# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1666 data_global # 1. SUBMISSION DETAILS _publ_contact_author ; Dr Andreas A Danopoulos Department of Chemistry Southampton University Highfield Southampton SO17 1BJ United Kingdom ; _publ_contact_author_phone '044 2380 594116' _publ_contact_author_fax '044 2380 596805' _publ_contact_author_email a.danopoulos@soton.ac.uk _publ_requested_journal 'Chemical Communications' _publ_requested_coeditor_name ; Arran A D Tulloch Sean M Cafferkey Sven Kleinhenz Michael B Hoursthouse Robert Tooze ; _publ_contact_letter ; ? ; #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Pyridine functionalised N-heterocyclic carbene complexes of Palladium ; loop_ _publ_author_name _publ_author_address 'Danopoulos, Andreas' ; Chemistry Department Department of Chemistry Southampton University Highfield Southampton SO17 1BJ United Kingdom ; #============================================================================== # 4. TEXT _publ_section_abstract ; ; _publ_section_comment ; ; _publ_section_experimental ; ; _publ_section_exptl_prep ; ; _publ_section_exptl_refinement ; ; _publ_section_references ; ; _publ_section_figure_captions ; ; _publ_section_acknowledgements ; ; #============================================================================== data_monomer _audit_creation_method SHELXL-97 _chemical_name_systematic ; (3-mesityl-1-(2-picolyl)-imidazolin-2-ylidene) palladium methyl bromide ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H22 Br N3 Pd' _chemical_formula_weight 478.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 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' '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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 24.521(4) _cell_length_b 24.521(4) _cell_length_c 20.201(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 10519(3) _cell_formula_units_Z 18 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 14346 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 26.373 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.360 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4284 _exptl_absorpt_coefficient_mu 2.507 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_process_details 'Sortav (Blessing, 1995,1997) ' _exptl_absorpt_correction_T_max 1.033 _exptl_absorpt_correction_T_min 0.960 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enraf Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf Nonius KappaCCD area detector' _diffrn_measurement_method '\p and \q scans to fill Ewald sphere' _diffrn_detector_area_resol_mean '9.091 pixels/mm' _diffrn_standards_number 'n/a' _diffrn_standards_interval_count 'n/a' _diffrn_standards_interval_time 'n/a' _diffrn_standards_decay_% 'n/a' _diffrn_reflns_number 25874 _diffrn_reflns_av_R_equivalents 0.0467 _diffrn_reflns_av_sigmaI/netI 0.0440 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 26.37 _reflns_number_total 4782 _reflns_number_gt 3712 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; DENZO (Otwinowski and minor, 1997) Collect (Hooft, 1998) ; _computing_cell_refinement 'DENZO and COLLECT' _computing_data_reduction 'DENZO and COLLECT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (L.J.Farrugia 1997)' _computing_publication_material 'PLATON (Spek, 1990)' _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. Fluent solvent (Dichloromethane) located in channels along the c axis was treated in the manner described by van der Sluis and Spek (Van der Sluis and Spek, 1990). ; _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^)+(0.0605P)^2^+14.8281P] 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 4782 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0636 _refine_ls_R_factor_gt 0.0439 _refine_ls_wR_factor_ref 0.1142 _refine_ls_wR_factor_gt 0.1072 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.687536(15) 0.055171(14) 0.058766(13) 0.04147(13) Uani 1 1 d . . . Br1 Br 0.73625(2) 0.157731(19) 0.119130(19) 0.05435(16) Uani 1 1 d . . . C1 C 0.65182(19) -0.02638(19) 0.01331(18) 0.0447(9) Uani 1 1 d . . . C10 C 0.59517(15) 0.03999(15) 0.08000(14) 0.0267(7) Uani 1 1 d . . . H10A H 0.5634 -0.0002 0.0609 0.040 Uiso 1 1 calc R . . H10B H 0.5907 0.0742 0.0608 0.040 Uiso 1 1 calc R . . H10C H 0.5892 0.0391 0.1281 0.040 Uiso 1 1 calc R . . C5 C 0.7849(2) 0.05334(18) -0.03614(18) 0.0468(10) Uani 1 1 d . . . N1 N 0.61038(16) -0.08649(15) 0.03003(17) 0.0469(8) Uani 1 1 d . . . N2 N 0.67548(16) -0.03034(15) -0.04594(15) 0.0451(8) Uani 1 1 d . . . N3 N 0.77887(16) 0.06978(15) 0.02662(15) 0.0474(8) Uani 1 1 d . . . C3 C 0.6494(2) -0.0926(2) -0.0662(2) 0.0549(11) Uani 1 1 d . . . H3A H 0.6585 -0.1073 -0.1058 0.066 Uiso 1 1 calc R . . C9 C 0.8294(2) 0.0946(2) 0.0657(2) 0.0559(11) Uani 1 1 d . . . H9A H 0.8252 0.1056 0.1097 0.067 Uiso 1 1 calc R . . C2 C 0.6090(2) -0.1275(2) -0.0190(2) 0.0597(12) Uani 1 1 d . . . H2A H 0.5839 -0.1721 -0.0188 0.072 Uiso 1 1 calc R . . C4 C 0.7270(2) 0.0243(2) -0.07878(19) 0.0504(10) Uani 1 1 d . . . H4A H 0.7141 0.0558 -0.0881 0.060 Uiso 1 1 calc R . . H4B H 0.7366 0.0111 -0.1215 0.060 Uiso 1 1 calc R . . C7 C 0.8941(2) 0.0898(3) -0.0191(2) 0.0761(16) Uani 1 1 d . . . H7A H 0.9336 0.0970 -0.0350 0.091 Uiso 1 1 calc R . . C8 C 0.8880(2) 0.1054(3) 0.0453(2) 0.0739(15) Uani 1 1 d . . . H8A H 0.9229 0.1229 0.0747 0.089 Uiso 1 1 calc R . . C6 C 0.8423(2) 0.0638(2) -0.0597(2) 0.0590(12) Uani 1 1 d . . . H6A H 0.8458 0.0530 -0.1040 0.071 Uiso 1 1 calc R . . C11 C 0.57525(19) -0.10626(18) 0.0903(2) 0.0461(10) Uani 1 1 d . . . C12 C 0.6055(2) -0.10627(19) 0.1484(2) 0.0501(10) Uani 1 1 d . . . C14 C 0.5075(2) -0.1414(2) 0.2075(2) 0.0527(11) Uani 1 1 d . . . C13 C 0.5701(2) -0.1241(2) 0.2064(2) 0.0555(11) Uani 1 1 d . . . H13A H 0.5900 -0.1244 0.2467 0.067 Uiso 1 1 calc R . . C16 C 0.5113(2) -0.1256(2) 0.0888(2) 0.0557(11) Uani 1 1 d . . . C15 C 0.4792(2) -0.1428(2) 0.1482(2) 0.0578(12) Uani 1 1 d . . . H15A H 0.4355 -0.1562 0.1482 0.069 Uiso 1 1 calc R . . C17 C 0.6745(2) -0.0872(3) 0.1503(3) 0.0699(14) Uani 1 1 d . . . H17A H 0.6924 -0.0752 0.1057 0.105 Uiso 1 1 calc R . . H17B H 0.6788 -0.1227 0.1660 0.105 Uiso 1 1 calc R . . H17C H 0.6970 -0.0513 0.1803 0.105 Uiso 1 1 calc R . . C18 C 0.4695(3) -0.1605(3) 0.2713(3) 0.0760(15) Uani 1 1 d . . . H18A H 0.4969 -0.1568 0.3084 0.114 Uiso 1 1 calc R . . H18B H 0.4351 -0.2042 0.2677 0.114 Uiso 1 1 calc R . . H18C H 0.4520 -0.1328 0.2789 0.114 Uiso 1 1 calc R . . C19 C 0.4787(3) -0.1259(3) 0.0251(3) 0.0796(15) Uani 1 1 d . . . H19A H 0.5090 -0.1122 -0.0114 0.119 Uiso 1 1 calc R . . H19B H 0.4621 -0.0971 0.0293 0.119 Uiso 1 1 calc R . . H19C H 0.4441 -0.1686 0.0164 0.119 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 0.0510(2) 0.0377(2) 0.03037(18) -0.00383(12) 0.00422(12) 0.01816(15) Br1 0.0678(3) 0.0403(3) 0.0381(2) -0.00660(16) 0.01362(19) 0.0145(2) C1 0.048(2) 0.048(2) 0.040(2) -0.0049(18) -0.0039(18) 0.025(2) C10 0.0372(19) 0.0215(16) 0.0164(14) -0.0020(12) -0.0014(13) 0.0108(15) C5 0.062(3) 0.036(2) 0.035(2) -0.0010(17) 0.0065(19) 0.019(2) N1 0.047(2) 0.0364(19) 0.052(2) -0.0086(15) -0.0015(16) 0.0167(16) N2 0.052(2) 0.0437(19) 0.0357(17) -0.0093(14) -0.0025(15) 0.0209(17) N3 0.054(2) 0.0431(19) 0.0355(17) -0.0063(14) 0.0064(16) 0.0168(17) C3 0.062(3) 0.046(3) 0.052(3) -0.019(2) -0.010(2) 0.023(2) C9 0.048(3) 0.060(3) 0.042(2) -0.018(2) 0.002(2) 0.013(2) C2 0.063(3) 0.043(2) 0.061(3) -0.016(2) 0.000(2) 0.017(2) C4 0.062(3) 0.055(3) 0.033(2) -0.0051(18) 0.0031(19) 0.028(2) C7 0.051(3) 0.092(4) 0.065(3) -0.026(3) 0.013(2) 0.020(3) C8 0.047(3) 0.093(4) 0.057(3) -0.024(3) 0.003(2) 0.016(3) C6 0.064(3) 0.061(3) 0.042(2) -0.009(2) 0.014(2) 0.024(2) C11 0.049(2) 0.033(2) 0.051(2) -0.0038(18) 0.003(2) 0.0167(19) C12 0.046(2) 0.043(2) 0.061(3) 0.004(2) 0.001(2) 0.021(2) C14 0.058(3) 0.044(2) 0.059(3) 0.002(2) 0.008(2) 0.028(2) C13 0.062(3) 0.053(3) 0.055(3) 0.005(2) -0.002(2) 0.031(2) C16 0.053(3) 0.049(3) 0.059(3) -0.003(2) 0.002(2) 0.020(2) C15 0.044(2) 0.050(3) 0.074(3) 0.003(2) 0.009(2) 0.020(2) C17 0.056(3) 0.082(4) 0.072(3) 0.012(3) -0.001(2) 0.035(3) C18 0.087(4) 0.092(4) 0.067(3) 0.008(3) 0.022(3) 0.058(3) C19 0.061(3) 0.098(4) 0.069(3) -0.009(3) -0.010(3) 0.032(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C1 1.964(4) . ? Pd1 C10 2.147(3) . ? Pd1 N3 2.183(3) . ? Pd1 Br1 2.4969(6) . ? C1 N1 1.350(5) . ? C1 N2 1.355(5) . ? C5 N3 1.360(5) . ? C5 C6 1.382(6) . ? C5 C4 1.501(6) . ? N1 C2 1.400(5) . ? N1 C11 1.429(5) . ? N2 C3 1.389(5) . ? N2 C4 1.462(5) . ? N3 C9 1.333(5) . ? C3 C2 1.331(6) . ? C9 C8 1.386(6) . ? C7 C6 1.372(7) . ? C7 C8 1.385(6) . ? C11 C12 1.388(6) . ? C11 C16 1.394(6) . ? C12 C13 1.393(6) . ? C12 C17 1.515(6) . ? C14 C13 1.373(6) . ? C14 C15 1.378(6) . ? C14 C18 1.520(6) . ? C16 C15 1.380(6) . ? C16 C19 1.512(7) . ? 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 C10 91.27(15) . . ? C1 Pd1 N3 85.79(14) . . ? C10 Pd1 N3 174.21(11) . . ? C1 Pd1 Br1 177.46(12) . . ? C10 Pd1 Br1 90.51(8) . . ? N3 Pd1 Br1 92.59(8) . . ? N1 C1 N2 105.0(3) . . ? N1 C1 Pd1 134.7(3) . . ? N2 C1 Pd1 119.8(3) . . ? N3 C5 C6 121.1(4) . . ? N3 C5 C4 117.3(4) . . ? C6 C5 C4 121.6(3) . . ? C1 N1 C2 110.0(3) . . ? C1 N1 C11 125.5(3) . . ? C2 N1 C11 124.5(3) . . ? C1 N2 C3 111.1(3) . . ? C1 N2 C4 122.7(3) . . ? C3 N2 C4 125.8(3) . . ? C9 N3 C5 118.2(4) . . ? C9 N3 Pd1 122.9(3) . . ? C5 N3 Pd1 118.9(3) . . ? C2 C3 N2 106.4(4) . . ? N3 C9 C8 123.4(4) . . ? C3 C2 N1 107.6(4) . . ? N2 C4 C5 110.7(3) . . ? C6 C7 C8 119.1(4) . . ? C7 C8 C9 118.1(4) . . ? C7 C6 C5 120.1(4) . . ? C12 C11 C16 121.9(4) . . ? C12 C11 N1 119.3(4) . . ? C16 C11 N1 118.8(4) . . ? C11 C12 C13 117.6(4) . . ? C11 C12 C17 122.4(4) . . ? C13 C12 C17 120.0(4) . . ? C13 C14 C15 117.8(4) . . ? C13 C14 C18 121.9(4) . . ? C15 C14 C18 120.3(4) . . ? C14 C13 C12 122.4(4) . . ? C15 C16 C11 117.3(4) . . ? C15 C16 C19 121.3(4) . . ? C11 C16 C19 121.4(4) . . ? C14 C15 C16 123.0(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 C10 Pd1 C1 N1 -54.9(4) . . . . ? N3 Pd1 C1 N1 130.1(4) . . . . ? Br1 Pd1 C1 N1 80(3) . . . . ? C10 Pd1 C1 N2 134.3(3) . . . . ? N3 Pd1 C1 N2 -40.7(3) . . . . ? Br1 Pd1 C1 N2 -91(3) . . . . ? N2 C1 N1 C2 0.4(5) . . . . ? Pd1 C1 N1 C2 -171.3(4) . . . . ? N2 C1 N1 C11 177.4(4) . . . . ? Pd1 C1 N1 C11 5.7(7) . . . . ? N1 C1 N2 C3 -0.4(4) . . . . ? Pd1 C1 N2 C3 172.9(3) . . . . ? N1 C1 N2 C4 -173.8(4) . . . . ? Pd1 C1 N2 C4 -0.5(5) . . . . ? C6 C5 N3 C9 -1.9(6) . . . . ? C4 C5 N3 C9 178.8(4) . . . . ? C6 C5 N3 Pd1 177.6(3) . . . . ? C4 C5 N3 Pd1 -1.7(5) . . . . ? C1 Pd1 N3 C9 -137.9(4) . . . . ? C10 Pd1 N3 C9 162.5(11) . . . . ? Br1 Pd1 N3 C9 40.1(3) . . . . ? C1 Pd1 N3 C5 42.6(3) . . . . ? C10 Pd1 N3 C5 -17.0(14) . . . . ? Br1 Pd1 N3 C5 -139.3(3) . . . . ? C1 N2 C3 C2 0.1(5) . . . . ? C4 N2 C3 C2 173.3(4) . . . . ? C5 N3 C9 C8 0.9(7) . . . . ? Pd1 N3 C9 C8 -178.6(4) . . . . ? N2 C3 C2 N1 0.1(5) . . . . ? C1 N1 C2 C3 -0.4(5) . . . . ? C11 N1 C2 C3 -177.4(4) . . . . ? C1 N2 C4 C5 59.9(5) . . . . ? C3 N2 C4 C5 -112.6(4) . . . . ? N3 C5 C4 N2 -54.2(5) . . . . ? C6 C5 C4 N2 126.5(4) . . . . ? C6 C7 C8 C9 -0.9(9) . . . . ? N3 C9 C8 C7 0.5(8) . . . . ? C8 C7 C6 C5 -0.1(8) . . . . ? N3 C5 C6 C7 1.6(7) . . . . ? C4 C5 C6 C7 -179.2(5) . . . . ? C1 N1 C11 C12 -75.1(5) . . . . ? C2 N1 C11 C12 101.5(5) . . . . ? C1 N1 C11 C16 105.5(5) . . . . ? C2 N1 C11 C16 -78.0(5) . . . . ? C16 C11 C12 C13 -2.4(6) . . . . ? N1 C11 C12 C13 178.2(4) . . . . ? C16 C11 C12 C17 178.2(4) . . . . ? N1 C11 C12 C17 -1.2(6) . . . . ? C15 C14 C13 C12 2.2(7) . . . . ? C18 C14 C13 C12 -179.7(4) . . . . ? C11 C12 C13 C14 0.1(6) . . . . ? C17 C12 C13 C14 179.5(4) . . . . ? C12 C11 C16 C15 2.2(6) . . . . ? N1 C11 C16 C15 -178.3(4) . . . . ? C12 C11 C16 C19 -179.5(4) . . . . ? N1 C11 C16 C19 0.0(6) . . . . ? C13 C14 C15 C16 -2.3(7) . . . . ? C18 C14 C15 C16 179.5(4) . . . . ? C11 C16 C15 C14 0.2(7) . . . . ? C19 C16 C15 C14 -178.1(5) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.837 _refine_diff_density_min -0.714 _refine_diff_density_rms 0.105 #===END data_tetramer _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H80 F12 N12 O8 Pd4 [C4 H8 O1]x' _chemical_formula_sum 'C68 H89 F12 N12 O9 Pd4' _chemical_formula_weight 1872.11 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' '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.852(2) _cell_length_b 20.026(4) _cell_length_c 21.056(4) _cell_angle_alpha 89.95(3) _cell_angle_beta 90.19(3) _cell_angle_gamma 90.04(3) _cell_volume 4154.2(14) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour 'clear, colourless' _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.025 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.497 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1890 _exptl_absorpt_coefficient_mu 0.935 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK/a _diffrn_radiation_source 'Enraf Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf Nonius KappaCCD area detector' _diffrn_measurement_method '\p and \q scans to fill Ewald sphere' _diffrn_detector_area_resol_mean '9.091 pixels/mm' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34221 _diffrn_reflns_av_R_equivalents 0.2498 _diffrn_reflns_av_sigmaI/netI 0.3118 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 22.50 _reflns_number_total 10208 _reflns_number_gt 3896 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DENZO (Otwinowski and minor, 1997) Collect (Hooft, 1998)' _computing_cell_refinement 'DENZO AND COLLECT' _computing_data_reduction 'DENZO AND COLLECT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1435P)^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 10208 _refine_ls_number_parameters 1007 _refine_ls_number_restraints 78 _refine_ls_R_factor_all 0.2650 _refine_ls_R_factor_gt 0.1095 _refine_ls_wR_factor_ref 0.3230 _refine_ls_wR_factor_gt 0.2539 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.880 _refine_ls_shift/su_mean 0.056 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 O01 O 0.592(3) 0.2590(15) 0.2511(14) 0.037(9) Uani 0.50 1 d P . . C01 C 0.551(9) 0.722(4) 0.666(5) 0.15(4) Uani 0.50 1 d P . . H01A H 0.5822 0.6791 0.6502 0.174 Uiso 0.50 1 calc PR . . H01B H 0.5529 0.7538 0.6315 0.174 Uiso 0.50 1 calc PR . . C02 C 0.582(7) 0.284(3) 0.311(3) 0.09(2) Uani 0.50 1 d P . . H02A H 0.6072 0.3311 0.3101 0.104 Uiso 0.50 1 calc PR . . H02B H 0.6436 0.2609 0.3387 0.104 Uiso 0.50 1 calc PR . . C03 C 0.450(12) 1.254(3) 0.242(4) 0.21(8) Uani 0.50 1 d P . . H03A H 0.4238 1.2892 0.2119 0.246 Uiso 0.50 1 calc PR . . H03B H 0.4310 1.2119 0.2215 0.246 Uiso 0.50 1 calc PR . . C04 C 0.625(7) 0.741(3) 0.709(3) 0.09(3) Uani 0.50 1 d P . . H04A H 0.6648 0.7835 0.6984 0.107 Uiso 0.50 1 calc PR . . H04B H 0.6971 0.7086 0.7161 0.107 Uiso 0.50 1 calc PR . . O02 O 1.008(5) 0.733(3) 0.704(2) 0.105(19) Uani 0.50 1 d P . . H02C H 0.9096 0.7287 0.7012 0.126 Uiso 0.50 1 calc PR . . H02D H 1.0438 0.7216 0.6622 0.126 Uiso 0.50 1 calc PR . . C05 C 1.044(5) 0.697(3) 0.737(4) 0.07(2) Uani 0.50 1 d P . . H05A H 1.1259 0.6721 0.7278 0.080 Uiso 0.50 1 calc PR . . H05B H 0.9837 0.6796 0.7691 0.080 Uiso 0.50 1 calc PR . . C06 C 1.039(5) 0.735(4) -0.204(2) 0.07(2) Uani 0.50 1 d P . . H06A H 1.1145 0.7237 -0.1763 0.087 Uiso 0.50 1 calc PR . . H06B H 0.9542 0.7277 -0.1820 0.087 Uiso 0.50 1 calc PR . . C07 C 0.949(7) 1.196(4) 0.231(4) 0.11(3) Uani 0.50 1 d P . . H07A H 0.8611 1.1756 0.2238 0.135 Uiso 0.50 1 calc PR . . H07B H 1.0208 1.1662 0.2165 0.135 Uiso 0.50 1 calc PR . . C08 C 1.035(7) 0.786(4) 0.715(3) 0.09(3) Uani 0.50 1 d P . . H08A H 0.9639 0.8141 0.6967 0.108 Uiso 0.50 1 calc PR . . H08B H 1.1175 0.7965 0.6923 0.108 Uiso 0.50 1 calc PR . . Pd1 Pd 0.57063(18) 0.63872(10) 0.11517(9) 0.0453(6) Uani 1 1 d . . . Pd2 Pd 0.94347(18) 0.59337(10) 0.35407(8) 0.0434(6) Uani 1 1 d . . . Pd3 Pd 0.57515(18) 0.86223(10) 0.38382(9) 0.0458(6) Uani 1 1 d . . . Pd4 Pd 0.94267(18) 0.90801(10) 0.14453(8) 0.0442(6) Uani 1 1 d . . . F1 F 0.7853(17) 0.5254(10) -0.0584(7) 0.083(6) Uani 1 1 d . . . F2 F 0.7921(16) 0.6256(11) -0.0903(7) 0.104(7) Uani 1 1 d . . . F3 F 0.9618(18) 0.5871(10) -0.0477(8) 0.113(7) Uani 1 1 d . . . F4 F 0.5440(13) 0.4380(10) 0.4258(9) 0.121(8) Uani 1 1 d . . . F5 F 0.6945(19) 0.4512(11) 0.4895(8) 0.128(8) Uani 1 1 d . . . F6 F 0.7225(19) 0.3860(8) 0.4161(10) 0.131(8) Uani 1 1 d . . . F7 F 0.7910(17) 0.8770(10) 0.5882(7) 0.104(6) Uani 1 1 d . . . F8 F 0.7893(15) 0.9771(8) 0.5606(6) 0.080(5) Uani 1 1 d . . . F9 F 0.9704(16) 0.9184(9) 0.5488(7) 0.100(6) Uani 1 1 d . . . F10 F 0.721(3) 1.1142(11) 0.093(2) 0.26(2) Uani 1 1 d . . . F11 F 0.5516(17) 1.0720(12) 0.0783(15) 0.216(15) Uani 1 1 d . . . F12 F 0.705(3) 1.067(2) 0.0229(15) 0.28(2) Uani 1 1 d . . . O1 O 0.6465(19) 0.6144(9) 0.0216(7) 0.055(5) Uani 1 1 d . . . O2 O 0.8573(19) 0.6192(9) 0.0630(10) 0.076(6) Uani 1 1 d . . . O3 O 0.6537(14) 0.5352(9) 0.3673(8) 0.064(5) Uani 1 1 d . . . O4 O 0.8583(14) 0.4988(8) 0.3951(7) 0.050(5) Uani 1 1 d . . . O5 O 0.6484(14) 0.8917(8) 0.4756(7) 0.052(5) Uani 1 1 d . . . O6 O 0.8632(15) 0.8864(9) 0.4364(7) 0.060(5) Uani 1 1 d . . . O7 O 0.8613(14) 1.0002(8) 0.1059(6) 0.052(5) Uani 1 1 d . . . O8 O 0.6546(16) 0.9657(8) 0.1305(8) 0.062(5) Uani 1 1 d . . . N1 N 0.373(2) 0.7428(12) 0.0682(10) 0.055(6) Uani 1 1 d . . . N2 N 0.560(2) 0.7845(13) 0.0977(10) 0.060(7) Uani 1 1 d . . . N3 N 0.888(2) 0.8613(10) 0.0649(10) 0.062(7) Uani 1 1 d . . . N4 N 0.6176(18) 0.5408(10) 0.1457(8) 0.054(6) Uani 1 1 d . . . N5 N 0.9513(18) 0.5540(10) 0.2224(9) 0.066(7) Uani 1 1 d . . . N6 N 1.1277(17) 0.5217(10) 0.2604(9) 0.051(6) Uani 1 1 d . . . N7 N 0.8822(16) 0.6426(9) 0.4370(8) 0.039(5) Uani 1 1 d . . . N8 N 0.5673(17) 0.7182(10) 0.4074(9) 0.049(6) Uani 1 1 d . . . N9 N 0.3790(18) 0.7592(10) 0.4360(9) 0.058(6) Uani 1 1 d . . . N10 N 0.6194(17) 0.9580(10) 0.3498(8) 0.052(6) Uani 1 1 d . . . N11 N 0.9503(17) 0.9502(11) 0.2773(8) 0.055(6) Uani 1 1 d . . . N12 N 1.1235(18) 0.9839(10) 0.2326(8) 0.049(6) Uani 1 1 d . . . C1 C 0.516(3) 0.6630(12) 0.2086(12) 0.085(11) Uani 1 1 d . . . H1A H 0.4508 0.6984 0.2080 0.128 Uiso 1 1 calc R . . H1B H 0.5955 0.6772 0.2316 0.128 Uiso 1 1 calc R . . H1C H 0.4780 0.6244 0.2289 0.128 Uiso 1 1 calc R . . C2 C 0.765(4) 0.6093(14) 0.0208(14) 0.058(9) Uani 1 1 d . . . C3 C 0.833(3) 0.583(2) -0.0451(13) 0.068(10) Uani 1 1 d . . . C4 C 0.492(3) 0.7253(13) 0.0928(11) 0.042(7) Uani 1 1 d U . . C5 C 0.366(3) 0.8141(15) 0.0638(13) 0.067(9) Uani 1 1 d U . . H5 H 0.2905 0.8389 0.0512 0.080 Uiso 1 1 calc R . . C6 C 0.476(3) 0.8361(16) 0.0797(15) 0.084(11) Uani 1 1 d . . . H6 H 0.5003 0.8810 0.0796 0.101 Uiso 1 1 calc R . . C7 C 0.264(3) 0.6955(16) 0.0512(15) 0.076(10) Uani 1 1 d . . . C8 C 0.319(3) 0.6487(14) 0.0031(13) 0.081(10) Uani 1 1 d . . . H8A H 0.2597 0.6474 -0.0330 0.121 Uiso 1 1 calc R . . H8B H 0.3264 0.6049 0.0213 0.121 Uiso 1 1 calc R . . H8C H 0.4073 0.6638 -0.0099 0.121 Uiso 1 1 calc R . . C9 C 0.145(3) 0.7305(16) 0.0203(13) 0.086(11) Uani 1 1 d . . . H9A H 0.1148 0.7660 0.0472 0.130 Uiso 1 1 calc R . . H9B H 0.0729 0.6992 0.0137 0.130 Uiso 1 1 calc R . . H9C H 0.1733 0.7485 -0.0199 0.130 Uiso 1 1 calc R . . C10 C 0.209(3) 0.6566(14) 0.1112(13) 0.093(10) Uani 1 1 d U . . H10A H 0.2842 0.6441 0.1378 0.140 Uiso 1 1 calc R . . H10B H 0.1617 0.6172 0.0976 0.140 Uiso 1 1 calc R . . H10C H 0.1485 0.6848 0.1346 0.140 Uiso 1 1 calc R . . C11 C 0.705(2) 0.7913(14) 0.1127(11) 0.070(9) Uani 1 1 d . . . H11A H 0.7391 0.7492 0.1292 0.085 Uiso 1 1 calc R . . H11B H 0.7170 0.8248 0.1455 0.085 Uiso 1 1 calc R . . C12 C 0.788(2) 0.8110(12) 0.0551(12) 0.053(8) Uani 1 1 d . . . C13 C 0.759(3) 0.7813(16) -0.0038(13) 0.078(10) Uani 1 1 d . . . H13 H 0.6917 0.7488 -0.0071 0.094 Uiso 1 1 calc R . . C14 C 0.831(3) 0.8008(17) -0.0568(13) 0.088(11) Uani 1 1 d . . . H14 H 0.8158 0.7807 -0.0960 0.106 Uiso 1 1 calc R . . C15 C 0.928(3) 0.8513(14) -0.0504(12) 0.054(7) Uani 1 1 d U . . H15 H 0.9801 0.8647 -0.0849 0.065 Uiso 1 1 calc R . . C16 C 0.945(2) 0.8804(14) 0.0074(12) 0.062(8) Uani 1 1 d . . . H16 H 1.0014 0.9176 0.0086 0.075 Uiso 1 1 calc R . . C17 C 0.709(3) 0.5220(15) 0.1880(10) 0.051(8) Uani 1 1 d . . . C18 C 0.722(3) 0.4561(15) 0.2114(13) 0.063(9) Uani 1 1 d . . . H18 H 0.7823 0.4451 0.2438 0.075 Uiso 1 1 calc R . . C19 C 0.643(4) 0.4115(14) 0.1844(14) 0.074(10) Uani 1 1 d . . . H19 H 0.6526 0.3673 0.1971 0.089 Uiso 1 1 calc R . . C20 C 0.546(3) 0.4260(14) 0.1374(14) 0.064(9) Uani 1 1 d . . . H20 H 0.4897 0.3937 0.1193 0.076 Uiso 1 1 calc R . . C21 C 0.540(2) 0.4916(13) 0.1209(12) 0.057(8) Uani 1 1 d . . . H21 H 0.4782 0.5036 0.0896 0.068 Uiso 1 1 calc R . . C22 C 0.808(2) 0.5791(13) 0.2102(11) 0.063(9) Uani 1 1 d . . . H22A H 0.8101 0.6136 0.1779 0.075 Uiso 1 1 calc R . . H22B H 0.7725 0.5989 0.2488 0.075 Uiso 1 1 calc R . . C23 C 1.019(3) 0.5230(13) 0.1712(13) 0.061(8) Uani 1 1 d . . . H23 H 0.9868 0.5149 0.1303 0.073 Uiso 1 1 calc R . . C24 C 1.134(3) 0.5091(15) 0.1951(11) 0.072(10) Uani 1 1 d . . . H24 H 1.2097 0.4933 0.1732 0.087 Uiso 1 1 calc R . . C25 C 1.009(2) 0.5525(12) 0.2783(11) 0.053(7) Uani 1 1 d . . . C26 C 1.239(3) 0.5013(16) 0.3068(12) 0.071(9) Uani 1 1 d . . . C27 C 1.288(3) 0.5733(16) 0.3437(15) 0.112(12) Uani 1 1 d U . . H27A H 1.3583 0.5945 0.3195 0.168 Uiso 1 1 calc R . . H27B H 1.3216 0.5631 0.3855 0.168 Uiso 1 1 calc R . . H27C H 1.2117 0.6029 0.3470 0.168 Uiso 1 1 calc R . . C28 C 1.359(4) 0.493(2) 0.2741(18) 0.177(17) Uani 1 1 d U . . H28A H 1.4332 0.4897 0.3037 0.266 Uiso 1 1 calc R . . H28B H 1.3734 0.5298 0.2461 0.266 Uiso 1 1 calc R . . H28C H 1.3544 0.4522 0.2496 0.266 Uiso 1 1 calc R . . C29 C 1.180(3) 0.464(2) 0.3597(17) 0.160(16) Uani 1 1 d U . . H29A H 1.0834 0.4633 0.3557 0.240 Uiso 1 1 calc R . . H29B H 1.2055 0.4847 0.3991 0.240 Uiso 1 1 calc R . . H29C H 1.2142 0.4188 0.3591 0.240 Uiso 1 1 calc R . . C30 C 1.004(3) 0.6772(13) 0.3169(10) 0.067(8) Uani 1 1 d U . . H30A H 1.0933 0.6718 0.3001 0.100 Uiso 1 1 calc R . . H30B H 1.0045 0.7113 0.3489 0.100 Uiso 1 1 calc R . . H30C H 0.9425 0.6898 0.2834 0.100 Uiso 1 1 calc R . . C31 C 0.737(2) 0.4977(12) 0.3940(11) 0.055(8) Uani 1 1 d . . . C32 C 0.674(3) 0.4437(17) 0.4263(11) 0.081(10) Uani 1 1 d . . . C33 C 0.958(2) 0.6226(13) 0.4907(11) 0.057(8) Uani 1 1 d . . . H33 H 1.0168 0.5865 0.4870 0.068 Uiso 1 1 calc R . . C34 C 0.948(3) 0.6548(15) 0.5491(11) 0.059(8) Uani 1 1 d . . . H34 H 1.0091 0.6452 0.5815 0.070 Uiso 1 1 calc R . . C35 C 0.852(3) 0.6986(18) 0.5581(15) 0.095(12) Uani 1 1 d . . . H35 H 0.8336 0.7147 0.5986 0.114 Uiso 1 1 calc R . . C36 C 0.776(3) 0.7212(13) 0.5051(13) 0.062(8) Uani 1 1 d . . . H36 H 0.7167 0.7571 0.5087 0.075 Uiso 1 1 calc R . . C37 C 0.793(2) 0.6879(11) 0.4466(10) 0.035(6) Uani 1 1 d . . . C38 C 0.712(2) 0.7081(14) 0.3900(12) 0.068(9) Uani 1 1 d . . . H38A H 0.7482 0.7492 0.3725 0.081 Uiso 1 1 calc R . . H38B H 0.7181 0.6738 0.3577 0.081 Uiso 1 1 calc R . . C39 C 0.485(3) 0.6609(14) 0.4296(13) 0.073(9) Uani 1 1 d . . . H39 H 0.5063 0.6157 0.4300 0.088 Uiso 1 1 calc R . . C40 C 0.372(3) 0.6917(16) 0.4489(13) 0.078(10) Uani 1 1 d . . . H40 H 0.2991 0.6706 0.4683 0.093 Uiso 1 1 calc R . . C41 C 0.502(2) 0.7775(13) 0.4117(12) 0.063(8) Uani 1 1 d U . . C42 C 0.272(3) 0.8089(15) 0.4494(14) 0.068(9) Uani 1 1 d . . . C43 C 0.228(3) 0.8481(15) 0.3897(14) 0.094(12) Uani 1 1 d . . . H43A H 0.2144 0.8177 0.3551 0.141 Uiso 1 1 calc R . . H43B H 0.2982 0.8795 0.3787 0.141 Uiso 1 1 calc R . . H43C H 0.1455 0.8717 0.3980 0.141 Uiso 1 1 calc R . . C44 C 0.326(3) 0.8575(14) 0.4985(13) 0.083(10) Uani 1 1 d . . . H44A H 0.3766 0.8335 0.5302 0.124 Uiso 1 1 calc R . . H44B H 0.2519 0.8805 0.5182 0.124 Uiso 1 1 calc R . . H44C H 0.3845 0.8894 0.4781 0.124 Uiso 1 1 calc R . . C45 C 0.154(2) 0.7708(12) 0.4797(12) 0.062(8) Uani 1 1 d . . . H45A H 0.1443 0.7282 0.4593 0.092 Uiso 1 1 calc R . . H45B H 0.0719 0.7959 0.4747 0.092 Uiso 1 1 calc R . . H45C H 0.1725 0.7643 0.5241 0.092 Uiso 1 1 calc R . . C46 C 0.522(3) 0.8341(12) 0.2940(11) 0.071(9) Uani 1 1 d . . . H46A H 0.5876 0.8028 0.2781 0.107 Uiso 1 1 calc R . . H46B H 0.5202 0.8727 0.2669 0.107 Uiso 1 1 calc R . . H46C H 0.4341 0.8137 0.2946 0.107 Uiso 1 1 calc R . . C47 C 0.774(2) 0.8974(12) 0.4783(9) 0.047(7) Uani 1 1 d . . . C48 C 0.829(3) 0.9179(14) 0.5397(12) 0.075(9) Uani 1 1 d . . . C49 C 0.546(2) 1.0069(15) 0.3750(12) 0.061(8) Uani 1 1 d . . . H49 H 0.4961 0.9956 0.4110 0.073 Uiso 1 1 calc R . . C50 C 0.533(3) 1.0749(18) 0.3537(13) 0.089(11) Uani 1 1 d . . . H50 H 0.4682 1.1052 0.3677 0.107 Uiso 1 1 calc R . . C51 C 0.630(3) 1.0881(15) 0.3103(17) 0.106(13) Uani 1 1 d . . . H51 H 0.6396 1.1323 0.2977 0.127 Uiso 1 1 calc R . . C52 C 0.719(3) 1.0405(14) 0.2818(11) 0.054(8) Uani 1 1 d . . . H52 H 0.7783 1.0511 0.2491 0.065 Uiso 1 1 calc R . . C53 C 0.707(2) 0.9764(14) 0.3079(11) 0.050(7) Uani 1 1 d . . . C54 C 0.811(2) 0.9224(12) 0.2905(12) 0.060(8) Uani 1 1 d . . . H54A H 0.8175 0.8905 0.3251 0.072 Uiso 1 1 calc R . . H54B H 0.7792 0.8986 0.2532 0.072 Uiso 1 1 calc R . . C55 C 1.021(3) 0.9822(14) 0.3262(11) 0.060(8) Uani 1 1 d . . . H55 H 0.9939 0.9874 0.3681 0.072 Uiso 1 1 calc R . . C56 C 1.136(3) 1.0035(14) 0.3002(12) 0.067(9) Uani 1 1 d . . . H56 H 1.2075 1.0257 0.3199 0.080 Uiso 1 1 calc R . . C57 C 1.000(2) 0.9518(11) 0.2193(10) 0.044(7) Uani 1 1 d . . . C58 C 1.234(3) 0.9965(15) 0.1923(11) 0.060(8) Uani 1 1 d U . . C59 C 1.360(3) 0.9672(18) 0.2173(15) 0.124(13) Uani 1 1 d U . . H59A H 1.4318 0.9998 0.2153 0.186 Uiso 1 1 calc R . . H59B H 1.3847 0.9290 0.1923 0.186 Uiso 1 1 calc R . . H59C H 1.3472 0.9537 0.2606 0.186 Uiso 1 1 calc R . . C60 C 1.290(3) 1.0744(17) 0.1974(16) 0.131(13) Uani 1 1 d U . . H60A H 1.2222 1.1045 0.1816 0.196 Uiso 1 1 calc R . . H60B H 1.3713 1.0790 0.1725 0.196 Uiso 1 1 calc R . . H60C H 1.3103 1.0848 0.2409 0.196 Uiso 1 1 calc R . . C61 C 1.200(3) 0.991(2) 0.1261(14) 0.140(14) Uani 1 1 d U . . H61A H 1.2163 0.9467 0.1118 0.210 Uiso 1 1 calc R . . H61B H 1.2561 1.0218 0.1023 0.210 Uiso 1 1 calc R . . H61C H 1.1066 1.0026 0.1199 0.210 Uiso 1 1 calc R . . C62 C 1.010(3) 0.8177(12) 0.1819(10) 0.068(9) Uani 1 1 d . . . H62A H 1.1037 0.8221 0.1947 0.102 Uiso 1 1 calc R . . H62B H 1.0026 0.7835 0.1503 0.102 Uiso 1 1 calc R . . H62C H 0.9563 0.8060 0.2181 0.102 Uiso 1 1 calc R . . C63 C 0.732(2) 1.0046(12) 0.1077(11) 0.045(7) Uani 1 1 d . . . C64 C 0.667(4) 1.0576(15) 0.0790(14) 0.103(12) Uani 1 1 d . . . 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 O01 0.04(2) 0.03(2) 0.04(2) -0.009(16) 0.040(17) -0.017(16) C01 0.11(7) 0.04(6) 0.28(13) -0.01(7) 0.01(8) 0.00(5) C02 0.12(6) 0.04(4) 0.10(5) 0.03(4) 0.04(5) 0.06(4) C03 0.5(2) 0.00(4) 0.16(9) 0.00(4) 0.25(13) -0.06(7) C04 0.11(6) 0.06(5) 0.10(6) -0.03(4) -0.08(5) -0.04(4) O02 0.12(5) 0.10(5) 0.09(4) -0.03(4) -0.08(3) 0.05(4) C05 0.02(3) 0.02(4) 0.16(7) -0.05(4) -0.03(4) 0.05(3) C06 0.04(4) 0.16(7) 0.02(3) 0.00(4) 0.01(3) -0.03(4) C07 0.10(5) 0.12(8) 0.12(6) -0.12(6) -0.03(5) 0.07(5) C08 0.10(5) 0.09(7) 0.08(5) 0.05(5) -0.04(4) -0.11(5) Pd1 0.0415(13) 0.0480(16) 0.0463(13) -0.0015(11) 0.0030(10) 0.0003(10) Pd2 0.0421(13) 0.0514(16) 0.0366(12) 0.0003(10) -0.0004(10) 0.0050(10) Pd3 0.0411(13) 0.0494(16) 0.0469(13) 0.0012(11) 0.0017(10) 0.0038(10) Pd4 0.0373(13) 0.0564(17) 0.0388(13) 0.0028(11) 0.0031(10) -0.0009(10) F1 0.091(13) 0.086(16) 0.071(12) -0.004(11) 0.008(9) -0.020(11) F2 0.089(14) 0.17(2) 0.049(11) -0.008(12) -0.006(9) 0.034(13) F3 0.062(13) 0.19(2) 0.088(13) -0.042(13) 0.027(11) -0.021(12) F4 0.023(10) 0.15(2) 0.189(19) 0.078(15) -0.007(10) -0.028(10) F5 0.153(18) 0.15(2) 0.085(13) 0.042(13) -0.017(12) -0.036(14) F6 0.138(17) 0.041(13) 0.21(2) 0.019(13) 0.057(15) -0.022(11) F7 0.138(16) 0.127(19) 0.047(10) -0.024(10) -0.015(10) 0.000(12) F8 0.092(12) 0.081(14) 0.066(11) -0.020(9) -0.003(9) 0.008(10) F9 0.103(14) 0.128(18) 0.070(11) -0.031(11) -0.028(10) -0.001(11) F10 0.23(3) 0.067(18) 0.49(5) -0.06(2) -0.31(3) 0.078(17) F11 0.046(13) 0.17(2) 0.43(4) 0.15(2) 0.09(2) 0.058(13) F12 0.23(3) 0.39(6) 0.23(3) 0.18(3) 0.04(3) 0.18(4) O1 0.056(13) 0.072(15) 0.036(10) 0.033(9) -0.018(10) 0.009(10) O2 0.060(14) 0.080(17) 0.089(16) 0.012(13) 0.046(12) 0.018(11) O3 0.030(10) 0.081(16) 0.080(13) -0.003(11) -0.001(9) -0.026(9) O4 0.041(10) 0.047(12) 0.061(11) 0.017(9) 0.012(8) 0.004(8) O5 0.049(11) 0.057(13) 0.049(11) -0.009(9) 0.010(8) -0.019(9) O6 0.058(12) 0.089(16) 0.033(10) 0.008(9) -0.004(8) 0.014(10) O7 0.039(10) 0.085(15) 0.032(9) 0.024(9) -0.006(8) 0.014(9) O8 0.068(12) 0.034(12) 0.084(13) 0.001(10) 0.021(10) -0.003(9) N1 0.037(15) 0.060(19) 0.069(16) 0.000(13) -0.004(12) -0.020(12) N2 0.041(17) 0.08(2) 0.064(16) -0.012(14) -0.011(12) 0.014(15) N3 0.065(16) 0.043(16) 0.079(16) -0.008(12) 0.055(13) 0.005(12) N4 0.056(14) 0.066(18) 0.039(12) 0.002(11) 0.000(10) 0.011(11) N5 0.051(14) 0.070(18) 0.078(16) -0.022(13) 0.047(12) -0.002(12) N6 0.029(12) 0.062(17) 0.062(14) 0.011(12) -0.035(10) -0.002(10) N7 0.044(12) 0.035(14) 0.037(11) 0.024(10) -0.013(9) 0.011(9) N8 0.035(13) 0.048(16) 0.064(14) 0.000(11) -0.012(10) 0.006(10) N9 0.051(14) 0.048(16) 0.076(15) 0.024(12) 0.015(11) 0.022(11) N10 0.033(12) 0.085(19) 0.037(12) 0.008(11) -0.013(10) 0.007(11) N11 0.029(12) 0.10(2) 0.038(12) -0.016(12) -0.021(10) 0.016(11) N12 0.062(14) 0.056(16) 0.030(11) -0.010(10) 0.013(10) 0.000(11) C1 0.12(3) 0.04(2) 0.10(2) 0.002(16) 0.08(2) 0.030(17) C2 0.06(2) 0.05(2) 0.06(2) 0.015(16) -0.03(2) -0.019(18) C3 0.05(2) 0.12(4) 0.04(2) 0.02(2) 0.005(17) -0.01(2) C4 0.046(14) 0.035(14) 0.044(13) 0.006(11) 0.004(11) -0.024(12) C5 0.071(16) 0.043(16) 0.087(16) 0.018(13) -0.009(14) -0.004(13) C6 0.06(2) 0.06(3) 0.13(3) 0.03(2) -0.01(2) -0.02(2) C7 0.03(2) 0.08(3) 0.12(3) 0.01(2) 0.037(19) -0.020(17) C8 0.07(2) 0.07(3) 0.10(3) -0.02(2) -0.015(19) -0.033(18) C9 0.04(2) 0.12(3) 0.09(2) -0.01(2) -0.023(17) 0.011(19) C10 0.100(17) 0.073(17) 0.107(17) 0.006(14) -0.003(14) -0.053(14) C11 0.07(2) 0.09(3) 0.049(18) -0.028(16) 0.002(15) -0.021(17) C12 0.08(2) 0.028(18) 0.054(18) -0.032(14) 0.012(15) -0.006(14) C13 0.06(2) 0.13(3) 0.046(19) -0.01(2) -0.014(16) -0.029(18) C14 0.11(3) 0.12(3) 0.039(19) -0.010(19) -0.027(19) -0.02(2) C15 0.063(15) 0.069(16) 0.029(12) 0.026(12) 0.005(12) -0.006(13) C16 0.045(18) 0.08(2) 0.07(2) 0.030(17) -0.017(15) 0.002(15) C17 0.07(2) 0.06(2) 0.020(14) -0.002(14) -0.002(13) 0.030(16) C18 0.06(2) 0.05(2) 0.08(2) 0.008(19) 0.000(16) -0.020(17) C19 0.10(3) 0.02(2) 0.10(3) 0.036(18) 0.00(2) 0.021(18) C20 0.041(18) 0.05(2) 0.10(3) -0.007(18) 0.020(17) 0.026(15) C21 0.056(18) 0.04(2) 0.08(2) -0.015(16) 0.010(15) -0.013(14) C22 0.09(2) 0.06(2) 0.038(16) -0.014(14) 0.014(15) -0.031(17) C23 0.038(19) 0.08(2) 0.07(2) -0.021(17) 0.016(16) -0.014(16) C24 0.06(2) 0.12(3) 0.035(17) -0.033(17) 0.005(15) 0.026(19) C25 0.065(18) 0.043(19) 0.052(16) 0.040(14) -0.021(13) -0.002(13) C26 0.07(2) 0.09(3) 0.053(18) 0.000(17) 0.030(16) 0.034(17) C27 0.14(2) 0.08(2) 0.12(2) -0.001(19) -0.046(19) -0.007(19) C28 0.13(2) 0.26(3) 0.14(3) 0.01(2) -0.01(2) 0.02(2) C29 0.12(2) 0.21(3) 0.15(3) 0.06(2) -0.03(2) 0.00(2) C30 0.094(16) 0.076(17) 0.030(12) 0.027(12) 0.016(12) 0.003(13) C31 0.068(19) 0.033(19) 0.063(18) 0.011(14) -0.007(15) 0.023(14) C32 0.08(2) 0.13(3) 0.035(17) 0.018(18) -0.020(15) -0.02(2) C33 0.037(16) 0.07(2) 0.068(19) -0.018(16) 0.015(14) -0.002(14) C34 0.06(2) 0.09(3) 0.025(15) -0.014(15) -0.011(13) -0.003(17) C35 0.10(3) 0.12(3) 0.07(2) -0.05(2) 0.00(2) 0.03(2) C36 0.07(2) 0.05(2) 0.06(2) 0.010(17) 0.015(17) -0.006(15) C37 0.061(17) 0.011(15) 0.035(14) -0.011(11) 0.005(13) -0.006(12) C38 0.06(2) 0.08(3) 0.053(19) -0.021(17) -0.014(15) 0.012(16) C39 0.06(2) 0.04(2) 0.11(2) -0.012(17) 0.025(18) -0.014(16) C40 0.037(19) 0.11(3) 0.08(2) 0.045(19) 0.012(16) -0.015(18) C41 0.044(13) 0.072(16) 0.074(14) 0.038(13) -0.012(11) 0.027(12) C42 0.052(19) 0.07(3) 0.08(2) -0.050(19) 0.014(17) -0.020(16) C43 0.11(3) 0.09(3) 0.08(2) -0.02(2) -0.02(2) 0.07(2) C44 0.06(2) 0.08(3) 0.11(3) 0.00(2) 0.048(19) 0.008(17) C45 0.044(17) 0.032(18) 0.11(2) 0.013(16) 0.040(16) 0.008(13) C46 0.12(2) 0.018(18) 0.073(19) -0.029(14) -0.060(17) 0.019(15) C47 0.069(18) 0.06(2) 0.015(13) -0.013(12) -0.007(12) -0.011(14) C48 0.10(2) 0.07(2) 0.049(18) 0.005(16) -0.016(16) -0.005(18) C49 0.020(15) 0.09(3) 0.07(2) 0.022(18) -0.013(13) -0.002(14) C50 0.08(2) 0.11(3) 0.08(2) 0.04(2) 0.030(19) -0.01(2) C51 0.11(3) 0.03(2) 0.17(4) 0.05(2) 0.04(3) 0.01(2) C52 0.06(2) 0.05(2) 0.048(17) 0.016(15) 0.008(14) -0.019(16) C53 0.014(15) 0.07(2) 0.067(19) -0.006(16) -0.014(13) 0.005(13) C54 0.043(18) 0.05(2) 0.09(2) 0.010(16) 0.001(15) 0.002(14) C55 0.05(2) 0.09(3) 0.039(16) -0.023(15) -0.035(14) 0.033(16) C56 0.036(18) 0.08(3) 0.08(2) -0.032(17) -0.011(16) -0.023(16) C57 0.051(16) 0.043(18) 0.039(14) -0.009(12) 0.022(12) -0.034(13) C58 0.067(15) 0.085(17) 0.029(12) -0.028(12) 0.000(11) -0.006(13) C59 0.08(2) 0.15(3) 0.14(2) 0.05(2) 0.022(19) 0.020(19) C60 0.15(2) 0.11(2) 0.13(2) -0.039(16) 0.023(16) -0.031(16) C61 0.13(2) 0.20(3) 0.09(2) 0.02(2) 0.008(19) -0.05(2) C62 0.12(2) 0.06(2) 0.027(14) 0.027(14) -0.022(14) -0.022(17) C63 0.053(17) 0.030(18) 0.054(17) 0.009(13) 0.019(13) 0.001(13) C64 0.18(3) 0.05(2) 0.08(2) 0.025(19) 0.06(2) 0.04(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 O01 C02 1.36(6) . ? O01 C03 1.41(12) 1_545 ? C01 C04 1.21(9) . ? C01 C02 1.40(8) 2_666 ? C01 C03 2.00(12) 2_676 ? C02 C01 1.40(8) 2_666 ? C02 C03 2.03(13) 1_545 ? C03 C04 1.29(8) 2_676 ? C03 O01 1.41(12) 1_565 ? C03 C01 2.00(12) 2_676 ? C03 C02 2.03(13) 1_565 ? C04 C03 1.29(8) 2_676 ? O02 C05 1.06(6) . ? O02 C08 1.13(7) . ? C05 C08 1.84(9) . ? C06 C05 1.45(7) 1_554 ? C06 C07 1.51(8) 2_775 ? C06 C08 1.99(8) 1_554 ? C07 C08 1.20(7) 2_776 ? C07 C06 1.51(8) 2_775 ? C08 C07 1.20(7) 2_776 ? C08 C06 1.99(8) 1_556 ? Pd1 C4 1.96(3) . ? Pd1 C1 2.10(2) . ? Pd1 N4 2.11(2) . ? Pd1 O1 2.165(16) . ? Pd2 C25 1.91(2) . ? Pd2 C30 1.94(2) . ? Pd2 N7 2.097(17) . ? Pd2 O4 2.245(14) . ? Pd3 C41 1.94(3) . ? Pd3 C46 2.04(2) . ? Pd3 N10 2.09(2) . ? Pd3 O5 2.145(15) . ? Pd4 C57 1.89(2) . ? Pd4 N3 1.99(2) . ? Pd4 C62 2.08(2) . ? Pd4 O7 2.170(15) . ? F1 C3 1.27(4) . ? F2 C3 1.34(3) . ? F3 C3 1.27(3) . ? F4 C32 1.29(3) . ? F5 C32 1.35(2) . ? F6 C32 1.27(3) . ? F7 C48 1.36(3) . ? F8 C48 1.32(3) . ? F9 C48 1.41(3) . ? F10 C64 1.29(3) . ? F10 F12 1.76(4) . ? F11 C64 1.17(3) . ? F12 C64 1.26(3) . ? O1 C2 1.17(3) . ? O2 C2 1.28(3) . ? O3 C31 1.25(2) . ? O4 C31 1.19(2) . ? O5 C47 1.24(2) . ? O6 C47 1.27(2) . ? O7 C63 1.28(2) . ? O8 C63 1.19(2) . ? N1 C4 1.33(3) . ? N1 C5 1.43(3) . ? N1 C7 1.48(3) . ? N2 C4 1.37(3) . ? N2 C6 1.37(3) . ? N2 C11 1.47(3) . ? N3 C16 1.39(2) . ? N3 C12 1.42(3) . ? N4 C17 1.32(2) . ? N4 C21 1.35(2) . ? N5 C25 1.31(2) . ? N5 C23 1.41(2) . ? N5 C22 1.52(3) . ? N6 C25 1.37(2) . ? N6 C24 1.40(2) . ? N6 C26 1.52(3) . ? N7 C37 1.28(2) . ? N7 C33 1.41(3) . ? N8 C41 1.36(2) . ? N8 C39 1.48(3) . ? N8 C38 1.49(2) . ? N9 C41 1.36(2) . ? N9 C40 1.38(3) . ? N9 C42 1.48(3) . ? N10 C53 1.29(2) . ? N10 C49 1.33(3) . ? N11 C57 1.317(19) . ? N11 C55 1.40(2) . ? N11 C54 1.51(2) . ? N12 C58 1.40(2) . ? N12 C57 1.40(2) . ? N12 C56 1.48(2) . ? C2 C3 1.64(4) . ? C5 C6 1.22(3) . ? C7 C8 1.49(3) . ? C7 C9 1.50(4) . ? C7 C10 1.58(3) . ? C11 C12 1.52(3) . ? C12 C13 1.40(3) . ? C13 C14 1.38(3) . ? C14 C15 1.40(3) . ? C15 C16 1.36(3) . ? C17 C18 1.41(3) . ? C17 C22 1.57(3) . ? C18 C19 1.31(3) . ? C19 C20 1.41(4) . ? C20 C21 1.36(3) . ? C23 C24 1.28(3) . ? C26 C28 1.38(4) . ? C26 C29 1.46(4) . ? C26 C27 1.71(4) . ? C31 C32 1.42(3) . ? C33 C34 1.39(3) . ? C34 C35 1.30(3) . ? C35 C36 1.41(4) . ? C36 C37 1.41(3) . ? C37 C38 1.49(3) . ? C39 C40 1.34(3) . ? C42 C44 1.52(3) . ? C42 C45 1.53(3) . ? C42 C43 1.54(4) . ? C47 C48 1.46(3) . ? C49 C50 1.44(4) . ? C50 C51 1.35(3) . ? C51 C52 1.43(4) . ? C52 C53 1.40(3) . ? C53 C54 1.54(3) . ? C55 C56 1.33(3) . ? C58 C61 1.44(3) . ? C58 C59 1.47(4) . ? C58 C60 1.66(4) . ? C63 C64 1.38(3) . ? 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 C02 O01 C03 94(4) . 1_545 ? C04 C01 C02 109(9) . 2_666 ? C04 C01 C03 38(6) . 2_676 ? C02 C01 C03 71(6) 2_666 2_676 ? O01 C02 C01 111(7) . 2_666 ? O01 C02 C03 44(3) . 1_545 ? C01 C02 C03 68(5) 2_666 1_545 ? C04 C03 O01 117(9) 2_676 1_565 ? C04 C03 C01 36(4) 2_676 2_676 ? O01 C03 C01 82(7) 1_565 2_676 ? C04 C03 C02 76(6) 2_676 1_565 ? O01 C03 C02 42(4) 1_565 1_565 ? C01 C03 C02 41(3) 2_676 1_565 ? C01 C04 C03 106(9) . 2_676 ? C05 O02 C08 114(7) . . ? O02 C05 C08 34(4) . . ? C05 C06 C07 99(4) 1_554 2_775 ? C05 C06 C08 62(4) 1_554 1_554 ? C07 C06 C08 37(3) 2_775 1_554 ? C08 C07 C06 94(6) 2_776 2_775 ? O02 C08 C07 121(7) . 2_776 ? O02 C08 C05 32(4) . . ? C07 C08 C05 93(5) 2_776 . ? O02 C08 C06 72(4) . 1_556 ? C07 C08 C06 49(4) 2_776 1_556 ? C05 C08 C06 44(3) . 1_556 ? C4 Pd1 C1 85.3(10) . . ? C4 Pd1 N4 169.0(8) . . ? C1 Pd1 N4 89.2(8) . . ? C4 Pd1 O1 96.8(8) . . ? C1 Pd1 O1 174.6(10) . . ? N4 Pd1 O1 89.5(6) . . ? C25 Pd2 C30 86.0(10) . . ? C25 Pd2 N7 176.2(7) . . ? C30 Pd2 N7 91.0(7) . . ? C25 Pd2 O4 95.0(6) . . ? C30 Pd2 O4 175.8(8) . . ? N7 Pd2 O4 88.2(6) . . ? C41 Pd3 C46 86.8(11) . . ? C41 Pd3 N10 170.0(6) . . ? C46 Pd3 N10 89.3(7) . . ? C41 Pd3 O5 95.3(8) . . ? C46 Pd3 O5 175.1(8) . . ? N10 Pd3 O5 89.2(6) . . ? C57 Pd4 N3 178.3(6) . . ? C57 Pd4 C62 89.6(10) . . ? N3 Pd4 C62 89.8(7) . . ? C57 Pd4 O7 91.5(7) . . ? N3 Pd4 O7 89.2(7) . . ? C62 Pd4 O7 177.0(7) . . ? C64 F10 F12 45.5(13) . . ? C64 F12 F10 46.9(16) . . ? C2 O1 Pd1 112.3(19) . . ? C31 O4 Pd2 112.4(12) . . ? C47 O5 Pd3 113.4(9) . . ? C63 O7 Pd4 114.5(10) . . ? C4 N1 C5 110(2) . . ? C4 N1 C7 125(3) . . ? C5 N1 C7 126(3) . . ? C4 N2 C6 110(3) . . ? C4 N2 C11 125(3) . . ? C6 N2 C11 125(3) . . ? C16 N3 C12 110.4(18) . . ? C16 N3 Pd4 119.7(13) . . ? C12 N3 Pd4 129.8(15) . . ? C17 N4 C21 115.8(18) . . ? C17 N4 Pd1 128.2(13) . . ? C21 N4 Pd1 115.9(13) . . ? C25 N5 C23 118.2(17) . . ? C25 N5 C22 124.1(14) . . ? C23 N5 C22 117.1(15) . . ? C25 N6 C24 113.2(15) . . ? C25 N6 C26 123.8(13) . . ? C24 N6 C26 123.0(15) . . ? C37 N7 C33 115.8(14) . . ? C37 N7 Pd2 131.8(10) . . ? C33 N7 Pd2 112.4(10) . . ? C41 N8 C39 113.4(15) . . ? C41 N8 C38 126.4(15) . . ? C39 N8 C38 119.8(16) . . ? C41 N9 C40 112.3(16) . . ? C41 N9 C42 121.7(15) . . ? C40 N9 C42 125.8(16) . . ? C53 N10 C49 115.5(17) . . ? C53 N10 Pd3 129.5(13) . . ? C49 N10 Pd3 115.0(12) . . ? C57 N11 C55 119.1(15) . . ? C57 N11 C54 121.4(14) . . ? C55 N11 C54 119.1(16) . . ? C58 N12 C57 129.4(13) . . ? C58 N12 C56 118.1(14) . . ? C57 N12 C56 112.4(13) . . ? O1 C2 O2 133(3) . . ? O1 C2 C3 117(3) . . ? O2 C2 C3 110(3) . . ? F1 C3 F3 115(3) . . ? F1 C3 F2 108(3) . . ? F3 C3 F2 103(3) . . ? F1 C3 C2 109(2) . . ? F3 C3 C2 115(3) . . ? F2 C3 C2 105(3) . . ? N1 C4 N2 103(2) . . ? N1 C4 Pd1 133(2) . . ? N2 C4 Pd1 124(2) . . ? C6 C5 N1 107(3) . . ? C5 C6 N2 110(3) . . ? N1 C7 C8 107(2) . . ? N1 C7 C9 112(3) . . ? C8 C7 C9 107(3) . . ? N1 C7 C10 112(2) . . ? C8 C7 C10 111(3) . . ? C9 C7 C10 108(2) . . ? N2 C11 C12 112(2) . . ? C13 C12 N3 125(2) . . ? C13 C12 C11 119(2) . . ? N3 C12 C11 116(2) . . ? C14 C13 C12 119(3) . . ? C13 C14 C15 119(3) . . ? C16 C15 C14 119(2) . . ? C15 C16 N3 128(2) . . ? N4 C17 C18 124(3) . . ? N4 C17 C22 114(2) . . ? C18 C17 C22 121(2) . . ? C19 C18 C17 116(3) . . ? C18 C19 C20 125(3) . . ? C21 C20 C19 114(3) . . ? N4 C21 C20 126(3) . . ? N5 C22 C17 112.6(19) . . ? C24 C23 N5 103(2) . . ? C23 C24 N6 108(2) . . ? N5 C25 N6 97.6(16) . . ? N5 C25 Pd2 126.6(16) . . ? N6 C25 Pd2 135.4(15) . . ? C28 C26 C29 131(3) . . ? C28 C26 N6 109(2) . . ? C29 C26 N6 110(2) . . ? C28 C26 C27 95(3) . . ? C29 C26 C27 101(2) . . ? N6 C26 C27 105(2) . . ? O4 C31 O3 131(2) . . ? O4 C31 C32 116(2) . . ? O3 C31 C32 112(2) . . ? F6 C32 F4 107(2) . . ? F6 C32 F5 102.4(19) . . ? F4 C32 F5 99.4(17) . . ? F6 C32 C31 116(2) . . ? F4 C32 C31 120(2) . . ? F5 C32 C31 109(2) . . ? C34 C33 N7 122(2) . . ? C35 C34 C33 120(3) . . ? C34 C35 C36 119(3) . . ? C37 C36 C35 118(3) . . ? N7 C37 C36 124(2) . . ? N7 C37 C38 115.7(18) . . ? C36 C37 C38 120(2) . . ? N8 C38 C37 110.8(18) . . ? C40 C39 N8 101(2) . . ? C39 C40 N9 111(2) . . ? N8 C41 N9 102.3(17) . . ? N8 C41 Pd3 124.7(15) . . ? N9 C41 Pd3 132.9(16) . . ? N9 C42 C44 108(2) . . ? N9 C42 C45 107(2) . . ? C44 C42 C45 108(2) . . ? N9 C42 C43 112.5(18) . . ? C44 C42 C43 109(3) . . ? C45 C42 C43 113(2) . . ? O5 C47 O6 130.3(17) . . ? O5 C47 C48 115.7(18) . . ? O6 C47 C48 114(2) . . ? F8 C48 F7 101.9(17) . . ? F8 C48 F9 104.0(19) . . ? F7 C48 F9 100.2(17) . . ? F8 C48 C47 116(2) . . ? F7 C48 C47 113(2) . . ? F9 C48 C47 119(2) . . ? N10 C49 C50 128(2) . . ? C51 C50 C49 110(3) . . ? C50 C51 C52 126(3) . . ? C53 C52 C51 113(2) . . ? N10 C53 C52 126(2) . . ? N10 C53 C54 114(2) . . ? C52 C53 C54 120(2) . . ? N11 C54 C53 113.1(19) . . ? C56 C55 N11 106(2) . . ? C55 C56 N12 104.1(19) . . ? N11 C57 N12 98.6(14) . . ? N11 C57 Pd4 130.7(13) . . ? N12 C57 Pd4 129.5(12) . . ? N12 C58 C61 114(2) . . ? N12 C58 C59 112(2) . . ? C61 C58 C59 121(3) . . ? N12 C58 C60 113(2) . . ? C61 C58 C60 102(3) . . ? C59 C58 C60 94(2) . . ? O8 C63 O7 127(2) . . ? O8 C63 C64 112(2) . . ? O7 C63 C64 120(2) . . ? F11 C64 F12 104(2) . . ? F11 C64 F10 101(2) . . ? F12 C64 F10 88(2) . . ? F11 C64 C63 130(3) . . ? F12 C64 C63 113(2) . . ? F10 C64 C63 113(3) . . ? _diffrn_measured_fraction_theta_max 0.939 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.939 _refine_diff_density_max 1.053 _refine_diff_density_min -0.839 _refine_diff_density_rms 0.163 #===END