# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Su, Cheng-Yong' _publ_contact_author_email cesscy@mail.sysu.edu.cn _publ_section_title ; Pd2L2 metallacycles as molecular container for small molecules ; _publ_author_name 'Cheng-Yong Su' data_1 _database_code_depnum_ccdc_archive 'CCDC 767078' #TrackingRef 'Compds-rev.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53.50 H55 Cl7 N8 Pd2' _chemical_formula_weight 1271.01 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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.7450(5) _cell_length_b 19.4066(8) _cell_length_c 12.5835(5) _cell_angle_alpha 90.00 _cell_angle_beta 109.4970(10) _cell_angle_gamma 90.00 _cell_volume 2703.70(19) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8301 _cell_measurement_theta_min 2.308 _cell_measurement_theta_max 25.045 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.561 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1286 _exptl_absorpt_coefficient_mu 1.056 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7384 _exptl_absorpt_correction_T_max 0.9621 _exptl_absorpt_process_details '(SADABS, Bruker, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19000 _diffrn_reflns_av_R_equivalents 0.0582 _diffrn_reflns_av_sigmaI/netI 0.0517 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 25.08 _reflns_number_total 4775 _reflns_number_gt 4208 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; The dichloromethane solvent molecules are disordered over two partial positions, which were modelled by using SADI and EADP to make Cl-C bonds and anisotropic displacement parameters reasonable (6+6 restaints). 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^)+(0.0330P)^2^+28.1141P] 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 4775 _refine_ls_number_parameters 320 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0816 _refine_ls_R_factor_gt 0.0702 _refine_ls_wR_factor_ref 0.1485 _refine_ls_wR_factor_gt 0.1418 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd 0.45608(4) 0.47573(3) 0.79615(4) 0.02523(17) Uani 1 1 d . . . Cl1 Cl 0.60199(16) 0.55754(9) 0.81305(15) 0.0343(4) Uani 1 1 d . . . Cl2 Cl 0.30884(16) 0.39202(10) 0.75331(17) 0.0399(5) Uani 1 1 d . . . C1 C 0.2968(6) 0.5963(4) 0.6882(6) 0.0274(15) Uani 1 1 d . . . H1 H 0.3394 0.6057 0.6375 0.033 Uiso 1 1 calc R . . C2 C 0.1632(6) 0.6050(4) 0.7750(6) 0.0285(15) Uani 1 1 d . . . C3 C 0.0680(6) 0.6220(4) 0.8133(6) 0.0333(17) Uani 1 1 d . . . H3 H 0.0115 0.6572 0.7790 0.040 Uiso 1 1 calc R . . C4 C 0.0613(7) 0.5845(4) 0.9036(6) 0.0356(17) Uani 1 1 d . . . H4 H -0.0024 0.5940 0.9321 0.043 Uiso 1 1 calc R . . C5 C 0.1432(6) 0.5338(4) 0.9544(6) 0.0343(17) Uani 1 1 d . . . H5 H 0.1356 0.5104 1.0180 0.041 Uiso 1 1 calc R . . C6 C 0.2358(6) 0.5158(4) 0.9159(6) 0.0328(16) Uani 1 1 d . . . H6 H 0.2915 0.4804 0.9509 0.039 Uiso 1 1 calc R . . C7 C 0.2443(6) 0.5520(4) 0.8228(6) 0.0278(15) Uani 1 1 d . . . C8 C 0.1389(7) 0.6892(4) 0.6167(6) 0.0338(17) Uani 1 1 d . . . H8A H 0.1717 0.7332 0.6544 0.041 Uiso 1 1 calc R . . H8B H 0.0513 0.6881 0.6054 0.041 Uiso 1 1 calc R . . C9 C 0.1566(6) 0.6867(4) 0.5028(6) 0.0266(15) Uani 1 1 d . . . C10 C 0.0911(6) 0.6384(4) 0.4237(6) 0.0290(15) Uani 1 1 d . . . C11 C 0.0966(6) 0.6395(4) 0.3139(6) 0.0296(16) Uani 1 1 d . . . C12 C 0.1647(6) 0.6904(4) 0.2852(6) 0.0274(15) Uani 1 1 d . . . C13 C 0.2364(6) 0.7367(4) 0.3666(6) 0.0311(16) Uani 1 1 d . . . C14 C 0.2329(6) 0.7335(4) 0.4765(6) 0.0286(15) Uani 1 1 d . . . C15 C 0.0139(7) 0.5842(4) 0.4537(7) 0.0423(19) Uani 1 1 d . . . H15A H 0.0544 0.5394 0.4623 0.063 Uiso 1 1 calc R . . H15B H -0.0646 0.5814 0.3935 0.063 Uiso 1 1 calc R . . H15C H 0.0018 0.5968 0.5246 0.063 Uiso 1 1 calc R . . C16 C 0.0303(7) 0.5846(4) 0.2323(7) 0.045(2) Uani 1 1 d . . . H16A H 0.0575 0.5847 0.1667 0.068 Uiso 1 1 calc R . . H16B H -0.0567 0.5938 0.2078 0.068 Uiso 1 1 calc R . . H16C H 0.0469 0.5394 0.2693 0.068 Uiso 1 1 calc R . . C17 C 0.3158(8) 0.7878(5) 0.3367(8) 0.052(2) Uani 1 1 d . . . H17A H 0.2986 0.8341 0.3586 0.078 Uiso 1 1 calc R . . H17B H 0.3004 0.7865 0.2553 0.078 Uiso 1 1 calc R . . H17C H 0.4006 0.7764 0.3768 0.078 Uiso 1 1 calc R . . C18 C 0.3107(7) 0.7829(5) 0.5639(8) 0.049(2) Uani 1 1 d . . . H18A H 0.2685 0.8270 0.5583 0.074 Uiso 1 1 calc R . . H18B H 0.3874 0.7901 0.5506 0.074 Uiso 1 1 calc R . . H18C H 0.3265 0.7634 0.6393 0.074 Uiso 1 1 calc R . . C19 C 0.1611(7) 0.6982(5) 0.1653(6) 0.0398(19) Uani 1 1 d . . . H19A H 0.0874 0.6755 0.1148 0.048 Uiso 1 1 calc R . . H19B H 0.1557 0.7478 0.1459 0.048 Uiso 1 1 calc R . . C20 C 0.3348(6) 0.6148(4) 0.1993(6) 0.0282(15) Uani 1 1 d . . . H20 H 0.3222 0.5914 0.2607 0.034 Uiso 1 1 calc R . . C21 C 0.3124(6) 0.6889(4) 0.0609(5) 0.0256(14) Uani 1 1 d . . . C22 C 0.2779(6) 0.7405(4) -0.0204(6) 0.0320(16) Uani 1 1 d . . . H22 H 0.2126 0.7707 -0.0257 0.038 Uiso 1 1 calc R . . C23 C 0.3428(7) 0.7455(4) -0.0926(6) 0.0326(16) Uani 1 1 d . . . H23 H 0.3227 0.7804 -0.1488 0.039 Uiso 1 1 calc R . . C24 C 0.4370(6) 0.7010(4) -0.0855(6) 0.0308(16) Uani 1 1 d . . . H24 H 0.4788 0.7059 -0.1380 0.037 Uiso 1 1 calc R . . C25 C 0.4725(6) 0.6500(4) -0.0053(6) 0.0293(16) Uani 1 1 d . . . H25 H 0.5378 0.6199 -0.0009 0.035 Uiso 1 1 calc R . . C26 C 0.4078(6) 0.6446(3) 0.0692(6) 0.0253(14) Uani 1 1 d . . . N1 N 0.3278(5) 0.5466(3) 0.7658(5) 0.0302(13) Uani 1 1 d . . . N2 N 0.1979(5) 0.6321(3) 0.6895(5) 0.0290(13) Uani 1 1 d . . . N3 N 0.4213(5) 0.5979(3) 0.1569(5) 0.0291(13) Uani 1 1 d . . . N4 N 0.2672(5) 0.6686(3) 0.1455(5) 0.0291(13) Uani 1 1 d . . . C1A C 0.6584(10) 0.5702(6) 0.5238(13) 0.086(4) Uiso 0.38 1 d PDU A 1 H1A1 H 0.6929 0.5792 0.4633 0.104 Uiso 0.38 1 calc PR A 1 H1A2 H 0.7217 0.5802 0.5968 0.104 Uiso 0.38 1 calc PR A 1 Cl3A Cl 0.5351(6) 0.6266(4) 0.5064(6) 0.150(2) Uiso 0.38 1 d PDU A 1 Cl4A Cl 0.6198(8) 0.4858(5) 0.5202(8) 0.092(2) Uiso 0.38 1 d PDU A 1 C1B C 0.6584(10) 0.5702(6) 0.5238(13) 0.086(4) Uiso 0.38 1 d PDU B 2 H1B1 H 0.6356 0.5240 0.5430 0.104 Uiso 0.38 1 calc PR B 2 H1B2 H 0.6722 0.5663 0.4506 0.104 Uiso 0.38 1 calc PR B 2 Cl3B Cl 0.5351(6) 0.6266(4) 0.5064(6) 0.150(2) Uiso 0.38 1 d PDU B 2 Cl4B Cl 0.7856(7) 0.5926(4) 0.6199(7) 0.080(2) Uiso 0.38 1 d PDU B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd 0.0244(3) 0.0291(3) 0.0224(3) 0.0010(2) 0.0081(2) 0.0049(2) Cl1 0.0343(9) 0.0365(10) 0.0353(10) 0.0035(8) 0.0159(8) -0.0014(7) Cl2 0.0336(9) 0.0401(11) 0.0416(11) -0.0045(9) 0.0069(8) -0.0055(8) C1 0.029(3) 0.033(4) 0.022(4) -0.001(3) 0.011(3) 0.006(3) C2 0.029(3) 0.032(4) 0.024(4) -0.005(3) 0.007(3) 0.000(3) C3 0.030(4) 0.044(4) 0.026(4) 0.001(3) 0.009(3) 0.010(3) C4 0.036(4) 0.043(4) 0.031(4) -0.003(3) 0.016(3) 0.005(3) C5 0.040(4) 0.041(4) 0.025(4) -0.005(3) 0.015(3) -0.008(3) C6 0.035(4) 0.032(4) 0.029(4) -0.003(3) 0.006(3) -0.005(3) C7 0.031(4) 0.026(4) 0.027(4) -0.005(3) 0.011(3) 0.001(3) C8 0.038(4) 0.042(4) 0.025(4) 0.010(3) 0.015(3) 0.015(3) C9 0.029(3) 0.031(4) 0.023(3) 0.004(3) 0.012(3) 0.007(3) C10 0.026(3) 0.027(4) 0.035(4) 0.007(3) 0.013(3) 0.006(3) C11 0.023(3) 0.035(4) 0.031(4) 0.003(3) 0.009(3) 0.004(3) C12 0.027(3) 0.031(4) 0.027(4) 0.003(3) 0.014(3) 0.007(3) C13 0.029(4) 0.030(4) 0.042(4) 0.004(3) 0.023(3) 0.005(3) C14 0.026(3) 0.033(4) 0.027(4) -0.002(3) 0.009(3) 0.007(3) C15 0.042(4) 0.044(5) 0.045(5) 0.013(4) 0.020(4) -0.002(4) C16 0.041(4) 0.050(5) 0.042(5) -0.014(4) 0.011(4) -0.005(4) C17 0.053(5) 0.046(5) 0.067(6) -0.007(5) 0.035(5) -0.007(4) C18 0.038(4) 0.056(5) 0.059(6) -0.027(5) 0.023(4) -0.012(4) C19 0.035(4) 0.057(5) 0.032(4) 0.006(4) 0.017(3) 0.022(4) C20 0.031(4) 0.037(4) 0.019(3) 0.006(3) 0.012(3) 0.007(3) C21 0.028(3) 0.032(4) 0.017(3) 0.001(3) 0.008(3) -0.003(3) C22 0.034(4) 0.031(4) 0.033(4) 0.004(3) 0.013(3) 0.006(3) C23 0.046(4) 0.029(4) 0.023(4) 0.003(3) 0.013(3) -0.002(3) C24 0.033(4) 0.037(4) 0.025(4) -0.003(3) 0.012(3) -0.010(3) C25 0.026(3) 0.038(4) 0.028(4) -0.007(3) 0.015(3) -0.002(3) C26 0.027(3) 0.026(4) 0.023(3) -0.003(3) 0.008(3) -0.002(3) N1 0.029(3) 0.032(3) 0.033(3) 0.001(3) 0.015(3) 0.009(2) N2 0.030(3) 0.038(3) 0.021(3) 0.005(3) 0.011(2) 0.010(3) N3 0.027(3) 0.034(3) 0.030(3) 0.000(3) 0.015(3) 0.008(2) N4 0.032(3) 0.037(3) 0.023(3) 0.005(3) 0.016(3) 0.008(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd N3 1.974(5) 3_666 ? Pd N1 1.981(5) . ? Pd Cl1 2.2934(18) . ? Pd Cl2 2.3016(19) . ? C1 N1 1.334(9) . ? C1 N2 1.358(8) . ? C1 H1 0.9500 . ? C2 N2 1.375(9) . ? C2 C7 1.395(9) . ? C2 C3 1.396(9) . ? C3 C4 1.373(10) . ? C3 H3 0.9500 . ? C4 C5 1.377(10) . ? C4 H4 0.9500 . ? C5 C6 1.375(10) . ? C5 H5 0.9500 . ? C6 C7 1.397(10) . ? C6 H6 0.9500 . ? C7 N1 1.398(9) . ? C8 N2 1.459(9) . ? C8 C9 1.517(9) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C14 1.392(10) . ? C9 C10 1.396(10) . ? C10 C11 1.405(10) . ? C10 C15 1.517(10) . ? C11 C12 1.393(10) . ? C11 C16 1.504(10) . ? C12 C13 1.411(10) . ? C12 C19 1.502(10) . ? C13 C14 1.398(10) . ? C13 C17 1.493(10) . ? C14 C18 1.513(10) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 N4 1.468(8) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 N3 1.336(8) . ? C20 N4 1.350(8) . ? C20 H20 0.9500 . ? C21 C26 1.388(9) . ? C21 C22 1.391(9) . ? C21 N4 1.396(8) . ? C22 C23 1.370(10) . ? C22 H22 0.9500 . ? C23 C24 1.382(10) . ? C23 H23 0.9500 . ? C24 C25 1.376(10) . ? C24 H24 0.9500 . ? C25 C26 1.394(9) . ? C25 H25 0.9500 . ? C26 N3 1.396(9) . ? N3 Pd 1.974(5) 3_666 ? C1A Cl4A 1.696(11) . ? C1A Cl3A 1.769(10) . ? C1A H1A1 0.9900 . ? C1A H1A2 0.9900 . ? 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 N3 Pd N1 172.9(2) 3_666 . ? N3 Pd Cl1 91.48(18) 3_666 . ? N1 Pd Cl1 91.95(18) . . ? N3 Pd Cl2 88.56(18) 3_666 . ? N1 Pd Cl2 88.92(18) . . ? Cl1 Pd Cl2 171.93(7) . . ? N1 C1 N2 112.7(6) . . ? N1 C1 H1 123.7 . . ? N2 C1 H1 123.7 . . ? N2 C2 C7 106.3(6) . . ? N2 C2 C3 131.3(6) . . ? C7 C2 C3 122.4(7) . . ? C4 C3 C2 115.7(7) . . ? C4 C3 H3 122.1 . . ? C2 C3 H3 122.1 . . ? C3 C4 C5 122.7(7) . . ? C3 C4 H4 118.7 . . ? C5 C4 H4 118.7 . . ? C6 C5 C4 122.0(7) . . ? C6 C5 H5 119.0 . . ? C4 C5 H5 119.0 . . ? C5 C6 C7 117.0(7) . . ? C5 C6 H6 121.5 . . ? C7 C6 H6 121.5 . . ? C2 C7 C6 120.2(6) . . ? C2 C7 N1 109.2(6) . . ? C6 C7 N1 130.6(6) . . ? N2 C8 C9 112.5(6) . . ? N2 C8 H8A 109.1 . . ? C9 C8 H8A 109.1 . . ? N2 C8 H8B 109.1 . . ? C9 C8 H8B 109.1 . . ? H8A C8 H8B 107.8 . . ? C14 C9 C10 121.0(6) . . ? C14 C9 C8 120.4(6) . . ? C10 C9 C8 118.6(6) . . ? C9 C10 C11 119.7(6) . . ? C9 C10 C15 121.4(7) . . ? C11 C10 C15 118.9(7) . . ? C12 C11 C10 119.0(7) . . ? C12 C11 C16 122.5(7) . . ? C10 C11 C16 118.5(7) . . ? C11 C12 C13 121.2(6) . . ? C11 C12 C19 120.4(7) . . ? C13 C12 C19 118.3(7) . . ? C14 C13 C12 118.9(6) . . ? C14 C13 C17 120.3(7) . . ? C12 C13 C17 120.8(7) . . ? C9 C14 C13 119.8(6) . . ? C9 C14 C18 121.4(7) . . ? C13 C14 C18 118.7(7) . . ? C10 C15 H15A 109.5 . . ? C10 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C10 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C13 C17 H17A 109.5 . . ? C13 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C13 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C14 C18 H18A 109.5 . . ? C14 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C14 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N4 C19 C12 112.9(6) . . ? N4 C19 H19A 109.0 . . ? C12 C19 H19A 109.0 . . ? N4 C19 H19B 109.0 . . ? C12 C19 H19B 109.0 . . ? H19A C19 H19B 107.8 . . ? N3 C20 N4 112.8(6) . . ? N3 C20 H20 123.6 . . ? N4 C20 H20 123.6 . . ? C26 C21 C22 122.1(6) . . ? C26 C21 N4 105.7(6) . . ? C22 C21 N4 132.3(6) . . ? C23 C22 C21 116.6(7) . . ? C23 C22 H22 121.7 . . ? C21 C22 H22 121.7 . . ? C22 C23 C24 121.6(7) . . ? C22 C23 H23 119.2 . . ? C24 C23 H23 119.2 . . ? C25 C24 C23 122.4(7) . . ? C25 C24 H24 118.8 . . ? C23 C24 H24 118.8 . . ? C24 C25 C26 116.6(6) . . ? C24 C25 H25 121.7 . . ? C26 C25 H25 121.7 . . ? C21 C26 C25 120.7(6) . . ? C21 C26 N3 109.7(6) . . ? C25 C26 N3 129.5(6) . . ? C1 N1 C7 104.8(5) . . ? C1 N1 Pd 130.3(5) . . ? C7 N1 Pd 124.8(5) . . ? C1 N2 C2 107.0(6) . . ? C1 N2 C8 127.6(6) . . ? C2 N2 C8 125.4(6) . . ? C20 N3 C26 104.8(5) . . ? C20 N3 Pd 129.3(5) . 3_666 ? C26 N3 Pd 125.9(4) . 3_666 ? C20 N4 C21 106.9(5) . . ? C20 N4 C19 127.5(6) . . ? C21 N4 C19 125.5(6) . . ? Cl4A C1A Cl3A 113.2(8) . . ? Cl4A C1A H1A1 108.9 . . ? Cl3A C1A H1A1 108.9 . . ? Cl4A C1A H1A2 108.9 . . ? Cl3A C1A H1A2 108.9 . . ? H1A1 C1A H1A2 107.8 . . ? 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 N2 C2 C3 C4 -178.8(7) . . . . ? C7 C2 C3 C4 2.0(11) . . . . ? C2 C3 C4 C5 0.5(11) . . . . ? C3 C4 C5 C6 -1.8(12) . . . . ? C4 C5 C6 C7 0.6(11) . . . . ? N2 C2 C7 C6 177.4(6) . . . . ? C3 C2 C7 C6 -3.2(10) . . . . ? N2 C2 C7 N1 -0.4(8) . . . . ? C3 C2 C7 N1 179.0(6) . . . . ? C5 C6 C7 C2 1.8(10) . . . . ? C5 C6 C7 N1 179.0(7) . . . . ? N2 C8 C9 C14 -107.8(8) . . . . ? N2 C8 C9 C10 74.8(8) . . . . ? C14 C9 C10 C11 -3.8(10) . . . . ? C8 C9 C10 C11 173.6(6) . . . . ? C14 C9 C10 C15 176.1(6) . . . . ? C8 C9 C10 C15 -6.5(10) . . . . ? C9 C10 C11 C12 -2.0(10) . . . . ? C15 C10 C11 C12 178.2(6) . . . . ? C9 C10 C11 C16 176.9(6) . . . . ? C15 C10 C11 C16 -3.0(10) . . . . ? C10 C11 C12 C13 5.7(10) . . . . ? C16 C11 C12 C13 -173.1(7) . . . . ? C10 C11 C12 C19 -172.8(6) . . . . ? C16 C11 C12 C19 8.4(10) . . . . ? C11 C12 C13 C14 -3.7(10) . . . . ? C19 C12 C13 C14 174.9(6) . . . . ? C11 C12 C13 C17 175.6(7) . . . . ? C19 C12 C13 C17 -5.9(10) . . . . ? C10 C9 C14 C13 5.8(10) . . . . ? C8 C9 C14 C13 -171.5(6) . . . . ? C10 C9 C14 C18 -175.8(7) . . . . ? C8 C9 C14 C18 6.8(10) . . . . ? C12 C13 C14 C9 -2.1(10) . . . . ? C17 C13 C14 C9 178.6(7) . . . . ? C12 C13 C14 C18 179.5(6) . . . . ? C17 C13 C14 C18 0.2(10) . . . . ? C11 C12 C19 N4 -101.9(8) . . . . ? C13 C12 C19 N4 79.6(9) . . . . ? C26 C21 C22 C23 0.1(10) . . . . ? N4 C21 C22 C23 -179.1(7) . . . . ? C21 C22 C23 C24 0.7(11) . . . . ? C22 C23 C24 C25 -1.0(11) . . . . ? C23 C24 C25 C26 0.5(10) . . . . ? C22 C21 C26 C25 -0.5(10) . . . . ? N4 C21 C26 C25 178.8(6) . . . . ? C22 C21 C26 N3 -179.4(6) . . . . ? N4 C21 C26 N3 0.0(7) . . . . ? C24 C25 C26 C21 0.3(10) . . . . ? C24 C25 C26 N3 178.9(6) . . . . ? N2 C1 N1 C7 -1.5(8) . . . . ? N2 C1 N1 Pd 175.9(5) . . . . ? C2 C7 N1 C1 1.1(8) . . . . ? C6 C7 N1 C1 -176.4(7) . . . . ? C2 C7 N1 Pd -176.5(5) . . . . ? C6 C7 N1 Pd 6.0(11) . . . . ? N3 Pd N1 C1 173.3(17) 3_666 . . . ? Cl1 Pd N1 C1 54.5(6) . . . . ? Cl2 Pd N1 C1 -117.4(6) . . . . ? N3 Pd N1 C7 -10(2) 3_666 . . . ? Cl1 Pd N1 C7 -128.5(5) . . . . ? Cl2 Pd N1 C7 59.5(5) . . . . ? N1 C1 N2 C2 1.3(8) . . . . ? N1 C1 N2 C8 -179.7(7) . . . . ? C7 C2 N2 C1 -0.5(7) . . . . ? C3 C2 N2 C1 -179.8(7) . . . . ? C7 C2 N2 C8 -179.6(6) . . . . ? C3 C2 N2 C8 1.1(12) . . . . ? C9 C8 N2 C1 27.4(10) . . . . ? C9 C8 N2 C2 -153.7(6) . . . . ? N4 C20 N3 C26 -0.1(8) . . . . ? N4 C20 N3 Pd 179.9(5) . . . 3_666 ? C21 C26 N3 C20 0.1(7) . . . . ? C25 C26 N3 C20 -178.7(7) . . . . ? C21 C26 N3 Pd -179.9(5) . . . 3_666 ? C25 C26 N3 Pd 1.4(10) . . . 3_666 ? N3 C20 N4 C21 0.1(8) . . . . ? N3 C20 N4 C19 176.3(7) . . . . ? C26 C21 N4 C20 0.0(7) . . . . ? C22 C21 N4 C20 179.3(7) . . . . ? C26 C21 N4 C19 -176.4(7) . . . . ? C22 C21 N4 C19 2.9(12) . . . . ? C12 C19 N4 C20 29.8(11) . . . . ? C12 C19 N4 C21 -154.6(7) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.08 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.537 _refine_diff_density_min -1.099 _refine_diff_density_rms 0.123 #===============# data_2 _database_code_depnum_ccdc_archive 'CCDC 767079' #TrackingRef 'Compds-rev.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H54 Cl10 N8 Pd2' _chemical_formula_weight 1382.35 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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.7459(17) _cell_length_b 19.650(3) _cell_length_c 12.5948(18) _cell_angle_alpha 90.00 _cell_angle_beta 109.831(2) _cell_angle_gamma 90.00 _cell_volume 2734.5(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(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 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.679 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1392 _exptl_absorpt_coefficient_mu 1.193 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7014 _exptl_absorpt_correction_T_max 0.7877 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 APEX _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14888 _diffrn_reflns_av_R_equivalents 0.0330 _diffrn_reflns_av_sigmaI/netI 0.0411 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 27.00 _reflns_number_total 5751 _reflns_number_gt 5220 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; The solvated chloroform solvent molecule was modelled by using SADI, ISOR and SIMU to make Cl-C bonds and anisotropic displacement parameters of Cl and C atoms reasonable (3+24+6). 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^)+(0.0743P)^2^+20.1522P] 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 5751 _refine_ls_number_parameters 338 _refine_ls_number_restraints 33 _refine_ls_R_factor_all 0.0641 _refine_ls_R_factor_gt 0.0588 _refine_ls_wR_factor_ref 0.1645 _refine_ls_wR_factor_gt 0.1607 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd 0.45420(2) 0.476282(13) 0.79794(2) 0.01481(6) Uani 1 1 d . . . Cl1 Cl 0.60050(7) 0.55712(4) 0.81422(7) 0.02135(19) Uani 1 1 d . . . Cl2 Cl 0.30532(8) 0.39377(5) 0.75466(8) 0.0249(2) Uani 1 1 d . . . C1 C 0.2962(3) 0.59667(18) 0.6914(3) 0.0174(8) Uani 1 1 d . . . H1 H 0.3391 0.6055 0.6412 0.021 Uiso 1 1 calc R . . C2 C 0.1630(3) 0.60585(18) 0.7779(3) 0.0176(8) Uani 1 1 d . . . C3 C 0.0689(3) 0.6236(2) 0.8164(3) 0.0220(8) Uani 1 1 d . . . H3 H 0.0143 0.6594 0.7829 0.026 Uiso 1 1 calc R . . C4 C 0.0594(3) 0.5862(2) 0.9059(3) 0.0234(9) Uani 1 1 d . . . H4 H -0.0041 0.5961 0.9343 0.028 Uiso 1 1 calc R . . C5 C 0.1416(3) 0.5339(2) 0.9559(3) 0.0219(8) Uani 1 1 d . . . H5 H 0.1331 0.5100 1.0184 0.026 Uiso 1 1 calc R . . C6 C 0.2341(3) 0.51632(18) 0.9172(3) 0.0193(8) Uani 1 1 d . . . H6 H 0.2893 0.4809 0.9515 0.023 Uiso 1 1 calc R . . C7 C 0.2430(3) 0.55267(18) 0.8258(3) 0.0159(7) Uani 1 1 d . . . C8 C 0.1394(3) 0.6894(2) 0.6184(3) 0.0214(8) Uani 1 1 d . . . H8A H 0.1725 0.7329 0.6560 0.026 Uiso 1 1 calc R . . H8B H 0.0516 0.6886 0.6062 0.026 Uiso 1 1 calc R . . C9 C 0.1585(3) 0.68593(18) 0.5050(3) 0.0159(7) Uani 1 1 d . . . C10 C 0.0934(3) 0.63735(17) 0.4253(3) 0.0164(7) Uani 1 1 d . . . C11 C 0.1001(3) 0.63777(17) 0.3172(3) 0.0166(7) Uani 1 1 d . . . C12 C 0.1683(3) 0.68869(18) 0.2888(3) 0.0171(7) Uani 1 1 d . . . C13 C 0.2395(3) 0.73422(18) 0.3698(3) 0.0193(8) Uani 1 1 d . . . C14 C 0.2352(3) 0.73230(18) 0.4796(3) 0.0181(8) Uani 1 1 d . . . C15 C 0.0173(3) 0.5835(2) 0.4547(4) 0.0278(9) Uani 1 1 d . . . H15A H 0.0502 0.5384 0.4487 0.042 Uiso 1 1 calc R . . H15B H -0.0662 0.5866 0.4025 0.042 Uiso 1 1 calc R . . H15C H 0.0187 0.5907 0.5322 0.042 Uiso 1 1 calc R . . C16 C 0.0338(4) 0.5842(2) 0.2331(3) 0.0287(10) Uani 1 1 d . . . H16A H 0.0625 0.5847 0.1686 0.043 Uiso 1 1 calc R . . H16B H -0.0532 0.5937 0.2071 0.043 Uiso 1 1 calc R . . H16C H 0.0491 0.5393 0.2691 0.043 Uiso 1 1 calc R . . C17 C 0.3208(4) 0.7849(2) 0.3413(4) 0.0346(10) Uani 1 1 d . . . H17A H 0.2939 0.8311 0.3498 0.052 Uiso 1 1 calc R . . H17B H 0.3172 0.7780 0.2632 0.052 Uiso 1 1 calc R . . H17C H 0.4042 0.7786 0.3923 0.052 Uiso 1 1 calc R . . C18 C 0.3124(4) 0.7817(2) 0.5677(4) 0.0355(11) Uani 1 1 d . . . H18A H 0.2692 0.8250 0.5619 0.053 Uiso 1 1 calc R . . H18B H 0.3891 0.7896 0.5548 0.053 Uiso 1 1 calc R . . H18C H 0.3288 0.7625 0.6432 0.053 Uiso 1 1 calc R . . C19 C 0.1640(3) 0.6967(2) 0.1676(3) 0.0240(9) Uani 1 1 d . . . H19A H 0.0896 0.6747 0.1169 0.029 Uiso 1 1 calc R . . H19B H 0.1594 0.7458 0.1486 0.029 Uiso 1 1 calc R . . C20 C 0.3367(3) 0.61303(18) 0.1998(3) 0.0174(8) Uani 1 1 d . . . H20 H 0.3244 0.5891 0.2605 0.021 Uiso 1 1 calc R . . C21 C 0.3142(3) 0.68746(18) 0.0626(3) 0.0161(7) Uani 1 1 d . . . C22 C 0.2787(3) 0.73967(18) -0.0169(3) 0.0190(8) Uani 1 1 d . . . H22 H 0.2133 0.7692 -0.0210 0.023 Uiso 1 1 calc R . . C23 C 0.3438(3) 0.74596(19) -0.0893(3) 0.0211(8) Uani 1 1 d . . . H23 H 0.3239 0.7814 -0.1439 0.025 Uiso 1 1 calc R . . C24 C 0.4388(3) 0.70134(18) -0.0840(3) 0.0189(8) Uani 1 1 d . . . H24 H 0.4803 0.7066 -0.1364 0.023 Uiso 1 1 calc R . . C25 C 0.4736(3) 0.64995(19) -0.0047(3) 0.0182(8) Uani 1 1 d . . . H25 H 0.5380 0.6199 -0.0015 0.022 Uiso 1 1 calc R . . C26 C 0.4096(3) 0.64410(17) 0.0708(3) 0.0146(7) Uani 1 1 d . . . N1 N 0.3253(2) 0.54780(16) 0.7683(2) 0.0174(7) Uani 1 1 d . . . N2 N 0.1988(2) 0.63236(15) 0.6924(2) 0.0166(6) Uani 1 1 d . . . N3 N 0.4211(2) 0.59767(15) 0.1570(2) 0.0150(6) Uani 1 1 d . . . N4 N 0.2695(3) 0.66697(16) 0.1471(2) 0.0179(7) Uani 1 1 d . . . C27 C 0.3306(5) 0.4280(3) 0.4817(6) 0.0739(19) Uani 1 1 d DU . . H27A H 0.3113 0.4215 0.5526 0.089 Uiso 1 1 calc R . . Cl3 Cl 0.2057(2) 0.40434(12) 0.37516(19) 0.0955(7) Uani 1 1 d DU . . Cl4 Cl 0.4563(2) 0.37109(12) 0.49290(19) 0.0956(7) Uani 1 1 d DU . . Cl5 Cl 0.3703(3) 0.51123(12) 0.4803(2) 0.1170(10) Uani 1 1 d DU . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd 0.01324(11) 0.01640(13) 0.01441(12) 0.00117(9) 0.00422(9) 0.00341(9) Cl1 0.0200(3) 0.0214(4) 0.0238(4) 0.0025(3) 0.0090(3) -0.0004(3) Cl2 0.0191(4) 0.0240(4) 0.0284(4) -0.0030(3) 0.0039(3) -0.0037(3) C1 0.0165(14) 0.0204(16) 0.0159(14) -0.0008(13) 0.0063(12) 0.0033(13) C2 0.0178(14) 0.0189(16) 0.0152(14) -0.0017(13) 0.0042(12) 0.0012(13) C3 0.0197(15) 0.0255(18) 0.0228(16) 0.0001(14) 0.0097(13) 0.0071(14) C4 0.0240(16) 0.0273(19) 0.0218(16) -0.0039(14) 0.0117(13) 0.0002(15) C5 0.0245(16) 0.0268(18) 0.0168(15) -0.0033(13) 0.0104(13) -0.0060(14) C6 0.0187(15) 0.0183(16) 0.0184(16) 0.0004(13) 0.0029(13) -0.0016(13) C7 0.0129(13) 0.0179(16) 0.0150(14) -0.0017(12) 0.0024(12) 0.0006(12) C8 0.0250(15) 0.0272(18) 0.0137(15) 0.0060(13) 0.0086(12) 0.0127(14) C9 0.0126(13) 0.0193(16) 0.0158(14) 0.0035(12) 0.0050(11) 0.0065(12) C10 0.0155(13) 0.0126(15) 0.0227(15) 0.0041(12) 0.0084(12) 0.0022(12) C11 0.0134(13) 0.0162(15) 0.0199(15) -0.0002(13) 0.0054(12) 0.0031(12) C12 0.0177(14) 0.0202(16) 0.0156(14) 0.0034(12) 0.0085(11) 0.0090(13) C13 0.0192(14) 0.0166(16) 0.0265(16) 0.0000(13) 0.0134(12) 0.0005(13) C14 0.0155(14) 0.0175(16) 0.0218(16) -0.0016(13) 0.0072(12) 0.0017(13) C15 0.0238(16) 0.0261(19) 0.0349(19) 0.0091(16) 0.0117(15) -0.0058(15) C16 0.0260(17) 0.029(2) 0.0293(19) -0.0088(16) 0.0071(15) -0.0046(16) C17 0.0394(18) 0.026(2) 0.051(2) -0.0029(17) 0.0312(17) -0.0085(17) C18 0.0270(18) 0.044(2) 0.037(2) -0.0190(19) 0.0128(16) -0.0125(18) C19 0.0223(15) 0.034(2) 0.0181(15) 0.0076(14) 0.0104(13) 0.0158(15) C20 0.0201(14) 0.0206(16) 0.0134(14) 0.0047(12) 0.0081(12) 0.0040(13) C21 0.0186(14) 0.0182(16) 0.0132(14) -0.0010(12) 0.0076(11) -0.0011(13) C22 0.0216(15) 0.0194(16) 0.0155(15) -0.0009(13) 0.0057(12) 0.0024(13) C23 0.0276(17) 0.0166(16) 0.0187(16) 0.0012(13) 0.0072(13) -0.0019(14) C24 0.0205(15) 0.0223(17) 0.0154(15) -0.0014(13) 0.0080(12) -0.0060(13) C25 0.0132(13) 0.0230(17) 0.0195(15) -0.0031(13) 0.0068(12) -0.0016(13) C26 0.0152(13) 0.0158(15) 0.0128(14) -0.0003(12) 0.0048(11) -0.0016(12) N1 0.0125(12) 0.0226(14) 0.0153(13) 0.0001(11) 0.0022(10) 0.0006(11) N2 0.0184(12) 0.0200(14) 0.0132(12) 0.0015(11) 0.0074(10) 0.0068(11) N3 0.0143(11) 0.0170(13) 0.0151(12) -0.0006(10) 0.0068(10) 0.0014(11) N4 0.0182(12) 0.0225(15) 0.0155(12) 0.0040(11) 0.0089(10) 0.0073(11) C27 0.105(4) 0.057(3) 0.074(3) -0.016(3) 0.048(3) -0.013(3) Cl3 0.1134(15) 0.0895(14) 0.0847(12) 0.0049(11) 0.0352(11) 0.0103(12) Cl4 0.1139(15) 0.0943(14) 0.0782(12) 0.0054(11) 0.0319(11) -0.0161(12) Cl5 0.197(3) 0.0712(13) 0.0846(13) -0.0125(11) 0.0499(15) -0.0018(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd N3 2.004(3) 3_666 ? Pd N1 2.006(3) . ? Pd Cl1 2.2977(9) . ? Pd Cl2 2.3102(10) . ? C1 N1 1.324(5) . ? C1 N2 1.345(5) . ? C1 H1 0.9500 . ? C2 N2 1.384(5) . ? C2 C3 1.393(5) . ? C2 C7 1.398(5) . ? C3 C4 1.382(6) . ? C3 H3 0.9500 . ? C4 C5 1.403(5) . ? C4 H4 0.9500 . ? C5 C6 1.377(6) . ? C5 H5 0.9500 . ? C6 C7 1.389(5) . ? C6 H6 0.9500 . ? C7 N1 1.395(5) . ? C8 N2 1.474(4) . ? C8 C9 1.521(5) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C14 1.392(5) . ? C9 C10 1.408(5) . ? C10 C11 1.390(5) . ? C10 C15 1.509(5) . ? C11 C12 1.402(5) . ? C11 C16 1.509(5) . ? C12 C13 1.400(5) . ? C12 C19 1.518(5) . ? C13 C14 1.402(5) . ? C13 C17 1.505(5) . ? C14 C18 1.521(5) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 N4 1.470(5) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 N3 1.314(5) . ? C20 N4 1.353(4) . ? C20 H20 0.9500 . ? C21 C26 1.383(5) . ? C21 C22 1.395(5) . ? C21 N4 1.397(5) . ? C22 C23 1.380(6) . ? C22 H22 0.9500 . ? C23 C24 1.403(5) . ? C23 H23 0.9500 . ? C24 C25 1.381(5) . ? C24 H24 0.9500 . ? C25 C26 1.403(5) . ? C25 H25 0.9500 . ? C26 N3 1.389(4) . ? N3 Pd 2.004(3) 3_666 ? C27 Cl3 1.683(6) . ? C27 Cl5 1.703(6) . ? C27 Cl4 1.819(6) . ? C27 H27A 1.0000 . ? 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 N3 Pd N1 173.69(12) 3_666 . ? N3 Pd Cl1 91.34(9) 3_666 . ? N1 Pd Cl1 91.52(9) . . ? N3 Pd Cl2 88.85(8) 3_666 . ? N1 Pd Cl2 89.12(9) . . ? Cl1 Pd Cl2 171.73(4) . . ? N1 C1 N2 112.4(3) . . ? N1 C1 H1 123.8 . . ? N2 C1 H1 123.8 . . ? N2 C2 C3 131.5(3) . . ? N2 C2 C7 106.3(3) . . ? C3 C2 C7 122.2(3) . . ? C4 C3 C2 116.4(3) . . ? C4 C3 H3 121.8 . . ? C2 C3 H3 121.8 . . ? C3 C4 C5 121.4(4) . . ? C3 C4 H4 119.3 . . ? C5 C4 H4 119.3 . . ? C6 C5 C4 122.0(4) . . ? C6 C5 H5 119.0 . . ? C4 C5 H5 119.0 . . ? C5 C6 C7 117.0(3) . . ? C5 C6 H6 121.5 . . ? C7 C6 H6 121.5 . . ? C6 C7 N1 131.0(3) . . ? C6 C7 C2 120.9(3) . . ? N1 C7 C2 108.0(3) . . ? N2 C8 C9 111.7(3) . . ? N2 C8 H8A 109.3 . . ? C9 C8 H8A 109.3 . . ? N2 C8 H8B 109.3 . . ? C9 C8 H8B 109.3 . . ? H8A C8 H8B 107.9 . . ? C14 C9 C10 121.2(3) . . ? C14 C9 C8 119.9(3) . . ? C10 C9 C8 118.9(3) . . ? C11 C10 C9 119.8(3) . . ? C11 C10 C15 118.7(3) . . ? C9 C10 C15 121.5(3) . . ? C10 C11 C12 118.8(3) . . ? C10 C11 C16 119.7(3) . . ? C12 C11 C16 121.6(3) . . ? C13 C12 C11 121.5(3) . . ? C13 C12 C19 118.3(3) . . ? C11 C12 C19 120.2(3) . . ? C12 C13 C14 119.3(3) . . ? C12 C13 C17 121.3(3) . . ? C14 C13 C17 119.5(3) . . ? C9 C14 C13 119.1(3) . . ? C9 C14 C18 121.5(3) . . ? C13 C14 C18 119.3(3) . . ? C10 C15 H15A 109.5 . . ? C10 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C10 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C13 C17 H17A 109.5 . . ? C13 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C13 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C14 C18 H18A 109.5 . . ? C14 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C14 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N4 C19 C12 113.1(3) . . ? N4 C19 H19A 109.0 . . ? C12 C19 H19A 109.0 . . ? N4 C19 H19B 109.0 . . ? C12 C19 H19B 109.0 . . ? H19A C19 H19B 107.8 . . ? N3 C20 N4 112.0(3) . . ? N3 C20 H20 124.0 . . ? N4 C20 H20 124.0 . . ? C26 C21 C22 123.0(3) . . ? C26 C21 N4 105.6(3) . . ? C22 C21 N4 131.3(3) . . ? C23 C22 C21 116.2(3) . . ? C23 C22 H22 121.9 . . ? C21 C22 H22 121.9 . . ? C22 C23 C24 121.6(3) . . ? C22 C23 H23 119.2 . . ? C24 C23 H23 119.2 . . ? C25 C24 C23 121.8(3) . . ? C25 C24 H24 119.1 . . ? C23 C24 H24 119.1 . . ? C24 C25 C26 117.1(3) . . ? C24 C25 H25 121.5 . . ? C26 C25 H25 121.5 . . ? C21 C26 N3 109.0(3) . . ? C21 C26 C25 120.3(3) . . ? N3 C26 C25 130.6(3) . . ? C1 N1 C7 106.1(3) . . ? C1 N1 Pd 129.5(3) . . ? C7 N1 Pd 124.3(2) . . ? C1 N2 C2 107.1(3) . . ? C1 N2 C8 127.8(3) . . ? C2 N2 C8 125.1(3) . . ? C20 N3 C26 106.4(3) . . ? C20 N3 Pd 129.1(2) . 3_666 ? C26 N3 Pd 124.4(2) . 3_666 ? C20 N4 C21 106.9(3) . . ? C20 N4 C19 127.7(3) . . ? C21 N4 C19 125.2(3) . . ? Cl3 C27 Cl5 115.1(4) . . ? Cl3 C27 Cl4 111.0(3) . . ? Cl5 C27 Cl4 111.9(4) . . ? Cl3 C27 H27A 106.1 . . ? Cl5 C27 H27A 106.1 . . ? Cl4 C27 H27A 106.1 . . ? _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 1.111 _refine_diff_density_min -1.580 _refine_diff_density_rms 0.170 #==========# data_3 _database_code_depnum_ccdc_archive 'CCDC 767080' #TrackingRef '- Compds-R1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C66 H78 Cl8 N10 Pd2' _chemical_formula_weight 1507.78 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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.0928(8) _cell_length_b 14.3947(8) _cell_length_c 34.027(2) _cell_angle_alpha 90.00 _cell_angle_beta 101.7330(10) _cell_angle_gamma 90.00 _cell_volume 6758.6(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(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 0.28 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.482 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3088 _exptl_absorpt_coefficient_mu 0.897 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7875 _exptl_absorpt_correction_T_max 0.8273 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 APEX _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39794 _diffrn_reflns_av_R_equivalents 0.0315 _diffrn_reflns_av_sigmaI/netI 0.0380 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 26.50 _reflns_number_total 13853 _reflns_number_gt 12240 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0560P)^2^+16.0506P] 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 13853 _refine_ls_number_parameters 823 _refine_ls_number_restraints 184 _refine_ls_R_factor_all 0.0537 _refine_ls_R_factor_gt 0.0466 _refine_ls_wR_factor_ref 0.1191 _refine_ls_wR_factor_gt 0.1149 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.030 _refine_ls_shift/su_mean 0.001 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 0.309117(19) 0.237470(18) 1.035155(8) 0.01829(8) Uani 1 1 d . . . Pd2 Pd 0.067492(18) 0.305316(19) 0.802195(8) 0.01911(8) Uani 1 1 d . . . N1 N 0.1925(2) 0.2656(2) 0.78829(9) 0.0225(6) Uani 1 1 d . . . N2 N 0.3496(2) 0.2560(2) 0.78963(9) 0.0223(6) Uani 1 1 d . . . N3 N 0.4393(2) 0.2745(2) 1.02489(9) 0.0211(6) Uani 1 1 d . . . N4 N 0.5551(2) 0.3348(2) 0.99739(8) 0.0203(6) Uani 1 1 d . . . N5 N -0.0611(2) 0.3404(2) 0.81446(9) 0.0218(6) Uani 1 1 d . . . N6 N -0.1903(2) 0.3227(2) 0.84122(8) 0.0208(6) Uani 1 1 d . . . Cl1 Cl 0.11396(7) 0.45828(6) 0.80192(3) 0.0270(2) Uani 1 1 d . . . Cl2 Cl 0.02440(8) 0.15240(7) 0.80423(4) 0.0457(3) Uani 1 1 d . . . Cl3 Cl 0.25105(7) 0.38201(6) 1.01470(3) 0.0298(2) Uani 1 1 d . . . Cl4 Cl 0.36582(7) 0.08928(7) 1.05212(3) 0.0334(2) Uani 1 1 d . . . N8 N 0.1817(2) 0.2054(2) 1.04953(9) 0.0212(6) Uani 1 1 d . . . C1 C 0.2798(3) 0.2857(3) 0.80850(11) 0.0245(8) Uani 1 1 d . . . H1A H 0.2923 0.3174 0.8335 0.029 Uiso 1 1 calc R . . C2 C 0.3036(3) 0.2159(2) 0.75390(10) 0.0201(7) Uani 1 1 d . . . C3 C 0.3393(3) 0.1799(2) 0.72155(10) 0.0220(7) Uani 1 1 d . . . H3A H 0.4068 0.1781 0.7219 0.026 Uiso 1 1 calc R . . C4 C 0.2724(3) 0.1469(2) 0.68901(10) 0.0230(7) Uani 1 1 d . . . C5 C 0.1713(3) 0.1482(2) 0.68908(11) 0.0230(7) Uani 1 1 d . . . C6 C 0.1382(3) 0.1849(2) 0.72109(11) 0.0227(7) Uani 1 1 d . . . H6A H 0.0708 0.1861 0.7211 0.027 Uiso 1 1 calc R . . C7 C 0.2049(3) 0.2204(2) 0.75350(10) 0.0199(7) Uani 1 1 d . . . C8 C 0.0995(3) 0.1094(3) 0.65382(12) 0.0322(9) Uani 1 1 d . . . H8A H 0.0339 0.1136 0.6592 0.048 Uiso 1 1 calc R . . H8B H 0.1152 0.0442 0.6497 0.048 Uiso 1 1 calc R . . H8C H 0.1029 0.1452 0.6296 0.048 Uiso 1 1 calc R . . C9 C 0.3083(3) 0.1107(3) 0.65305(11) 0.0292(8) Uani 1 1 d . . . H9A H 0.3781 0.1224 0.6566 0.044 Uiso 1 1 calc R . . H9B H 0.2742 0.1424 0.6288 0.044 Uiso 1 1 calc R . . H9C H 0.2961 0.0437 0.6504 0.044 Uiso 1 1 calc R . . C10 C 0.4545(3) 0.2712(3) 0.80185(11) 0.0268(8) Uani 1 1 d . . . H10A H 0.4738 0.3214 0.7852 0.032 Uiso 1 1 calc R . . H10B H 0.4888 0.2139 0.7967 0.032 Uiso 1 1 calc R . . C11 C 0.4850(2) 0.3904(3) 0.85743(11) 0.0232(8) Uani 1 1 d . . . C12 C 0.5218(2) 0.4138(3) 0.89779(11) 0.0214(7) Uani 1 1 d . . . C13 C 0.5607(2) 0.3436(3) 0.92490(10) 0.0200(7) Uani 1 1 d . . . C14 C 0.5572(3) 0.2506(2) 0.91356(11) 0.0210(7) Uani 1 1 d . . . C15 C 0.5169(3) 0.2263(3) 0.87381(11) 0.0230(7) Uani 1 1 d . . . C16 C 0.4857(2) 0.2972(3) 0.84567(10) 0.0223(7) Uani 1 1 d . . . C17 C 0.4416(3) 0.4653(3) 0.82799(12) 0.0342(9) Uani 1 1 d . . . H17A H 0.4517 0.5261 0.8411 0.051 Uiso 0.50 1 calc PR . . H17B H 0.3719 0.4540 0.8190 0.051 Uiso 0.50 1 calc PR . . H17C H 0.4729 0.4642 0.8048 0.051 Uiso 0.50 1 calc PR . . H17D H 0.4127 0.4367 0.8022 0.051 Uiso 0.50 1 calc PR . . H17E H 0.4924 0.5088 0.8243 0.051 Uiso 0.50 1 calc PR . . H17F H 0.3914 0.4987 0.8385 0.051 Uiso 0.50 1 calc PR . . C18 C 0.5178(3) 0.5134(3) 0.91131(13) 0.0325(9) Uani 1 1 d . . . H18A H 0.5058 0.5543 0.8878 0.049 Uiso 0.50 1 calc PR . . H18B H 0.5797 0.5300 0.9288 0.049 Uiso 0.50 1 calc PR . . H18C H 0.4655 0.5205 0.9261 0.049 Uiso 0.50 1 calc PR . . H18D H 0.5282 0.5155 0.9407 0.049 Uiso 0.50 1 calc PR . . H18E H 0.4542 0.5399 0.8997 0.049 Uiso 0.50 1 calc PR . . H18F H 0.5685 0.5494 0.9024 0.049 Uiso 0.50 1 calc PR . . C19 C 0.5945(3) 0.1749(3) 0.94396(12) 0.0292(8) Uani 1 1 d . . . H19A H 0.5656 0.1152 0.9341 0.044 Uiso 0.50 1 calc PR . . H19B H 0.5767 0.1899 0.9696 0.044 Uiso 0.50 1 calc PR . . H19C H 0.6652 0.1709 0.9477 0.044 Uiso 0.50 1 calc PR . . H19D H 0.6394 0.2021 0.9669 0.044 Uiso 0.50 1 calc PR . . H19E H 0.6282 0.1274 0.9314 0.044 Uiso 0.50 1 calc PR . . H19F H 0.5398 0.1465 0.9532 0.044 Uiso 0.50 1 calc PR . . C20 C 0.5068(3) 0.1257(3) 0.86109(13) 0.0342(9) Uani 1 1 d . . . H20A H 0.4865 0.1221 0.8318 0.051 Uiso 0.50 1 calc PR . . H20B H 0.4581 0.0956 0.8736 0.051 Uiso 0.50 1 calc PR . . H20C H 0.5692 0.0941 0.8696 0.051 Uiso 0.50 1 calc PR . . H20D H 0.5227 0.0858 0.8849 0.051 Uiso 0.50 1 calc PR . . H20E H 0.5511 0.1123 0.8431 0.051 Uiso 0.50 1 calc PR . . H20F H 0.4400 0.1137 0.8471 0.051 Uiso 0.50 1 calc PR . . C21 C 0.6086(3) 0.3697(3) 0.96753(10) 0.0246(8) Uani 1 1 d . . . H21A H 0.6752 0.3443 0.9736 0.030 Uiso 1 1 calc R . . H21B H 0.6133 0.4382 0.9697 0.030 Uiso 1 1 calc R . . C22 C 0.4613(3) 0.3089(3) 0.99192(11) 0.0228(7) Uani 1 1 d . . . H22A H 0.4163 0.3148 0.9672 0.027 Uiso 1 1 calc R . . C23 C 0.5970(3) 0.3166(2) 1.03729(10) 0.0217(7) Uani 1 1 d . . . C24 C 0.6898(3) 0.3323(3) 1.05937(11) 0.0257(8) Uani 1 1 d . . . H24A H 0.7390 0.3577 1.0472 0.031 Uiso 1 1 calc R . . C25 C 0.7079(3) 0.3097(3) 1.09970(12) 0.0306(9) Uani 1 1 d . . . C26 C 0.6339(3) 0.2710(3) 1.11736(11) 0.0300(9) Uani 1 1 d . . . C27 C 0.5421(3) 0.2544(3) 1.09471(11) 0.0259(8) Uani 1 1 d . . . H27A H 0.4929 0.2275 1.1065 0.031 Uiso 1 1 calc R . . C28 C 0.5238(3) 0.2785(2) 1.05410(11) 0.0208(7) Uani 1 1 d . . . C29 C 0.8081(3) 0.3257(3) 1.12501(13) 0.0421(11) Uani 1 1 d . . . H29A H 0.8508 0.3502 1.1081 0.063 Uiso 1 1 calc R . . H29B H 0.8342 0.2668 1.1370 0.063 Uiso 1 1 calc R . . H29C H 0.8041 0.3704 1.1463 0.063 Uiso 1 1 calc R . . C30 C 0.6536(4) 0.2489(3) 1.16160(13) 0.0471(12) Uani 1 1 d . . . H30A H 0.5964 0.2194 1.1684 0.071 Uiso 1 1 calc R . . H30B H 0.6682 0.3065 1.1770 0.071 Uiso 1 1 calc R . . H30C H 0.7090 0.2066 1.1681 0.071 Uiso 1 1 calc R . . C31 C 0.0944(3) 0.2146(2) 1.02675(10) 0.0211(7) Uani 1 1 d . . . H31A H 0.0827 0.2355 0.9997 0.025 Uiso 1 1 calc R . . C32 C 0.1676(3) 0.1736(2) 1.08667(10) 0.0196(7) Uani 1 1 d . . . C33 C 0.2329(3) 0.1506(2) 1.12203(10) 0.0226(7) Uani 1 1 d . . . H33A H 0.3008 0.1563 1.1238 0.027 Uiso 1 1 calc R . . C34 C 0.1962(3) 0.1195(3) 1.15448(11) 0.0251(8) Uani 1 1 d . . . C35 C 0.0950(3) 0.1120(2) 1.15218(10) 0.0233(8) Uani 1 1 d . . . C36 C 0.0303(3) 0.1346(2) 1.11717(10) 0.0225(7) Uani 1 1 d . . . H36A H -0.0377 0.1296 1.1153 0.027 Uiso 1 1 calc R . . C37 C 0.0687(3) 0.1649(2) 1.08473(10) 0.0199(7) Uani 1 1 d . . . C38 C 0.2658(3) 0.0882(3) 1.19185(12) 0.0342(9) Uani 1 1 d . . . H38A H 0.3319 0.1061 1.1901 0.051 Uiso 1 1 calc R . . H38B H 0.2622 0.0205 1.1943 0.051 Uiso 1 1 calc R . . H38C H 0.2486 0.1176 1.2154 0.051 Uiso 1 1 calc R . . C39 C 0.0556(3) 0.0796(3) 1.18789(11) 0.0334(9) Uani 1 1 d . . . H39A H -0.0153 0.0798 1.1811 0.050 Uiso 1 1 calc R . . H39B H 0.0779 0.1215 1.2106 0.050 Uiso 1 1 calc R . . H39C H 0.0788 0.0165 1.1952 0.050 Uiso 1 1 calc R . . C40 C -0.0818(3) 0.1919(3) 1.03189(11) 0.0251(8) Uani 1 1 d . . . H40A H -0.1106 0.2364 1.0483 0.030 Uiso 1 1 calc R . . H40B H -0.1078 0.1295 1.0359 0.030 Uiso 1 1 calc R . . C41 C -0.1129(2) 0.2183(3) 0.98827(10) 0.0202(7) Uani 1 1 d . . . C42 C -0.1202(3) 0.3124(2) 0.97745(10) 0.0212(7) Uani 1 1 d . . . C43 C -0.1623(3) 0.3369(2) 0.93802(11) 0.0223(7) Uani 1 1 d . . . C44 C -0.1957(2) 0.2671(3) 0.90994(10) 0.0204(7) Uani 1 1 d . . . C45 C -0.1789(3) 0.1735(3) 0.91954(11) 0.0226(7) Uani 1 1 d . . . C46 C -0.1377(3) 0.1483(3) 0.95930(11) 0.0234(7) Uani 1 1 d . . . C47 C -0.1221(3) 0.0470(3) 0.96924(14) 0.0361(10) Uani 1 1 d . . . H47A H -0.1428 0.0099 0.9449 0.054 Uiso 0.50 1 calc PR . . H47B H -0.1602 0.0292 0.9892 0.054 Uiso 0.50 1 calc PR . . H47C H -0.0533 0.0357 0.9802 0.054 Uiso 0.50 1 calc PR . . H47D H -0.0947 0.0400 0.9980 0.054 Uiso 0.50 1 calc PR . . H47E H -0.0773 0.0207 0.9536 0.054 Uiso 0.50 1 calc PR . . H47F H -0.1843 0.0142 0.9626 0.054 Uiso 0.50 1 calc PR . . C48 C -0.2033(3) 0.0976(3) 0.88824(13) 0.0361(10) Uani 1 1 d . . . H48A H -0.1844 0.0372 0.9007 0.054 Uiso 0.50 1 calc PR . . H48B H -0.1682 0.1086 0.8666 0.054 Uiso 0.50 1 calc PR . . H48C H -0.2732 0.0978 0.8772 0.054 Uiso 0.50 1 calc PR . . H48D H -0.2328 0.1252 0.8623 0.054 Uiso 0.50 1 calc PR . . H48E H -0.2490 0.0538 0.8964 0.054 Uiso 0.50 1 calc PR . . H48F H -0.1440 0.0646 0.8858 0.054 Uiso 0.50 1 calc PR . . C49 C -0.1710(3) 0.4383(3) 0.92619(13) 0.0336(9) Uani 1 1 d . . . H49A H -0.2241 0.4461 0.9029 0.050 Uiso 0.50 1 calc PR . . H49B H -0.1102 0.4593 0.9194 0.050 Uiso 0.50 1 calc PR . . H49C H -0.1844 0.4752 0.9487 0.050 Uiso 0.50 1 calc PR . . H49D H -0.1217 0.4743 0.9444 0.050 Uiso 0.50 1 calc PR . . H49E H -0.2356 0.4611 0.9279 0.050 Uiso 0.50 1 calc PR . . H49F H -0.1614 0.4452 0.8986 0.050 Uiso 0.50 1 calc PR . . C50 C -0.0824(3) 0.3877(3) 1.00754(12) 0.0328(9) Uani 1 1 d . . . H50A H -0.0329 0.3617 1.0292 0.049 Uiso 0.50 1 calc PR . . H50B H -0.1359 0.4126 1.0188 0.049 Uiso 0.50 1 calc PR . . H50C H -0.0540 0.4377 0.9942 0.049 Uiso 0.50 1 calc PR . . H50D H -0.1156 0.4463 0.9989 0.049 Uiso 0.50 1 calc PR . . H50E H -0.0126 0.3954 1.0093 0.049 Uiso 0.50 1 calc PR . . H50F H -0.0945 0.3702 1.0339 0.049 Uiso 0.50 1 calc PR . . C51 C -0.0951(3) 0.3067(3) 0.84505(10) 0.0228(8) Uani 1 1 d . . . H51A H -0.0566 0.2750 0.8671 0.027 Uiso 1 1 calc R . . C52 C -0.2215(2) 0.3682(2) 0.80535(10) 0.0183(7) Uani 1 1 d . . . C53 C -0.3129(2) 0.3970(2) 0.78542(10) 0.0197(7) Uani 1 1 d . . . H53A H -0.3680 0.3885 0.7971 0.024 Uiso 1 1 calc R . . C54 C -0.3213(3) 0.4384(2) 0.74807(10) 0.0205(7) Uani 1 1 d . . . C55 C -0.2382(3) 0.4540(2) 0.73144(10) 0.0203(7) Uani 1 1 d . . . C56 C -0.1469(3) 0.4249(2) 0.75183(10) 0.0204(7) Uani 1 1 d . . . H56A H -0.0910 0.4353 0.7409 0.024 Uiso 1 1 calc R . . C57 C -0.1398(2) 0.3804(2) 0.78870(10) 0.0183(7) Uani 1 1 d . . . C58 C -0.4202(3) 0.4683(3) 0.72572(11) 0.0274(8) Uani 1 1 d . . . H58A H -0.4696 0.4456 0.7399 0.041 Uiso 1 1 calc R . . H58B H -0.4322 0.4424 0.6985 0.041 Uiso 1 1 calc R . . H58C H -0.4229 0.5362 0.7242 0.041 Uiso 1 1 calc R . . C59 C -0.2476(3) 0.5023(3) 0.69183(11) 0.0285(8) Uani 1 1 d . . . H59A H -0.1835 0.5087 0.6852 0.043 Uiso 1 1 calc R . . H59B H -0.2760 0.5640 0.6934 0.043 Uiso 1 1 calc R . . H59C H -0.2896 0.4658 0.6710 0.043 Uiso 1 1 calc R . . C66 C -0.2527(3) 0.2952(3) 0.86905(11) 0.0255(8) Uani 1 1 d . . . H65A H -0.2941 0.2426 0.8573 0.031 Uiso 1 1 calc R . . H65B H -0.2958 0.3478 0.8723 0.031 Uiso 1 1 calc R . . N7 N 0.0238(2) 0.1909(2) 1.04624(8) 0.0197(6) Uani 1 1 d . . . C60 C 0.1715(6) 0.1305(7) 0.8958(3) 0.106(3) Uani 1 1 d U A 1 H60A H 0.1752 0.0637 0.8893 0.128 Uiso 1 1 calc R A 1 H60B H 0.1583 0.1653 0.8701 0.128 Uiso 1 1 calc R A 1 Cl5 Cl 0.2828(4) 0.1663(3) 0.9243(2) 0.128(2) Uani 0.60 1 d PDU A 1 Cl6 Cl 0.0742(2) 0.1482(2) 0.92093(7) 0.0589(6) Uani 0.60 1 d PDU A 1 Cl5' Cl 0.2781(6) 0.1653(6) 0.90508(19) 0.090(2) Uiso 0.40 1 d PDU B 2 Cl6' Cl 0.1139(9) 0.1248(9) 0.9315(4) 0.195(5) Uiso 0.40 1 d PDU C 2 C62 C 0.3123(4) 0.6442(3) 0.74058(14) 0.0398(10) Uani 1 1 d U . . C63 C 0.2126(3) 0.6484(3) 0.74526(14) 0.0407(10) Uani 1 1 d U . . H63D H 0.2014 0.7073 0.7580 0.061 Uiso 1 1 calc R . . H63E H 0.1996 0.5966 0.7621 0.061 Uiso 1 1 calc R . . H63F H 0.1694 0.6442 0.7188 0.061 Uiso 1 1 calc R . . C64 C 0.3000(4) 0.9314(3) 0.93319(17) 0.0457(12) Uani 1 1 d U . . C65 C 0.3907(4) 0.9596(4) 0.95908(18) 0.0617(15) Uani 1 1 d U . . H66D H 0.4326 0.9052 0.9660 0.093 Uiso 1 1 calc R . . H66E H 0.3773 0.9874 0.9837 0.093 Uiso 1 1 calc R . . H66F H 0.4233 1.0053 0.9451 0.093 Uiso 1 1 calc R . . N9 N 0.3901(4) 0.6399(3) 0.73701(18) 0.0755(16) Uani 1 1 d U . . N10 N 0.2295(4) 0.9103(3) 0.91361(17) 0.0641(13) Uani 1 1 d U . . C61 C 0.1669(10) 0.3763(9) 0.9097(4) 0.076(3) Uani 0.60 1 d PU D 1 H61E H 0.1454 0.3373 0.8856 0.091 Uiso 0.60 1 calc PR D 1 H61F H 0.1781 0.3348 0.9334 0.091 Uiso 0.60 1 calc PR D 1 Cl7 Cl 0.2809(2) 0.4327(2) 0.90629(9) 0.0636(7) Uani 0.60 1 d PDU D 1 Cl8 Cl 0.0763(2) 0.4537(2) 0.91364(8) 0.0728(7) Uani 0.60 1 d PDU D 1 C61' C 0.1391(15) 0.4191(17) 0.9107(9) 0.107(5) Uiso 0.40 1 d PDU E 2 H61G H 0.1014 0.4347 0.8837 0.128 Uiso 0.40 1 calc PR E 2 H61H H 0.1414 0.4763 0.9270 0.128 Uiso 0.40 1 calc PR E 2 Cl7' Cl 0.0751(9) 0.3470(9) 0.9293(4) 0.218(4) Uani 0.40 1 d PDU E 2 Cl8' Cl 0.2455(9) 0.4012(8) 0.9055(3) 0.183(4) Uani 0.40 1 d PDU E 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 0.01594(14) 0.02046(14) 0.01974(14) -0.00098(10) 0.00660(10) -0.00064(10) Pd2 0.01118(13) 0.02366(15) 0.02367(14) -0.00083(10) 0.00629(10) 0.00070(10) N1 0.0142(15) 0.0275(16) 0.0262(16) -0.0046(12) 0.0056(12) 0.0003(12) N2 0.0123(14) 0.0316(17) 0.0227(15) -0.0051(12) 0.0027(12) -0.0013(12) N3 0.0185(15) 0.0233(15) 0.0220(15) -0.0036(12) 0.0056(12) -0.0013(12) N4 0.0165(15) 0.0271(16) 0.0178(14) -0.0036(12) 0.0043(11) -0.0042(12) N5 0.0154(15) 0.0275(16) 0.0237(15) 0.0015(12) 0.0067(12) 0.0032(12) N6 0.0140(14) 0.0312(16) 0.0180(14) 0.0031(12) 0.0054(11) 0.0033(12) Cl1 0.0275(5) 0.0252(4) 0.0299(5) -0.0011(4) 0.0098(4) -0.0025(4) Cl2 0.0251(5) 0.0266(5) 0.0903(9) -0.0003(5) 0.0236(6) -0.0020(4) Cl3 0.0318(5) 0.0247(5) 0.0353(5) 0.0054(4) 0.0122(4) 0.0055(4) Cl4 0.0282(5) 0.0231(5) 0.0526(6) 0.0033(4) 0.0168(4) 0.0043(4) N8 0.0206(15) 0.0238(15) 0.0203(15) 0.0016(12) 0.0065(12) 0.0006(12) C1 0.0163(18) 0.030(2) 0.0279(19) -0.0067(15) 0.0067(15) -0.0033(15) C2 0.0165(17) 0.0222(18) 0.0206(17) -0.0024(13) 0.0015(13) 0.0006(14) C3 0.0187(18) 0.0255(19) 0.0223(17) -0.0004(14) 0.0054(14) 0.0032(14) C4 0.027(2) 0.0200(18) 0.0209(17) 0.0013(14) 0.0031(15) 0.0058(15) C5 0.0218(18) 0.0189(17) 0.0252(18) -0.0001(14) -0.0023(14) 0.0026(14) C6 0.0145(17) 0.0214(18) 0.0312(19) 0.0001(14) 0.0021(14) 0.0005(14) C7 0.0187(17) 0.0197(17) 0.0214(17) -0.0014(13) 0.0046(14) 0.0000(14) C8 0.028(2) 0.036(2) 0.028(2) -0.0072(17) -0.0047(16) -0.0001(17) C9 0.034(2) 0.030(2) 0.0233(19) -0.0048(15) 0.0052(16) 0.0069(17) C10 0.0102(17) 0.048(2) 0.0231(18) -0.0082(16) 0.0049(14) -0.0031(16) C11 0.0125(16) 0.033(2) 0.0264(18) -0.0015(15) 0.0087(14) -0.0026(14) C12 0.0143(17) 0.0255(19) 0.0254(18) -0.0034(14) 0.0062(14) -0.0020(14) C13 0.0135(16) 0.0276(19) 0.0206(17) -0.0055(14) 0.0078(13) -0.0061(14) C14 0.0145(17) 0.0259(19) 0.0246(18) -0.0002(14) 0.0088(14) -0.0027(14) C15 0.0143(17) 0.0284(19) 0.0282(19) -0.0080(15) 0.0089(14) -0.0044(14) C16 0.0110(16) 0.034(2) 0.0228(18) -0.0061(15) 0.0055(13) -0.0049(14) C17 0.026(2) 0.041(2) 0.034(2) 0.0071(18) 0.0019(17) -0.0009(18) C18 0.031(2) 0.026(2) 0.039(2) -0.0093(17) 0.0026(18) 0.0004(17) C19 0.028(2) 0.030(2) 0.031(2) 0.0010(16) 0.0090(16) 0.0004(16) C20 0.028(2) 0.031(2) 0.043(2) -0.0139(18) 0.0068(18) -0.0038(17) C21 0.0201(18) 0.035(2) 0.0207(17) -0.0035(15) 0.0086(14) -0.0078(15) C22 0.0173(17) 0.030(2) 0.0213(17) -0.0059(14) 0.0052(14) -0.0037(14) C23 0.0224(18) 0.0204(18) 0.0223(17) -0.0055(13) 0.0046(14) 0.0006(14) C24 0.0208(19) 0.0259(19) 0.0286(19) -0.0067(15) 0.0007(15) -0.0023(15) C25 0.029(2) 0.025(2) 0.033(2) -0.0099(16) -0.0054(17) 0.0030(16) C26 0.041(2) 0.0219(19) 0.0233(19) -0.0010(15) -0.0034(17) 0.0034(17) C27 0.035(2) 0.0215(19) 0.0215(18) -0.0001(14) 0.0052(16) -0.0005(15) C28 0.0210(18) 0.0175(17) 0.0241(18) -0.0054(13) 0.0048(14) 0.0003(14) C29 0.035(2) 0.046(3) 0.037(2) -0.004(2) -0.0132(19) -0.002(2) C30 0.062(3) 0.045(3) 0.028(2) 0.0048(19) -0.005(2) -0.002(2) C31 0.0219(18) 0.0251(18) 0.0175(16) 0.0046(13) 0.0071(14) 0.0000(14) C32 0.0212(18) 0.0201(17) 0.0174(16) -0.0018(13) 0.0041(13) -0.0009(14) C33 0.0209(18) 0.0217(18) 0.0242(18) -0.0016(14) 0.0022(14) -0.0002(14) C34 0.033(2) 0.0216(18) 0.0191(17) -0.0022(14) 0.0019(15) -0.0003(15) C35 0.033(2) 0.0188(17) 0.0186(17) -0.0009(13) 0.0069(15) -0.0058(15) C36 0.0262(19) 0.0212(18) 0.0217(17) -0.0020(14) 0.0087(14) -0.0039(14) C37 0.0235(18) 0.0183(17) 0.0177(16) -0.0009(13) 0.0038(14) 0.0003(14) C38 0.043(3) 0.031(2) 0.025(2) 0.0017(16) -0.0025(18) 0.0025(18) C39 0.046(3) 0.034(2) 0.0218(19) 0.0030(16) 0.0098(17) -0.0079(19) C40 0.0149(17) 0.037(2) 0.0228(18) 0.0067(15) 0.0026(14) -0.0014(15) C41 0.0116(16) 0.0289(19) 0.0202(17) 0.0031(14) 0.0037(13) -0.0010(14) C42 0.0168(17) 0.0251(19) 0.0231(17) -0.0015(14) 0.0077(14) -0.0003(14) C43 0.0225(18) 0.0227(18) 0.0245(18) 0.0026(14) 0.0117(15) 0.0041(14) C44 0.0137(16) 0.033(2) 0.0161(16) 0.0012(14) 0.0060(13) 0.0005(14) C45 0.0171(17) 0.0273(19) 0.0237(18) -0.0041(14) 0.0049(14) -0.0021(14) C46 0.0155(17) 0.0239(19) 0.0303(19) 0.0031(15) 0.0038(14) 0.0010(14) C47 0.032(2) 0.026(2) 0.048(3) 0.0053(18) 0.0012(19) 0.0039(17) C48 0.033(2) 0.037(2) 0.037(2) -0.0126(18) 0.0028(18) -0.0018(18) C49 0.043(3) 0.027(2) 0.034(2) 0.0074(17) 0.0145(19) 0.0061(18) C50 0.038(2) 0.027(2) 0.033(2) -0.0079(16) 0.0081(18) -0.0040(17) C51 0.0148(17) 0.036(2) 0.0184(17) 0.0031(14) 0.0047(13) 0.0052(15) C52 0.0171(17) 0.0215(17) 0.0170(16) -0.0016(13) 0.0053(13) -0.0005(13) C53 0.0144(16) 0.0235(18) 0.0222(17) -0.0010(14) 0.0057(13) -0.0004(13) C54 0.0190(18) 0.0207(17) 0.0205(17) 0.0000(13) 0.0004(14) -0.0003(14) C55 0.0233(18) 0.0190(17) 0.0184(16) -0.0002(13) 0.0039(14) -0.0014(14) C56 0.0183(17) 0.0232(18) 0.0214(17) -0.0008(13) 0.0078(14) 0.0001(14) C57 0.0140(16) 0.0187(17) 0.0224(17) -0.0040(13) 0.0042(13) 0.0011(13) C58 0.0209(19) 0.032(2) 0.0273(19) 0.0089(16) 0.0009(15) 0.0019(16) C59 0.028(2) 0.032(2) 0.0261(19) 0.0072(16) 0.0072(16) 0.0014(16) C66 0.0155(17) 0.041(2) 0.0210(18) 0.0079(15) 0.0070(14) 0.0036(15) N7 0.0157(14) 0.0272(16) 0.0159(14) 0.0031(11) 0.0025(11) -0.0003(12) C60 0.106(6) 0.123(6) 0.098(5) 0.041(5) 0.040(5) 0.048(5) Cl5 0.104(3) 0.072(2) 0.179(5) -0.025(3) -0.039(4) 0.0064(19) Cl6 0.0657(16) 0.0696(16) 0.0444(12) -0.0028(11) 0.0182(11) 0.0058(12) C62 0.048(3) 0.032(2) 0.043(2) -0.0035(18) 0.018(2) -0.011(2) C63 0.034(2) 0.044(3) 0.041(2) 0.002(2) 0.0001(19) -0.004(2) C64 0.044(3) 0.034(2) 0.067(3) 0.002(2) 0.029(3) 0.002(2) C65 0.057(3) 0.064(4) 0.063(3) -0.002(3) 0.011(3) 0.023(3) N9 0.072(3) 0.053(3) 0.122(4) -0.019(3) 0.066(3) -0.021(2) N10 0.048(3) 0.046(3) 0.106(4) -0.009(3) 0.033(3) -0.011(2) C61 0.087(7) 0.065(6) 0.065(6) -0.003(5) -0.008(6) -0.012(6) Cl7 0.0509(14) 0.0798(19) 0.0574(14) 0.0096(13) 0.0043(11) -0.0263(13) Cl8 0.0661(17) 0.0844(19) 0.0666(15) -0.0131(14) 0.0106(13) 0.0059(14) Cl7' 0.223(8) 0.215(8) 0.201(7) 0.007(7) 0.009(7) 0.031(7) Cl8' 0.226(8) 0.170(7) 0.135(6) 0.026(5) -0.008(6) -0.090(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N8 2.008(3) . ? Pd1 N3 2.009(3) . ? Pd1 Cl3 2.2916(9) . ? Pd1 Cl4 2.3097(10) . ? Pd2 N1 1.999(3) . ? Pd2 N5 2.005(3) . ? Pd2 Cl2 2.2882(11) . ? Pd2 Cl1 2.2978(10) . ? N1 C1 1.313(5) . ? N1 C7 1.392(4) . ? N2 C1 1.349(5) . ? N2 C2 1.383(4) . ? N2 C10 1.467(4) . ? N3 C22 1.319(5) . ? N3 C28 1.388(5) . ? N4 C22 1.350(4) . ? N4 C23 1.391(4) . ? N4 C21 1.471(4) . ? N5 C51 1.324(4) . ? N5 C57 1.391(4) . ? N6 C51 1.341(4) . ? N6 C52 1.376(4) . ? N6 C66 1.471(4) . ? N8 C31 1.321(5) . ? N8 C32 1.395(4) . ? C1 H1A 0.9500 . ? C2 C7 1.390(5) . ? C2 C3 1.399(5) . ? C3 C4 1.384(5) . ? C3 H3A 0.9500 . ? C4 C5 1.426(5) . ? C4 C9 1.509(5) . ? C5 C6 1.375(5) . ? C5 C8 1.510(5) . ? C6 C7 1.393(5) . ? C6 H6A 0.9500 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C16 1.513(5) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C16 1.400(5) . ? C11 C12 1.406(5) . ? C11 C17 1.514(5) . ? C12 C13 1.402(5) . ? C12 C18 1.510(5) . ? C13 C14 1.392(5) . ? C13 C21 1.517(5) . ? C14 C15 1.401(5) . ? C14 C19 1.520(5) . ? C15 C16 1.408(5) . ? C15 C20 1.510(5) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C17 H17D 0.9800 . ? C17 H17E 0.9800 . ? C17 H17F 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C18 H18D 0.9800 . ? C18 H18E 0.9800 . ? C18 H18F 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C19 H19D 0.9800 . ? C19 H19E 0.9800 . ? C19 H19F 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C20 H20D 0.9800 . ? C20 H20E 0.9800 . ? C20 H20F 0.9800 . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9500 . ? C23 C24 1.387(5) . ? C23 C28 1.390(5) . ? C24 C25 1.383(6) . ? C24 H24A 0.9500 . ? C25 C26 1.419(6) . ? C25 C29 1.515(6) . ? C26 C27 1.385(6) . ? C26 C30 1.508(6) . ? C27 C28 1.397(5) . ? C27 H27A 0.9500 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 N7 1.348(4) . ? C31 H31A 0.9500 . ? C32 C37 1.388(5) . ? C32 C33 1.398(5) . ? C33 C34 1.386(5) . ? C33 H33A 0.9500 . ? C34 C35 1.416(5) . ? C34 C38 1.508(5) . ? C35 C36 1.384(5) . ? C35 C39 1.509(5) . ? C36 C37 1.395(5) . ? C36 H36A 0.9500 . ? C37 N7 1.385(4) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 N7 1.469(4) . ? C40 C41 1.508(5) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.403(5) . ? C41 C46 1.403(5) . ? C42 C43 1.397(5) . ? C42 C50 1.511(5) . ? C43 C44 1.401(5) . ? C43 C49 1.512(5) . ? C44 C45 1.395(5) . ? C44 C66 1.513(5) . ? C45 C46 1.407(5) . ? C45 C48 1.516(5) . ? C46 C47 1.503(5) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C47 H47D 0.9800 . ? C47 H47E 0.9800 . ? C47 H47F 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C48 H48D 0.9800 . ? C48 H48E 0.9800 . ? C48 H48F 0.9800 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C49 H49D 0.9800 . ? C49 H49E 0.9800 . ? C49 H49F 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C50 H50D 0.9800 . ? C50 H50E 0.9800 . ? C50 H50F 0.9800 . ? C51 H51A 0.9500 . ? C52 C53 1.391(5) . ? C52 C57 1.393(5) . ? C53 C54 1.387(5) . ? C53 H53A 0.9500 . ? C54 C55 1.419(5) . ? C54 C58 1.507(5) . ? C55 C56 1.395(5) . ? C55 C59 1.498(5) . ? C56 C57 1.394(5) . ? C56 H56A 0.9500 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C66 H65A 0.9900 . ? C66 H65B 0.9900 . ? C60 Cl5 1.745(11) . ? C60 Cl6 1.777(8) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C62 N9 1.129(6) . ? C62 C63 1.447(6) . ? C63 H63D 0.9800 . ? C63 H63E 0.9800 . ? C63 H63F 0.9800 . ? C64 N10 1.120(7) . ? C64 C65 1.455(8) . ? C65 H66D 0.9800 . ? C65 H66E 0.9800 . ? C65 H66F 0.9800 . ? C61 Cl8 1.720(14) . ? C61 Cl7 1.824(14) . ? C61 H61E 0.9900 . ? C61 H61F 0.9900 . ? C61' Cl8' 1.566(17) . ? C61' Cl7' 1.588(17) . ? C61' H61G 0.9900 . ? C61' H61H 0.9900 . ? 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 N8 Pd1 N3 175.58(12) . . ? N8 Pd1 Cl3 90.06(9) . . ? N3 Pd1 Cl3 89.35(9) . . ? N8 Pd1 Cl4 90.45(9) . . ? N3 Pd1 Cl4 90.38(9) . . ? Cl3 Pd1 Cl4 176.85(4) . . ? N1 Pd2 N5 177.32(12) . . ? N1 Pd2 Cl2 89.09(9) . . ? N5 Pd2 Cl2 88.83(9) . . ? N1 Pd2 Cl1 90.43(9) . . ? N5 Pd2 Cl1 91.69(9) . . ? Cl2 Pd2 Cl1 178.31(4) . . ? C1 N1 C7 106.4(3) . . ? C1 N1 Pd2 126.1(3) . . ? C7 N1 Pd2 127.2(2) . . ? C1 N2 C2 107.1(3) . . ? C1 N2 C10 127.4(3) . . ? C2 N2 C10 125.2(3) . . ? C22 N3 C28 106.1(3) . . ? C22 N3 Pd1 128.9(3) . . ? C28 N3 Pd1 124.5(2) . . ? C22 N4 C23 107.0(3) . . ? C22 N4 C21 128.6(3) . . ? C23 N4 C21 124.3(3) . . ? C51 N5 C57 106.1(3) . . ? C51 N5 Pd2 124.0(2) . . ? C57 N5 Pd2 127.7(2) . . ? C51 N6 C52 107.4(3) . . ? C51 N6 C66 127.5(3) . . ? C52 N6 C66 125.0(3) . . ? C31 N8 C32 106.1(3) . . ? C31 N8 Pd1 127.3(2) . . ? C32 N8 Pd1 126.5(2) . . ? N1 C1 N2 112.2(3) . . ? N1 C1 H1A 123.9 . . ? N2 C1 H1A 123.9 . . ? N2 C2 C7 106.2(3) . . ? N2 C2 C3 131.9(3) . . ? C7 C2 C3 121.9(3) . . ? C4 C3 C2 117.5(3) . . ? C4 C3 H3A 121.3 . . ? C2 C3 H3A 121.3 . . ? C3 C4 C5 120.8(3) . . ? C3 C4 C9 118.7(3) . . ? C5 C4 C9 120.4(3) . . ? C6 C5 C4 120.4(3) . . ? C6 C5 C8 119.5(3) . . ? C4 C5 C8 120.1(3) . . ? C5 C6 C7 119.0(3) . . ? C5 C6 H6A 120.5 . . ? C7 C6 H6A 120.5 . . ? C2 C7 N1 108.2(3) . . ? C2 C7 C6 120.3(3) . . ? N1 C7 C6 131.5(3) . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N2 C10 C16 113.0(3) . . ? N2 C10 H10A 109.0 . . ? C16 C10 H10A 109.0 . . ? N2 C10 H10B 109.0 . . ? C16 C10 H10B 109.0 . . ? H10A C10 H10B 107.8 . . ? C16 C11 C12 119.1(3) . . ? C16 C11 C17 121.2(3) . . ? C12 C11 C17 119.6(3) . . ? C13 C12 C11 119.1(3) . . ? C13 C12 C18 121.1(3) . . ? C11 C12 C18 119.7(3) . . ? C14 C13 C12 121.6(3) . . ? C14 C13 C21 119.1(3) . . ? C12 C13 C21 119.3(3) . . ? C13 C14 C15 119.5(3) . . ? C13 C14 C19 120.9(3) . . ? C15 C14 C19 119.6(3) . . ? C14 C15 C16 119.0(3) . . ? C14 C15 C20 120.8(4) . . ? C16 C15 C20 120.2(3) . . ? C11 C16 C15 121.3(3) . . ? C11 C16 C10 120.1(3) . . ? C15 C16 C10 118.6(3) . . ? C11 C17 H17A 109.5 . . ? C11 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C11 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C11 C17 H17D 109.5 . . ? H17A C17 H17D 141.1 . . ? H17B C17 H17D 56.3 . . ? H17C C17 H17D 56.3 . . ? C11 C17 H17E 109.5 . . ? H17A C17 H17E 56.3 . . ? H17B C17 H17E 141.1 . . ? H17C C17 H17E 56.3 . . ? H17D C17 H17E 109.5 . . ? C11 C17 H17F 109.5 . . ? H17A C17 H17F 56.3 . . ? H17B C17 H17F 56.3 . . ? H17C C17 H17F 141.1 . . ? H17D C17 H17F 109.5 . . ? H17E C17 H17F 109.5 . . ? C12 C18 H18A 109.5 . . ? C12 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C12 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C12 C18 H18D 109.5 . . ? H18A C18 H18D 141.1 . . ? H18B C18 H18D 56.3 . . ? H18C C18 H18D 56.3 . . ? C12 C18 H18E 109.5 . . ? H18A C18 H18E 56.3 . . ? H18B C18 H18E 141.1 . . ? H18C C18 H18E 56.3 . . ? H18D C18 H18E 109.5 . . ? C12 C18 H18F 109.5 . . ? H18A C18 H18F 56.3 . . ? H18B C18 H18F 56.3 . . ? H18C C18 H18F 141.1 . . ? H18D C18 H18F 109.5 . . ? H18E C18 H18F 109.5 . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C14 C19 H19D 109.5 . . ? H19A C19 H19D 141.1 . . ? H19B C19 H19D 56.3 . . ? H19C C19 H19D 56.3 . . ? C14 C19 H19E 109.5 . . ? H19A C19 H19E 56.3 . . ? H19B C19 H19E 141.1 . . ? H19C C19 H19E 56.3 . . ? H19D C19 H19E 109.5 . . ? C14 C19 H19F 109.5 . . ? H19A C19 H19F 56.3 . . ? H19B C19 H19F 56.3 . . ? H19C C19 H19F 141.1 . . ? H19D C19 H19F 109.5 . . ? H19E C19 H19F 109.5 . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C15 C20 H20D 109.5 . . ? H20A C20 H20D 141.1 . . ? H20B C20 H20D 56.3 . . ? H20C C20 H20D 56.3 . . ? C15 C20 H20E 109.5 . . ? H20A C20 H20E 56.3 . . ? H20B C20 H20E 141.1 . . ? H20C C20 H20E 56.3 . . ? H20D C20 H20E 109.5 . . ? C15 C20 H20F 109.5 . . ? H20A C20 H20F 56.3 . . ? H20B C20 H20F 56.3 . . ? H20C C20 H20F 141.1 . . ? H20D C20 H20F 109.5 . . ? H20E C20 H20F 109.5 . . ? N4 C21 C13 112.7(3) . . ? N4 C21 H21A 109.1 . . ? C13 C21 H21A 109.1 . . ? N4 C21 H21B 109.1 . . ? C13 C21 H21B 109.1 . . ? H21A C21 H21B 107.8 . . ? N3 C22 N4 112.3(3) . . ? N3 C22 H22A 123.9 . . ? N4 C22 H22A 123.9 . . ? C24 C23 C28 122.5(3) . . ? C24 C23 N4 131.6(3) . . ? C28 C23 N4 105.8(3) . . ? C25 C24 C23 117.6(4) . . ? C25 C24 H24A 121.2 . . ? C23 C24 H24A 121.2 . . ? C24 C25 C26 120.6(4) . . ? C24 C25 C29 119.4(4) . . ? C26 C25 C29 119.9(4) . . ? C27 C26 C25 121.0(4) . . ? C27 C26 C30 118.7(4) . . ? C25 C26 C30 120.2(4) . . ? C26 C27 C28 118.1(4) . . ? C26 C27 H27A 121.0 . . ? C28 C27 H27A 121.0 . . ? N3 C28 C23 108.8(3) . . ? N3 C28 C27 131.1(3) . . ? C23 C28 C27 120.1(3) . . ? C25 C29 H29A 109.5 . . ? C25 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C25 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C26 C30 H30A 109.5 . . ? C26 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C26 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N8 C31 N7 112.3(3) . . ? N8 C31 H31A 123.9 . . ? N7 C31 H31A 123.9 . . ? C37 C32 N8 108.3(3) . . ? C37 C32 C33 119.9(3) . . ? N8 C32 C33 131.9(3) . . ? C34 C33 C32 118.4(3) . . ? C34 C33 H33A 120.8 . . ? C32 C33 H33A 120.8 . . ? C33 C34 C35 121.0(3) . . ? C33 C34 C38 118.9(4) . . ? C35 C34 C38 119.9(3) . . ? C36 C35 C34 120.7(3) . . ? C36 C35 C39 118.7(4) . . ? C34 C35 C39 120.7(3) . . ? C35 C36 C37 117.4(3) . . ? C35 C36 H36A 121.3 . . ? C37 C36 H36A 121.3 . . ? N7 C37 C32 106.4(3) . . ? N7 C37 C36 131.0(3) . . ? C32 C37 C36 122.6(3) . . ? C34 C38 H38A 109.5 . . ? C34 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C34 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C35 C39 H39A 109.5 . . ? C35 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C35 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? N7 C40 C41 113.7(3) . . ? N7 C40 H40A 108.8 . . ? C41 C40 H40A 108.8 . . ? N7 C40 H40B 108.8 . . ? C41 C40 H40B 108.8 . . ? H40A C40 H40B 107.7 . . ? C42 C41 C46 121.0(3) . . ? C42 C41 C40 119.5(3) . . ? C46 C41 C40 119.4(3) . . ? C43 C42 C41 119.3(3) . . ? C43 C42 C50 119.5(3) . . ? C41 C42 C50 121.2(3) . . ? C42 C43 C44 119.5(3) . . ? C42 C43 C49 119.6(3) . . ? C44 C43 C49 120.9(3) . . ? C45 C44 C43 121.0(3) . . ? C45 C44 C66 120.4(3) . . ? C43 C44 C66 118.5(3) . . ? C44 C45 C46 119.4(3) . . ? C44 C45 C48 121.9(3) . . ? C46 C45 C48 118.7(3) . . ? C41 C46 C45 119.0(3) . . ? C41 C46 C47 122.3(3) . . ? C45 C46 C47 118.6(3) . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C46 C47 H47D 109.5 . . ? H47A C47 H47D 141.1 . . ? H47B C47 H47D 56.3 . . ? H47C C47 H47D 56.3 . . ? C46 C47 H47E 109.5 . . ? H47A C47 H47E 56.3 . . ? H47B C47 H47E 141.1 . . ? H47C C47 H47E 56.3 . . ? H47D C47 H47E 109.5 . . ? C46 C47 H47F 109.5 . . ? H47A C47 H47F 56.3 . . ? H47B C47 H47F 56.3 . . ? H47C C47 H47F 141.1 . . ? H47D C47 H47F 109.5 . . ? H47E C47 H47F 109.5 . . ? C45 C48 H48A 109.5 . . ? C45 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C45 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C45 C48 H48D 109.5 . . ? H48A C48 H48D 141.1 . . ? H48B C48 H48D 56.3 . . ? H48C C48 H48D 56.3 . . ? C45 C48 H48E 109.5 . . ? H48A C48 H48E 56.3 . . ? H48B C48 H48E 141.1 . . ? H48C C48 H48E 56.3 . . ? H48D C48 H48E 109.5 . . ? C45 C48 H48F 109.5 . . ? H48A C48 H48F 56.3 . . ? H48B C48 H48F 56.3 . . ? H48C C48 H48F 141.1 . . ? H48D C48 H48F 109.5 . . ? H48E C48 H48F 109.5 . . ? C43 C49 H49A 109.5 . . ? C43 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C43 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C43 C49 H49D 109.5 . . ? H49A C49 H49D 141.1 . . ? H49B C49 H49D 56.3 . . ? H49C C49 H49D 56.3 . . ? C43 C49 H49E 109.5 . . ? H49A C49 H49E 56.3 . . ? H49B C49 H49E 141.1 . . ? H49C C49 H49E 56.3 . . ? H49D C49 H49E 109.5 . . ? C43 C49 H49F 109.5 . . ? H49A C49 H49F 56.3 . . ? H49B C49 H49F 56.3 . . ? H49C C49 H49F 141.1 . . ? H49D C49 H49F 109.5 . . ? H49E C49 H49F 109.5 . . ? C42 C50 H50A 109.5 . . ? C42 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C42 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C42 C50 H50D 109.5 . . ? H50A C50 H50D 141.1 . . ? H50B C50 H50D 56.3 . . ? H50C C50 H50D 56.3 . . ? C42 C50 H50E 109.5 . . ? H50A C50 H50E 56.3 . . ? H50B C50 H50E 141.1 . . ? H50C C50 H50E 56.3 . . ? H50D C50 H50E 109.5 . . ? C42 C50 H50F 109.5 . . ? H50A C50 H50F 56.3 . . ? H50B C50 H50F 56.3 . . ? H50C C50 H50F 141.1 . . ? H50D C50 H50F 109.5 . . ? H50E C50 H50F 109.5 . . ? N5 C51 N6 112.1(3) . . ? N5 C51 H51A 123.9 . . ? N6 C51 H51A 123.9 . . ? N6 C52 C53 132.1(3) . . ? N6 C52 C57 106.2(3) . . ? C53 C52 C57 121.6(3) . . ? C54 C53 C52 118.2(3) . . ? C54 C53 H53A 120.9 . . ? C52 C53 H53A 120.9 . . ? C53 C54 C55 120.6(3) . . ? C53 C54 C58 118.9(3) . . ? C55 C54 C58 120.5(3) . . ? C56 C55 C54 120.4(3) . . ? C56 C55 C59 119.4(3) . . ? C54 C55 C59 120.1(3) . . ? C57 C56 C55 118.4(3) . . ? C57 C56 H56A 120.8 . . ? C55 C56 H56A 120.8 . . ? N5 C57 C52 108.1(3) . . ? N5 C57 C56 131.2(3) . . ? C52 C57 C56 120.6(3) . . ? C54 C58 H58A 109.5 . . ? C54 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C54 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C55 C59 H59A 109.5 . . ? C55 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C55 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? N6 C66 C44 112.9(3) . . ? N6 C66 H65A 109.0 . . ? C44 C66 H65A 109.0 . . ? N6 C66 H65B 109.0 . . ? C44 C66 H65B 109.0 . . ? H65A C66 H65B 107.8 . . ? C31 N7 C37 107.0(3) . . ? C31 N7 C40 129.3(3) . . ? C37 N7 C40 123.7(3) . . ? Cl5 C60 Cl6 112.6(6) . . ? Cl5 C60 H60A 109.1 . . ? Cl6 C60 H60A 109.1 . . ? Cl5 C60 H60B 109.1 . . ? Cl6 C60 H60B 109.1 . . ? H60A C60 H60B 107.8 . . ? N9 C62 C63 179.3(6) . . ? C62 C63 H63D 109.5 . . ? C62 C63 H63E 109.5 . . ? H63D C63 H63E 109.5 . . ? C62 C63 H63F 109.5 . . ? H63D C63 H63F 109.5 . . ? H63E C63 H63F 109.5 . . ? N10 C64 C65 179.0(6) . . ? C64 C65 H66D 109.5 . . ? C64 C65 H66E 109.5 . . ? H66D C65 H66E 109.5 . . ? C64 C65 H66F 109.5 . . ? H66D C65 H66F 109.5 . . ? H66E C65 H66F 109.5 . . ? Cl8 C61 Cl7 113.2(7) . . ? Cl8 C61 H61E 108.9 . . ? Cl7 C61 H61E 108.9 . . ? Cl8 C61 H61F 108.9 . . ? Cl7 C61 H61F 108.9 . . ? H61E C61 H61F 107.8 . . ? Cl8' C61' Cl7' 124.8(16) . . ? Cl8' C61' H61G 106.1 . . ? Cl7' C61' H61G 106.1 . . ? Cl8' C61' H61H 106.1 . . ? Cl7' C61' H61H 106.1 . . ? H61G C61' H61H 106.3 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.924 _refine_diff_density_min -1.208 _refine_diff_density_rms 0.101 #=============# data_4 _database_code_depnum_ccdc_archive 'CCDC 767081' #TrackingRef 'Compds-rev.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C66 H76 Cl10 N10 Pd2' _chemical_formula_weight 1576.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 17.6272(10) _cell_length_b 16.7990(10) _cell_length_c 14.8756(10) _cell_angle_alpha 90.00 _cell_angle_beta 122.780(10) _cell_angle_gamma 90.00 _cell_volume 3703.5(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 5 _cell_measurement_theta_max 12 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.414 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1608 _exptl_absorpt_coefficient_mu 0.891 _exptl_absorpt_correction_type PSI-scan _exptl_absorpt_correction_T_min 0.7059 _exptl_absorpt_correction_T_max 0.8079 _exptl_absorpt_process_details PSI-scan _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 CAD4 _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count 800 _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 4433 _diffrn_reflns_av_R_equivalents 0.0379 _diffrn_reflns_av_sigmaI/netI 0.0327 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 26.11 _reflns_number_total 3770 _reflns_number_gt 2795 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Both acetontrile and chloroform solvents are disordered over two partial positions, which were modelled by using SADI to make Cl-C bonds similar (4 restraints) and ISOR and SIMU to make anisotropic displacement parameters of N, Cl and C atoms reasonable (72+48 restaints). 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^)+(0.0910P)^2^+38.4236P] 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 geom _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3770 _refine_ls_number_parameters 249 _refine_ls_number_restraints 126 _refine_ls_R_factor_all 0.1029 _refine_ls_R_factor_gt 0.0730 _refine_ls_wR_factor_ref 0.2148 _refine_ls_wR_factor_gt 0.1801 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.070 _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 -0.56045(5) -0.5000 1.25023(6) 0.0463(3) Uani 1 2 d S . . N1 N -0.5617(4) -0.6195(3) 1.2501(4) 0.0475(13) Uani 1 1 d . . . N2 N -0.5555(4) -0.7427(3) 1.2070(4) 0.0487(13) Uani 1 1 d . . . C1 C -0.5446(5) -0.6660(3) 1.1927(5) 0.0486(16) Uani 1 1 d . . . H1A H -0.5271 -0.6479 1.1475 0.058 Uiso 1 1 calc R . . C2 C -0.5835(4) -0.6672(3) 1.3084(5) 0.0403(13) Uani 1 1 d . . . C3 C -0.6058(4) -0.6508(4) 1.3826(5) 0.0449(14) Uani 1 1 d . . . H3A H -0.6086 -0.5986 1.4013 0.054 Uiso 1 1 calc R . . C4 C -0.6237(4) -0.7128(4) 1.4276(5) 0.0484(15) Uani 1 1 d . . . C5 C -0.6209(5) -0.7923(4) 1.3988(5) 0.0525(16) Uani 1 1 d . . . C6 C -0.5980(5) -0.8099(4) 1.3263(5) 0.0504(16) Uani 1 1 d . . . H6A H -0.5948 -0.8622 1.3080 0.061 Uiso 1 1 calc R . . C7 C -0.5796(4) -0.7460(4) 1.2817(5) 0.0409(13) Uani 1 1 d . . . C8 C -0.6439(7) -0.8600(6) 1.4463(7) 0.082(3) Uani 1 1 d . . . H8A H -0.6594 -0.8392 1.4945 0.122 Uiso 1 1 calc R . . H8B H -0.5928 -0.8947 1.4846 0.122 Uiso 1 1 calc R . . H8C H -0.6942 -0.8892 1.3902 0.122 Uiso 1 1 calc R . . C9 C -0.6485(5) -0.6938(6) 1.5086(6) 0.068(2) Uani 1 1 d . . . H9A H -0.6455 -0.6373 1.5199 0.103 Uiso 1 1 calc R . . H9B H -0.6070 -0.7200 1.5750 0.103 Uiso 1 1 calc R . . H9C H -0.7087 -0.7122 1.4820 0.103 Uiso 1 1 calc R . . C10 C -0.5426(7) -0.8143(4) 1.1599(7) 0.071(2) Uani 1 1 d . . . H10A H -0.5971 -0.8462 1.1274 0.086 Uiso 1 1 calc R . . H10B H -0.4940 -0.8456 1.2166 0.086 Uiso 1 1 calc R . . C11 C -0.5207(4) -0.7967(3) 1.0760(5) 0.0421(14) Uani 1 1 d . . . C12 C -0.4315(4) -0.7934(4) 1.1080(5) 0.0454(14) Uani 1 1 d . . . C13 C -0.5896(4) -0.7937(4) 0.9706(5) 0.0471(15) Uani 1 1 d . . . C14 C -0.3560(7) -0.7899(7) 1.2253(6) 0.099(3) Uani 1 1 d . . . H14A H -0.3812 -0.7896 1.2685 0.149 Uiso 1 1 calc R . . H14B H -0.3212 -0.7424 1.2386 0.149 Uiso 1 1 calc R . . H14C H -0.3177 -0.8356 1.2430 0.149 Uiso 1 1 calc R . . C15 C -0.6861(6) -0.7926(7) 0.9370(9) 0.092(3) Uani 1 1 d . . . H15A H -0.6896 -0.7941 0.9991 0.138 Uiso 1 1 calc R . . H15B H -0.7165 -0.8380 0.8928 0.138 Uiso 1 1 calc R . . H15C H -0.7142 -0.7448 0.8973 0.138 Uiso 1 1 calc R . . Cl1 Cl -0.4102(2) -0.5000 1.3107(3) 0.0794(9) Uani 1 2 d S . . Cl2 Cl -0.7106(2) -0.5000 1.1877(4) 0.0909(11) Uani 1 2 d S . . N3 N -0.0468(16) -0.5000 1.692(2) 0.126(8) Uani 0.60 2 d SPDU A 1 C17 C -0.1197(15) -0.5000 1.654(2) 0.089(6) Uani 0.60 2 d SPDU A 1 C18 C -0.2166(15) -0.5000 1.607(2) 0.098(7) Uani 0.60 2 d SPDU A 1 H18A H -0.2353 -0.5518 1.6149 0.147 Uiso 0.50 1 calc PR A 1 H18B H -0.2473 -0.4869 1.5325 0.147 Uiso 0.50 1 calc PR A 1 H18C H -0.2312 -0.4613 1.6429 0.147 Uiso 0.50 1 calc PR A 1 N3' N -0.016(4) -0.5000 1.822(3) 0.182(15) Uani 0.40 2 d SPDU B 2 C17' C 0.006(4) -0.5000 1.907(3) 0.165(13) Uani 0.40 2 d SPDU B 2 C18' C 0.0000 -0.5000 2.0000 0.137(11) Uani 0.80 4 d SPDU . 2 C16 C -0.292(2) -0.5000 1.054(5) 0.176(12) Uani 0.50 2 d SPDU . 1 H16A H -0.3122 -0.5000 0.9785 0.211 Uiso 0.50 2 calc SPR . 1 Cl3 Cl -0.3234(9) -0.4124(7) 1.0974(12) 0.194(5) Uani 0.50 1 d PDU . 1 Cl4 Cl -0.1703(10) -0.5000 1.1480(13) 0.161(5) Uani 0.50 2 d SPDU . 1 C16' C -0.346(3) -0.5000 1.135(4) 0.146(10) Uani 0.50 2 d SPU . 2 H16B H -0.3407 -0.5000 1.2043 0.175 Uiso 0.50 2 calc SPR . 2 Cl3' Cl -0.3981(11) -0.4164(8) 1.0704(12) 0.203(5) Uani 0.50 1 d PU . 2 Cl4' Cl -0.2388(17) -0.5000 1.157(2) 0.236(7) Uani 0.50 2 d SPU . 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 0.0675(5) 0.0324(4) 0.0497(4) 0.000 0.0387(4) 0.000 N1 0.071(4) 0.033(3) 0.055(3) 0.001(2) 0.045(3) 0.003(2) N2 0.078(4) 0.034(3) 0.058(3) -0.001(2) 0.052(3) -0.003(3) C1 0.084(5) 0.027(3) 0.063(4) 0.001(3) 0.057(4) 0.000(3) C2 0.055(4) 0.031(3) 0.042(3) 0.000(2) 0.031(3) 0.001(3) C3 0.052(4) 0.046(3) 0.042(3) -0.009(3) 0.029(3) -0.002(3) C4 0.043(3) 0.067(4) 0.038(3) 0.000(3) 0.024(3) -0.006(3) C5 0.065(4) 0.053(4) 0.049(4) 0.003(3) 0.037(3) -0.008(3) C6 0.074(5) 0.032(3) 0.054(4) 0.004(3) 0.041(3) -0.004(3) C7 0.055(4) 0.037(3) 0.043(3) 0.000(2) 0.035(3) -0.003(3) C8 0.110(7) 0.079(6) 0.081(6) 0.014(5) 0.068(6) -0.013(5) C9 0.069(5) 0.098(6) 0.055(4) -0.012(4) 0.045(4) -0.017(4) C10 0.144(8) 0.029(3) 0.091(6) 0.000(3) 0.096(6) 0.002(4) C11 0.066(4) 0.024(3) 0.050(3) 0.000(2) 0.041(3) 0.001(3) C12 0.049(3) 0.037(3) 0.043(3) 0.003(3) 0.020(3) 0.003(3) C13 0.052(4) 0.032(3) 0.058(4) -0.006(3) 0.031(3) -0.001(3) C14 0.086(6) 0.114(9) 0.046(4) 0.007(5) 0.002(4) 0.001(6) C15 0.059(5) 0.102(8) 0.119(8) -0.016(6) 0.052(5) -0.003(5) Cl1 0.0742(19) 0.0516(15) 0.131(3) 0.000 0.068(2) 0.000 Cl2 0.0673(19) 0.0481(15) 0.142(3) 0.000 0.047(2) 0.000 N3 0.123(13) 0.071(10) 0.139(13) 0.000 0.042(11) 0.000 C17 0.109(11) 0.043(8) 0.104(11) 0.000 0.050(10) 0.000 C18 0.114(13) 0.080(11) 0.107(12) 0.000 0.064(10) 0.000 N3' 0.195(19) 0.139(18) 0.18(2) 0.000 0.084(14) 0.000 C17' 0.184(17) 0.121(15) 0.168(18) 0.000 0.082(13) 0.000 C18' 0.170(17) 0.084(14) 0.154(17) 0.000 0.085(13) 0.000 C16 0.184(17) 0.180(17) 0.191(17) 0.000 0.120(13) 0.000 Cl3 0.182(9) 0.109(6) 0.249(10) -0.007(7) 0.090(8) 0.019(7) Cl4 0.168(10) 0.105(7) 0.197(10) 0.000 0.090(8) 0.000 C16' 0.174(16) 0.134(16) 0.172(15) 0.000 0.121(12) 0.000 Cl3' 0.254(10) 0.158(8) 0.206(8) 0.063(7) 0.131(8) 0.050(8) Cl4' 0.218(12) 0.202(11) 0.259(12) 0.000 0.110(10) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N1 2.008(5) 6_545 ? Pd1 N1 2.008(5) . ? Pd1 Cl2 2.282(3) . ? Pd1 Cl1 2.290(3) . ? N1 C1 1.306(7) . ? N1 C2 1.378(7) . ? N2 C1 1.336(8) . ? N2 C7 1.389(7) . ? N2 C10 1.471(8) . ? C1 H1A 0.9300 . ? C2 C3 1.385(8) . ? C2 C7 1.395(8) . ? C3 C4 1.365(9) . ? C3 H3A 0.9300 . ? C4 C5 1.410(10) . ? C4 C9 1.522(9) . ? C5 C6 1.373(9) . ? C5 C8 1.506(10) . ? C6 C7 1.389(8) . ? C6 H6A 0.9300 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C11 1.522(8) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C13 1.368(9) . ? C11 C12 1.374(9) . ? C12 C13 1.406(9) 2_457 ? C12 C14 1.519(10) . ? C13 C12 1.406(9) 2_457 ? C13 C15 1.491(10) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? N3 C17 1.088(17) . ? C17 C18 1.455(17) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? N3' C17' 1.11(2) . ? C17' C18' 1.44(3) . ? C18' C17' 1.44(3) 5_549 ? C16 Cl3 1.81(3) . ? C16 Cl3 1.81(3) 6_545 ? C16 Cl4 1.82(3) . ? C16 H16A 0.9800 . ? C16' Cl3' 1.67(3) 6_545 ? C16' Cl3' 1.67(3) . ? C16' Cl4' 1.74(5) . ? C16' H16B 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 N1 Pd1 N1 178.8(3) 6_545 . ? N1 Pd1 Cl2 89.43(16) 6_545 . ? N1 Pd1 Cl2 89.43(16) . . ? N1 Pd1 Cl1 90.58(16) 6_545 . ? N1 Pd1 Cl1 90.58(16) . . ? Cl2 Pd1 Cl1 179.26(15) . . ? C1 N1 C2 107.7(5) . . ? C1 N1 Pd1 126.3(4) . . ? C2 N1 Pd1 125.9(4) . . ? C1 N2 C7 107.4(5) . . ? C1 N2 C10 129.8(5) . . ? C7 N2 C10 122.8(5) . . ? N1 C1 N2 111.6(5) . . ? N1 C1 H1A 124.2 . . ? N2 C1 H1A 124.2 . . ? N1 C2 C3 133.0(6) . . ? N1 C2 C7 107.4(5) . . ? C3 C2 C7 119.6(5) . . ? C4 C3 C2 118.7(6) . . ? C4 C3 H3A 120.7 . . ? C2 C3 H3A 120.7 . . ? C3 C4 C5 121.2(6) . . ? C3 C4 C9 118.0(7) . . ? C5 C4 C9 120.7(6) . . ? C6 C5 C4 121.1(6) . . ? C6 C5 C8 118.3(7) . . ? C4 C5 C8 120.6(6) . . ? C5 C6 C7 116.9(6) . . ? C5 C6 H6A 121.6 . . ? C7 C6 H6A 121.6 . . ? N2 C7 C6 131.7(6) . . ? N2 C7 C2 105.8(5) . . ? C6 C7 C2 122.5(5) . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N2 C10 C11 113.9(5) . . ? N2 C10 H10A 108.8 . . ? C11 C10 H10A 108.8 . . ? N2 C10 H10B 108.8 . . ? C11 C10 H10B 108.8 . . ? H10A C10 H10B 107.7 . . ? C13 C11 C12 122.3(6) . . ? C13 C11 C10 119.0(7) . . ? C12 C11 C10 118.3(6) . . ? C11 C12 C13 118.6(6) . 2_457 ? C11 C12 C14 121.8(7) . . ? C13 C12 C14 119.6(7) 2_457 . ? C11 C13 C12 118.9(6) . 2_457 ? C11 C13 C15 121.9(7) . . ? C12 C13 C15 119.2(7) 2_457 . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N3 C17 C18 178(3) . . ? N3' C17' C18' 160(7) . . ? C17' C18' C17' 180.00(5) . 5_549 ? Cl3 C16 Cl3 109(3) . 6_545 ? Cl3 C16 Cl4 101(2) . . ? Cl3 C16 Cl4 101(2) 6_545 . ? Cl3 C16 H16A 114.9 . . ? Cl3 C16 H16A 114.9 6_545 . ? Cl4 C16 H16A 114.9 . . ? Cl3' C16' Cl3' 115(3) 6_545 . ? Cl3' C16' Cl4' 108.0(18) 6_545 . ? Cl3' C16' Cl4' 108.0(18) . . ? Cl3' C16' H16B 108.6 6_545 . ? Cl3' C16' H16B 108.6 . . ? Cl4' C16' H16B 108.6 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 26.11 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.152 _refine_diff_density_min -0.990 _refine_diff_density_rms 0.145 #=====================================# data_5 _database_code_depnum_ccdc_archive 'CCDC 767082' #TrackingRef 'Compds-rev.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53 H56 Cl6 N14 Pd2' _chemical_formula_weight 1314.62 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 Orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 17.0274(7) _cell_length_b 25.876(2) _cell_length_c 13.1365(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5788.0(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(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 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.509 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2664 _exptl_absorpt_coefficient_mu 0.947 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7642 _exptl_absorpt_correction_T_max 0.7976 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 Gemini _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22869 _diffrn_reflns_av_R_equivalents 0.0478 _diffrn_reflns_av_sigmaI/netI 0.0877 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 28.00 _reflns_number_total 7034 _reflns_number_gt 3647 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; The solvated dichloromethane is disordered over two partial positions, which was modelled by using SADI to make Cl-C bonds similar (6 restraints) and ISOR and SIMU to make anisotropic displacement parameters of Cl and C atoms reasonable (54+42 restaints). 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^)+(0.0399P)^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 7034 _refine_ls_number_parameters 370 _refine_ls_number_restraints 102 _refine_ls_R_factor_all 0.1111 _refine_ls_R_factor_gt 0.0467 _refine_ls_wR_factor_ref 0.1043 _refine_ls_wR_factor_gt 0.0928 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd 0.023209(15) 0.586905(14) 0.98232(2) 0.04460(11) Uani 1 1 d . . . N1 N -0.14754(18) 0.60958(14) 0.7718(2) 0.0501(9) Uani 1 1 d . . . N2 N -0.10781(18) 0.61986(14) 0.8581(2) 0.0514(9) Uani 1 1 d . . . N3 N -0.05238(17) 0.58517(14) 0.8646(2) 0.0457(8) Uani 1 1 d . . . N4 N 0.16634(18) 0.60803(14) 1.2267(2) 0.0502(9) Uani 1 1 d . . . N5 N 0.10427(17) 0.61953(13) 1.1673(2) 0.0490(9) Uani 1 1 d . . . N6 N 0.10290(17) 0.58485(13) 1.0952(2) 0.0444(8) Uani 1 1 d . . . C1 C -0.1176(2) 0.56767(17) 0.7229(3) 0.0469(10) Uani 1 1 d . . . C2 C -0.1367(3) 0.54195(19) 0.6330(3) 0.0638(13) Uani 1 1 d . . . H2A H -0.1794 0.5527 0.5916 0.077 Uiso 1 1 calc R . . C3 C -0.0912(3) 0.50082(19) 0.6077(3) 0.0707(14) Uani 1 1 d . . . H3A H -0.1027 0.4826 0.5467 0.085 Uiso 1 1 calc R . . C4 C -0.0288(3) 0.48426(19) 0.6671(3) 0.0685(13) Uani 1 1 d . . . H4A H 0.0012 0.4552 0.6460 0.082 Uiso 1 1 calc R . . C5 C -0.0094(2) 0.50916(17) 0.7560(3) 0.0561(12) Uani 1 1 d . . . H5A H 0.0329 0.4977 0.7974 0.067 Uiso 1 1 calc R . . C6 C -0.0545(2) 0.55203(17) 0.7830(3) 0.0450(10) Uani 1 1 d . . . C7 C -0.2204(2) 0.63881(18) 0.7511(3) 0.0611(12) Uani 1 1 d . . . H7A H -0.2607 0.6281 0.8012 0.073 Uiso 1 1 calc R . . H7B H -0.2399 0.6291 0.6827 0.073 Uiso 1 1 calc R . . C8 C -0.2122(2) 0.69647(17) 0.7554(3) 0.0485(10) Uani 1 1 d . . . C9 C -0.1928(2) 0.72304(16) 0.6662(3) 0.0592(12) Uani 1 1 d . . . C10 C -0.1735(3) 0.6928(2) 0.5688(3) 0.0976(18) Uani 1 1 d . . . H10A H -0.1763 0.6556 0.5828 0.146 Uiso 0.50 1 calc PR . . H10B H -0.1205 0.7017 0.5458 0.146 Uiso 0.50 1 calc PR . . H10C H -0.2116 0.7017 0.5156 0.146 Uiso 0.50 1 calc PR . . H10D H -0.1626 0.7170 0.5133 0.146 Uiso 0.50 1 calc PR . . H10E H -0.2184 0.6710 0.5504 0.146 Uiso 0.50 1 calc PR . . H10F H -0.1273 0.6710 0.5805 0.146 Uiso 0.50 1 calc PR . . C11 C -0.22760(19) 0.72323(14) 0.8453(3) 0.0462(10) Uani 1 1 d . . . C12 C -0.2443(2) 0.6941(2) 0.9434(3) 0.0730(14) Uani 1 1 d . . . H12A H -0.2421 0.6569 0.9304 0.109 Uiso 0.50 1 calc PR . . H12B H -0.2966 0.7034 0.9684 0.109 Uiso 0.50 1 calc PR . . H12C H -0.2048 0.7034 0.9946 0.109 Uiso 0.50 1 calc PR . . H12D H -0.2536 0.7189 0.9985 0.109 Uiso 0.50 1 calc PR . . H12E H -0.1991 0.6724 0.9605 0.109 Uiso 0.50 1 calc PR . . H12F H -0.2908 0.6724 0.9344 0.109 Uiso 0.50 1 calc PR . . C13 C 0.1629(2) 0.54953(17) 1.1073(3) 0.0439(10) Uani 1 1 d . . . C14 C 0.1839(2) 0.50586(17) 1.0519(3) 0.0535(11) Uani 1 1 d . . . H14A H 0.1545 0.4950 0.9943 0.064 Uiso 1 1 calc R . . C15 C 0.2486(2) 0.47933(18) 1.0842(3) 0.0599(12) Uani 1 1 d . . . H15A H 0.2650 0.4495 1.0478 0.072 Uiso 1 1 calc R . . C16 C 0.2912(2) 0.49521(19) 1.1696(4) 0.0665(13) Uani 1 1 d . . . H16A H 0.3363 0.4760 1.1891 0.080 Uiso 1 1 calc R . . C17 C 0.2705(2) 0.5374(2) 1.2262(3) 0.0629(13) Uani 1 1 d . . . H17A H 0.2993 0.5475 1.2849 0.076 Uiso 1 1 calc R . . C18 C 0.2042(2) 0.56479(17) 1.1928(3) 0.0473(10) Uani 1 1 d . . . C19 C 0.1799(2) 0.63868(17) 1.3208(3) 0.0581(12) Uani 1 1 d . . . H19A H 0.2324 0.6300 1.3481 0.070 Uiso 1 1 calc R . . H19B H 0.1405 0.6283 1.3724 0.070 Uiso 1 1 calc R . . C20 C 0.1752(2) 0.69584(17) 1.3060(2) 0.0471(10) Uani 1 1 d . . . C21 C 0.1055(2) 0.72299(16) 1.3297(2) 0.0521(11) Uani 1 1 d . . . C22 C 0.0310(2) 0.6933(2) 1.3537(3) 0.0828(16) Uani 1 1 d . . . H22A H 0.0416 0.6561 1.3502 0.124 Uiso 0.50 1 calc PR . . H22B H -0.0098 0.7023 1.3040 0.124 Uiso 0.50 1 calc PR . . H22C H 0.0129 0.7022 1.4223 0.124 Uiso 0.50 1 calc PR . . H22D H -0.0118 0.7176 1.3675 0.124 Uiso 0.50 1 calc PR . . H22E H 0.0396 0.6715 1.4136 0.124 Uiso 0.50 1 calc PR . . H22F H 0.0169 0.6715 1.2954 0.124 Uiso 0.50 1 calc PR . . C23 C 0.2422(2) 0.72285(15) 1.2733(3) 0.0493(11) Uani 1 1 d . . . C24 C 0.3153(2) 0.69363(18) 1.2408(3) 0.0704(13) Uani 1 1 d . . . H24A H 0.3561 0.7183 1.2206 0.106 Uiso 0.50 1 calc PR . . H24B H 0.3027 0.6711 1.1832 0.106 Uiso 0.50 1 calc PR . . H24C H 0.3344 0.6726 1.2978 0.106 Uiso 0.50 1 calc PR . . H24D H 0.3061 0.6564 1.2471 0.106 Uiso 0.50 1 calc PR . . H24E H 0.3595 0.7036 1.2845 0.106 Uiso 0.50 1 calc PR . . H24F H 0.3277 0.7020 1.1699 0.106 Uiso 0.50 1 calc PR . . Cl1 Cl -0.07920(5) 0.59194(4) 1.09592(6) 0.0546(3) Uani 1 1 d . . . Cl2 Cl 0.12568(6) 0.58782(6) 0.86995(8) 0.0749(4) Uani 1 1 d . . . N7 N 0.0730(5) 0.6071(3) 0.5706(5) 0.151(3) Uani 1 1 d U . . C26 C 0.0611(5) 0.6387(4) 0.6248(7) 0.132(3) Uani 1 1 d U . . C27 C 0.0408(5) 0.6806(3) 0.6948(6) 0.163(3) Uani 1 1 d U . . H27D H -0.0154 0.6882 0.6894 0.244 Uiso 1 1 calc R . . H27E H 0.0712 0.7115 0.6773 0.244 Uiso 1 1 calc R . . H27F H 0.0532 0.6701 0.7647 0.244 Uiso 1 1 calc R . . C25 C 0.0371(10) 0.7500 1.0729(17) 0.158(7) Uani 0.50 2 d SPDU A 1 Cl4 Cl 0.1308(7) 0.7500 1.0112(8) 0.203(4) Uani 0.50 2 d SPDU A 1 Cl3 Cl -0.0330(6) 0.7500 0.9729(9) 0.227(5) Uani 0.50 2 d SPDU A 1 C28 C 0.0555(13) 0.7691(11) 1.040(2) 0.161(8) Uani 0.25 1 d PDU B -2 H28C H 0.0802 0.7740 1.1079 0.194 Uiso 0.25 1 calc PR B -2 H28D H 0.0411 0.8030 1.0108 0.194 Uiso 0.25 1 calc PR B -2 Cl5 Cl -0.0242(8) 0.7261(4) 1.0445(8) 0.179(4) Uani 0.25 1 d PDU B -2 Cl6 Cl 0.1162(8) 0.7307(6) 0.9549(8) 0.216(6) Uani 0.25 1 d PDU B -2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd 0.03360(16) 0.0606(2) 0.03957(16) -0.00120(16) -0.00376(13) -0.00498(17) N1 0.0449(19) 0.052(2) 0.0534(19) 0.0002(18) -0.0153(16) -0.0050(18) N2 0.0425(19) 0.062(3) 0.0499(18) -0.0023(18) -0.0131(15) -0.0047(19) N3 0.0469(18) 0.057(2) 0.0337(15) -0.0023(18) -0.0046(13) -0.0004(18) N4 0.050(2) 0.053(2) 0.0477(18) -0.0023(18) -0.0180(16) -0.0052(18) N5 0.0482(19) 0.054(2) 0.0450(18) 0.0014(18) -0.0097(15) 0.0000(17) N6 0.0462(18) 0.051(2) 0.0363(16) -0.0063(17) -0.0058(13) -0.0109(18) C1 0.049(2) 0.049(3) 0.042(2) -0.002(2) -0.0058(18) -0.003(2) C2 0.066(3) 0.068(4) 0.057(2) -0.010(3) -0.017(2) -0.008(3) C3 0.074(3) 0.076(4) 0.062(3) -0.026(3) -0.007(2) -0.011(3) C4 0.071(3) 0.065(3) 0.070(3) -0.015(3) 0.005(3) 0.000(3) C5 0.048(2) 0.063(4) 0.057(3) 0.007(2) 0.0017(19) -0.004(2) C6 0.037(2) 0.054(3) 0.044(2) 0.002(2) -0.0011(17) -0.003(2) C7 0.046(2) 0.066(4) 0.071(3) 0.000(3) -0.0168(19) -0.003(2) C8 0.045(2) 0.049(3) 0.051(2) 0.004(2) -0.0128(18) -0.006(2) C9 0.064(3) 0.069(3) 0.044(2) -0.003(2) -0.0083(18) 0.000(2) C10 0.139(5) 0.100(5) 0.054(3) -0.016(3) 0.000(3) 0.013(4) C11 0.0363(19) 0.057(3) 0.045(2) 0.0025(19) 0.0003(16) 0.0005(18) C12 0.071(3) 0.089(4) 0.059(2) 0.011(3) 0.011(2) -0.004(3) C13 0.033(2) 0.054(3) 0.044(2) -0.001(2) -0.0035(17) -0.004(2) C14 0.049(2) 0.063(3) 0.049(2) -0.006(2) -0.0012(18) -0.011(2) C15 0.056(3) 0.054(3) 0.069(3) 0.000(2) 0.002(2) -0.001(2) C16 0.052(3) 0.056(4) 0.092(3) 0.011(3) -0.012(2) 0.004(2) C17 0.049(3) 0.067(4) 0.073(3) 0.010(3) -0.023(2) -0.001(2) C18 0.044(2) 0.045(3) 0.052(2) 0.000(2) -0.0063(19) -0.005(2) C19 0.076(3) 0.050(3) 0.048(2) 0.002(2) -0.018(2) -0.010(3) C20 0.049(2) 0.055(3) 0.0375(19) -0.004(2) -0.0099(17) -0.003(2) C21 0.047(2) 0.070(3) 0.0388(19) 0.0013(18) -0.0092(16) -0.008(2) C22 0.055(3) 0.107(5) 0.086(3) 0.000(3) 0.007(2) -0.015(3) C23 0.043(2) 0.059(3) 0.0455(19) -0.0047(19) -0.0106(16) 0.002(2) C24 0.055(3) 0.072(4) 0.084(3) 0.000(3) -0.003(2) 0.007(3) Cl1 0.0429(5) 0.0733(8) 0.0475(5) -0.0040(5) 0.0067(4) 0.0011(6) Cl2 0.0442(6) 0.1264(12) 0.0542(6) 0.0068(7) 0.0093(5) -0.0140(7) N7 0.195(6) 0.135(7) 0.123(5) 0.014(4) 0.005(5) -0.007(5) C26 0.126(5) 0.128(8) 0.142(7) 0.058(6) -0.015(6) -0.023(6) C27 0.172(7) 0.123(7) 0.194(7) 0.007(6) 0.012(6) -0.019(6) C25 0.129(11) 0.178(13) 0.166(12) 0.000 0.009(11) 0.000 Cl4 0.148(6) 0.240(11) 0.223(9) 0.000 -0.020(7) 0.000 Cl3 0.130(6) 0.237(10) 0.315(11) 0.000 -0.046(8) 0.000 C28 0.127(12) 0.188(14) 0.168(13) 0.005(11) 0.018(11) -0.004(11) Cl5 0.152(7) 0.152(8) 0.233(9) 0.009(7) 0.021(8) -0.041(6) Cl6 0.214(10) 0.225(14) 0.208(9) -0.069(8) 0.057(8) 0.034(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd N6 2.011(3) . ? Pd N3 2.012(3) . ? Pd Cl2 2.2856(10) . ? Pd Cl1 2.2988(9) . ? N1 N2 1.348(4) . ? N1 C1 1.359(5) . ? N1 C7 1.478(5) . ? N2 N3 1.305(4) . ? N3 C6 1.373(5) . ? N4 N5 1.347(4) . ? N4 C18 1.366(5) . ? N4 C19 1.486(4) . ? N5 N6 1.305(4) . ? N6 C13 1.380(5) . ? C1 C6 1.393(5) . ? C1 C2 1.394(5) . ? C2 C3 1.357(6) . ? C2 H2A 0.9500 . ? C3 C4 1.387(6) . ? C3 H3A 0.9500 . ? C4 C5 1.374(6) . ? C4 H4A 0.9500 . ? C5 C6 1.395(5) . ? C5 H5A 0.9500 . ? C7 C8 1.500(6) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C11 1.394(5) . ? C8 C9 1.399(5) . ? C9 C9 1.395(8) 7_575 ? C9 C10 1.536(5) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C10 H10D 0.9800 . ? C10 H10E 0.9800 . ? C10 H10F 0.9800 . ? C11 C11 1.386(7) 7_575 ? C11 C12 1.519(5) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C12 H12D 0.9800 . ? C12 H12E 0.9800 . ? C12 H12F 0.9800 . ? C13 C18 1.383(5) . ? C13 C14 1.390(5) . ? C14 C15 1.366(5) . ? C14 H14A 0.9500 . ? C15 C16 1.398(6) . ? C15 H15A 0.9500 . ? C16 C17 1.367(6) . ? C16 H16A 0.9500 . ? C17 C18 1.404(5) . ? C17 H17A 0.9500 . ? C19 C20 1.494(6) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C23 1.405(5) . ? C20 C21 1.413(5) . ? C21 C21 1.398(8) 7_575 ? C21 C22 1.517(5) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C22 H22D 0.9800 . ? C22 H22E 0.9800 . ? C22 H22F 0.9800 . ? C23 C23 1.405(8) 7_575 ? C23 C24 1.519(5) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C24 H24D 0.9800 . ? C24 H24E 0.9800 . ? C24 H24F 0.9800 . ? N7 C26 1.103(10) . ? C26 C27 1.463(10) . ? C27 H27D 0.9800 . ? C27 H27E 0.9800 . ? C27 H27F 0.9800 . ? C25 Cl3 1.775(17) . ? C25 Cl4 1.789(17) . ? C28 Cl5 1.756(18) . ? C28 Cl6 1.820(17) . ? C28 H28C 0.9900 . ? C28 H28D 0.9900 . ? 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 N6 Pd N3 176.13(14) . . ? N6 Pd Cl2 87.79(9) . . ? N3 Pd Cl2 89.56(9) . . ? N6 Pd Cl1 91.99(8) . . ? N3 Pd Cl1 90.85(9) . . ? Cl2 Pd Cl1 176.14(5) . . ? N2 N1 C1 111.5(3) . . ? N2 N1 C7 118.3(3) . . ? C1 N1 C7 129.5(3) . . ? N3 N2 N1 106.4(3) . . ? N2 N3 C6 111.0(3) . . ? N2 N3 Pd 119.8(2) . . ? C6 N3 Pd 129.1(3) . . ? N5 N4 C18 111.3(3) . . ? N5 N4 C19 119.0(3) . . ? C18 N4 C19 129.4(3) . . ? N6 N5 N4 106.4(3) . . ? N5 N6 C13 111.0(3) . . ? N5 N6 Pd 122.0(3) . . ? C13 N6 Pd 127.0(3) . . ? N1 C1 C6 104.7(3) . . ? N1 C1 C2 133.9(4) . . ? C6 C1 C2 121.4(4) . . ? C3 C2 C1 116.7(4) . . ? C3 C2 H2A 121.7 . . ? C1 C2 H2A 121.7 . . ? C2 C3 C4 122.8(4) . . ? C2 C3 H3A 118.6 . . ? C4 C3 H3A 118.6 . . ? C5 C4 C3 121.2(4) . . ? C5 C4 H4A 119.4 . . ? C3 C4 H4A 119.4 . . ? C4 C5 C6 117.2(4) . . ? C4 C5 H5A 121.4 . . ? C6 C5 H5A 121.4 . . ? N3 C6 C1 106.4(3) . . ? N3 C6 C5 132.9(4) . . ? C1 C6 C5 120.8(4) . . ? N1 C7 C8 115.0(3) . . ? N1 C7 H7A 108.5 . . ? C8 C7 H7A 108.5 . . ? N1 C7 H7B 108.5 . . ? C8 C7 H7B 108.5 . . ? H7A C7 H7B 107.5 . . ? C11 C8 C9 120.7(4) . . ? C11 C8 C7 120.5(4) . . ? C9 C8 C7 118.7(4) . . ? C9 C9 C8 119.4(2) 7_575 . ? C9 C9 C10 120.7(3) 7_575 . ? C8 C9 C10 119.9(4) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C10 H10D 109.5 . . ? H10A C10 H10D 141.1 . . ? H10B C10 H10D 56.3 . . ? H10C C10 H10D 56.3 . . ? C9 C10 H10E 109.5 . . ? H10A C10 H10E 56.3 . . ? H10B C10 H10E 141.1 . . ? H10C C10 H10E 56.3 . . ? H10D C10 H10E 109.5 . . ? C9 C10 H10F 109.5 . . ? H10A C10 H10F 56.3 . . ? H10B C10 H10F 56.3 . . ? H10C C10 H10F 141.1 . . ? H10D C10 H10F 109.5 . . ? H10E C10 H10F 109.5 . . ? C11 C11 C8 119.8(2) 7_575 . ? C11 C11 C12 119.7(2) 7_575 . ? C8 C11 C12 120.5(4) . . ? 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 . . ? C11 C12 H12D 109.5 . . ? H12A C12 H12D 141.1 . . ? H12B C12 H12D 56.3 . . ? H12C C12 H12D 56.3 . . ? C11 C12 H12E 109.5 . . ? H12A C12 H12E 56.3 . . ? H12B C12 H12E 141.1 . . ? H12C C12 H12E 56.3 . . ? H12D C12 H12E 109.5 . . ? C11 C12 H12F 109.5 . . ? H12A C12 H12F 56.3 . . ? H12B C12 H12F 56.3 . . ? H12C C12 H12F 141.1 . . ? H12D C12 H12F 109.5 . . ? H12E C12 H12F 109.5 . . ? N6 C13 C18 106.3(4) . . ? N6 C13 C14 131.9(3) . . ? C18 C13 C14 121.8(4) . . ? C15 C14 C13 117.0(4) . . ? C15 C14 H14A 121.5 . . ? C13 C14 H14A 121.5 . . ? C14 C15 C16 121.3(4) . . ? C14 C15 H15A 119.3 . . ? C16 C15 H15A 119.3 . . ? C17 C16 C15 122.5(4) . . ? C17 C16 H16A 118.8 . . ? C15 C16 H16A 118.8 . . ? C16 C17 C18 116.2(4) . . ? C16 C17 H17A 121.9 . . ? C18 C17 H17A 121.9 . . ? N4 C18 C13 105.0(3) . . ? N4 C18 C17 133.8(4) . . ? C13 C18 C17 121.2(4) . . ? N4 C19 C20 114.3(3) . . ? N4 C19 H19A 108.7 . . ? C20 C19 H19A 108.7 . . ? N4 C19 H19B 108.7 . . ? C20 C19 H19B 108.7 . . ? H19A C19 H19B 107.6 . . ? C23 C20 C21 120.1(4) . . ? C23 C20 C19 119.3(4) . . ? C21 C20 C19 120.6(4) . . ? C21 C21 C20 119.8(2) 7_575 . ? C21 C21 C22 120.5(3) 7_575 . ? C20 C21 C22 119.7(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 . . ? C21 C22 H22D 109.5 . . ? H22A C22 H22D 141.1 . . ? H22B C22 H22D 56.3 . . ? H22C C22 H22D 56.3 . . ? C21 C22 H22E 109.5 . . ? H22A C22 H22E 56.3 . . ? H22B C22 H22E 141.1 . . ? H22C C22 H22E 56.3 . . ? H22D C22 H22E 109.5 . . ? C21 C22 H22F 109.5 . . ? H22A C22 H22F 56.3 . . ? H22B C22 H22F 56.3 . . ? H22C C22 H22F 141.1 . . ? H22D C22 H22F 109.5 . . ? H22E C22 H22F 109.5 . . ? C20 C23 C23 119.8(2) . 7_575 ? C20 C23 C24 120.3(4) . . ? C23 C23 C24 119.9(2) 7_575 . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C24 H24D 109.5 . . ? H24A C24 H24D 141.1 . . ? H24B C24 H24D 56.3 . . ? H24C C24 H24D 56.3 . . ? C23 C24 H24E 109.5 . . ? H24A C24 H24E 56.3 . . ? H24B C24 H24E 141.1 . . ? H24C C24 H24E 56.3 . . ? H24D C24 H24E 109.5 . . ? C23 C24 H24F 109.5 . . ? H24A C24 H24F 56.3 . . ? H24B C24 H24F 56.3 . . ? H24C C24 H24F 141.1 . . ? H24D C24 H24F 109.5 . . ? H24E C24 H24F 109.5 . . ? N7 C26 C27 176.9(11) . . ? C26 C27 H27D 109.5 . . ? C26 C27 H27E 109.5 . . ? H27D C27 H27E 109.5 . . ? C26 C27 H27F 109.5 . . ? H27D C27 H27F 109.5 . . ? H27E C27 H27F 109.5 . . ? Cl3 C25 Cl4 105.3(13) . . ? Cl5 C28 Cl6 96.5(14) . . ? Cl5 C28 H28C 112.5 . . ? Cl6 C28 H28C 112.5 . . ? Cl5 C28 H28D 112.5 . . ? Cl6 C28 H28D 112.5 . . ? H28C C28 H28D 110.0 . . ? 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 C1 N1 N2 N3 0.5(4) . . . . ? C7 N1 N2 N3 172.3(3) . . . . ? N1 N2 N3 C6 0.4(4) . . . . ? N1 N2 N3 Pd 178.9(2) . . . . ? N6 Pd N3 N2 -172.5(17) . . . . ? Cl2 Pd N3 N2 -125.7(3) . . . . ? Cl1 Pd N3 N2 50.4(3) . . . . ? N6 Pd N3 C6 6(2) . . . . ? Cl2 Pd N3 C6 52.5(3) . . . . ? Cl1 Pd N3 C6 -131.3(3) . . . . ? C18 N4 N5 N6 -1.2(4) . . . . ? C19 N4 N5 N6 -175.4(3) . . . . ? N4 N5 N6 C13 1.3(4) . . . . ? N4 N5 N6 Pd -177.3(2) . . . . ? N3 Pd N6 N5 170.3(17) . . . . ? Cl2 Pd N6 N5 123.6(3) . . . . ? Cl1 Pd N6 N5 -52.6(3) . . . . ? N3 Pd N6 C13 -8(2) . . . . ? Cl2 Pd N6 C13 -54.7(3) . . . . ? Cl1 Pd N6 C13 129.1(3) . . . . ? N2 N1 C1 C6 -1.0(4) . . . . ? C7 N1 C1 C6 -171.8(4) . . . . ? N2 N1 C1 C2 -179.7(4) . . . . ? C7 N1 C1 C2 9.6(7) . . . . ? N1 C1 C2 C3 179.0(4) . . . . ? C6 C1 C2 C3 0.5(6) . . . . ? C1 C2 C3 C4 0.3(7) . . . . ? C2 C3 C4 C5 -0.1(7) . . . . ? C3 C4 C5 C6 -0.8(6) . . . . ? N2 N3 C6 C1 -1.0(4) . . . . ? Pd N3 C6 C1 -179.3(3) . . . . ? N2 N3 C6 C5 -179.2(4) . . . . ? Pd N3 C6 C5 2.5(6) . . . . ? N1 C1 C6 N3 1.2(4) . . . . ? C2 C1 C6 N3 -179.9(4) . . . . ? N1 C1 C6 C5 179.6(3) . . . . ? C2 C1 C6 C5 -1.5(6) . . . . ? C4 C5 C6 N3 179.5(4) . . . . ? C4 C5 C6 C1 1.6(6) . . . . ? N2 N1 C7 C8 53.3(5) . . . . ? C1 N1 C7 C8 -136.5(4) . . . . ? N1 C7 C8 C11 -93.1(4) . . . . ? N1 C7 C8 C9 90.3(4) . . . . ? C11 C8 C9 C9 -3.2(4) . . . 7_575 ? C7 C8 C9 C9 173.4(2) . . . 7_575 ? C11 C8 C9 C10 178.2(4) . . . . ? C7 C8 C9 C10 -5.2(5) . . . . ? C9 C8 C11 C11 3.2(4) . . . 7_575 ? C7 C8 C11 C11 -173.3(2) . . . 7_575 ? C9 C8 C11 C12 -176.6(3) . . . . ? C7 C8 C11 C12 6.8(5) . . . . ? N5 N6 C13 C18 -0.9(4) . . . . ? Pd N6 C13 C18 177.5(2) . . . . ? N5 N6 C13 C14 178.4(4) . . . . ? Pd N6 C13 C14 -3.2(6) . . . . ? N6 C13 C14 C15 179.0(4) . . . . ? C18 C13 C14 C15 -1.8(6) . . . . ? C13 C14 C15 C16 0.6(6) . . . . ? C14 C15 C16 C17 0.8(7) . . . . ? C15 C16 C17 C18 -1.1(6) . . . . ? N5 N4 C18 C13 0.6(4) . . . . ? C19 N4 C18 C13 174.1(4) . . . . ? N5 N4 C18 C17 179.7(4) . . . . ? C19 N4 C18 C17 -6.8(7) . . . . ? N6 C13 C18 N4 0.1(4) . . . . ? C14 C13 C18 N4 -179.2(3) . . . . ? N6 C13 C18 C17 -179.1(3) . . . . ? C14 C13 C18 C17 1.5(6) . . . . ? C16 C17 C18 N4 -179.0(4) . . . . ? C16 C17 C18 C13 -0.1(6) . . . . ? N5 N4 C19 C20 -47.7(5) . . . . ? C18 N4 C19 C20 139.2(4) . . . . ? N4 C19 C20 C23 -85.4(4) . . . . ? N4 C19 C20 C21 98.0(4) . . . . ? C23 C20 C21 C21 -5.9(4) . . . 7_575 ? C19 C20 C21 C21 170.7(2) . . . 7_575 ? C23 C20 C21 C22 173.3(3) . . . . ? C19 C20 C21 C22 -10.1(5) . . . . ? C21 C20 C23 C23 5.9(4) . . . 7_575 ? C19 C20 C23 C23 -170.7(2) . . . 7_575 ? C21 C20 C23 C24 -175.8(3) . . . . ? C19 C20 C23 C24 7.6(5) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.987 _refine_diff_density_min -0.525 _refine_diff_density_rms 0.068 #============# data_1a _database_code_depnum_ccdc_archive 'CCDC 767084' #TrackingRef 'Compds-rev.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H64 Cl4 N8 O6 Pd2' _chemical_formula_weight 1251.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.8379(11) _cell_length_b 18.9967(19) _cell_length_c 12.7049(11) _cell_angle_alpha 90.00 _cell_angle_beta 109.101(8) _cell_angle_gamma 90.00 _cell_volume 2699.8(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2470 _cell_measurement_theta_min 3.6899 _cell_measurement_theta_max 61.5536 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.540 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1280 _exptl_absorpt_coefficient_mu 7.651 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2232 _exptl_absorpt_correction_T_max 0.3740 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 16.0855 _diffrn_measurement_device_type Oxford _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7657 _diffrn_reflns_av_R_equivalents 0.0524 _diffrn_reflns_av_sigmaI/netI 0.0526 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 4.36 _diffrn_reflns_theta_max 59.97 _reflns_number_total 3502 _reflns_number_gt 2625 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; The solvated water molecules were restrained by ISOR to make anisotropic displacement parameters reasonable (18 restaints). 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^)+(0.0910P)^2^+48.9230P] 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 3502 _refine_ls_number_parameters 329 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.1219 _refine_ls_R_factor_gt 0.0926 _refine_ls_wR_factor_ref 0.2364 _refine_ls_wR_factor_gt 0.2152 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.019 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd 0.45766(8) 0.47715(6) 0.79706(7) 0.0496(3) Uani 1 1 d . . . Cl1 Cl 0.6004(3) 0.56230(19) 0.8179(3) 0.0560(8) Uani 1 1 d . . . Cl2 Cl 0.3148(3) 0.3909(2) 0.7552(3) 0.0600(9) Uani 1 1 d . . . C1 C 0.2937(12) 0.5960(7) 0.6883(10) 0.051(3) Uani 1 1 d . . . H1 H 0.3337 0.6030 0.6372 0.061 Uiso 1 1 calc R . . C2 C 0.1636(11) 0.6043(7) 0.7756(10) 0.050(3) Uani 1 1 d . . . C3 C 0.0662(12) 0.6214(9) 0.8125(11) 0.064(4) Uani 1 1 d . . . H3 H 0.0096 0.6552 0.7776 0.077 Uiso 1 1 calc R . . C4 C 0.0613(12) 0.5837(8) 0.9046(11) 0.063(4) Uani 1 1 d . . . H4 H -0.0004 0.5925 0.9330 0.075 Uiso 1 1 calc R . . C5 C 0.1480(12) 0.5323(8) 0.9564(10) 0.058(4) Uani 1 1 d . . . H5 H 0.1436 0.5090 1.0193 0.070 Uiso 1 1 calc R . . C6 C 0.2361(11) 0.5166(8) 0.9163(10) 0.052(3) Uani 1 1 d . . . H6 H 0.2915 0.4818 0.9498 0.062 Uiso 1 1 calc R . . C7 C 0.2442(11) 0.5530(7) 0.8235(10) 0.050(3) Uani 1 1 d . . . C8 C 0.1356(12) 0.6911(8) 0.6170(11) 0.061(4) Uani 1 1 d . . . H8A H 0.1670 0.7353 0.6531 0.073 Uiso 1 1 calc R . . H8B H 0.0507 0.6896 0.6067 0.073 Uiso 1 1 calc R . . C9 C 0.1540(11) 0.6876(7) 0.5032(10) 0.048(3) Uani 1 1 d . . . C10 C 0.0914(11) 0.6394(7) 0.4245(10) 0.049(3) Uani 1 1 d . . . C11 C 0.0958(11) 0.6401(8) 0.3188(10) 0.052(3) Uani 1 1 d . . . C12 C 0.1622(11) 0.6914(8) 0.2882(10) 0.050(3) Uani 1 1 d . . . C13 C 0.2340(11) 0.7370(7) 0.3683(11) 0.050(3) Uani 1 1 d . . . C14 C 0.2285(11) 0.7349(7) 0.4760(11) 0.051(3) Uani 1 1 d . . . C15 C 0.0126(14) 0.5848(8) 0.4548(14) 0.073(4) Uani 1 1 d . . . H15A H 0.0583 0.5429 0.4819 0.110 Uiso 1 1 calc R . . H15B H -0.0541 0.5736 0.3899 0.110 Uiso 1 1 calc R . . H15C H -0.0161 0.6035 0.5115 0.110 Uiso 1 1 calc R . . C16 C 0.0287(14) 0.5842(10) 0.2358(13) 0.079(5) Uani 1 1 d . . . H16A H 0.0557 0.5847 0.1723 0.119 Uiso 1 1 calc R . . H16B H -0.0554 0.5939 0.2123 0.119 Uiso 1 1 calc R . . H16C H 0.0437 0.5387 0.2706 0.119 Uiso 1 1 calc R . . C17 C 0.3182(14) 0.7895(8) 0.3404(15) 0.081(5) Uani 1 1 d . . . H17A H 0.3060 0.8355 0.3659 0.121 Uiso 1 1 calc R . . H17B H 0.3020 0.7905 0.2613 0.121 Uiso 1 1 calc R . . H17C H 0.3996 0.7753 0.3766 0.121 Uiso 1 1 calc R . . C18 C 0.3099(13) 0.7841(9) 0.5641(14) 0.081(5) Uani 1 1 d . . . H18A H 0.3460 0.8178 0.5286 0.122 Uiso 1 1 calc R . . H18B H 0.3712 0.7571 0.6168 0.122 Uiso 1 1 calc R . . H18C H 0.2634 0.8084 0.6021 0.122 Uiso 1 1 calc R . . C19 C 0.1622(13) 0.7004(9) 0.1705(11) 0.070(5) Uani 1 1 d . . . H19A H 0.0899 0.6794 0.1201 0.083 Uiso 1 1 calc R . . H19B H 0.1604 0.7502 0.1536 0.083 Uiso 1 1 calc R . . C20 C 0.3340(12) 0.6149(7) 0.1999(10) 0.052(3) Uani 1 1 d . . . H20 H 0.3223 0.5908 0.2591 0.062 Uiso 1 1 calc R . . C21 C 0.3132(12) 0.6897(8) 0.0681(9) 0.053(4) Uani 1 1 d . . . C22 C 0.2756(12) 0.7424(8) -0.0156(10) 0.055(4) Uani 1 1 d . . . H22 H 0.2115 0.7719 -0.0202 0.066 Uiso 1 1 calc R . . C23 C 0.3376(12) 0.7477(7) -0.0887(10) 0.053(3) Uani 1 1 d . . . H23 H 0.3160 0.7823 -0.1434 0.064 Uiso 1 1 calc R . . C24 C 0.4315(12) 0.7032(7) -0.0842(10) 0.052(3) Uani 1 1 d . . . H24 H 0.4708 0.7085 -0.1363 0.062 Uiso 1 1 calc R . . C25 C 0.4684(11) 0.6510(7) -0.0040(10) 0.051(3) Uani 1 1 d . . . H25 H 0.5324 0.6214 0.0002 0.062 Uiso 1 1 calc R . . C26 C 0.4028(11) 0.6453(7) 0.0713(10) 0.045(3) Uani 1 1 d . . . N1 N 0.3249(8) 0.5515(5) 0.7656(7) 0.038(2) Uani 1 1 d . . . N2 N 0.1953(9) 0.6328(6) 0.6875(8) 0.054(3) Uani 1 1 d . . . N3 N 0.4173(8) 0.5986(5) 0.1602(7) 0.039(2) Uani 1 1 d . . . N4 N 0.2660(10) 0.6685(6) 0.1503(8) 0.053(3) Uani 1 1 d . . . O1 O 0.3630(17) 0.5679(11) 0.4584(14) 0.159(7) Uani 1 1 d U . . O2 O 0.2748(19) 0.4436(12) 0.4946(17) 0.176(7) Uani 1 1 d U . . O3 O 0.439(2) 0.3690(12) 0.4257(19) 0.193(8) Uani 1 1 d U . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd 0.0488(5) 0.0609(6) 0.0400(5) 0.0038(5) 0.0159(4) 0.0076(5) Cl1 0.0440(16) 0.068(2) 0.0584(19) 0.0057(17) 0.0193(14) 0.0028(15) Cl2 0.0430(17) 0.073(2) 0.0584(19) -0.0076(17) 0.0089(14) -0.0043(16) C1 0.057(8) 0.061(9) 0.033(6) 0.000(6) 0.015(6) -0.001(7) C2 0.052(7) 0.065(9) 0.043(7) 0.001(6) 0.030(6) 0.010(7) C3 0.055(8) 0.092(11) 0.052(8) -0.006(8) 0.026(7) 0.011(8) C4 0.057(8) 0.094(12) 0.046(7) -0.004(8) 0.028(7) -0.003(8) C5 0.063(8) 0.082(11) 0.035(6) 0.001(7) 0.024(6) -0.006(8) C6 0.047(7) 0.071(9) 0.035(6) 0.009(7) 0.009(5) 0.005(7) C7 0.045(7) 0.064(9) 0.034(6) -0.005(6) 0.005(6) 0.002(7) C8 0.055(8) 0.083(10) 0.052(8) 0.008(8) 0.027(7) 0.028(8) C9 0.038(6) 0.063(9) 0.045(7) 0.023(7) 0.015(6) 0.020(6) C10 0.043(7) 0.059(9) 0.046(7) 0.008(6) 0.013(6) 0.010(6) C11 0.038(7) 0.065(9) 0.048(7) 0.012(7) 0.009(6) 0.009(6) C12 0.037(6) 0.070(9) 0.041(7) 0.006(7) 0.010(6) 0.021(7) C13 0.045(7) 0.055(8) 0.057(8) 0.000(7) 0.024(6) -0.003(6) C14 0.036(7) 0.059(9) 0.052(8) -0.014(7) 0.008(6) 0.008(6) C15 0.062(9) 0.069(10) 0.088(11) 0.013(9) 0.023(8) -0.008(8) C16 0.061(9) 0.104(13) 0.068(10) 0.001(9) 0.014(8) 0.001(9) C17 0.078(10) 0.068(11) 0.123(14) 0.019(9) 0.069(10) 0.012(9) C18 0.058(9) 0.091(13) 0.100(12) -0.032(10) 0.033(9) -0.030(9) C19 0.060(8) 0.108(13) 0.040(7) 0.016(8) 0.015(6) 0.043(9) C20 0.062(8) 0.056(9) 0.030(6) 0.008(6) 0.007(6) 0.001(7) C21 0.050(8) 0.074(10) 0.029(6) -0.003(6) 0.003(6) 0.011(7) C22 0.049(8) 0.070(10) 0.039(7) -0.004(7) 0.005(6) 0.009(7) C23 0.071(9) 0.059(9) 0.033(6) 0.007(6) 0.022(6) 0.003(7) C24 0.057(8) 0.066(9) 0.034(6) 0.003(6) 0.017(6) -0.009(7) C25 0.046(7) 0.068(9) 0.039(7) -0.014(6) 0.012(6) -0.017(7) C26 0.044(7) 0.051(8) 0.036(6) -0.006(6) 0.009(5) -0.012(6) N1 0.027(5) 0.053(6) 0.029(5) -0.002(5) 0.005(4) -0.008(4) N2 0.053(6) 0.069(8) 0.042(6) 0.012(5) 0.017(5) 0.024(6) N3 0.041(5) 0.053(6) 0.022(4) -0.001(4) 0.010(4) -0.009(5) N4 0.052(6) 0.065(8) 0.043(6) 0.002(5) 0.015(5) 0.015(6) O1 0.171(13) 0.194(14) 0.120(10) 0.042(10) 0.059(10) 0.008(12) O2 0.176(14) 0.203(15) 0.161(13) 0.009(12) 0.070(11) 0.010(12) O3 0.231(16) 0.186(15) 0.189(14) 0.016(12) 0.107(12) -0.004(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd N3 2.008(10) 3_666 ? Pd N1 2.052(10) . ? Pd Cl2 2.288(4) . ? Pd Cl1 2.291(4) . ? C1 N1 1.257(15) . ? C1 N2 1.355(16) . ? C1 H1 0.9300 . ? C2 C7 1.361(18) . ? C2 N2 1.401(16) . ? C2 C3 1.417(17) . ? C3 C4 1.389(19) . ? C3 H3 0.9300 . ? C4 C5 1.413(19) . ? C4 H4 0.9300 . ? C5 C6 1.336(18) . ? C5 H5 0.9300 . ? C6 C7 1.397(18) . ? C6 H6 0.9300 . ? C7 N1 1.383(15) . ? C8 N2 1.455(16) . ? C8 C9 1.532(17) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.379(18) . ? C9 C14 1.379(19) . ? C10 C11 1.362(18) . ? C10 C15 1.527(19) . ? C11 C12 1.385(19) . ? C11 C16 1.52(2) . ? C12 C13 1.394(18) . ? C12 C19 1.505(18) . ? C13 C14 1.391(18) . ? C13 C17 1.531(19) . ? C14 C18 1.534(19) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 N4 1.466(17) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 N3 1.283(16) . ? C20 N4 1.323(16) . ? C20 H20 0.9300 . ? C21 C26 1.345(18) . ? C21 N4 1.396(17) . ? C21 C22 1.421(19) . ? C22 C23 1.363(18) . ? C22 H22 0.9300 . ? C23 C24 1.382(19) . ? C23 H23 0.9300 . ? C24 C25 1.387(18) . ? C24 H24 0.9300 . ? C25 C26 1.420(17) . ? C25 H25 0.9300 . ? C26 N3 1.402(15) . ? N3 Pd 2.008(10) 3_666 ? 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 N3 Pd N1 174.6(4) 3_666 . ? N3 Pd Cl2 88.5(3) 3_666 . ? N1 Pd Cl2 89.2(3) . . ? N3 Pd Cl1 91.4(3) 3_666 . ? N1 Pd Cl1 91.5(3) . . ? Cl2 Pd Cl1 173.32(13) . . ? N1 C1 N2 112.6(11) . . ? N1 C1 H1 123.7 . . ? N2 C1 H1 123.7 . . ? C7 C2 N2 107.5(10) . . ? C7 C2 C3 122.9(12) . . ? N2 C2 C3 129.6(12) . . ? C4 C3 C2 115.1(13) . . ? C4 C3 H3 122.5 . . ? C2 C3 H3 122.5 . . ? C3 C4 C5 121.6(12) . . ? C3 C4 H4 119.2 . . ? C5 C4 H4 119.2 . . ? C6 C5 C4 121.0(12) . . ? C6 C5 H5 119.5 . . ? C4 C5 H5 119.5 . . ? C5 C6 C7 119.3(13) . . ? C5 C6 H6 120.3 . . ? C7 C6 H6 120.3 . . ? C2 C7 N1 106.4(11) . . ? C2 C7 C6 120.0(12) . . ? N1 C7 C6 133.5(12) . . ? N2 C8 C9 110.9(10) . . ? N2 C8 H8A 109.5 . . ? C9 C8 H8A 109.5 . . ? N2 C8 H8B 109.5 . . ? C9 C8 H8B 109.5 . . ? H8A C8 H8B 108.0 . . ? C10 C9 C14 119.1(12) . . ? C10 C9 C8 120.3(12) . . ? C14 C9 C8 120.6(13) . . ? C11 C10 C9 121.6(13) . . ? C11 C10 C15 118.6(13) . . ? C9 C10 C15 119.8(12) . . ? C10 C11 C12 119.5(13) . . ? C10 C11 C16 119.7(13) . . ? C12 C11 C16 120.8(12) . . ? C11 C12 C13 119.9(12) . . ? C11 C12 C19 122.8(13) . . ? C13 C12 C19 117.2(13) . . ? C14 C13 C12 119.1(12) . . ? C14 C13 C17 119.4(13) . . ? C12 C13 C17 121.5(13) . . ? C9 C14 C13 120.4(12) . . ? C9 C14 C18 120.9(12) . . ? C13 C14 C18 118.7(13) . . ? C10 C15 H15A 109.5 . . ? C10 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C10 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C13 C17 H17A 109.5 . . ? C13 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C13 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C14 C18 H18A 109.5 . . ? C14 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C14 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N4 C19 C12 113.6(10) . . ? N4 C19 H19A 108.9 . . ? C12 C19 H19A 108.9 . . ? N4 C19 H19B 108.9 . . ? C12 C19 H19B 108.9 . . ? H19A C19 H19B 107.7 . . ? N3 C20 N4 115.1(11) . . ? N3 C20 H20 122.4 . . ? N4 C20 H20 122.4 . . ? C26 C21 N4 107.6(12) . . ? C26 C21 C22 121.0(12) . . ? N4 C21 C22 131.2(12) . . ? C23 C22 C21 117.1(13) . . ? C23 C22 H22 121.5 . . ? C21 C22 H22 121.5 . . ? C22 C23 C24 122.1(12) . . ? C22 C23 H23 118.9 . . ? C24 C23 H23 118.9 . . ? C23 C24 C25 121.6(12) . . ? C23 C24 H24 119.2 . . ? C25 C24 H24 119.2 . . ? C24 C25 C26 116.0(13) . . ? C24 C25 H25 122.0 . . ? C26 C25 H25 122.0 . . ? C21 C26 N3 107.9(11) . . ? C21 C26 C25 122.1(12) . . ? N3 C26 C25 129.9(12) . . ? C1 N1 C7 108.9(11) . . ? C1 N1 Pd 128.8(9) . . ? C7 N1 Pd 121.9(8) . . ? C1 N2 C2 104.5(10) . . ? C1 N2 C8 129.9(11) . . ? C2 N2 C8 125.6(10) . . ? C20 N3 C26 104.9(10) . . ? C20 N3 Pd 131.3(8) . 3_666 ? C26 N3 Pd 123.8(8) . 3_666 ? C20 N4 C21 104.4(11) . . ? C20 N4 C19 130.4(12) . . ? C21 N4 C19 125.2(11) . . ? _diffrn_measured_fraction_theta_max 0.874 _diffrn_reflns_theta_full 59.97 _diffrn_measured_fraction_theta_full 0.874 _refine_diff_density_max 1.806 _refine_diff_density_min -0.934 _refine_diff_density_rms 0.159 #=================END