# 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 yhshi_2000@126.com _publ_contact_author_name 'Yanhui Shi' loop_ _publ_author_name 'Longguang Yang' 'Pei Guan' 'Pan He' 'Qian Chen' 'Changsheng Cao' 'Yu Peng' 'Zhan Shi' 'Guangsheng Pang' 'Yanhui Shi' data_110226g _database_code_depnum_ccdc_archive 'CCDC 858709' #TrackingRef '- 3a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H39 Br2 N3 Pd' _chemical_formula_weight 755.90 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.6900(10) _cell_length_b 11.0661(11) _cell_length_c 14.7279(15) _cell_angle_alpha 109.010(2) _cell_angle_beta 90.6700(10) _cell_angle_gamma 96.2090(10) _cell_volume 1635.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 3447 _cell_measurement_theta_min 2.576 _cell_measurement_theta_max 27.954 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.43 _exptl_crystal_size_min 0.38 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.535 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 760 _exptl_absorpt_coefficient_mu 3.037 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3419 _exptl_absorpt_correction_T_max 0.3916 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8476 _diffrn_reflns_av_R_equivalents 0.0210 _diffrn_reflns_av_sigmaI/netI 0.0488 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.58 _diffrn_reflns_theta_max 25.02 _reflns_number_total 5672 _reflns_number_gt 4102 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SMART' _computing_publication_material 'Bruker SMART' _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^)+(0.0594P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5672 _refine_ls_number_parameters 361 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0686 _refine_ls_R_factor_gt 0.0400 _refine_ls_wR_factor_ref 0.1103 _refine_ls_wR_factor_gt 0.0964 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _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 0.32925(3) 0.16925(3) 0.23492(2) 0.03008(12) Uani 1 1 d . . . Br1 Br 0.51566(4) 0.32493(5) 0.25877(4) 0.04283(16) Uani 1 1 d . . . Br2 Br 0.14928(5) 0.01711(6) 0.23989(5) 0.0661(2) Uani 1 1 d . . . N1 N 0.1947(3) 0.4024(4) 0.2744(2) 0.0314(9) Uani 1 1 d . . . N2 N 0.2352(3) 0.3526(4) 0.4026(2) 0.0338(9) Uani 1 1 d . . . N3 N 0.4293(3) 0.0167(4) 0.1569(3) 0.0342(9) Uani 1 1 d . . . C1 C 0.2427(4) 0.3169(4) 0.3062(3) 0.0292(10) Uani 1 1 d . . . C2 C 0.2013(4) 0.4851(4) 0.4421(3) 0.0347(11) Uani 1 1 d . . . H2A H 0.1388 0.4900 0.4910 0.042 Uiso 1 1 calc R . . C3 C 0.1414(4) 0.5011(5) 0.3525(3) 0.0362(11) Uani 1 1 d . . . H3A H 0.0502 0.4846 0.3507 0.043 Uiso 1 1 calc R . . H3B H 0.1652 0.5866 0.3493 0.043 Uiso 1 1 calc R . . C4 C 0.1748(4) 0.3930(5) 0.1746(3) 0.0411(12) Uani 1 1 d . . . C5 C 0.2559(5) 0.4719(6) 0.1372(4) 0.0502(14) Uani 1 1 d . . . C6 C 0.2319(6) 0.4609(7) 0.0407(4) 0.078(2) Uani 1 1 d . . . H6A H 0.2836 0.5108 0.0129 0.093 Uiso 1 1 calc R . . C7 C 0.1334(7) 0.3780(8) -0.0129(5) 0.092(2) Uani 1 1 d . . . H7A H 0.1208 0.3713 -0.0770 0.111 Uiso 1 1 calc R . . C8 C 0.0542(6) 0.3057(8) 0.0247(4) 0.083(2) Uani 1 1 d . . . H8A H -0.0115 0.2499 -0.0138 0.099 Uiso 1 1 calc R . . C9 C 0.0698(5) 0.3139(6) 0.1209(4) 0.0554(15) Uani 1 1 d . . . C10 C 0.3578(5) 0.5719(6) 0.1967(4) 0.0539(15) Uani 1 1 d . . . H10A H 0.3718 0.5558 0.2574 0.065 Uiso 1 1 calc R . . C11 C 0.4833(6) 0.5660(7) 0.1451(5) 0.0741(19) Uani 1 1 d . . . H11A H 0.5089 0.4815 0.1309 0.111 Uiso 1 1 calc R . . H11B H 0.5470 0.6285 0.1860 0.111 Uiso 1 1 calc R . . H11C H 0.4719 0.5843 0.0863 0.111 Uiso 1 1 calc R . . C12 C 0.3164(7) 0.7073(6) 0.2196(5) 0.088(2) Uani 1 1 d . . . H12A H 0.2385 0.7107 0.2517 0.132 Uiso 1 1 calc R . . H12B H 0.3049 0.7257 0.1609 0.132 Uiso 1 1 calc R . . H12C H 0.3800 0.7698 0.2606 0.132 Uiso 1 1 calc R . . C13 C -0.0312(5) 0.2467(6) 0.1640(4) 0.0618(16) Uani 1 1 d . . . H13A H 0.0019 0.2459 0.2262 0.074 Uiso 1 1 calc R . . C14 C -0.1424(6) 0.3258(8) 0.1818(5) 0.089(2) Uani 1 1 d . . . H14A H -0.1142 0.4126 0.2213 0.134 Uiso 1 1 calc R . . H14B H -0.2057 0.2887 0.2139 0.134 Uiso 1 1 calc R . . H14C H -0.1774 0.3258 0.1215 0.134 Uiso 1 1 calc R . . C15 C -0.0742(8) 0.1071(8) 0.1008(6) 0.115(3) Uani 1 1 d . . . H15A H -0.0034 0.0586 0.0903 0.173 Uiso 1 1 calc R . . H15B H -0.1089 0.1063 0.0402 0.173 Uiso 1 1 calc R . . H15C H -0.1372 0.0692 0.1326 0.173 Uiso 1 1 calc R . . C16 C 0.2935(4) 0.2916(5) 0.4635(3) 0.0389(12) Uani 1 1 d . . . H16A H 0.3739 0.3406 0.4902 0.047 Uiso 1 1 calc R . . H16B H 0.3092 0.2057 0.4248 0.047 Uiso 1 1 calc R . . C17 C 0.2115(5) 0.2828(4) 0.5449(3) 0.0364(11) Uani 1 1 d . . . C18 C 0.2560(5) 0.3405(5) 0.6385(3) 0.0521(14) Uani 1 1 d . . . H18A H 0.3350 0.3884 0.6527 0.062 Uiso 1 1 calc R . . C19 C 0.1805(6) 0.3261(6) 0.7131(4) 0.0619(16) Uani 1 1 d . . . H19A H 0.2099 0.3645 0.7768 0.074 Uiso 1 1 calc R . . C20 C 0.0649(5) 0.2565(6) 0.6921(4) 0.0565(15) Uani 1 1 d . . . H20A H 0.0154 0.2481 0.7417 0.068 Uiso 1 1 calc R . . C21 C 0.0213(5) 0.1992(6) 0.5996(4) 0.0552(15) Uani 1 1 d . . . H21A H -0.0575 0.1507 0.5858 0.066 Uiso 1 1 calc R . . C22 C 0.0940(5) 0.2128(5) 0.5254(4) 0.0494(14) Uani 1 1 d . . . H22A H 0.0632 0.1744 0.4621 0.059 Uiso 1 1 calc R . . C23 C 0.3196(5) 0.5806(5) 0.4854(3) 0.0436(12) Uani 1 1 d . . . H23A H 0.3559 0.5586 0.5378 0.052 Uiso 1 1 calc R . . H23B H 0.3814 0.5717 0.4366 0.052 Uiso 1 1 calc R . . C24 C 0.2931(5) 0.7181(5) 0.5222(3) 0.0438(12) Uani 1 1 d . . . C25 C 0.3553(6) 0.8095(6) 0.4872(4) 0.0655(16) Uani 1 1 d . . . H25A H 0.4122 0.7847 0.4392 0.079 Uiso 1 1 calc R . . C26 C 0.3332(7) 0.9375(7) 0.5232(6) 0.082(2) Uani 1 1 d . . . H26A H 0.3750 0.9976 0.4988 0.099 Uiso 1 1 calc R . . C27 C 0.2505(7) 0.9758(6) 0.5941(5) 0.077(2) Uani 1 1 d . . . H27A H 0.2375 1.0620 0.6186 0.092 Uiso 1 1 calc R . . C28 C 0.1872(6) 0.8886(6) 0.6292(5) 0.0674(17) Uani 1 1 d . . . H28A H 0.1294 0.9144 0.6764 0.081 Uiso 1 1 calc R . . C29 C 0.2095(5) 0.7600(5) 0.5937(4) 0.0537(14) Uani 1 1 d . . . H29A H 0.1671 0.7009 0.6188 0.064 Uiso 1 1 calc R . . C30 C 0.3829(5) -0.0629(5) 0.0708(3) 0.0444(12) Uani 1 1 d . . . H30A H 0.3029 -0.0548 0.0497 0.053 Uiso 1 1 calc R . . C31 C 0.4484(6) -0.1559(5) 0.0125(4) 0.0550(15) Uani 1 1 d . . . H31A H 0.4141 -0.2082 -0.0476 0.066 Uiso 1 1 calc R . . C32 C 0.5638(6) -0.1705(5) 0.0438(4) 0.0614(16) Uani 1 1 d . . . H32A H 0.6098 -0.2328 0.0052 0.074 Uiso 1 1 calc R . . C33 C 0.6118(5) -0.0932(5) 0.1323(4) 0.0594(15) Uani 1 1 d . . . H33A H 0.6901 -0.1031 0.1554 0.071 Uiso 1 1 calc R . . C34 C 0.5419(5) 0.0010(5) 0.1878(4) 0.0463(13) Uani 1 1 d . . . H34A H 0.5748 0.0543 0.2480 0.056 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0296(2) 0.0282(2) 0.0287(2) 0.00462(15) 0.00544(14) 0.00156(15) Br1 0.0334(3) 0.0361(3) 0.0502(3) 0.0043(2) 0.0046(2) -0.0028(2) Br2 0.0474(4) 0.0438(4) 0.0996(5) 0.0161(3) 0.0252(3) -0.0062(3) N1 0.036(2) 0.037(2) 0.0230(18) 0.0113(17) 0.0065(15) 0.0069(18) N2 0.042(2) 0.036(2) 0.026(2) 0.0119(17) 0.0054(16) 0.0094(18) N3 0.032(2) 0.032(2) 0.035(2) 0.0064(18) 0.0057(17) 0.0014(17) C1 0.028(2) 0.031(3) 0.027(2) 0.009(2) 0.0024(18) -0.002(2) C2 0.039(3) 0.040(3) 0.027(2) 0.010(2) 0.007(2) 0.012(2) C3 0.037(3) 0.038(3) 0.033(2) 0.010(2) 0.007(2) 0.009(2) C4 0.039(3) 0.058(3) 0.031(3) 0.019(2) 0.009(2) 0.012(3) C5 0.044(3) 0.079(4) 0.040(3) 0.033(3) 0.011(2) 0.015(3) C6 0.071(5) 0.119(6) 0.052(4) 0.044(4) 0.015(3) 0.002(4) C7 0.087(6) 0.150(8) 0.044(4) 0.043(5) -0.003(4) -0.005(5) C8 0.066(5) 0.131(7) 0.041(4) 0.020(4) -0.010(3) -0.002(4) C9 0.044(3) 0.081(4) 0.036(3) 0.013(3) -0.001(2) 0.006(3) C10 0.057(4) 0.067(4) 0.052(3) 0.037(3) 0.013(3) 0.010(3) C11 0.064(4) 0.094(5) 0.084(5) 0.056(4) 0.020(3) 0.007(4) C12 0.103(6) 0.072(5) 0.108(6) 0.052(5) 0.038(4) 0.020(4) C13 0.053(4) 0.073(4) 0.048(3) 0.012(3) -0.012(3) -0.012(3) C14 0.047(4) 0.141(7) 0.084(5) 0.043(5) 0.005(3) 0.010(4) C15 0.119(7) 0.104(7) 0.090(6) 0.007(5) -0.046(5) -0.035(5) C16 0.046(3) 0.041(3) 0.034(3) 0.017(2) 0.003(2) 0.010(2) C17 0.048(3) 0.035(3) 0.030(3) 0.014(2) 0.006(2) 0.009(2) C18 0.060(4) 0.052(4) 0.038(3) 0.010(3) 0.008(3) -0.003(3) C19 0.072(4) 0.075(4) 0.030(3) 0.010(3) 0.011(3) -0.003(4) C20 0.059(4) 0.069(4) 0.047(3) 0.025(3) 0.022(3) 0.013(3) C21 0.045(3) 0.065(4) 0.060(4) 0.027(3) 0.007(3) 0.005(3) C22 0.054(4) 0.060(4) 0.034(3) 0.015(3) -0.001(2) 0.006(3) C23 0.044(3) 0.044(3) 0.038(3) 0.007(2) 0.000(2) 0.007(2) C24 0.041(3) 0.038(3) 0.047(3) 0.009(2) -0.009(2) 0.002(2) C25 0.059(4) 0.056(4) 0.079(4) 0.020(3) 0.009(3) 0.000(3) C26 0.084(5) 0.054(4) 0.110(6) 0.032(4) -0.001(4) -0.004(4) C27 0.071(5) 0.049(4) 0.099(6) 0.009(4) -0.020(4) 0.013(4) C28 0.062(4) 0.056(4) 0.068(4) -0.003(3) -0.009(3) 0.015(3) C29 0.056(4) 0.050(4) 0.047(3) 0.005(3) 0.001(3) 0.003(3) C30 0.050(3) 0.041(3) 0.038(3) 0.010(2) 0.003(2) -0.004(2) C31 0.069(4) 0.042(3) 0.044(3) 0.003(3) 0.020(3) -0.004(3) C32 0.068(4) 0.038(3) 0.071(4) 0.007(3) 0.032(3) 0.008(3) C33 0.048(4) 0.047(4) 0.080(4) 0.015(3) 0.009(3) 0.009(3) C34 0.049(3) 0.032(3) 0.053(3) 0.008(2) -0.001(3) 0.002(2) _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 C1 1.965(4) . ? Pd1 N3 2.114(4) . ? Pd1 Br1 2.4309(6) . ? Pd1 Br2 2.4339(7) . ? N1 C1 1.328(5) . ? N1 C4 1.451(5) . ? N1 C3 1.473(5) . ? N2 C1 1.349(5) . ? N2 C16 1.457(5) . ? N2 C2 1.478(5) . ? N3 C34 1.330(6) . ? N3 C30 1.339(6) . ? C2 C3 1.529(6) . ? C2 C23 1.541(7) . ? C2 H2A 0.9800 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C9 1.403(7) . ? C4 C5 1.406(7) . ? C5 C6 1.404(7) . ? C5 C10 1.506(8) . ? C6 C7 1.369(9) . ? C6 H6A 0.9300 . ? C7 C8 1.347(9) . ? C7 H7A 0.9300 . ? C8 C9 1.396(7) . ? C8 H8A 0.9300 . ? C9 C13 1.507(8) . ? C10 C12 1.540(8) . ? C10 C11 1.546(7) . ? C10 H10A 0.9800 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14 1.528(8) . ? C13 C15 1.537(9) . ? C13 H13A 0.9800 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 C17 1.515(6) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.371(7) . ? C17 C22 1.377(7) . ? C18 C19 1.410(7) . ? C18 H18A 0.9300 . ? C19 C20 1.359(8) . ? C19 H19A 0.9300 . ? C20 C21 1.354(7) . ? C20 H20A 0.9300 . ? C21 C22 1.386(7) . ? C21 H21A 0.9300 . ? C22 H22A 0.9300 . ? C23 C24 1.500(6) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C29 1.384(7) . ? C24 C25 1.391(8) . ? C25 C26 1.390(8) . ? C25 H25A 0.9300 . ? C26 C27 1.366(9) . ? C26 H26A 0.9300 . ? C27 C28 1.360(9) . ? C27 H27A 0.9300 . ? C28 C29 1.395(7) . ? C28 H28A 0.9300 . ? C29 H29A 0.9300 . ? C30 C31 1.371(7) . ? C30 H30A 0.9300 . ? C31 C32 1.357(8) . ? C31 H31A 0.9300 . ? C32 C33 1.363(8) . ? C32 H32A 0.9300 . ? C33 C34 1.393(7) . ? C33 H33A 0.9300 . ? C34 H34A 0.9300 . ? 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 C1 Pd1 N3 177.22(16) . . ? C1 Pd1 Br1 85.64(13) . . ? N3 Pd1 Br1 91.73(10) . . ? C1 Pd1 Br2 91.93(13) . . ? N3 Pd1 Br2 90.81(10) . . ? Br1 Pd1 Br2 170.15(2) . . ? C1 N1 C4 126.3(4) . . ? C1 N1 C3 111.6(3) . . ? C4 N1 C3 121.3(3) . . ? C1 N2 C16 124.5(4) . . ? C1 N2 C2 111.0(3) . . ? C16 N2 C2 121.3(3) . . ? C34 N3 C30 118.0(4) . . ? C34 N3 Pd1 122.1(3) . . ? C30 N3 Pd1 119.8(3) . . ? N1 C1 N2 109.2(4) . . ? N1 C1 Pd1 128.9(3) . . ? N2 C1 Pd1 121.6(3) . . ? N2 C2 C3 100.9(3) . . ? N2 C2 C23 110.3(3) . . ? C3 C2 C23 114.4(4) . . ? N2 C2 H2A 110.3 . . ? C3 C2 H2A 110.3 . . ? C23 C2 H2A 110.3 . . ? N1 C3 C2 102.0(3) . . ? N1 C3 H3A 111.4 . . ? C2 C3 H3A 111.4 . . ? N1 C3 H3B 111.4 . . ? C2 C3 H3B 111.4 . . ? H3A C3 H3B 109.2 . . ? C9 C4 C5 122.0(5) . . ? C9 C4 N1 119.2(4) . . ? C5 C4 N1 118.6(4) . . ? C6 C5 C4 116.6(5) . . ? C6 C5 C10 119.6(5) . . ? C4 C5 C10 123.5(4) . . ? C7 C6 C5 120.9(6) . . ? C7 C6 H6A 119.6 . . ? C5 C6 H6A 119.6 . . ? C8 C7 C6 121.8(6) . . ? C8 C7 H7A 119.1 . . ? C6 C7 H7A 119.1 . . ? C7 C8 C9 120.7(6) . . ? C7 C8 H8A 119.7 . . ? C9 C8 H8A 119.7 . . ? C8 C9 C4 117.7(6) . . ? C8 C9 C13 119.0(5) . . ? C4 C9 C13 123.1(5) . . ? C5 C10 C12 110.2(5) . . ? C5 C10 C11 111.7(5) . . ? C12 C10 C11 109.6(5) . . ? C5 C10 H10A 108.4 . . ? C12 C10 H10A 108.4 . . ? C11 C10 H10A 108.4 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C9 C13 C14 107.7(5) . . ? C9 C13 C15 113.4(6) . . ? C14 C13 C15 110.4(6) . . ? C9 C13 H13A 108.4 . . ? C14 C13 H13A 108.4 . . ? C15 C13 H13A 108.4 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 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 . . ? N2 C16 C17 112.1(4) . . ? N2 C16 H16A 109.2 . . ? C17 C16 H16A 109.2 . . ? N2 C16 H16B 109.2 . . ? C17 C16 H16B 109.2 . . ? H16A C16 H16B 107.9 . . ? C18 C17 C22 119.5(4) . . ? C18 C17 C16 120.1(5) . . ? C22 C17 C16 120.3(4) . . ? C17 C18 C19 119.2(5) . . ? C17 C18 H18A 120.4 . . ? C19 C18 H18A 120.4 . . ? C20 C19 C18 120.2(5) . . ? C20 C19 H19A 119.9 . . ? C18 C19 H19A 119.9 . . ? C21 C20 C19 120.6(5) . . ? C21 C20 H20A 119.7 . . ? C19 C20 H20A 119.7 . . ? C20 C21 C22 120.0(5) . . ? C20 C21 H21A 120.0 . . ? C22 C21 H21A 120.0 . . ? C17 C22 C21 120.5(5) . . ? C17 C22 H22A 119.7 . . ? C21 C22 H22A 119.7 . . ? C24 C23 C2 113.2(4) . . ? C24 C23 H23A 108.9 . . ? C2 C23 H23A 108.9 . . ? C24 C23 H23B 108.9 . . ? C2 C23 H23B 108.9 . . ? H23A C23 H23B 107.7 . . ? C29 C24 C25 117.5(5) . . ? C29 C24 C23 121.9(5) . . ? C25 C24 C23 120.6(5) . . ? C26 C25 C24 120.6(6) . . ? C26 C25 H25A 119.7 . . ? C24 C25 H25A 119.7 . . ? C27 C26 C25 120.5(7) . . ? C27 C26 H26A 119.8 . . ? C25 C26 H26A 119.8 . . ? C28 C27 C26 120.4(6) . . ? C28 C27 H27A 119.8 . . ? C26 C27 H27A 119.8 . . ? C27 C28 C29 119.5(6) . . ? C27 C28 H28A 120.3 . . ? C29 C28 H28A 120.3 . . ? C24 C29 C28 121.6(6) . . ? C24 C29 H29A 119.2 . . ? C28 C29 H29A 119.2 . . ? N3 C30 C31 122.8(5) . . ? N3 C30 H30A 118.6 . . ? C31 C30 H30A 118.6 . . ? C32 C31 C30 119.0(5) . . ? C32 C31 H31A 120.5 . . ? C30 C31 H31A 120.5 . . ? C31 C32 C33 119.4(5) . . ? C31 C32 H32A 120.3 . . ? C33 C32 H32A 120.3 . . ? C32 C33 C34 119.0(6) . . ? C32 C33 H33A 120.5 . . ? C34 C33 H33A 120.5 . . ? N3 C34 C33 121.7(5) . . ? N3 C34 H34A 119.1 . . ? C33 C34 H34A 119.1 . . ? 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 Pd1 N3 C34 66(3) . . . . ? Br1 Pd1 N3 C34 46.8(4) . . . . ? Br2 Pd1 N3 C34 -123.6(4) . . . . ? C1 Pd1 N3 C30 -110(3) . . . . ? Br1 Pd1 N3 C30 -129.0(3) . . . . ? Br2 Pd1 N3 C30 60.5(3) . . . . ? C4 N1 C1 N2 -174.1(4) . . . . ? C3 N1 C1 N2 -4.2(5) . . . . ? C4 N1 C1 Pd1 12.1(7) . . . . ? C3 N1 C1 Pd1 -178.0(3) . . . . ? C16 N2 C1 N1 -171.5(4) . . . . ? C2 N2 C1 N1 -11.5(5) . . . . ? C16 N2 C1 Pd1 2.9(6) . . . . ? C2 N2 C1 Pd1 162.9(3) . . . . ? N3 Pd1 C1 N1 63(3) . . . . ? Br1 Pd1 C1 N1 82.0(4) . . . . ? Br2 Pd1 C1 N1 -107.5(4) . . . . ? N3 Pd1 C1 N2 -110(3) . . . . ? Br1 Pd1 C1 N2 -91.2(3) . . . . ? Br2 Pd1 C1 N2 79.3(3) . . . . ? C1 N2 C2 C3 21.0(5) . . . . ? C16 N2 C2 C3 -178.2(4) . . . . ? C1 N2 C2 C23 -100.3(4) . . . . ? C16 N2 C2 C23 60.4(5) . . . . ? C1 N1 C3 C2 16.9(5) . . . . ? C4 N1 C3 C2 -172.6(4) . . . . ? N2 C2 C3 N1 -21.3(4) . . . . ? C23 C2 C3 N1 97.1(4) . . . . ? C1 N1 C4 C9 78.8(6) . . . . ? C3 N1 C4 C9 -90.2(6) . . . . ? C1 N1 C4 C5 -106.4(6) . . . . ? C3 N1 C4 C5 84.6(5) . . . . ? C9 C4 C5 C6 -4.4(8) . . . . ? N1 C4 C5 C6 -179.0(5) . . . . ? C9 C4 C5 C10 170.7(5) . . . . ? N1 C4 C5 C10 -3.9(7) . . . . ? C4 C5 C6 C7 0.6(10) . . . . ? C10 C5 C6 C7 -174.8(6) . . . . ? C5 C6 C7 C8 1.4(13) . . . . ? C6 C7 C8 C9 0.4(13) . . . . ? C7 C8 C9 C4 -4.1(10) . . . . ? C7 C8 C9 C13 171.1(7) . . . . ? C5 C4 C9 C8 6.2(9) . . . . ? N1 C4 C9 C8 -179.3(5) . . . . ? C5 C4 C9 C13 -168.8(5) . . . . ? N1 C4 C9 C13 5.8(8) . . . . ? C6 C5 C10 C12 71.6(7) . . . . ? C4 C5 C10 C12 -103.4(6) . . . . ? C6 C5 C10 C11 -50.5(7) . . . . ? C4 C5 C10 C11 134.5(5) . . . . ? C8 C9 C13 C14 -75.0(7) . . . . ? C4 C9 C13 C14 99.9(6) . . . . ? C8 C9 C13 C15 47.4(8) . . . . ? C4 C9 C13 C15 -137.7(6) . . . . ? C1 N2 C16 C17 -142.6(4) . . . . ? C2 N2 C16 C17 59.4(6) . . . . ? N2 C16 C17 C18 -120.8(5) . . . . ? N2 C16 C17 C22 61.7(6) . . . . ? C22 C17 C18 C19 0.4(8) . . . . ? C16 C17 C18 C19 -177.1(5) . . . . ? C17 C18 C19 C20 -0.3(9) . . . . ? C18 C19 C20 C21 0.6(9) . . . . ? C19 C20 C21 C22 -0.9(9) . . . . ? C18 C17 C22 C21 -0.7(8) . . . . ? C16 C17 C22 C21 176.8(5) . . . . ? C20 C21 C22 C17 1.0(8) . . . . ? N2 C2 C23 C24 177.0(4) . . . . ? C3 C2 C23 C24 64.0(5) . . . . ? C2 C23 C24 C29 59.6(6) . . . . ? C2 C23 C24 C25 -122.3(5) . . . . ? C29 C24 C25 C26 -0.1(9) . . . . ? C23 C24 C25 C26 -178.3(5) . . . . ? C24 C25 C26 C27 0.4(10) . . . . ? C25 C26 C27 C28 -1.2(10) . . . . ? C26 C27 C28 C29 1.5(10) . . . . ? C25 C24 C29 C28 0.5(8) . . . . ? C23 C24 C29 C28 178.6(5) . . . . ? C27 C28 C29 C24 -1.2(9) . . . . ? C34 N3 C30 C31 -2.4(7) . . . . ? Pd1 N3 C30 C31 173.6(4) . . . . ? N3 C30 C31 C32 1.6(8) . . . . ? C30 C31 C32 C33 0.3(8) . . . . ? C31 C32 C33 C34 -1.3(8) . . . . ? C30 N3 C34 C33 1.3(7) . . . . ? Pd1 N3 C34 C33 -174.6(4) . . . . ? C32 C33 C34 N3 0.5(8) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.642 _refine_diff_density_min -1.310 _refine_diff_density_rms 0.104 # Attachment '- 3c.cif' data_110227c _database_code_depnum_ccdc_archive 'CCDC 858710' #TrackingRef '- 3c.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H37 Br2 N3 O Pd' _chemical_formula_weight 709.84 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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 10.4260(11) _cell_length_b 17.3900(18) _cell_length_c 16.7852(15) _cell_angle_alpha 90.00 _cell_angle_beta 95.8990(10) _cell_angle_gamma 90.00 _cell_volume 3027.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 5138 _cell_measurement_theta_min 2.287 _cell_measurement_theta_max 24.529 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.558 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1424 _exptl_absorpt_coefficient_mu 3.278 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3330 _exptl_absorpt_correction_T_max 0.4396 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14987 _diffrn_reflns_av_R_equivalents 0.0362 _diffrn_reflns_av_sigmaI/netI 0.0472 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 25.02 _reflns_number_total 5293 _reflns_number_gt 3816 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0180P)^2^+25.6770P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5293 _refine_ls_number_parameters 358 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0894 _refine_ls_R_factor_gt 0.0630 _refine_ls_wR_factor_ref 0.1334 _refine_ls_wR_factor_gt 0.1253 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _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 0.08070(6) 0.21715(4) 0.86285(4) 0.03751(17) Uani 1 1 d . . . Br1 Br -0.11168(9) 0.29683(6) 0.84484(7) 0.0682(3) Uani 1 1 d . . . Br2 Br 0.27836(10) 0.14480(6) 0.89415(7) 0.0693(3) Uani 1 1 d . . . N1 N 0.2284(6) 0.3216(4) 0.7638(4) 0.0411(16) Uani 1 1 d . B . N2 N 0.2390(7) 0.3528(4) 0.8901(4) 0.056(2) Uani 1 1 d . . . N3 N -0.0287(7) 0.1247(4) 0.9014(4) 0.0511(18) Uani 1 1 d . . . O1 O 0.1506(18) 0.4874(12) 0.9795(10) 0.122(9) Uani 0.59(3) 1 d P A 1 H1 H 0.1908 0.4880 0.9400 0.146 Uiso 0.59(3) 1 calc PR A 1 O1' O 0.032(3) 0.4424(16) 0.9469(17) 0.124(13) Uani 0.41(3) 1 d P A 2 H1' H -0.0070 0.4085 0.9202 0.149 Uiso 0.41(3) 1 calc PR A 2 C1 C 0.1887(8) 0.3036(5) 0.8344(5) 0.043(2) Uani 1 1 d . B . C2 C 0.356(4) 0.390(2) 0.860(2) 0.061(8) Uani 0.52(5) 1 d P B 1 H2 H 0.4289 0.3541 0.8684 0.073 Uiso 0.52(5) 1 calc PR B 1 C2' C 0.304(4) 0.419(2) 0.856(2) 0.059(9) Uani 0.48(5) 1 d P B 2 H2' H 0.2595 0.4684 0.8613 0.071 Uiso 0.48(5) 1 calc PR B 2 C3 C 0.3074(9) 0.3923(5) 0.7702(5) 0.058(2) Uani 1 1 d . . . H3A H 0.2560 0.4378 0.7566 0.070 Uiso 1 1 calc R B 1 H3B H 0.3780 0.3898 0.7369 0.070 Uiso 1 1 calc R B 1 C4 C 0.1987(8) 0.2864(5) 0.6864(5) 0.0416(19) Uani 1 1 d . . . C5 C 0.0919(8) 0.3100(5) 0.6366(5) 0.045(2) Uani 1 1 d . B . C6 C 0.0738(9) 0.2776(6) 0.5593(5) 0.055(2) Uani 1 1 d . . . H6 H 0.0018 0.2913 0.5250 0.066 Uiso 1 1 calc R B . C7 C 0.1595(9) 0.2267(6) 0.5342(5) 0.059(2) Uani 1 1 d . B . H7 H 0.1460 0.2063 0.4828 0.071 Uiso 1 1 calc R . . C8 C 0.2666(9) 0.2050(5) 0.5842(5) 0.056(2) Uani 1 1 d . . . H8 H 0.3246 0.1702 0.5659 0.067 Uiso 1 1 calc R B . C9 C 0.2896(8) 0.2341(5) 0.6614(5) 0.045(2) Uani 1 1 d . B . C10 C -0.0038(8) 0.3693(5) 0.6586(5) 0.053(2) Uani 1 1 d . . . H10 H 0.0116 0.3777 0.7165 0.063 Uiso 1 1 calc R B . C11 C -0.1443(9) 0.3426(6) 0.6401(6) 0.067(3) Uani 1 1 d . B . H11A H -0.1643 0.3375 0.5833 0.101 Uiso 1 1 calc R . . H11B H -0.2009 0.3798 0.6602 0.101 Uiso 1 1 calc R . . H11C H -0.1554 0.2939 0.6654 0.101 Uiso 1 1 calc R . . C12 C 0.0191(10) 0.4474(6) 0.6168(6) 0.072(3) Uani 1 1 d . B . H12A H 0.1088 0.4607 0.6255 0.107 Uiso 1 1 calc R . . H12B H -0.0314 0.4868 0.6387 0.107 Uiso 1 1 calc R . . H12C H -0.0060 0.4428 0.5603 0.107 Uiso 1 1 calc R . . C13 C 0.4125(8) 0.2119(5) 0.7127(6) 0.055(2) Uani 1 1 d . . . H13 H 0.4050 0.2293 0.7676 0.066 Uiso 1 1 calc R B . C14 C 0.4326(11) 0.1235(6) 0.7147(6) 0.074(3) Uani 1 1 d . B . H14A H 0.3541 0.0987 0.7257 0.112 Uiso 1 1 calc R . . H14B H 0.5001 0.1107 0.7558 0.112 Uiso 1 1 calc R . . H14C H 0.4561 0.1065 0.6637 0.112 Uiso 1 1 calc R . . C15 C 0.5290(10) 0.2518(7) 0.6829(7) 0.082(3) Uani 1 1 d . B . H15A H 0.5424 0.2323 0.6309 0.123 Uiso 1 1 calc R . . H15B H 0.6041 0.2419 0.7196 0.123 Uiso 1 1 calc R . . H15C H 0.5136 0.3061 0.6796 0.123 Uiso 1 1 calc R . . C16 C 0.2200(11) 0.3506(7) 0.9745(6) 0.076(3) Uani 1 1 d . A . H16A H 0.3027 0.3584 1.0055 0.092 Uiso 1 1 calc R . . H16B H 0.1898 0.2997 0.9871 0.092 Uiso 1 1 calc R . . C17 C 0.1258(17) 0.4094(9) 1.0009(9) 0.100(4) Uani 1 1 d . . . H17A H 0.0398 0.3956 0.9777 0.120 Uiso 0.59(3) 1 calc PR A 1 H17B H 0.1267 0.4065 1.0586 0.120 Uiso 0.59(3) 1 calc PR A 1 H17C H 0.0813 0.3862 1.0428 0.120 Uiso 0.41(3) 1 d PR A 2 H17D H 0.1773 0.4510 1.0258 0.120 Uiso 0.41(3) 1 d PR A 2 C18 C 0.395(3) 0.466(2) 0.9020(14) 0.067(10) Uani 0.52(5) 1 d P B 1 H18A H 0.3255 0.5032 0.8935 0.080 Uiso 0.52(5) 1 calc PR B 1 H18B H 0.4153 0.4581 0.9591 0.080 Uiso 0.52(5) 1 calc PR B 1 C18' C 0.446(3) 0.421(2) 0.8909(16) 0.064(9) Uani 0.48(5) 1 d P B 2 H18C H 0.4509 0.4199 0.9489 0.077 Uiso 0.48(5) 1 calc PR B 2 H18D H 0.4887 0.3750 0.8736 0.077 Uiso 0.48(5) 1 calc PR B 2 C19 C 0.5127(11) 0.4920(8) 0.8632(7) 0.076(3) Uani 1 1 d . . . C20 C 0.6262(13) 0.4637(7) 0.8409(8) 0.090(4) Uani 1 1 d . B . H20 H 0.6435 0.4114 0.8462 0.107 Uiso 1 1 calc R . . C21 C 0.7149(11) 0.5113(8) 0.8110(8) 0.089(4) Uani 1 1 d . . . H21 H 0.7939 0.4913 0.8000 0.107 Uiso 1 1 calc R B . C22 C 0.6903(12) 0.5847(8) 0.7976(7) 0.083(4) Uani 1 1 d . B . H22 H 0.7497 0.6159 0.7754 0.100 Uiso 1 1 calc R . . C23 C 0.5773(12) 0.6141(7) 0.8166(7) 0.079(3) Uani 1 1 d . . . H23 H 0.5587 0.6659 0.8078 0.095 Uiso 1 1 calc R B . C24 C 0.4907(11) 0.5673(7) 0.8487(7) 0.076(3) Uani 1 1 d . B . H24 H 0.4133 0.5884 0.8611 0.092 Uiso 1 1 calc R . . C25 C -0.0176(10) 0.0539(6) 0.8749(6) 0.061(3) Uani 1 1 d . . . H25 H 0.0392 0.0444 0.8368 0.073 Uiso 1 1 calc R . . C26 C -0.0874(11) -0.0067(6) 0.9019(6) 0.076(3) Uani 1 1 d . . . H26 H -0.0758 -0.0562 0.8829 0.092 Uiso 1 1 calc R . . C27 C -0.1727(12) 0.0064(7) 0.9561(7) 0.083(4) Uani 1 1 d . . . H27 H -0.2227 -0.0335 0.9730 0.099 Uiso 1 1 calc R . . C28 C -0.1844(11) 0.0795(7) 0.9856(7) 0.080(3) Uani 1 1 d . . . H28 H -0.2391 0.0897 1.0247 0.096 Uiso 1 1 calc R . . C29 C -0.1119(10) 0.1378(6) 0.9551(6) 0.071(3) Uani 1 1 d . . . H29 H -0.1219 0.1878 0.9730 0.085 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0407(3) 0.0344(3) 0.0387(3) 0.0038(3) 0.0100(2) -0.0041(3) Br1 0.0526(6) 0.0698(7) 0.0849(8) 0.0237(6) 0.0205(5) 0.0144(5) Br2 0.0565(6) 0.0740(7) 0.0806(7) 0.0327(6) 0.0223(5) 0.0177(5) N1 0.042(4) 0.039(4) 0.043(4) -0.003(3) 0.011(3) -0.014(3) N2 0.069(5) 0.057(5) 0.044(4) -0.008(4) 0.019(4) -0.026(4) N3 0.055(5) 0.050(5) 0.050(4) 0.013(4) 0.012(4) -0.008(4) O1 0.132(17) 0.129(18) 0.108(14) -0.038(12) 0.029(11) -0.003(12) O1' 0.13(3) 0.13(2) 0.11(2) -0.042(17) 0.028(18) -0.003(19) C1 0.046(5) 0.043(5) 0.042(5) -0.005(4) 0.012(4) -0.006(4) C2 0.07(2) 0.06(2) 0.057(14) -0.012(15) 0.016(16) -0.021(15) C2' 0.06(2) 0.06(2) 0.055(15) -0.010(16) 0.020(16) -0.019(14) C3 0.065(6) 0.058(6) 0.052(6) -0.010(5) 0.012(5) -0.025(5) C4 0.048(5) 0.042(5) 0.036(4) -0.004(4) 0.013(4) -0.011(4) C5 0.050(5) 0.046(5) 0.041(5) 0.000(4) 0.011(4) -0.007(4) C6 0.057(6) 0.061(6) 0.046(5) -0.002(5) -0.002(4) -0.007(5) C7 0.070(6) 0.064(6) 0.044(5) -0.008(5) 0.006(5) -0.004(5) C8 0.064(6) 0.054(6) 0.053(6) -0.007(5) 0.021(5) 0.001(5) C9 0.048(5) 0.041(5) 0.049(5) 0.002(4) 0.015(4) -0.004(4) C10 0.054(6) 0.058(6) 0.046(5) 0.001(4) 0.008(4) 0.003(4) C11 0.055(6) 0.074(7) 0.071(7) 0.015(6) 0.005(5) 0.018(5) C12 0.076(7) 0.054(6) 0.084(8) 0.006(6) 0.006(6) 0.008(5) C13 0.051(5) 0.060(6) 0.055(5) 0.003(5) 0.010(4) 0.004(5) C14 0.080(8) 0.066(7) 0.080(8) 0.011(6) 0.019(6) 0.015(6) C15 0.061(7) 0.081(8) 0.106(9) 0.009(7) 0.019(6) 0.001(6) C16 0.095(8) 0.080(8) 0.057(6) -0.012(6) 0.020(6) -0.035(7) C17 0.126(13) 0.098(12) 0.079(10) -0.021(8) 0.028(9) -0.019(10) C18 0.070(17) 0.07(2) 0.064(14) -0.009(13) 0.016(12) -0.020(15) C18' 0.065(18) 0.06(2) 0.065(15) -0.007(13) 0.007(12) -0.012(15) C19 0.068(8) 0.087(9) 0.071(7) 0.001(6) -0.009(6) -0.035(7) C20 0.081(9) 0.077(8) 0.105(10) 0.007(7) -0.020(7) -0.021(7) C21 0.057(7) 0.093(10) 0.116(11) -0.008(8) -0.008(7) -0.006(7) C22 0.077(8) 0.082(9) 0.090(9) -0.003(7) 0.006(7) -0.037(7) C23 0.077(8) 0.062(7) 0.092(9) -0.008(6) -0.019(7) -0.012(6) C24 0.068(7) 0.084(9) 0.076(8) -0.023(7) 0.005(6) -0.014(7) C25 0.077(7) 0.052(6) 0.053(6) 0.007(5) 0.000(5) -0.016(5) C26 0.097(9) 0.064(7) 0.064(7) 0.004(6) -0.011(6) -0.030(6) C27 0.091(9) 0.074(8) 0.080(8) 0.023(7) -0.002(7) -0.034(7) C28 0.081(8) 0.087(9) 0.075(8) 0.015(7) 0.024(6) -0.019(7) C29 0.077(7) 0.071(7) 0.070(7) 0.010(6) 0.029(6) -0.010(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 C1 1.967(8) . ? Pd1 N3 2.111(7) . ? Pd1 Br2 2.4256(12) . ? Pd1 Br1 2.4311(12) . ? N1 C1 1.332(9) . ? N1 C4 1.439(10) . ? N1 C3 1.478(10) . ? N2 C1 1.333(10) . ? N2 C16 1.452(11) . ? N2 C2' 1.48(4) . ? N2 C2 1.51(3) . ? N3 C25 1.317(11) . ? N3 C29 1.335(11) . ? O1 C17 1.43(2) . ? O1 H1 0.8200 . ? O1 H17D 1.0189 . ? O1' C17 1.39(3) . ? O1' H1' 0.8200 . ? C2 C18 1.53(6) . ? C2 C3 1.55(4) . ? C2 H2 0.9800 . ? C2' C3 1.52(4) . ? C2' C18' 1.53(6) . ? C2' H2' 0.9800 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.385(11) . ? C4 C9 1.409(11) . ? C5 C6 1.409(11) . ? C5 C10 1.506(12) . ? C6 C7 1.355(12) . ? C6 H6 0.9300 . ? C7 C8 1.379(13) . ? C7 H7 0.9300 . ? C8 C9 1.388(12) . ? C8 H8 0.9300 . ? C9 C13 1.519(12) . ? C10 C11 1.538(12) . ? C10 C12 1.559(13) . ? C10 H10 0.9800 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C15 1.526(12) . ? C13 C14 1.551(13) . ? C13 H13 0.9800 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 C17 1.515(16) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? C17 H17D 0.9700 . ? C18 C19 1.52(3) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18' C19 1.52(3) . ? C18' H18C 0.9700 . ? C18' H18D 0.9700 . ? C19 C24 1.347(16) . ? C19 C20 1.369(16) . ? C20 C21 1.375(16) . ? C20 H20 0.9300 . ? C21 C22 1.317(16) . ? C21 H21 0.9300 . ? C22 C23 1.351(15) . ? C22 H22 0.9300 . ? C23 C24 1.366(15) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 C26 1.384(13) . ? C25 H25 0.9300 . ? C26 C27 1.355(15) . ? C26 H26 0.9300 . ? C27 C28 1.374(16) . ? C27 H27 0.9300 . ? C28 C29 1.392(13) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? 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 C1 Pd1 N3 176.1(3) . . ? C1 Pd1 Br2 87.4(2) . . ? N3 Pd1 Br2 90.7(2) . . ? C1 Pd1 Br1 91.1(2) . . ? N3 Pd1 Br1 90.4(2) . . ? Br2 Pd1 Br1 173.91(5) . . ? C1 N1 C4 130.2(7) . . ? C1 N1 C3 110.6(7) . . ? C4 N1 C3 119.1(6) . . ? C1 N2 C16 125.8(7) . . ? C1 N2 C2' 113.3(15) . . ? C16 N2 C2' 120.4(15) . . ? C1 N2 C2 108.4(15) . . ? C16 N2 C2 122.0(15) . . ? C2' N2 C2 28.7(12) . . ? C25 N3 C29 118.3(8) . . ? C25 N3 Pd1 122.6(6) . . ? C29 N3 Pd1 119.1(7) . . ? C17 O1 H1 109.5 . . ? C17 O1 H17D 42.5 . . ? H1 O1 H17D 120.1 . . ? C17 O1' H1' 109.5 . . ? N1 C1 N2 109.8(7) . . ? N1 C1 Pd1 129.3(6) . . ? N2 C1 Pd1 120.9(6) . . ? N2 C2 C18 114(3) . . ? N2 C2 C3 98(2) . . ? C18 C2 C3 118(3) . . ? N2 C2 H2 108.9 . . ? C18 C2 H2 108.9 . . ? C3 C2 H2 108.9 . . ? N2 C2' C3 100(2) . . ? N2 C2' C18' 109(4) . . ? C3 C2' C18' 104(3) . . ? N2 C2' H2' 113.9 . . ? C3 C2' H2' 113.9 . . ? C18' C2' H2' 113.9 . . ? N1 C3 C2' 105.0(15) . . ? N1 C3 C2 100.0(15) . . ? C2' C3 C2 28.0(11) . . ? N1 C3 H3A 111.8 . . ? C2' C3 H3A 84.7 . . ? C2 C3 H3A 111.8 . . ? N1 C3 H3B 111.8 . . ? C2' C3 H3B 130.8 . . ? C2 C3 H3B 111.8 . . ? H3A C3 H3B 109.5 . . ? C5 C4 C9 122.3(7) . . ? C5 C4 N1 120.3(7) . . ? C9 C4 N1 117.1(8) . . ? C4 C5 C6 117.4(8) . . ? C4 C5 C10 124.5(8) . . ? C6 C5 C10 118.1(8) . . ? C7 C6 C5 121.2(9) . . ? C7 C6 H6 119.4 . . ? C5 C6 H6 119.4 . . ? C6 C7 C8 120.5(9) . . ? C6 C7 H7 119.8 . . ? C8 C7 H7 119.8 . . ? C7 C8 C9 121.3(9) . . ? C7 C8 H8 119.3 . . ? C9 C8 H8 119.3 . . ? C8 C9 C4 117.2(8) . . ? C8 C9 C13 119.4(8) . . ? C4 C9 C13 123.3(8) . . ? C5 C10 C11 112.6(8) . . ? C5 C10 C12 110.5(7) . . ? C11 C10 C12 111.0(8) . . ? C5 C10 H10 107.5 . . ? C11 C10 H10 107.5 . . ? C12 C10 H10 107.5 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C9 C13 C15 110.6(8) . . ? C9 C13 C14 111.6(8) . . ? C15 C13 C14 110.3(8) . . ? C9 C13 H13 108.1 . . ? C15 C13 H13 108.1 . . ? C14 C13 H13 108.1 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 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 . . ? N2 C16 C17 115.2(10) . . ? N2 C16 H16A 108.5 . . ? C17 C16 H16A 108.5 . . ? N2 C16 H16B 108.5 . . ? C17 C16 H16B 108.5 . . ? H16A C16 H16B 107.5 . . ? O1' C17 O1 65.2(14) . . ? O1' C17 C16 121.6(14) . . ? O1 C17 C16 115.3(13) . . ? O1' C17 H17A 43.8 . . ? O1 C17 H17A 108.5 . . ? C16 C17 H17A 108.5 . . ? O1' C17 H17B 127.3 . . ? O1 C17 H17B 108.5 . . ? C16 C17 H17B 108.5 . . ? H17A C17 H17B 107.5 . . ? O1' C17 H17C 106.5 . . ? O1 C17 H17C 133.4 . . ? C16 C17 H17C 107.7 . . ? H17A C17 H17C 72.3 . . ? H17B C17 H17C 37.7 . . ? O1' C17 H17D 107.2 . . ? O1 C17 H17D 45.2 . . ? C16 C17 H17D 106.4 . . ? H17A C17 H17D 143.6 . . ? H17B C17 H17D 70.1 . . ? H17C C17 H17D 106.4 . . ? C19 C18 C2 104(3) . . ? C19 C18 H18A 110.9 . . ? C2 C18 H18A 110.9 . . ? C19 C18 H18B 110.9 . . ? C2 C18 H18B 110.9 . . ? H18A C18 H18B 108.9 . . ? C19 C18' C2' 111(3) . . ? C19 C18' H18C 109.5 . . ? C2' C18' H18C 109.5 . . ? C19 C18' H18D 109.5 . . ? C2' C18' H18D 109.5 . . ? H18C C18' H18D 108.1 . . ? C24 C19 C20 115.8(11) . . ? C24 C19 C18 104(2) . . ? C20 C19 C18 140(2) . . ? C24 C19 C18' 141(2) . . ? C20 C19 C18' 103(2) . . ? C18 C19 C18' 37.5(10) . . ? C19 C20 C21 121.1(12) . . ? C19 C20 H20 119.4 . . ? C21 C20 H20 119.4 . . ? C22 C21 C20 121.2(13) . . ? C22 C21 H21 119.4 . . ? C20 C21 H21 119.4 . . ? C21 C22 C23 119.1(12) . . ? C21 C22 H22 120.5 . . ? C23 C22 H22 120.5 . . ? C22 C23 C24 119.7(12) . . ? C22 C23 H23 120.1 . . ? C24 C23 H23 120.1 . . ? C19 C24 C23 122.9(12) . . ? C19 C24 H24 118.6 . . ? C23 C24 H24 118.6 . . ? N3 C25 C26 122.3(10) . . ? N3 C25 H25 118.9 . . ? C26 C25 H25 118.9 . . ? C27 C26 C25 119.7(11) . . ? C27 C26 H26 120.2 . . ? C25 C26 H26 120.2 . . ? C26 C27 C28 119.1(11) . . ? C26 C27 H27 120.5 . . ? C28 C27 H27 120.5 . . ? C27 C28 C29 118.0(11) . . ? C27 C28 H28 121.0 . . ? C29 C28 H28 121.0 . . ? N3 C29 C28 122.6(11) . . ? N3 C29 H29 118.7 . . ? C28 C29 H29 118.7 . . ? 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 C1 Pd1 N3 C25 -112(5) . . . . ? Br2 Pd1 N3 C25 -51.8(7) . . . . ? Br1 Pd1 N3 C25 134.2(7) . . . . ? C1 Pd1 N3 C29 67(5) . . . . ? Br2 Pd1 N3 C29 127.6(7) . . . . ? Br1 Pd1 N3 C29 -46.4(7) . . . . ? C4 N1 C1 N2 -179.0(8) . . . . ? C3 N1 C1 N2 -3.5(10) . . . . ? C4 N1 C1 Pd1 4.1(13) . . . . ? C3 N1 C1 Pd1 179.5(7) . . . . ? C16 N2 C1 N1 -178.6(9) . . . . ? C2' N2 C1 N1 10(2) . . . . ? C2 N2 C1 N1 -21(2) . . . . ? C16 N2 C1 Pd1 -1.4(13) . . . . ? C2' N2 C1 Pd1 -173(2) . . . . ? C2 N2 C1 Pd1 156.6(19) . . . . ? N3 Pd1 C1 N1 151(4) . . . . ? Br2 Pd1 C1 N1 90.7(8) . . . . ? Br1 Pd1 C1 N1 -95.2(8) . . . . ? N3 Pd1 C1 N2 -25(5) . . . . ? Br2 Pd1 C1 N2 -86.0(7) . . . . ? Br1 Pd1 C1 N2 88.1(7) . . . . ? C1 N2 C2 C18 159(3) . . . . ? C16 N2 C2 C18 -42(5) . . . . ? C2' N2 C2 C18 54(5) . . . . ? C1 N2 C2 C3 34(3) . . . . ? C16 N2 C2 C3 -166.9(12) . . . . ? C2' N2 C2 C3 -71(5) . . . . ? C1 N2 C2' C3 -11(3) . . . . ? C16 N2 C2' C3 176.7(14) . . . . ? C2 N2 C2' C3 75(5) . . . . ? C1 N2 C2' C18' -120(3) . . . . ? C16 N2 C2' C18' 67(4) . . . . ? C2 N2 C2' C18' -34(5) . . . . ? C1 N1 C3 C2' -4(2) . . . . ? C4 N1 C3 C2' 172(2) . . . . ? C1 N1 C3 C2 24.7(19) . . . . ? C4 N1 C3 C2 -159.3(18) . . . . ? N2 C2' C3 N1 8(3) . . . . ? C18' C2' C3 N1 121(3) . . . . ? N2 C2' C3 C2 -75(5) . . . . ? C18' C2' C3 C2 38(5) . . . . ? N2 C2 C3 N1 -33(2) . . . . ? C18 C2 C3 N1 -155(3) . . . . ? N2 C2 C3 C2' 70(5) . . . . ? C18 C2 C3 C2' -52(5) . . . . ? C1 N1 C4 C5 88.1(11) . . . . ? C3 N1 C4 C5 -87.0(10) . . . . ? C1 N1 C4 C9 -98.5(10) . . . . ? C3 N1 C4 C9 86.4(10) . . . . ? C9 C4 C5 C6 2.1(12) . . . . ? N1 C4 C5 C6 175.1(7) . . . . ? C9 C4 C5 C10 -176.1(8) . . . . ? N1 C4 C5 C10 -3.1(12) . . . . ? C4 C5 C6 C7 -1.6(13) . . . . ? C10 C5 C6 C7 176.8(8) . . . . ? C5 C6 C7 C8 0.4(14) . . . . ? C6 C7 C8 C9 0.2(14) . . . . ? C7 C8 C9 C4 0.3(13) . . . . ? C7 C8 C9 C13 -176.7(8) . . . . ? C5 C4 C9 C8 -1.5(12) . . . . ? N1 C4 C9 C8 -174.7(7) . . . . ? C5 C4 C9 C13 175.3(8) . . . . ? N1 C4 C9 C13 2.1(11) . . . . ? C4 C5 C10 C11 -131.6(9) . . . . ? C6 C5 C10 C11 50.2(10) . . . . ? C4 C5 C10 C12 103.6(10) . . . . ? C6 C5 C10 C12 -74.7(10) . . . . ? C8 C9 C13 C15 72.5(11) . . . . ? C4 C9 C13 C15 -104.3(10) . . . . ? C8 C9 C13 C14 -50.7(11) . . . . ? C4 C9 C13 C14 132.5(9) . . . . ? C1 N2 C16 C17 -103.3(13) . . . . ? C2' N2 C16 C17 68(3) . . . . ? C2 N2 C16 C17 101(2) . . . . ? N2 C16 C17 O1' 23(2) . . . . ? N2 C16 C17 O1 -52.6(18) . . . . ? N2 C2 C18 C19 179.9(19) . . . . ? C3 C2 C18 C19 -66(5) . . . . ? N2 C2' C18' C19 -175.1(18) . . . . ? C3 C2' C18' C19 79(4) . . . . ? C2 C18 C19 C24 135(3) . . . . ? C2 C18 C19 C20 -45(4) . . . . ? C2 C18 C19 C18' -36(3) . . . . ? C2' C18' C19 C24 38(4) . . . . ? C2' C18' C19 C20 -135(3) . . . . ? C2' C18' C19 C18 51(3) . . . . ? C24 C19 C20 C21 4.4(18) . . . . ? C18 C19 C20 C21 -175.1(18) . . . . ? C18' C19 C20 C21 179.2(14) . . . . ? C19 C20 C21 C22 -5(2) . . . . ? C20 C21 C22 C23 2(2) . . . . ? C21 C22 C23 C24 -0.4(18) . . . . ? C20 C19 C24 C23 -2.4(17) . . . . ? C18 C19 C24 C23 177.3(13) . . . . ? C18' C19 C24 C23 -174.4(19) . . . . ? C22 C23 C24 C19 0.4(18) . . . . ? C29 N3 C25 C26 -1.0(15) . . . . ? Pd1 N3 C25 C26 178.4(7) . . . . ? N3 C25 C26 C27 1.5(16) . . . . ? C25 C26 C27 C28 -2.6(17) . . . . ? C26 C27 C28 C29 3.1(18) . . . . ? C25 N3 C29 C28 1.6(15) . . . . ? Pd1 N3 C29 C28 -177.8(8) . . . . ? C27 C28 C29 N3 -2.7(17) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.818 _refine_diff_density_min -0.845 _refine_diff_density_rms 0.105