 calc R . . H28B H 0.0685 0.8280 0.4785 0.060 Uiso 1 1 calc R . . H28C H -0.0404 0.7304 0.3271 0.060 Uiso 1 1 calc R . . C23 C -0.5256(3) 0.6865(2) 0.3623(2) 0.0337(5) Uani 1 1 d . . . H23 H -0.6407 0.6215 0.3037 0.040 Uiso 1 1 calc R . . C26 C -0.1939(3) 0.8780(2) 0.5294(2) 0.0372(5) Uani 1 1 d . . . H26 H -0.0797 0.9452 0.5874 0.045 Uiso 1 1 calc R . . C27 C -0.2037(3) 0.7575(2) 0.4317(2) 0.0291(4) Uani 1 1 d . . . C25 C -0.3452(4) 0.9020(3) 0.5439(2) 0.0419(6) Uani 1 1 d . . . H25 H -0.3346 0.9840 0.6121 0.050 Uiso 1 1 calc R . . C24 C -0.5116(4) 0.8067(3) 0.4593(3) 0.0406(6) Uani 1 1 d . . . H24 H -0.6164 0.8236 0.4677 0.049 Uiso 1 1 calc R . . C31 C -0.4579(3) 0.27278(19) 0.14544(19) 0.0250(4) Uani 1 1 d . . . H31A H -0.5670 0.2607 0.0746 0.030 Uiso 1 1 calc R A 1 H31B H -0.3551 0.3004 0.1189 0.030 Uiso 1 1 calc R A 1 C32A C -0.4743(6) 0.1328(4) 0.1573(6) 0.0267(17) Uani 0.50 1 d PG B 1 C37A C -0.6351(6) 0.0298(4) 0.1287(5) 0.0366(14) Uani 0.50 1 d PG B 1 C36A C -0.6363(7) -0.0991(4) 0.1352(5) 0.0481(18) Uani 0.50 1 d PG B 1 H36A H -0.7462 -0.1695 0.1156 0.058 Uiso 0.50 1 calc PR B 1 C35A C -0.4768(7) -0.1250(4) 0.1704(5) 0.054(2) Uani 0.50 1 d PG B 1 H35A H -0.4776 -0.2131 0.1749 0.065 Uiso 0.50 1 calc PR B 1 C34A C -0.3160(7) -0.0219(4) 0.1991(4) 0.0551(16) Uani 0.50 1 d PG B 1 H34A H -0.2069 -0.0396 0.2231 0.066 Uiso 0.50 1 calc PR B 1 C33A C -0.3147(6) 0.1070(4) 0.1925(5) 0.0356(13) Uani 0.50 1 d PG B 1 H33A H -0.2048 0.1774 0.2121 0.043 Uiso 0.50 1 calc PR B 1 C38A C -0.8168(7) 0.0444(6) 0.0800(6) 0.0585(16) Uani 0.50 1 d P B 1 H38A H -0.8501 0.0838 0.1546 0.088 Uiso 0.50 1 calc PR B 1 H38B H -0.9064 -0.0482 0.0215 0.088 Uiso 0.50 1 calc PR B 1 H38C H -0.8112 0.1072 0.0326 0.088 Uiso 0.50 1 calc PR B 1 C32B C -0.5075(6) 0.1269(4) 0.1488(6) 0.0309(18) Uani 0.50 1 d PG B 2 C33B C -0.6905(6) 0.0539(4) 0.1066(5) 0.0371(14) Uani 0.50 1 d PG B 2 H33B H -0.7745 0.0970 0.0805 0.045 Uiso 0.50 1 calc PR B 2 C34B C -0.7500(6) -0.0824(4) 0.1029(4) 0.0496(14) Uani 0.50 1 d PG B 2 H34B H -0.8745 -0.1321 0.0743 0.059 Uiso 0.50 1 calc PR B 2 C35B C -0.6265(7) -0.1458(4) 0.1413(5) 0.0528(19) Uani 0.50 1 d PG B 2 H35B H -0.6669 -0.2385 0.1388 0.063 Uiso 0.50 1 calc PR B 2 C36B C -0.4434(7) -0.0728(4) 0.1835(5) 0.0479(18) Uani 0.50 1 d PG B 2 H36B H -0.3594 -0.1159 0.2096 0.058 Uiso 0.50 1 calc PR B 2 C37B C -0.3839(6) 0.0636(4) 0.1872(5) 0.0341(13) Uani 0.50 1 d PG B 2 C38B C -0.1882(8) 0.1293(5) 0.2240(5) 0.0438(12) Uani 0.50 1 d P B 2 H38D H -0.1330 0.1865 0.3180 0.066 Uiso 0.50 1 calc PR B 2 H38E H -0.1664 0.1892 0.1755 0.066 Uiso 0.50 1 calc PR B 2 H38F H -0.1362 0.0556 0.2029 0.066 Uiso 0.50 1 calc PR 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 Pd1 0.01784(10) 0.03648(13) 0.02752(12) 0.01520(10) 0.01039(9) 0.01117(8) Cl2 0.0303(3) 0.0544(3) 0.0367(3) 0.0266(3) 0.0192(2) 0.0223(2) Cl1 0.0384(3) 0.0568(4) 0.0402(3) 0.0274(3) 0.0231(3) 0.0308(3) N1 0.0219(7) 0.0226(8) 0.0231(8) 0.0123(7) 0.0091(6) 0.0080(6) C11 0.0255(10) 0.0279(10) 0.0381(12) 0.0176(9) 0.0174(9) 0.0106(8) C12 0.0262(9) 0.0271(10) 0.0225(9) 0.0098(8) 0.0073(8) 0.0110(8) C21 0.0294(10) 0.0235(9) 0.0266(10) 0.0150(8) 0.0107(8) 0.0082(8) C22 0.0290(10) 0.0250(9) 0.0302(10) 0.0179(8) 0.0151(8) 0.0130(8) C28 0.0264(11) 0.0288(11) 0.0543(15) 0.0073(11) 0.0111(11) 0.0055(9) C23 0.0343(11) 0.0331(11) 0.0519(14) 0.0290(11) 0.0232(11) 0.0182(9) C26 0.0502(14) 0.0273(11) 0.0335(12) 0.0123(9) 0.0117(11) 0.0160(10) C27 0.0346(11) 0.0252(10) 0.0328(11) 0.0143(9) 0.0142(9) 0.0134(8) C25 0.0776(19) 0.0352(12) 0.0406(13) 0.0242(11) 0.0371(14) 0.0366(13) C24 0.0552(15) 0.0438(13) 0.0633(17) 0.0402(13) 0.0435(14) 0.0363(12) C31 0.0275(10) 0.0249(10) 0.0230(9) 0.0099(8) 0.0090(8) 0.0091(8) C32A 0.034(3) 0.019(3) 0.017(3) 0.005(3) 0.004(2) -0.001(2) C37A 0.056(4) 0.028(3) 0.028(3) 0.011(2) 0.021(3) 0.010(3) C36A 0.091(6) 0.022(3) 0.034(3) 0.010(2) 0.034(4) 0.014(3) C35A 0.114(7) 0.020(3) 0.022(3) 0.010(3) 0.021(3) 0.011(4) C34A 0.098(5) 0.034(3) 0.026(3) 0.010(2) 0.003(3) 0.035(3) C33A 0.046(4) 0.027(3) 0.026(2) 0.005(2) 0.004(3) 0.016(3) C38A 0.035(3) 0.049(3) 0.059(4) -0.003(3) 0.020(3) -0.012(2) C32B 0.044(3) 0.029(4) 0.024(4) 0.011(3) 0.012(3) 0.019(3) C33B 0.042(4) 0.030(3) 0.024(3) 0.011(2) 0.001(2) -0.001(2) C34B 0.065(4) 0.034(3) 0.032(3) 0.011(2) 0.011(3) -0.004(3) C35B 0.093(5) 0.030(4) 0.029(3) 0.014(3) 0.015(3) 0.017(3) C36B 0.091(5) 0.015(3) 0.027(3) 0.009(2) 0.013(3) 0.009(3) C37B 0.051(4) 0.024(3) 0.021(2) 0.008(2) 0.008(3) 0.010(2) C38B 0.057(3) 0.041(3) 0.035(3) 0.012(2) 0.013(3) 0.028(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 Cl1 2.3102(8) . ? Pd1 Cl1 2.3102(8) 2_565 ? Pd1 Cl2 2.3114(7) 2_565 ? Pd1 Cl2 2.3114(7) . ? N1 C12 1.488(2) . ? N1 C11 1.498(2) . ? N1 C31 1.535(3) . ? N1 C21 1.538(2) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C21 C22 1.507(3) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C27 1.400(3) . ? C22 C23 1.401(3) . ? C28 C27 1.510(3) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C23 C24 1.380(3) . ? C23 H23 0.9500 . ? C26 C25 1.379(3) . ? C26 C27 1.399(3) . ? C26 H26 0.9500 . ? C25 C24 1.377(4) . ? C25 H25 0.9500 . ? C24 H24 0.9500 . ? C31 C32A 1.509(4) . ? C31 C32B 1.519(4) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32A C37A 1.390(2) . ? C32A C33A 1.390(2) . ? C37A C36A 1.390(2) . ? C37A C38A 1.519(7) . ? C36A C35A 1.390(2) . ? C36A H36A 0.9500 . ? C35A C34A 1.390(2) . ? C35A H35A 0.9500 . ? C34A C33A 1.390(2) . ? C34A H34A 0.9500 . ? C33A H33A 0.9500 . ? C38A H38A 0.9800 . ? C38A H38B 0.9800 . ? C38A H38C 0.9800 . ? C32B C33B 1.397(2) . ? C32B C37B 1.397(2) . ? C33B C34B 1.397(2) . ? C33B H33B 0.9500 . ? C34B C35B 1.397(2) . ? C34B H34B 0.9500 . ? C35B C36B 1.397(2) . ? C35B H35B 0.9500 . ? C36B C37B 1.397(2) . ? C36B H36B 0.9500 . ? C37B C38B 1.484(7) . ? C38B H38D 0.9800 . ? C38B H38E 0.9800 . ? C38B H38F 0.9800 . ? 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 Cl1 Pd1 Cl1 180.0 . 2_565 ? Cl1 Pd1 Cl2 90.74(3) . 2_565 ? Cl1 Pd1 Cl2 89.26(3) 2_565 2_565 ? Cl1 Pd1 Cl2 89.26(3) . . ? Cl1 Pd1 Cl2 90.74(3) 2_565 . ? Cl2 Pd1 Cl2 180.000(1) 2_565 . ? C12 N1 C11 109.18(15) . . ? C12 N1 C31 110.49(14) . . ? C11 N1 C31 109.88(15) . . ? C12 N1 C21 110.28(15) . . ? C11 N1 C21 111.00(14) . . ? C31 N1 C21 105.98(14) . . ? N1 C11 H11A 109.5 . . ? N1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N1 C12 H12A 109.5 . . ? N1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C22 C21 N1 114.58(15) . . ? C22 C21 H21A 108.6 . . ? N1 C21 H21A 108.6 . . ? C22 C21 H21B 108.6 . . ? N1 C21 H21B 108.6 . . ? H21A C21 H21B 107.6 . . ? C27 C22 C23 119.23(19) . . ? C27 C22 C21 122.22(17) . . ? C23 C22 C21 118.43(19) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C24 C23 C22 121.2(2) . . ? C24 C23 H23 119.4 . . ? C22 C23 H23 119.4 . . ? C25 C26 C27 121.9(2) . . ? C25 C26 H26 119.1 . . ? C27 C26 H26 119.1 . . ? C26 C27 C22 118.1(2) . . ? C26 C27 C28 118.8(2) . . ? C22 C27 C28 122.98(19) . . ? C24 C25 C26 119.7(2) . . ? C24 C25 H25 120.1 . . ? C26 C25 H25 120.1 . . ? C25 C24 C23 119.7(2) . . ? C25 C24 H24 120.1 . . ? C23 C24 H24 120.1 . . ? C32A C31 C32B 9.5(3) . . ? C32A C31 N1 115.5(3) . . ? C32B C31 N1 115.7(3) . . ? C32A C31 H31A 108.4 . . ? C32B C31 H31A 100.0 . . ? N1 C31 H31A 108.4 . . ? C32A C31 H31B 108.4 . . ? C32B C31 H31B 116.0 . . ? N1 C31 H31B 108.4 . . ? H31A C31 H31B 107.5 . . ? C37A C32A C33A 120.0 . . ? C37A C32A C31 124.6(3) . . ? C33A C32A C31 115.3(3) . . ? C36A C37A C32A 120.0 . . ? C36A C37A C38A 116.1(3) . . ? C32A C37A C38A 123.7(3) . . ? C37A C36A C35A 120.0 . . ? C37A C36A H36A 120.0 . . ? C35A C36A H36A 120.0 . . ? C36A C35A C34A 120.0 . . ? C36A C35A H35A 120.0 . . ? C34A C35A H35A 120.0 . . ? C33A C34A C35A 120.0 . . ? C33A C34A H34A 120.0 . . ? C35A C34A H34A 120.0 . . ? C34A C33A C32A 120.0 . . ? C34A C33A H33A 120.0 . . ? C32A C33A H33A 120.0 . . ? C33B C32B C37B 120.0 . . ? C33B C32B C31 115.6(3) . . ? C37B C32B C31 124.4(3) . . ? C32B C33B C34B 120.0 . . ? C32B C33B H33B 120.0 . . ? C34B C33B H33B 120.0 . . ? C35B C34B C33B 120.0 . . ? C35B C34B H34B 120.0 . . ? C33B C34B H34B 120.0 . . ? C34B C35B C36B 120.0 . . ? C34B C35B H35B 120.0 . . ? C36B C35B H35B 120.0 . . ? C37B C36B C35B 120.0 . . ? C37B C36B H36B 120.0 . . ? C35B C36B H36B 120.0 . . ? C36B C37B C32B 120.0 . . ? C36B C37B C38B 116.3(3) . . ? C32B C37B C38B 123.5(3) . . ? C37B C38B H38D 109.5 . . ? C37B C38B H38E 109.5 . . ? H38D C38B H38E 109.5 . . ? C37B C38B H38F 109.5 . . ? H38D C38B H38F 109.5 . . ? H38E C38B H38F 109.5 . . ? 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 C12 N1 C21 C22 -61.6(2) . . . . ? C11 N1 C21 C22 59.5(2) . . . . ? C31 N1 C21 C22 178.78(16) . . . . ? N1 C21 C22 C27 100.2(2) . . . . ? N1 C21 C22 C23 -83.7(2) . . . . ? C27 C22 C23 C24 -2.7(3) . . . . ? C21 C22 C23 C24 -178.84(18) . . . . ? C25 C26 C27 C22 -1.0(3) . . . . ? C25 C26 C27 C28 176.1(2) . . . . ? C23 C22 C27 C26 2.9(3) . . . . ? C21 C22 C27 C26 178.88(17) . . . . ? C23 C22 C27 C28 -174.18(19) . . . . ? C21 C22 C27 C28 1.8(3) . . . . ? C27 C26 C25 C24 -1.1(3) . . . . ? C26 C25 C24 C23 1.3(3) . . . . ? C22 C23 C24 C25 0.5(3) . . . . ? C12 N1 C31 C32A 54.3(3) . . . . ? C11 N1 C31 C32A -66.3(3) . . . . ? C21 N1 C31 C32A 173.7(2) . . . . ? C12 N1 C31 C32B 64.8(3) . . . . ? C11 N1 C31 C32B -55.8(3) . . . . ? C21 N1 C31 C32B -175.8(2) . . . . ? C32B C31 C32A C37A -2(3) . . . . ? N1 C31 C32A C37A 91.7(4) . . . . ? C32B C31 C32A C33A 174(3) . . . . ? N1 C31 C32A C33A -92.1(3) . . . . ? C33A C32A C37A C36A 0.0 . . . . ? C31 C32A C37A C36A 176.0(5) . . . . ? C33A C32A C37A C38A -175.5(5) . . . . ? C31 C32A C37A C38A 0.6(5) . . . . ? C32A C37A C36A C35A 0.0 . . . . ? C38A C37A C36A C35A 175.8(4) . . . . ? C37A C36A C35A C34A 0.0 . . . . ? C36A C35A C34A C33A 0.0 . . . . ? C35A C34A C33A C32A 0.0 . . . . ? C37A C32A C33A C34A 0.0 . . . . ? C31 C32A C33A C34A -176.4(5) . . . . ? C32A C31 C32B C33B 180(3) . . . . ? N1 C31 C32B C33B 89.1(3) . . . . ? C32A C31 C32B C37B -2(3) . . . . ? N1 C31 C32B C37B -92.5(4) . . . . ? C37B C32B C33B C34B 0.0 . . . . ? C31 C32B C33B C34B 178.4(5) . . . . ? C32B C33B C34B C35B 0.0 . . . . ? C33B C34B C35B C36B 0.0 . . . . ? C34B C35B C36B C37B 0.0 . . . . ? C35B C36B C37B C32B 0.0 . . . . ? C35B C36B C37B C38B -175.7(4) . . . . ? C33B C32B C37B C36B 0.0 . . . . ? C31 C32B C37B C36B -178.3(5) . . . . ? C33B C32B C37B C38B 175.4(5) . . . . ? C31 C32B C37B C38B -2.9(5) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.72 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.323 _refine_diff_density_min -0.516 _refine_diff_density_rms 0.067