# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Axel Klein' _publ_contact_author_email AKLEIN2@UNI-KOELN.DE _publ_section_title ; Tuning the Electronic Properties of dppz-Ligands and their Palladium(II) Complexes ; loop_ _publ_author_name 'Axel Klein' 'Katharina Butsch' 'Ronald Gust ' 'Ingo Ott' 'Marco Romanski' # Attachment 'kb-d05.cif' data_shelxl _database_code_depnum_ccdc_archive 'CCDC 750425' #TrackingRef 'kb-d05.cif' _audit_creation_method SHELXL-97 _chemical_name_common ((CH3)(dppz)(pyridine)palladium(ii))SbF6 _chemical_melting_point ? _chemical_formula_moiety 'C24 H18 N5 Pd, F6 Sb' _chemical_formula_sum 'C24 H18 F6 N5 Pd Sb' _chemical_formula_weight 718.58 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' F F 0.0171 0.0103 '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' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.1171(16) _cell_length_b 10.1421(20) _cell_length_c 16.5134(31) _cell_angle_alpha 82.022(15) _cell_angle_beta 80.729(15) _cell_angle_gamma 68.043(14) _cell_volume 1392.52(47) _cell_formula_units_Z 2 _cell_measurement_temperature 170(2) _cell_measurement_reflns_used 5770 _cell_measurement_theta_min 0.95 _cell_measurement_theta_max 27.39 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.714 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 696 _exptl_absorpt_coefficient_mu 1.677 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 1.25 _exptl_absorpt_correction_T_max 27.35 _exptl_absorpt_process_details ; The absorption correction (X-RED; StoeCie, 2001) was performed after optimizing the crystal shape using X-SHAPE (SToe&Cie, 1999). ; _exptl_special_details ? _diffrn_ambient_temperature 170(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fixed in a loop with frozen oil' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS I' _diffrn_measurement_method 'w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21569 _diffrn_reflns_av_R_equivalents 0.1106 _diffrn_reflns_av_sigmaI/netI 0.1997 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.25 _diffrn_reflns_theta_max 27.36 _reflns_number_total 6186 _reflns_number_gt 2585 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-AREA (STOE & CIE 2001)' _computing_cell_refinement 'X-AREA (STOE & CIE 2001)' _computing_data_reduction 'X-RED (STOE & CIE 2001)' _computing_structure_solution 'SHELXL-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0410P)^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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6186 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1264 _refine_ls_R_factor_gt 0.0477 _refine_ls_wR_factor_ref 0.1088 _refine_ls_wR_factor_gt 0.0918 _refine_ls_goodness_of_fit_ref 0.734 _refine_ls_restrained_S_all 0.734 _refine_ls_shift/su_max 0.005 _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 Sb1 Sb 1.43640(7) 0.75654(7) 0.33329(3) 0.0387(2) Uani 1 1 d . . . Pd1 Pd 1.01644(7) 0.22746(7) 0.15329(4) 0.02627(17) Uani 1 1 d . . . F1 F 1.6445(8) 0.7586(10) 0.2966(4) 0.111(3) Uani 1 1 d . . . F2 F 1.4883(7) 0.6755(7) 0.4377(3) 0.0711(17) Uani 1 1 d . . . F3 F 1.3705(6) 0.8360(5) 0.2292(3) 0.0504(13) Uani 1 1 d . . . F4 F 1.2322(6) 0.7533(5) 0.3650(3) 0.0476(13) Uani 1 1 d . . . F5 F 1.4946(7) 0.5756(6) 0.2961(3) 0.0632(16) Uani 1 1 d . . . F6 F 1.3605(7) 0.9418(6) 0.3705(3) 0.0640(16) Uani 1 1 d . . . N1 N 1.3720(7) 0.5772(6) -0.1190(4) 0.0307(15) Uani 1 1 d . . . N2 N 1.1163(7) 0.2711(6) 0.0379(4) 0.0249(14) Uani 1 1 d . . . N3 N 1.0738(7) 0.4053(6) 0.1733(4) 0.0265(14) Uani 1 1 d . . . N4 N 1.3344(8) 0.7182(7) 0.0236(4) 0.0315(15) Uani 1 1 d . . . N5 N 0.9205(7) 0.1907(6) 0.2698(4) 0.0266(14) Uani 1 1 d . . . C1 C 0.9769(10) 0.0569(8) 0.1228(5) 0.0335(19) Uani 1 1 d . . . H1A H 1.0087 0.0466 0.0650 0.050 Uiso 1 1 calc . . . H1B H 0.8657 0.0715 0.1352 0.050 Uiso 1 1 calc . . . H1C H 1.0377 -0.0280 0.1537 0.050 Uiso 1 1 calc . . . C2 C 0.7887(9) 0.2877(8) 0.3056(5) 0.0336(19) Uani 1 1 d . . . H2 H 0.7420 0.3748 0.2761 0.040 Uiso 1 1 calc . . . C3 C 0.9867(9) 0.0655(9) 0.3142(5) 0.036(2) Uani 1 1 d . . . H3 H 1.0786 -0.0025 0.2908 0.044 Uiso 1 1 calc . . . C4 C 0.9240(11) 0.0345(10) 0.3928(5) 0.047(2) Uani 1 1 d . . . H4 H 0.9725 -0.0523 0.4221 0.056 Uiso 1 1 calc . . . C5 C 0.7866(11) 0.1360(10) 0.4270(5) 0.043(2) Uani 1 1 d . . . H5 H 0.7397 0.1174 0.4795 0.051 Uiso 1 1 calc . . . C6 C 0.7206(10) 0.2637(10) 0.3831(5) 0.041(2) Uani 1 1 d . . . H6 H 0.6299 0.3337 0.4059 0.049 Uiso 1 1 calc . . . C7 C 1.1386(9) 0.2005(8) -0.0294(4) 0.0273(17) Uani 1 1 d . . . H7 H 1.1019 0.1254 -0.0249 0.033 Uiso 1 1 calc . . . C8 C 1.2140(10) 0.2347(9) -0.1052(5) 0.0312(19) Uani 1 1 d . . . H8 H 1.2283 0.1827 -0.1499 0.037 Uiso 1 1 calc . . . C9 C 1.2668(9) 0.3467(8) -0.1128(4) 0.0297(19) Uani 1 1 d . . . H9 H 1.3153 0.3725 -0.1632 0.036 Uiso 1 1 calc . . . C10 C 1.2474(8) 0.4213(8) -0.0449(4) 0.0260(17) Uani 1 1 d . . . C11 C 1.1710(8) 0.3792(8) 0.0302(4) 0.0251(17) Uani 1 1 d . . . C12 C 1.1490(8) 0.4537(7) 0.1043(4) 0.0248(16) Uani 1 1 d . . . C13 C 1.2048(8) 0.5642(8) 0.1017(4) 0.0260(17) Uani 1 1 d . . . C14 C 1.1862(9) 0.6261(8) 0.1756(5) 0.0324(19) Uani 1 1 d . . . H14 H 1.2234 0.6995 0.1769 0.039 Uiso 1 1 calc . . . C15 C 1.1119(10) 0.5765(9) 0.2466(4) 0.0345(19) Uani 1 1 d . . . H15 H 1.0994 0.6155 0.2961 0.041 Uiso 1 1 calc . . . C16 C 1.0565(10) 0.4677(9) 0.2426(5) 0.0333(19) Uani 1 1 d . . . H16 H 1.0049 0.4365 0.2903 0.040 Uiso 1 1 calc . . . C17 C 1.3024(8) 0.5399(7) -0.0469(4) 0.0252(17) Uani 1 1 d . . . C18 C 1.2827(8) 0.6112(7) 0.0250(4) 0.0244(16) Uani 1 1 d . . . C19 C 1.4072(9) 0.7547(8) -0.0492(5) 0.0284(17) Uani 1 1 d . . . C20 C 1.4240(8) 0.6862(8) -0.1208(5) 0.0289(18) Uani 1 1 d . . . C21 C 1.5016(9) 0.7312(9) -0.1958(5) 0.0346(19) Uani 1 1 d . . . H21 H 1.5170 0.6851 -0.2431 0.042 Uiso 1 1 calc . . . C22 C 1.5525(9) 0.8414(9) -0.1977(5) 0.037(2) Uani 1 1 d . . . H22 H 1.6017 0.8711 -0.2468 0.044 Uiso 1 1 calc . . . C23 C 1.5325(10) 0.9111(9) -0.1273(5) 0.038(2) Uani 1 1 d . . . H23 H 1.5696 0.9857 -0.1303 0.046 Uiso 1 1 calc . . . C24 C 1.4600(9) 0.8722(9) -0.0547(5) 0.037(2) Uani 1 1 d . . . H24 H 1.4447 0.9216 -0.0088 0.045 Uiso 1 1 calc . . . 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 Sb1 0.0366(4) 0.0452(4) 0.0301(4) -0.0055(3) 0.0031(3) -0.0121(3) Pd1 0.0262(4) 0.0272(4) 0.0252(4) -0.0013(3) -0.0010(3) -0.0105(3) F1 0.073(5) 0.180(8) 0.067(4) -0.032(5) 0.027(4) -0.038(5) F2 0.058(4) 0.093(5) 0.042(3) -0.001(3) -0.002(3) -0.008(3) F3 0.072(4) 0.052(3) 0.035(3) -0.001(2) -0.004(3) -0.032(3) F4 0.042(3) 0.043(3) 0.056(3) -0.001(2) 0.004(2) -0.018(2) F5 0.072(4) 0.041(3) 0.058(4) -0.011(3) -0.001(3) 0.001(3) F6 0.090(4) 0.060(4) 0.048(3) -0.011(3) 0.009(3) -0.040(3) N1 0.026(4) 0.026(4) 0.039(4) 0.001(3) -0.001(3) -0.011(3) N2 0.025(3) 0.021(3) 0.027(3) -0.002(3) -0.007(3) -0.006(3) N3 0.025(3) 0.025(4) 0.029(3) -0.001(3) -0.003(3) -0.009(3) N4 0.035(4) 0.032(4) 0.036(4) 0.004(3) -0.009(3) -0.021(3) N5 0.023(3) 0.025(3) 0.034(4) -0.002(3) -0.004(3) -0.011(3) C1 0.040(5) 0.033(5) 0.026(4) -0.005(3) 0.000(4) -0.013(4) C2 0.033(5) 0.035(5) 0.028(4) 0.000(3) -0.001(4) -0.008(4) C3 0.028(4) 0.033(5) 0.042(5) 0.000(4) -0.010(4) -0.003(4) C4 0.049(6) 0.047(6) 0.037(5) 0.005(4) 0.002(4) -0.014(5) C5 0.043(5) 0.055(6) 0.025(4) 0.000(4) 0.001(4) -0.014(5) C6 0.037(5) 0.039(5) 0.034(5) -0.001(4) -0.002(4) 0.000(4) C7 0.030(4) 0.027(4) 0.027(4) -0.004(3) -0.003(3) -0.013(3) C8 0.036(5) 0.032(5) 0.024(4) -0.009(4) 0.000(4) -0.011(4) C9 0.035(5) 0.027(4) 0.020(4) -0.003(3) 0.000(3) -0.004(4) C10 0.023(4) 0.024(4) 0.030(4) -0.004(3) -0.002(3) -0.009(3) C11 0.024(4) 0.020(4) 0.031(4) -0.009(3) -0.004(3) -0.004(3) C12 0.025(4) 0.024(4) 0.025(4) 0.002(3) -0.002(3) -0.010(3) C13 0.025(4) 0.024(4) 0.029(4) -0.004(3) 0.001(3) -0.010(3) C14 0.031(4) 0.029(4) 0.042(5) -0.012(4) -0.007(4) -0.012(4) C15 0.045(5) 0.037(5) 0.021(4) -0.007(3) 0.005(4) -0.017(4) C16 0.038(5) 0.039(5) 0.026(4) -0.008(4) 0.000(4) -0.017(4) C17 0.023(4) 0.018(4) 0.029(4) 0.002(3) -0.003(3) -0.002(3) C18 0.016(4) 0.022(4) 0.029(4) 0.003(3) -0.005(3) -0.001(3) C19 0.025(4) 0.026(4) 0.035(4) 0.002(3) 0.001(3) -0.014(3) C20 0.018(4) 0.031(4) 0.034(4) 0.000(3) -0.004(3) -0.006(3) C21 0.030(4) 0.037(5) 0.033(4) 0.005(4) -0.002(4) -0.011(4) C22 0.026(4) 0.033(5) 0.050(5) 0.008(4) 0.001(4) -0.016(4) C23 0.033(5) 0.034(5) 0.051(5) 0.006(4) -0.013(4) -0.015(4) C24 0.029(5) 0.041(5) 0.046(5) -0.003(4) -0.004(4) -0.018(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sb1 F2 1.858(5) . ? Sb1 F4 1.863(5) . ? Sb1 F5 1.872(5) . ? Sb1 F3 1.884(5) . ? Sb1 F6 1.897(5) . ? Sb1 F1 1.903(7) . ? Pd1 N5 2.026(6) . ? Pd1 C1 2.036(8) . ? Pd1 N2 2.041(6) . ? Pd1 N3 2.136(6) . ? N1 C17 1.332(9) . ? N1 C20 1.351(10) . ? N2 C11 1.349(9) . ? N2 C7 1.352(9) . ? N3 C16 1.343(9) . ? N3 C12 1.362(9) . ? N4 C18 1.331(9) . ? N4 C19 1.351(9) . ? N5 C2 1.346(9) . ? N5 C3 1.351(10) . ? C2 C6 1.361(11) . ? C3 C4 1.375(11) . ? C4 C5 1.384(12) . ? C5 C6 1.365(12) . ? C7 C8 1.393(10) . ? C8 C9 1.374(11) . ? C9 C10 1.390(10) . ? C10 C11 1.416(10) . ? C10 C17 1.461(10) . ? C11 C12 1.473(10) . ? C12 C13 1.386(10) . ? C13 C14 1.408(10) . ? C13 C18 1.459(10) . ? C14 C15 1.386(11) . ? C15 C16 1.387(11) . ? C17 C18 1.427(10) . ? C19 C20 1.412(10) . ? C19 C24 1.430(11) . ? C20 C21 1.431(10) . ? C21 C22 1.356(11) . ? C22 C23 1.395(12) . ? C23 C24 1.357(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F2 Sb1 F4 88.8(2) . . ? F2 Sb1 F5 90.9(3) . . ? F4 Sb1 F5 88.0(2) . . ? F2 Sb1 F3 176.0(3) . . ? F4 Sb1 F3 87.2(2) . . ? F5 Sb1 F3 88.2(2) . . ? F2 Sb1 F6 90.5(3) . . ? F4 Sb1 F6 87.7(2) . . ? F5 Sb1 F6 175.5(3) . . ? F3 Sb1 F6 90.1(2) . . ? F2 Sb1 F1 93.1(3) . . ? F4 Sb1 F1 177.8(3) . . ? F5 Sb1 F1 90.7(3) . . ? F3 Sb1 F1 90.9(3) . . ? F6 Sb1 F1 93.5(3) . . ? N5 Pd1 C1 88.2(3) . . ? N5 Pd1 N2 177.4(3) . . ? C1 Pd1 N2 94.4(3) . . ? N5 Pd1 N3 97.7(2) . . ? C1 Pd1 N3 174.0(3) . . ? N2 Pd1 N3 79.8(2) . . ? C17 N1 C20 116.5(6) . . ? C11 N2 C7 117.6(6) . . ? C11 N2 Pd1 115.1(5) . . ? C7 N2 Pd1 127.3(5) . . ? C16 N3 C12 117.2(7) . . ? C16 N3 Pd1 130.4(5) . . ? C12 N3 Pd1 112.3(5) . . ? C18 N4 C19 116.5(6) . . ? C2 N5 C3 117.4(6) . . ? C2 N5 Pd1 121.9(5) . . ? C3 N5 Pd1 120.7(5) . . ? N5 C2 C6 122.8(7) . . ? N5 C3 C4 122.7(7) . . ? C3 C4 C5 118.2(8) . . ? C6 C5 C4 119.4(8) . . ? C2 C6 C5 119.5(8) . . ? N2 C7 C8 123.2(7) . . ? C9 C8 C7 118.8(7) . . ? C8 C9 C10 119.8(7) . . ? C9 C10 C11 118.0(7) . . ? C9 C10 C17 123.6(7) . . ? C11 C10 C17 118.4(6) . . ? N2 C11 C10 122.5(6) . . ? N2 C11 C12 117.2(6) . . ? C10 C11 C12 120.3(7) . . ? N3 C12 C13 123.8(6) . . ? N3 C12 C11 115.7(6) . . ? C13 C12 C11 120.5(6) . . ? C12 C13 C14 117.4(7) . . ? C12 C13 C18 120.6(6) . . ? C14 C13 C18 121.9(7) . . ? C15 C14 C13 119.3(7) . . ? C14 C15 C16 119.0(7) . . ? N3 C16 C15 123.3(7) . . ? N1 C17 C18 122.1(7) . . ? N1 C17 C10 116.5(6) . . ? C18 C17 C10 121.4(6) . . ? N4 C18 C17 121.5(6) . . ? N4 C18 C13 119.7(6) . . ? C17 C18 C13 118.8(7) . . ? N4 C19 C20 122.1(7) . . ? N4 C19 C24 118.7(7) . . ? C20 C19 C24 119.2(7) . . ? N1 C20 C19 121.3(7) . . ? N1 C20 C21 119.8(7) . . ? C19 C20 C21 118.9(7) . . ? C22 C21 C20 119.7(7) . . ? C21 C22 C23 121.2(7) . . ? C24 C23 C22 121.3(8) . . ? C23 C24 C19 119.5(7) . . ? 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 N5 Pd1 N2 C11 -7(6) . . . . ? C1 Pd1 N2 C11 -176.7(5) . . . . ? N3 Pd1 N2 C11 1.9(5) . . . . ? N5 Pd1 N2 C7 170(5) . . . . ? C1 Pd1 N2 C7 0.4(6) . . . . ? N3 Pd1 N2 C7 179.0(6) . . . . ? N5 Pd1 N3 C16 2.3(7) . . . . ? C1 Pd1 N3 C16 -163(3) . . . . ? N2 Pd1 N3 C16 -177.3(7) . . . . ? N5 Pd1 N3 C12 177.6(5) . . . . ? C1 Pd1 N3 C12 12(3) . . . . ? N2 Pd1 N3 C12 -2.0(5) . . . . ? C1 Pd1 N5 C2 -118.7(6) . . . . ? N2 Pd1 N5 C2 71(6) . . . . ? N3 Pd1 N5 C2 62.8(6) . . . . ? C1 Pd1 N5 C3 60.5(6) . . . . ? N2 Pd1 N5 C3 -109(5) . . . . ? N3 Pd1 N5 C3 -118.0(6) . . . . ? C3 N5 C2 C6 -0.6(12) . . . . ? Pd1 N5 C2 C6 178.6(7) . . . . ? C2 N5 C3 C4 0.7(12) . . . . ? Pd1 N5 C3 C4 -178.6(7) . . . . ? N5 C3 C4 C5 0.4(14) . . . . ? C3 C4 C5 C6 -1.6(15) . . . . ? N5 C2 C6 C5 -0.5(14) . . . . ? C4 C5 C6 C2 1.7(15) . . . . ? C11 N2 C7 C8 -0.3(11) . . . . ? Pd1 N2 C7 C8 -177.4(6) . . . . ? N2 C7 C8 C9 -0.8(12) . . . . ? C7 C8 C9 C10 1.4(12) . . . . ? C8 C9 C10 C11 -0.8(11) . . . . ? C8 C9 C10 C17 178.9(7) . . . . ? C7 N2 C11 C10 0.9(10) . . . . ? Pd1 N2 C11 C10 178.3(5) . . . . ? C7 N2 C11 C12 -178.8(6) . . . . ? Pd1 N2 C11 C12 -1.4(8) . . . . ? C9 C10 C11 N2 -0.4(11) . . . . ? C17 C10 C11 N2 179.9(7) . . . . ? C9 C10 C11 C12 179.3(7) . . . . ? C17 C10 C11 C12 -0.3(10) . . . . ? C16 N3 C12 C13 -1.3(11) . . . . ? Pd1 N3 C12 C13 -177.2(6) . . . . ? C16 N3 C12 C11 177.8(7) . . . . ? Pd1 N3 C12 C11 1.9(8) . . . . ? N2 C11 C12 N3 -0.4(10) . . . . ? C10 C11 C12 N3 179.8(6) . . . . ? N2 C11 C12 C13 178.8(7) . . . . ? C10 C11 C12 C13 -1.0(11) . . . . ? N3 C12 C13 C14 2.0(11) . . . . ? C11 C12 C13 C14 -177.1(7) . . . . ? N3 C12 C13 C18 -179.3(6) . . . . ? C11 C12 C13 C18 1.6(11) . . . . ? C12 C13 C14 C15 -1.0(11) . . . . ? C18 C13 C14 C15 -179.7(7) . . . . ? C13 C14 C15 C16 -0.5(12) . . . . ? C12 N3 C16 C15 -0.4(12) . . . . ? Pd1 N3 C16 C15 174.6(6) . . . . ? C14 C15 C16 N3 1.3(13) . . . . ? C20 N1 C17 C18 0.2(10) . . . . ? C20 N1 C17 C10 -179.5(6) . . . . ? C9 C10 C17 N1 1.1(11) . . . . ? C11 C10 C17 N1 -179.2(6) . . . . ? C9 C10 C17 C18 -178.6(7) . . . . ? C11 C10 C17 C18 1.0(10) . . . . ? C19 N4 C18 C17 -0.5(10) . . . . ? C19 N4 C18 C13 179.1(6) . . . . ? N1 C17 C18 N4 -0.5(11) . . . . ? C10 C17 C18 N4 179.2(7) . . . . ? N1 C17 C18 C13 179.9(6) . . . . ? C10 C17 C18 C13 -0.5(10) . . . . ? C12 C13 C18 N4 179.5(7) . . . . ? C14 C13 C18 N4 -1.9(11) . . . . ? C12 C13 C18 C17 -0.9(10) . . . . ? C14 C13 C18 C17 177.8(7) . . . . ? C18 N4 C19 C20 1.8(10) . . . . ? C18 N4 C19 C24 177.9(7) . . . . ? C17 N1 C20 C19 1.0(10) . . . . ? C17 N1 C20 C21 179.3(7) . . . . ? N4 C19 C20 N1 -2.2(11) . . . . ? C24 C19 C20 N1 -178.2(7) . . . . ? N4 C19 C20 C21 179.6(7) . . . . ? C24 C19 C20 C21 3.5(11) . . . . ? N1 C20 C21 C22 179.4(7) . . . . ? C19 C20 C21 C22 -2.3(11) . . . . ? C20 C21 C22 C23 0.8(12) . . . . ? C21 C22 C23 C24 -0.7(13) . . . . ? C22 C23 C24 C19 1.9(12) . . . . ? N4 C19 C24 C23 -179.6(7) . . . . ? C20 C19 C24 C23 -3.4(11) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.36 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 2.266 _refine_diff_density_min -1.658 _refine_diff_density_rms 0.159 #================================================================ end