# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email milaniba@units.it _publ_contact_author_name 'Barbara Milani' loop_ _publ_author_name 'Angelo Meduri' 'Daniela Cozzula' "Angela D'Amora" 'Ennio Zangrando' 'Serafino Gladiali' 'Barbara Milani' data_3a _database_code_depnum_ccdc_archive 'CCDC 864728' #TrackingRef '- data.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H40 N6 O2 Pd2 2+, 2(Cl 1-)' _chemical_formula_sum 'C46 H40 Cl2 N6 O2 Pd2' _chemical_formula_weight 992.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 4322' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x, -y, -z+1/2' '-x, y, -z' '-y, -x, -z+3/4' 'y, x, -z+1/4' 'y, -x, z+1/4' '-y, x, z+3/4' _cell_length_a 16.527(3) _cell_length_b 16.527(3) _cell_length_c 17.005(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4644.8(18) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.419 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2000 _exptl_absorpt_coefficient_mu 7.638 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.1340 _exptl_absorpt_correction_T_max 0.2323 _exptl_absorpt_process_details ; Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56 Quadratic fit to sin(theta)/lambda - 18 parameters ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28058 _diffrn_reflns_av_R_equivalents 0.0535 _diffrn_reflns_av_sigmaI/netI 0.0867 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.67 _diffrn_reflns_theta_max 57.87 _reflns_number_total 2988 _reflns_number_gt 1222 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Nonius, Supergui' _computing_cell_refinement 'Denzo (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELX97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELX97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep3 for Windows (Farrugia,1997)' _computing_publication_material 'Wingx 1.80.05 (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0196P)^2^+46.4302P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.09(5) _refine_ls_number_reflns 2988 _refine_ls_number_parameters 169 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1128 _refine_ls_R_factor_gt 0.0636 _refine_ls_wR_factor_ref 0.1739 _refine_ls_wR_factor_gt 0.1433 _refine_ls_goodness_of_fit_ref 1.109 _refine_ls_restrained_S_all 1.109 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd 0.92577(10) 0.47402(12) 0.83571(10) 0.0913(7) Uani 1 1 d . . . N2 N 0.8227(11) 0.5153(13) 0.8833(9) 0.093(6) Uani 1 1 d . . . N1 N 0.9482(10) 0.6023(11) 0.8388(10) 0.090(6) Uani 1 1 d . . . N3 N 1.0348(10) 0.5694(10) 0.6960(9) 0.088(5) Uani 1 1 d . . . O1 O 1.1323(9) 0.6495(10) 0.7479(9) 0.103(5) Uani 1 1 d . . . C1 C 1.0071(15) 0.6507(14) 0.8128(13) 0.089(8) Uiso 1 1 d . . . C2 C 1.0192(16) 0.7302(14) 0.8406(15) 0.116(8) Uiso 1 1 d . . . H9 H 1.0610 0.7618 0.8208 0.139 Uiso 1 1 calc R . . C3 C 0.9693(16) 0.7596(15) 0.8963(14) 0.117(8) Uiso 1 1 d . . . H8 H 0.9788 0.8108 0.9170 0.140 Uiso 1 1 calc R . . C4 C 0.9053(15) 0.7158(15) 0.9229(15) 0.104(8) Uiso 1 1 d . . . C5 C 0.8940(15) 0.6402(16) 0.8933(14) 0.101(8) Uiso 1 1 d . . . C6 C 0.8257(13) 0.5909(14) 0.9117(14) 0.088(7) Uiso 1 1 d . . . C7 C 0.7693(17) 0.6286(17) 0.9663(14) 0.110(8) Uiso 1 1 d . . . C8 C 0.7013(18) 0.5789(18) 0.9745(16) 0.137(11) Uiso 1 1 d . . . H3 H 0.6601 0.5987 1.0062 0.165 Uiso 1 1 calc R . . C9 C 0.6885(17) 0.5059(18) 0.9419(15) 0.141(11) Uiso 1 1 d . . . H2 H 0.6400 0.4781 0.9485 0.170 Uiso 1 1 calc R . . C10 C 0.7532(16) 0.4737(17) 0.8967(15) 0.121(9) Uiso 1 1 d . . . H1 H 0.7478 0.4221 0.8756 0.146 Uiso 1 1 calc R . . C11 C 0.7842(16) 0.7016(15) 0.9953(16) 0.112(9) Uiso 1 1 d . . . H11 H 0.7461 0.7230 1.0297 0.134 Uiso 1 1 calc R . . C12 C 0.8449(16) 0.7446(15) 0.9806(14) 0.115(9) Uiso 1 1 d . . . H12 H 0.8519 0.7941 1.0058 0.138 Uiso 1 1 calc R . . C13 C 1.0584(15) 0.6198(16) 0.7467(15) 0.092(8) Uiso 1 1 d . . . C14 C 1.1653(15) 0.6215(15) 0.6729(15) 0.111(8) Uiso 1 1 d . . . H14 H 1.2205 0.6019 0.6820 0.133 Uiso 1 1 calc R . . C15 C 1.1116(12) 0.5487(12) 0.6530(11) 0.084(6) Uiso 1 1 d . . . H15 H 1.1352 0.4995 0.6756 0.101 Uiso 1 1 calc R . . C16 C 1.0962(12) 0.5359(13) 0.5657(11) 0.110(8) Uiso 1 1 d . . . H16A H 1.0794 0.5860 0.5423 0.165 Uiso 1 1 calc R . . H16B H 1.0545 0.4961 0.5589 0.165 Uiso 1 1 calc R . . H16C H 1.1450 0.5175 0.5408 0.165 Uiso 1 1 calc R . . C17 C 1.1691(18) 0.6889(18) 0.6138(16) 0.129(10) Uiso 1 1 d . . . C18 C 1.1125(17) 0.7469(17) 0.6088(16) 0.133(10) Uiso 1 1 d . . . H18 H 1.0700 0.7488 0.6445 0.160 Uiso 1 1 calc R . . C19 C 1.119(2) 0.805(2) 0.5485(19) 0.176(14) Uiso 1 1 d . . . H19 H 1.0806 0.8455 0.5411 0.211 Uiso 1 1 calc R . . C20 C 1.188(2) 0.7965(18) 0.500(2) 0.148(11) Uiso 1 1 d . . . H20 H 1.1940 0.8343 0.4600 0.178 Uiso 1 1 calc R . . C21 C 1.246(2) 0.7398(18) 0.506(2) 0.159(12) Uiso 1 1 d . . . H21 H 1.2891 0.7394 0.4704 0.191 Uiso 1 1 calc R . . C22 C 1.2415(19) 0.6817(18) 0.5650(18) 0.161(11) Uiso 1 1 d . . . H22 H 1.2808 0.6422 0.5728 0.193 Uiso 1 1 calc R . . C23 C 0.8967(13) 0.3616(11) 0.8531(14) 0.112(9) Uani 1 1 d . . . H23A H 0.8748 0.3392 0.8055 0.168 Uiso 1 1 calc R . . H23B H 0.8570 0.3583 0.8942 0.168 Uiso 1 1 calc R . . H23C H 0.9440 0.3316 0.8682 0.168 Uiso 1 1 calc R . . Cl1 Cl 0.5000 0.6748(15) 1.0000 0.27(2) Uani 0.50 2 d SP . . Cl2 Cl 0.4737(11) 0.5263(11) 0.8750 0.202(10) Uani 0.50 2 d SP . . Cl3 Cl 0.6067(13) 0.5000 0.7500 0.149(8) Uani 0.50 2 d SP . . Cl4 Cl 0.461(4) 0.695(2) 0.9170(18) 0.20(2) Uani 0.25 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd 0.0905(13) 0.1124(15) 0.0711(9) -0.0025(11) 0.0036(10) 0.0032(12) N2 0.093(14) 0.106(16) 0.079(13) 0.018(12) -0.004(10) 0.029(13) N1 0.090(15) 0.121(16) 0.060(10) -0.011(11) -0.012(11) 0.015(11) N3 0.080(13) 0.095(13) 0.090(12) 0.001(11) 0.012(11) -0.034(10) O1 0.086(11) 0.146(16) 0.077(10) -0.016(10) 0.001(10) -0.014(11) C23 0.12(2) 0.050(15) 0.16(2) -0.016(16) 0.044(18) -0.035(13) Cl1 0.21(4) 0.074(18) 0.52(7) 0.000 0.19(5) 0.000 Cl2 0.195(14) 0.195(14) 0.22(3) 0.005(15) 0.005(15) 0.00(2) Cl3 0.17(2) 0.15(2) 0.129(16) 0.027(14) 0.000 0.000 Cl4 0.35(6) 0.13(3) 0.11(2) 0.02(2) 0.03(4) -0.08(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd C23 1.942(17) . ? Pd N2 2.006(16) . ? Pd N3 2.013(16) 3_566 ? Pd N1 2.154(18) . ? Pd Pd 3.039(4) 3_566 ? N2 C6 1.34(2) . ? N2 C10 1.36(3) . ? N1 C1 1.34(2) . ? N1 C5 1.43(2) . ? N3 C13 1.26(2) . ? N3 C15 1.51(2) . ? N3 Pd 2.013(16) 3_566 ? O1 C13 1.32(2) . ? O1 C14 1.46(3) . ? C1 C2 1.41(3) . ? C1 C13 1.50(3) . ? C2 C3 1.35(3) . ? C2 H9 0.9300 . ? C3 C4 1.36(3) . ? C3 H8 0.9300 . ? C4 C5 1.36(3) . ? C4 C12 1.48(3) . ? C5 C6 1.43(3) . ? C6 C7 1.46(3) . ? C7 C11 1.33(3) . ? C7 C8 1.40(3) . ? C8 C9 1.34(3) . ? C8 H3 0.9300 . ? C9 C10 1.42(3) . ? C9 H2 0.9300 . ? C10 H1 0.9300 . ? C11 C12 1.25(3) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C14 C17 1.50(3) . ? C14 C15 1.53(2) . ? C14 H14 0.9800 . ? C15 C16 1.52(2) . ? C15 H15 0.9800 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C18 1.34(3) . ? C17 C22 1.46(3) . ? C18 C19 1.41(4) . ? C18 H18 0.9300 . ? C19 C20 1.42(4) . ? C19 H19 0.9300 . ? C20 C21 1.34(3) . ? C20 H20 0.9300 . ? C21 C22 1.39(4) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? Cl1 Cl4 1.59(4) . ? Cl1 Cl4 1.59(4) 4_657 ? 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 C23 Pd N2 93.1(9) . . ? C23 Pd N3 85.5(8) . 3_566 ? N2 Pd N3 171.7(6) . 3_566 ? C23 Pd N1 168.9(8) . . ? N2 Pd N1 78.5(8) . . ? N3 Pd N1 101.8(7) 3_566 . ? C23 Pd Pd 114.6(7) . 3_566 ? N2 Pd Pd 106.9(4) . 3_566 ? N3 Pd Pd 81.0(4) 3_566 3_566 ? N1 Pd Pd 75.2(5) . 3_566 ? C6 N2 C10 116(2) . . ? C6 N2 Pd 115.5(17) . . ? C10 N2 Pd 127.8(19) . . ? C1 N1 C5 114(2) . . ? C1 N1 Pd 135.0(15) . . ? C5 N1 Pd 109.8(16) . . ? C13 N3 C15 102.8(18) . . ? C13 N3 Pd 134.1(17) . 3_566 ? C15 N3 Pd 123.0(13) . 3_566 ? C13 O1 C14 102.4(18) . . ? N1 C1 C2 123(2) . . ? N1 C1 C13 117(2) . . ? C2 C1 C13 119(3) . . ? C3 C2 C1 119(3) . . ? C3 C2 H9 120.5 . . ? C1 C2 H9 120.5 . . ? C2 C3 C4 121(3) . . ? C2 C3 H8 119.4 . . ? C4 C3 H8 119.4 . . ? C3 C4 C5 118(3) . . ? C3 C4 C12 125(3) . . ? C5 C4 C12 117(3) . . ? C4 C5 C6 123(3) . . ? C4 C5 N1 124(2) . . ? C6 C5 N1 113(2) . . ? N2 C6 C5 119(2) . . ? N2 C6 C7 127(2) . . ? C5 C6 C7 114(2) . . ? C11 C7 C8 130(3) . . ? C11 C7 C6 120(3) . . ? C8 C7 C6 109(3) . . ? C9 C8 C7 128(3) . . ? C9 C8 H3 116.1 . . ? C7 C8 H3 116.1 . . ? C8 C9 C10 116(3) . . ? C8 C9 H2 121.9 . . ? C10 C9 H2 121.9 . . ? N2 C10 C9 123(3) . . ? N2 C10 H1 118.7 . . ? C9 C10 H1 118.7 . . ? C12 C11 C7 126(3) . . ? C12 C11 H11 116.9 . . ? C7 C11 H11 116.9 . . ? C11 C12 C4 119(3) . . ? C11 C12 H12 120.3 . . ? C4 C12 H12 120.3 . . ? N3 C13 O1 123(2) . . ? N3 C13 C1 124(2) . . ? O1 C13 C1 113(2) . . ? O1 C14 C17 111(2) . . ? O1 C14 C15 103.0(18) . . ? C17 C14 C15 117(2) . . ? O1 C14 H14 108.3 . . ? C17 C14 H14 108.3 . . ? C15 C14 H14 108.3 . . ? N3 C15 C16 111.4(16) . . ? N3 C15 C14 101.7(17) . . ? C16 C15 C14 114.9(19) . . ? N3 C15 H15 109.5 . . ? C16 C15 H15 109.5 . . ? C14 C15 H15 109.5 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 C22 126(3) . . ? C18 C17 C14 123(3) . . ? C22 C17 C14 111(3) . . ? C17 C18 C19 119(3) . . ? C17 C18 H18 120.6 . . ? C19 C18 H18 120.6 . . ? C18 C19 C20 115(3) . . ? C18 C19 H19 122.7 . . ? C20 C19 H19 122.7 . . ? C21 C20 C19 127(4) . . ? C21 C20 H20 116.5 . . ? C19 C20 H20 116.5 . . ? C20 C21 C22 119(4) . . ? C20 C21 H21 120.3 . . ? C22 C21 H21 120.3 . . ? C21 C22 C17 114(3) . . ? C21 C22 H22 123.2 . . ? C17 C22 H22 123.2 . . ? Pd C23 H23A 109.5 . . ? Pd C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Pd C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Cl4 Cl1 Cl4 155(4) . 4_657 ? _diffrn_measured_fraction_theta_max 0.926 _diffrn_reflns_theta_full 57.87 _diffrn_measured_fraction_theta_full 0.926 _refine_diff_density_max 0.966 _refine_diff_density_min -0.550 _refine_diff_density_rms 0.110 #===END data_3b _database_code_depnum_ccdc_archive 'CCDC 864729' #TrackingRef '- data.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H40 N6 O2 Pd2 2+, 2(P F6 1-), C H2 Cl2' _chemical_formula_sum 'C47 H42 Cl2 F12 N6 O2 P2 Pd2' _chemical_formula_weight 1296.51 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0074 0.0035 '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 0.0135 0.0071 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0225 0.0128 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.3471 1.8595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1741 0.1882 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0348 0.0215 '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' _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M 'P 61 2 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y, -x, -z+5/6' 'y, x, -z+1/3' 'x-y, -y, -z' '-x+y, y, -z+1/2' 'x, x-y, -z+1/6' '-x, -x+y, -z+2/3' '-y, x-y, z+1/3' 'y, -x+y, z+5/6' 'x-y, x, z+1/6' '-x+y, -x, z+2/3' _cell_length_a 14.1900(11) _cell_length_b 14.1900(11) _cell_length_c 42.200(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 7358.8(10) _cell_formula_units_Z 6 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description cube _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.755 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3876 _exptl_absorpt_coefficient_mu 3.127 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.00000 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'PILATUS 2M detector' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 82509 _diffrn_reflns_av_R_equivalents 0.0228 _diffrn_reflns_av_sigmaI/netI 0.0379 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 28.08 _reflns_number_total 2120 _reflns_number_gt 2113 _reflns_threshold_expression >2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction 'CCP4 Suite, 1994' _computing_structure_solution 'SHELX97 (Sheldrick, 1998)' _computing_structure_refinement 'SHELX97 (Sheldrick, 1998)' _computing_molecular_graphics 'Ortep3/windows (Farrugia,1997)' _computing_publication_material 'Wingx 1.80.05 (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0485P)^2^+5.6616P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00328(16) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.48(2) _refine_ls_number_reflns 2120 _refine_ls_number_parameters 336 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0285 _refine_ls_R_factor_gt 0.0284 _refine_ls_wR_factor_ref 0.0714 _refine_ls_wR_factor_gt 0.0713 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _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 0.66625(3) 0.56669(3) 0.195071(8) 0.0242(3) Uani 1 1 d . . . N1 N 0.6035(3) 0.6644(3) 0.21534(9) 0.0219(10) Uani 1 1 d . . . N2 N 0.5354(3) 0.4502(3) 0.21894(10) 0.0295(11) Uani 1 1 d . . . C1 C 0.6360(4) 0.7703(5) 0.21356(12) 0.0279(14) Uani 1 1 d . . . C2 C 0.6008(5) 0.8230(5) 0.23439(13) 0.0388(16) Uani 1 1 d . . . H2 H 0.6303 0.8995 0.2332 0.047 Uiso 1 1 calc R . . C3 C 0.5235(5) 0.7631(5) 0.25658(14) 0.0438(16) Uani 1 1 d . . . H3 H 0.4984 0.7973 0.2710 0.053 Uiso 1 1 calc R . . C4 C 0.4817(5) 0.6504(5) 0.25774(12) 0.0354(16) Uani 1 1 d . . . C5 C 0.5247(4) 0.6052(4) 0.23730(11) 0.0238(14) Uani 1 1 d . . . C6 C 0.4866(4) 0.4893(4) 0.23870(12) 0.0279(14) Uani 1 1 d . . . C7 C 0.4024(4) 0.4244(5) 0.25923(13) 0.0383(16) Uani 1 1 d . . . C8 C 0.3619(5) 0.3114(5) 0.25813(16) 0.0518(18) Uani 1 1 d . . . H8 H 0.3024 0.2632 0.2711 0.062 Uiso 1 1 calc R . . C9 C 0.4094(6) 0.2726(5) 0.23829(15) 0.0510(18) Uani 1 1 d . . . H9 H 0.3825 0.1964 0.2373 0.061 Uiso 1 1 calc R . . C10 C 0.4970(5) 0.3423(5) 0.21930(14) 0.0388(15) Uani 1 1 d . . . H10 H 0.5305 0.3129 0.2062 0.047 Uiso 1 1 calc R . . C11 C 0.3976(5) 0.5796(6) 0.27947(14) 0.0555(19) Uani 1 1 d . . . H11 H 0.3693 0.6102 0.2940 0.067 Uiso 1 1 calc R . . C12 C 0.3585(5) 0.4730(6) 0.27978(15) 0.0483(17) Uani 1 1 d . . . H12 H 0.3008 0.4285 0.2938 0.058 Uiso 1 1 calc R . . C23 C 0.7109(5) 0.4583(4) 0.17914(13) 0.0368(15) Uani 1 1 d . . . H23A H 0.7809 0.4976 0.1681 0.055 Uiso 1 1 calc R . . H23B H 0.6554 0.4066 0.1645 0.055 Uiso 1 1 calc R . . H23C H 0.7179 0.4186 0.1972 0.055 Uiso 1 1 calc R . . N3 N 0.6858(3) 0.8066(3) 0.15742(9) 0.0230(10) Uani 1 1 d . . . O1 O 0.7833(3) 0.9340(3) 0.19385(8) 0.0353(10) Uani 1 1 d . . . C13 C 0.7035(4) 0.8343(4) 0.18680(13) 0.0266(14) Uani 1 1 d . . . C14 C 0.8336(5) 0.9871(4) 0.16385(12) 0.0329(14) Uani 1 1 d . . . H14 H 0.9076 0.9951 0.1627 0.039 Uiso 1 1 calc R . . C15 C 0.7609(5) 0.9048(4) 0.13808(12) 0.0347(14) Uani 1 1 d . . . H15 H 0.8067 0.8867 0.1242 0.042 Uiso 1 1 calc R . . C16 C 0.6955(6) 0.9402(5) 0.11750(14) 0.0541(19) Uani 1 1 d . . . H16A H 0.6484 0.8808 0.1031 0.081 Uiso 1 1 calc R . . H16B H 0.7454 1.0043 0.1051 0.081 Uiso 1 1 calc R . . H16C H 0.6506 0.9582 0.1311 0.081 Uiso 1 1 calc R . . C17 C 0.8464(5) 1.0991(4) 0.16406(12) 0.0323(14) Uani 1 1 d . . . C18 C 0.9404(5) 1.1856(5) 0.15068(12) 0.0379(15) Uani 1 1 d . . . H18 H 0.9935 1.1723 0.1413 0.045 Uiso 1 1 calc R . . C19 C 0.9566(5) 1.2906(5) 0.15096(13) 0.0396(15) Uani 1 1 d . . . H19 H 1.0206 1.3488 0.1419 0.048 Uiso 1 1 calc R . . C20 C 0.8800(5) 1.3094(5) 0.16428(14) 0.0415(17) Uani 1 1 d . . . H20 H 0.8915 1.3814 0.1645 0.050 Uiso 1 1 calc R . . C21 C 0.7860(5) 1.2261(5) 0.17737(13) 0.0381(15) Uani 1 1 d . . . H21 H 0.7328 1.2399 0.1864 0.046 Uiso 1 1 calc R . . C22 C 0.7711(5) 1.1214(4) 0.17702(12) 0.0344(15) Uani 1 1 d . . . H22 H 0.7068 1.0636 0.1860 0.041 Uiso 1 1 calc R . . P1 P 0.03529(9) 0.07059(18) 0.2500 0.0391(6) Uani 1 2 d S . . F1 F 0.0319(3) 0.0690(3) 0.21217(7) 0.0577(10) Uani 1 1 d . . . F2 F -0.0752(3) 0.0733(3) 0.25109(8) 0.0559(9) Uani 1 1 d . . . F3 F -0.02866(19) -0.0573(4) 0.2500 0.0679(17) Uani 1 2 d S . . F4 F 0.10089(19) 0.2018(4) 0.2500 0.0659(15) Uani 1 2 d S . . P2 P 0.53313(9) 0.06625(18) 0.2500 0.0367(6) Uani 1 2 d S . . F5 F 0.4198(2) 0.0648(2) 0.25209(8) 0.0466(9) Uani 1 1 d . . . F6 F 0.5719(4) 0.1530(4) 0.22343(13) 0.126(2) Uani 1 1 d . . . F7 F 0.4836(3) -0.0276(4) 0.22414(10) 0.0887(15) Uani 1 1 d . . . Cl1 Cl 0.26317(16) 0.36561(16) 0.18329(4) 0.0699(6) Uani 1 1 d . . . C24 C 0.2450(7) 0.2450(7) 0.1667 0.074(3) Uani 1 2 d S . . H24A H 0.1881 0.2198 0.1501 0.089 Uiso 0.50 1 calc PR . . H24B H 0.2198 0.1881 0.1832 0.089 Uiso 0.50 1 calc PR . . 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 0.0288(3) 0.0260(3) 0.0225(3) 0.00123(17) 0.0036(2) 0.0172(2) N1 0.024(2) 0.024(3) 0.017(2) -0.004(2) -0.002(2) 0.011(2) N2 0.031(3) 0.023(3) 0.031(3) -0.001(2) -0.007(2) 0.011(2) C1 0.035(3) 0.029(4) 0.020(3) -0.006(3) 0.000(3) 0.016(3) C2 0.056(4) 0.030(4) 0.030(3) -0.003(3) 0.000(4) 0.022(3) C3 0.067(5) 0.044(4) 0.033(3) 0.001(3) 0.013(4) 0.038(4) C4 0.039(4) 0.046(5) 0.027(3) 0.008(3) 0.017(3) 0.026(3) C5 0.024(3) 0.029(4) 0.017(3) 0.000(3) -0.006(3) 0.012(3) C6 0.035(4) 0.030(4) 0.020(3) -0.002(3) -0.009(3) 0.017(3) C7 0.027(4) 0.038(4) 0.036(4) 0.021(3) 0.008(3) 0.006(3) C8 0.040(4) 0.041(5) 0.048(4) 0.024(3) -0.007(4) 0.000(4) C9 0.069(5) 0.032(4) 0.048(4) 0.006(4) -0.004(4) 0.022(4) C10 0.041(4) 0.024(4) 0.049(4) 0.007(3) 0.006(3) 0.014(3) C11 0.050(4) 0.074(6) 0.057(5) 0.008(4) 0.028(4) 0.042(4) C12 0.043(4) 0.051(5) 0.052(4) 0.022(4) 0.026(3) 0.024(4) C23 0.055(4) 0.029(3) 0.039(3) 0.006(3) 0.012(3) 0.030(3) N3 0.033(3) 0.023(3) 0.016(3) -0.005(2) -0.003(2) 0.016(2) O1 0.055(3) 0.022(2) 0.019(2) 0.0015(17) -0.0025(19) 0.012(2) C13 0.033(4) 0.019(4) 0.027(4) -0.002(3) -0.003(3) 0.013(3) C14 0.044(4) 0.025(3) 0.028(3) 0.004(3) 0.007(3) 0.016(3) C15 0.046(4) 0.027(3) 0.028(3) 0.006(3) 0.009(3) 0.016(3) C16 0.090(5) 0.036(4) 0.034(3) 0.009(3) -0.016(4) 0.030(4) C17 0.038(4) 0.033(4) 0.020(3) 0.002(3) 0.001(3) 0.013(4) C18 0.039(4) 0.045(4) 0.031(3) 0.000(3) 0.003(3) 0.022(4) C19 0.043(4) 0.022(4) 0.043(3) 0.010(3) 0.007(3) 0.008(3) C20 0.069(5) 0.034(4) 0.031(3) -0.002(3) -0.005(4) 0.033(4) C21 0.051(4) 0.040(4) 0.033(3) 0.007(3) 0.011(3) 0.030(4) C22 0.039(4) 0.030(4) 0.027(3) 0.008(3) 0.011(3) 0.012(3) P1 0.0481(12) 0.0392(15) 0.0271(13) 0.000 -0.0034(9) 0.0196(7) F1 0.066(2) 0.081(3) 0.0229(18) 0.0095(17) 0.0009(18) 0.035(2) F2 0.061(2) 0.061(2) 0.048(2) 0.0056(19) -0.0008(18) 0.033(2) F3 0.097(4) 0.032(3) 0.053(3) 0.000 -0.017(3) 0.0161(15) F4 0.064(3) 0.030(3) 0.092(4) 0.000 -0.011(3) 0.0152(15) P2 0.0349(10) 0.0308(13) 0.0429(14) 0.000 0.0028(9) 0.0154(6) F5 0.037(2) 0.046(2) 0.063(2) 0.0160(18) 0.0179(17) 0.0250(17) F6 0.115(4) 0.127(4) 0.188(5) 0.121(4) 0.113(4) 0.100(4) F7 0.070(3) 0.114(4) 0.103(3) -0.058(3) -0.038(3) 0.062(3) Cl1 0.0880(14) 0.0964(15) 0.0565(10) -0.0036(10) 0.0063(10) 0.0696(12) C24 0.056(5) 0.056(5) 0.089(8) -0.009(3) 0.009(3) 0.012(6) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd N3 2.027(4) 4 ? Pd N2 2.032(4) . ? Pd C23 2.049(5) . ? Pd N1 2.164(4) . ? N1 C1 1.336(6) . ? N1 C5 1.369(6) . ? N2 C10 1.344(7) . ? N2 C6 1.366(7) . ? C1 C2 1.398(8) . ? C1 C13 1.465(8) . ? C2 C3 1.368(8) . ? C3 C4 1.401(8) . ? C4 C5 1.385(7) . ? C4 C11 1.441(8) . ? C5 C6 1.453(8) . ? C6 C7 1.387(7) . ? C7 C8 1.409(8) . ? C7 C12 1.429(9) . ? C8 C9 1.352(9) . ? C9 C10 1.391(8) . ? C11 C12 1.325(9) . ? N3 C13 1.287(6) . ? N3 C15 1.503(7) . ? N3 Pd 2.027(4) 4 ? O1 C13 1.330(6) . ? O1 C14 1.464(6) . ? C14 C17 1.505(7) . ? C14 C15 1.552(8) . ? C15 C16 1.528(8) . ? C17 C22 1.371(8) . ? C17 C18 1.402(8) . ? C18 C19 1.389(8) . ? C19 C20 1.364(8) . ? C20 C21 1.380(8) . ? C21 C22 1.393(8) . ? P1 F3 1.572(5) . ? P1 F2 1.588(4) . ? P1 F2 1.588(4) 6 ? P1 F1 1.597(3) . ? P1 F1 1.597(3) 6 ? P1 F4 1.612(5) . ? P2 F6 1.548(4) . ? P2 F6 1.548(4) 6_655 ? P2 F7 1.588(4) . ? P2 F7 1.588(4) 6_655 ? P2 F5 1.601(3) 6_655 ? P2 F5 1.601(3) . ? Cl1 C24 1.746(6) . ? C24 Cl1 1.746(5) 4 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Pd N2 173.45(16) 4 . ? N3 Pd C23 87.2(2) 4 . ? N2 Pd C23 93.0(2) . . ? N3 Pd N1 99.85(16) 4 . ? N2 Pd N1 79.84(17) . . ? C23 Pd N1 172.78(19) . . ? C1 N1 C5 116.4(4) . . ? C1 N1 Pd 132.6(3) . . ? C5 N1 Pd 110.3(3) . . ? C10 N2 C6 117.2(5) . . ? C10 N2 Pd 128.1(4) . . ? C6 N2 Pd 114.5(3) . . ? N1 C1 C2 123.5(5) . . ? N1 C1 C13 119.4(4) . . ? C2 C1 C13 116.8(5) . . ? C3 C2 C1 119.2(5) . . ? C2 C3 C4 118.9(5) . . ? C5 C4 C3 118.3(5) . . ? C5 C4 C11 118.4(5) . . ? C3 C4 C11 123.3(5) . . ? N1 C5 C4 123.4(5) . . ? N1 C5 C6 116.7(5) . . ? C4 C5 C6 119.9(5) . . ? N2 C6 C7 123.7(5) . . ? N2 C6 C5 117.2(5) . . ? C7 C6 C5 119.1(5) . . ? C6 C7 C8 117.4(6) . . ? C6 C7 C12 119.8(5) . . ? C8 C7 C12 122.8(6) . . ? C9 C8 C7 118.8(6) . . ? C8 C9 C10 121.1(6) . . ? N2 C10 C9 121.7(5) . . ? C12 C11 C4 122.0(6) . . ? C11 C12 C7 120.6(6) . . ? C13 N3 C15 107.5(4) . . ? C13 N3 Pd 128.6(4) . 4 ? C15 N3 Pd 123.4(3) . 4 ? C13 O1 C14 106.9(4) . . ? N3 C13 O1 118.2(5) . . ? N3 C13 C1 125.8(5) . . ? O1 C13 C1 115.6(5) . . ? O1 C14 C17 108.0(4) . . ? O1 C14 C15 104.4(4) . . ? C17 C14 C15 118.9(5) . . ? N3 C15 C16 110.4(5) . . ? N3 C15 C14 102.4(4) . . ? C16 C15 C14 115.8(5) . . ? C22 C17 C18 117.9(5) . . ? C22 C17 C14 123.3(5) . . ? C18 C17 C14 118.8(5) . . ? C19 C18 C17 120.7(5) . . ? C20 C19 C18 119.5(5) . . ? C19 C20 C21 121.4(5) . . ? C20 C21 C22 118.4(6) . . ? C17 C22 C21 122.1(5) . . ? F3 P1 F2 91.22(15) . . ? F3 P1 F2 91.22(15) . 6 ? F2 P1 F2 177.6(3) . 6 ? F3 P1 F1 89.29(16) . . ? F2 P1 F1 90.33(18) . . ? F2 P1 F1 89.70(18) 6 . ? F3 P1 F1 89.29(16) . 6 ? F2 P1 F1 89.70(18) . 6 ? F2 P1 F1 90.33(18) 6 6 ? F1 P1 F1 178.6(3) . 6 ? F3 P1 F4 180.000(1) . . ? F2 P1 F4 88.78(15) . . ? F2 P1 F4 88.78(15) 6 . ? F1 P1 F4 90.71(16) . . ? F1 P1 F4 90.71(16) 6 . ? F6 P2 F6 93.0(5) . 6_655 ? F6 P2 F7 90.1(3) . . ? F6 P2 F7 176.8(4) 6_655 . ? F6 P2 F7 176.8(4) . 6_655 ? F6 P2 F7 90.1(3) 6_655 6_655 ? F7 P2 F7 86.9(4) . 6_655 ? F6 P2 F5 90.6(2) . 6_655 ? F6 P2 F5 90.29(19) 6_655 6_655 ? F7 P2 F5 88.69(18) . 6_655 ? F7 P2 F5 90.4(2) 6_655 6_655 ? F6 P2 F5 90.29(19) . . ? F6 P2 F5 90.6(2) 6_655 . ? F7 P2 F5 90.4(2) . . ? F7 P2 F5 88.69(18) 6_655 . ? F5 P2 F5 178.8(3) 6_655 . ? Cl1 C24 Cl1 111.3(5) . 4 ? 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 N3 Pd N1 C1 7.2(5) 4 . . . ? N2 Pd N1 C1 -179.5(5) . . . . ? C23 Pd N1 C1 175.0(14) . . . . ? N3 Pd N1 C5 -162.7(3) 4 . . . ? N2 Pd N1 C5 10.7(3) . . . . ? C23 Pd N1 C5 5.2(16) . . . . ? N3 Pd N2 C10 -96.5(15) 4 . . . ? C23 Pd N2 C10 -5.2(5) . . . . ? N1 Pd N2 C10 175.5(5) . . . . ? N3 Pd N2 C6 78.2(16) 4 . . . ? C23 Pd N2 C6 169.6(4) . . . . ? N1 Pd N2 C6 -9.7(3) . . . . ? C5 N1 C1 C2 5.6(7) . . . . ? Pd N1 C1 C2 -163.8(4) . . . . ? C5 N1 C1 C13 -168.1(5) . . . . ? Pd N1 C1 C13 22.5(7) . . . . ? N1 C1 C2 C3 -4.6(8) . . . . ? C13 C1 C2 C3 169.2(5) . . . . ? C1 C2 C3 C4 0.0(8) . . . . ? C2 C3 C4 C5 3.1(8) . . . . ? C2 C3 C4 C11 -177.9(6) . . . . ? C1 N1 C5 C4 -2.2(7) . . . . ? Pd N1 C5 C4 169.5(4) . . . . ? C1 N1 C5 C6 178.2(4) . . . . ? Pd N1 C5 C6 -10.1(5) . . . . ? C3 C4 C5 N1 -2.1(8) . . . . ? C11 C4 C5 N1 178.9(5) . . . . ? C3 C4 C5 C6 177.5(5) . . . . ? C11 C4 C5 C6 -1.5(7) . . . . ? C10 N2 C6 C7 1.4(7) . . . . ? Pd N2 C6 C7 -174.0(4) . . . . ? C10 N2 C6 C5 -177.3(5) . . . . ? Pd N2 C6 C5 7.3(5) . . . . ? N1 C5 C6 N2 2.5(6) . . . . ? C4 C5 C6 N2 -177.2(5) . . . . ? N1 C5 C6 C7 -176.3(4) . . . . ? C4 C5 C6 C7 4.1(7) . . . . ? N2 C6 C7 C8 -3.5(8) . . . . ? C5 C6 C7 C8 175.1(5) . . . . ? N2 C6 C7 C12 178.0(5) . . . . ? C5 C6 C7 C12 -3.3(7) . . . . ? C6 C7 C8 C9 2.6(8) . . . . ? C12 C7 C8 C9 -179.0(6) . . . . ? C7 C8 C9 C10 0.3(9) . . . . ? C6 N2 C10 C9 1.7(8) . . . . ? Pd N2 C10 C9 176.4(4) . . . . ? C8 C9 C10 N2 -2.6(9) . . . . ? C5 C4 C11 C12 -2.0(9) . . . . ? C3 C4 C11 C12 179.1(6) . . . . ? C4 C11 C12 C7 2.8(10) . . . . ? C6 C7 C12 C11 -0.1(9) . . . . ? C8 C7 C12 C11 -178.4(6) . . . . ? C15 N3 C13 O1 -4.1(6) . . . . ? Pd N3 C13 O1 -176.0(3) 4 . . . ? C15 N3 C13 C1 168.6(5) . . . . ? Pd N3 C13 C1 -3.3(8) 4 . . . ? C14 O1 C13 N3 -1.4(6) . . . . ? C14 O1 C13 C1 -174.8(4) . . . . ? N1 C1 C13 N3 46.9(8) . . . . ? C2 C1 C13 N3 -127.2(6) . . . . ? N1 C1 C13 O1 -140.2(5) . . . . ? C2 C1 C13 O1 45.6(7) . . . . ? C13 O1 C14 C17 133.3(5) . . . . ? C13 O1 C14 C15 5.9(5) . . . . ? C13 N3 C15 C16 -116.6(5) . . . . ? Pd N3 C15 C16 55.8(5) 4 . . . ? C13 N3 C15 C14 7.2(5) . . . . ? Pd N3 C15 C14 179.6(3) 4 . . . ? O1 C14 C15 N3 -7.7(5) . . . . ? C17 C14 C15 N3 -128.0(5) . . . . ? O1 C14 C15 C16 112.4(5) . . . . ? C17 C14 C15 C16 -7.9(7) . . . . ? O1 C14 C17 C22 -37.4(7) . . . . ? C15 C14 C17 C22 81.1(6) . . . . ? O1 C14 C17 C18 141.9(5) . . . . ? C15 C14 C17 C18 -99.6(6) . . . . ? C22 C17 C18 C19 0.7(8) . . . . ? C14 C17 C18 C19 -178.6(5) . . . . ? C17 C18 C19 C20 -0.3(8) . . . . ? C18 C19 C20 C21 -0.4(8) . . . . ? C19 C20 C21 C22 0.6(8) . . . . ? C18 C17 C22 C21 -0.5(8) . . . . ? C14 C17 C22 C21 178.9(5) . . . . ? C20 C21 C22 C17 -0.2(8) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 28.08 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.351 _refine_diff_density_min -0.348 _refine_diff_density_rms 0.087