# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_120114 _database_code_depnum_ccdc_archive 'CCDC 911818' #TrackingRef 'CCDC911818_revised.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C25 H13 N' _chemical_formula_moiety 'C25 H13 N' _chemical_formula_weight 327.38 _chemical_melting_point ? _chemical_absolute_configuration ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P c a 21' _symmetry_space_group_name_Hall 'P 2c -2ac' _symmetry_Int_Tables_number 29 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 1/2-X,+Y,1/2+Z 3 1/2+X,-Y,+Z 4 -X,-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 20.712(3) _cell_length_b 9.4816(13) _cell_length_c 8.0453(12) _cell_angle_alpha 90.0000 _cell_angle_beta 90.0000 _cell_angle_gamma 90.0000 _cell_volume 1580.0(4) _cell_formula_units_Z 4 _cell_measurement_reflns_used 5926 _cell_measurement_theta_min 3.21 _cell_measurement_theta_max 25.60 _cell_measurement_temperature 93 #------------------------------------------------------------------------------ _exptl_crystal_description platelet _exptl_crystal_colour yellow _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.100 _exptl_crystal_density_diffrn 1.376 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 680.00 _exptl_absorpt_coefficient_mu 0.080 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'ABSCOR (Rigaku, 1995)' _exptl_absorpt_correction_T_min 0.380 _exptl_absorpt_correction_T_max 0.992 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 93 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_reflns_number 12478 _diffrn_reflns_av_R_equivalents 0.1352 _diffrn_reflns_theta_max 25.63 _diffrn_reflns_theta_full 25.62 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% ? #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). SIMU restraints were applied for the some part of the corannulene moiety (C8-C22, C14-C24 and C17-C25). ; _reflns_number_total 2964 _reflns_number_gt 1498 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0862 _refine_ls_wR_factor_ref 0.2365 _refine_ls_number_restraints 19 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 2964 _refine_ls_number_parameters 235 _refine_ls_goodness_of_fit_ref 1.134 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0908P)^2^+0.2137P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.000 _refine_diff_density_max 0.440 _refine_diff_density_min -0.280 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack, H. D. (1983), Acta Cryst. A39, 876-881. 1366 Friedel Pairs' _refine_ls_abs_structure_Flack 0.00000 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 for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.0000 0.0000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; N N 0.0061 0.0033 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 N1 N 0.7109(3) 0.8091(6) 0.1842(8) 0.0549(15) Uani 1.0 4 d . . . C1 C 0.7691(3) 0.8626(7) 0.2249(10) 0.0546(19) Uani 1.0 4 d . . . C2 C 0.7780(3) 0.9871(7) 0.3111(9) 0.0514(17) Uani 1.0 4 d . . . C3 C 0.7256(3) 1.0611(7) 0.3593(9) 0.0559(19) Uani 1.0 4 d . . . C4 C 0.6649(3) 1.0112(7) 0.3177(9) 0.0548(18) Uani 1.0 4 d . . . C5 C 0.6588(3) 0.8860(7) 0.2298(9) 0.0505(17) Uani 1.0 4 d . . . C6 C 0.5949(3) 0.8349(7) 0.1686(10) 0.0578(18) Uani 1.0 4 d . . . C7 C 0.5925(3) 0.7588(7) 0.0075(10) 0.0529(18) Uani 1.0 4 d . . . C8 C 0.5353(3) 0.7076(7) -0.0619(10) 0.0572(17) Uani 1.0 4 d . . . C9 C 0.5240(4) 0.6019(7) -0.1764(10) 0.061(2) Uani 1.0 4 d . . . C10 C 0.4622(3) 0.5278(7) -0.1951(10) 0.0547(18) Uani 1.0 4 d . . . C11 C 0.4108(3) 0.5633(8) -0.0892(10) 0.060(2) Uani 1.0 4 d . . . C12 C 0.3564(3) 0.4813(8) -0.0444(12) 0.067(3) Uani 1.0 4 d . . . C13 C 0.3193(4) 0.5037(8) 0.1081(11) 0.062(2) Uani 1.0 4 d . . . C14 C 0.3372(3) 0.6124(8) 0.2191(12) 0.066(2) Uani 1.0 4 d . . . C15 C 0.3259(4) 0.6227(9) 0.3935(12) 0.076(3) Uani 1.0 4 d . . . C16 C 0.3643(3) 0.7074(7) 0.5019(10) 0.0535(18) Uani 1.0 4 d . . . C17 C 0.4183(3) 0.7851(8) 0.4432(11) 0.062(2) Uani 1.0 4 d . . . C18 C 0.4729(4) 0.8372(7) 0.5198(12) 0.064(2) Uani 1.0 4 d . . . C19 C 0.5329(4) 0.8700(7) 0.4361(10) 0.0553(18) Uani 1.0 4 d . . . C20 C 0.5398(4) 0.8513(7) 0.2641(10) 0.0571(19) Uani 1.0 4 d . . . C21 C 0.4802(3) 0.8193(7) 0.1801(10) 0.0494(17) Uani 1.0 4 d . . . C22 C 0.4775(3) 0.7532(7) 0.0240(9) 0.0501(16) Uani 1.0 4 d . . . C23 C 0.4185(4) 0.6838(6) 0.0116(10) 0.0550(19) Uani 1.0 4 d . . . C24 C 0.3839(3) 0.7088(7) 0.1628(11) 0.0591(19) Uani 1.0 4 d . . . C25 C 0.4245(4) 0.7923(7) 0.2618(9) 0.0538(18) Uani 1.0 4 d . . . H1 H 0.8064 0.8113 0.1923 0.0655 Uiso 1.0 4 calc R . . H2 H 0.8202 1.0200 0.3359 0.0617 Uiso 1.0 4 calc R . . H3 H 0.7303 1.1460 0.4208 0.0671 Uiso 1.0 4 calc R . . H4 H 0.6275 1.0626 0.3493 0.0657 Uiso 1.0 4 calc R . . H7 H 0.6318 0.7443 -0.0512 0.0634 Uiso 1.0 4 calc R . . H9 H 0.5584 0.5755 -0.2479 0.0737 Uiso 1.0 4 calc R . . H10 H 0.4570 0.4569 -0.2775 0.0657 Uiso 1.0 4 calc R . . H12 H 0.3432 0.4079 -0.1173 0.0805 Uiso 1.0 4 calc R . . H13 H 0.2833 0.4452 0.1325 0.0741 Uiso 1.0 4 calc R . . H15 H 0.2911 0.5707 0.4399 0.0910 Uiso 1.0 4 calc R . . H16 H 0.3535 0.7118 0.6165 0.0642 Uiso 1.0 4 calc R . . H18 H 0.4709 0.8527 0.6364 0.0771 Uiso 1.0 4 calc R . . H19 H 0.5683 0.9049 0.4989 0.0664 Uiso 1.0 4 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 N1 0.054(4) 0.050(3) 0.061(4) -0.010(3) -0.007(3) 0.003(3) C1 0.039(4) 0.053(4) 0.072(5) -0.005(3) -0.006(4) 0.017(4) C2 0.051(4) 0.049(4) 0.055(5) -0.010(4) -0.007(4) 0.009(4) C3 0.056(4) 0.041(4) 0.070(6) -0.011(3) -0.013(4) -0.011(4) C4 0.053(4) 0.044(4) 0.067(5) -0.001(4) -0.004(4) 0.001(4) C5 0.047(4) 0.045(4) 0.060(5) -0.009(4) -0.009(4) 0.014(4) C6 0.051(4) 0.048(4) 0.074(6) -0.002(3) -0.008(4) 0.011(4) C7 0.049(4) 0.046(4) 0.063(5) -0.005(3) 0.002(4) 0.007(4) C8 0.059(4) 0.052(4) 0.061(5) -0.005(4) -0.010(4) 0.003(4) C9 0.076(5) 0.048(4) 0.060(5) 0.013(4) 0.000(5) 0.014(4) C10 0.052(4) 0.057(4) 0.055(5) 0.016(4) -0.006(4) 0.012(4) C11 0.054(4) 0.060(5) 0.067(6) 0.009(4) -0.014(4) 0.018(4) C12 0.045(4) 0.069(5) 0.087(6) -0.001(4) -0.032(5) 0.023(5) C13 0.046(4) 0.049(4) 0.090(6) -0.002(4) -0.018(5) 0.009(4) C14 0.049(4) 0.064(5) 0.086(6) 0.019(4) -0.006(5) 0.002(4) C15 0.053(5) 0.081(6) 0.094(7) 0.032(4) 0.016(5) 0.024(5) C16 0.036(4) 0.059(5) 0.065(5) 0.012(4) 0.012(4) 0.013(4) C17 0.042(4) 0.055(4) 0.090(6) 0.022(3) 0.002(4) 0.002(4) C18 0.071(5) 0.039(4) 0.083(6) 0.009(4) -0.012(5) -0.010(4) C19 0.060(5) 0.041(4) 0.064(5) 0.007(4) -0.010(4) -0.012(4) C20 0.064(5) 0.043(4) 0.065(6) 0.007(4) 0.001(4) -0.003(4) C21 0.042(4) 0.041(4) 0.066(5) 0.001(3) -0.020(4) 0.007(4) C22 0.051(4) 0.046(4) 0.053(5) 0.017(3) 0.012(4) 0.010(4) C23 0.078(5) 0.028(4) 0.059(5) 0.017(4) -0.028(5) -0.005(4) C24 0.038(3) 0.048(4) 0.092(6) 0.011(3) 0.008(4) 0.032(4) C25 0.069(5) 0.041(4) 0.051(5) 0.021(4) -0.001(4) -0.003(3) #============================================================================== _computing_data_collection 'RAPID AUTO (Rigaku)' _computing_cell_refinement 'RAPID AUTO' _computing_data_reduction 'RAPID AUTO' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_molecular_graphics 'CrystalStructure 4.0' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 N1 C1 1.349(8) yes . . N1 C5 1.354(8) yes . . C1 C2 1.381(10) yes . . C2 C3 1.350(10) yes . . C3 C4 1.384(9) yes . . C4 C5 1.388(9) yes . . C5 C6 1.493(9) yes . . C6 C7 1.484(11) yes . . C6 C20 1.383(10) yes . . C7 C8 1.398(10) yes . . C8 C9 1.381(10) yes . . C8 C22 1.447(10) yes . . C9 C10 1.468(10) yes . . C10 C11 1.403(10) yes . . C11 C12 1.417(10) yes . . C11 C23 1.410(10) yes . . C12 C13 1.463(12) yes . . C13 C14 1.413(12) yes . . C14 C15 1.426(13) yes . . C14 C24 1.407(10) yes . . C15 C16 1.427(11) yes . . C16 C17 1.419(10) yes . . C17 C18 1.380(10) yes . . C17 C25 1.467(11) yes . . C18 C19 1.449(11) yes . . C19 C20 1.403(11) yes . . C20 C21 1.439(10) yes . . C21 C22 1.405(11) yes . . C21 C25 1.352(10) yes . . C22 C23 1.391(9) yes . . C23 C24 1.431(11) yes . . C24 C25 1.403(10) yes . . C1 H1 0.950 no . . C2 H2 0.950 no . . C3 H3 0.950 no . . C4 H4 0.950 no . . C7 H7 0.950 no . . C9 H9 0.950 no . . C10 H10 0.950 no . . C12 H12 0.950 no . . C13 H13 0.950 no . . C15 H15 0.950 no . . C16 H16 0.950 no . . C18 H18 0.950 no . . C19 H19 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 C1 N1 C5 116.4(6) yes . . . N1 C1 C2 124.2(6) yes . . . C1 C2 C3 118.8(6) yes . . . C2 C3 C4 118.9(6) yes . . . C3 C4 C5 119.9(6) yes . . . N1 C5 C4 121.8(6) yes . . . N1 C5 C6 116.3(6) yes . . . C4 C5 C6 121.7(6) yes . . . C5 C6 C7 118.3(6) yes . . . C5 C6 C20 120.7(7) yes . . . C7 C6 C20 120.8(6) yes . . . C6 C7 C8 123.0(6) yes . . . C7 C8 C9 131.5(7) yes . . . C7 C8 C22 114.0(7) yes . . . C9 C8 C22 113.2(6) yes . . . C8 C9 C10 124.3(7) yes . . . C9 C10 C11 118.9(7) yes . . . C10 C11 C12 128.7(7) yes . . . C10 C11 C23 117.3(6) yes . . . C12 C11 C23 112.9(7) yes . . . C11 C12 C13 123.5(7) yes . . . C12 C13 C14 119.9(7) yes . . . C13 C14 C15 129.0(8) yes . . . C13 C14 C24 116.8(8) yes . . . C15 C14 C24 112.7(8) yes . . . C14 C15 C16 123.3(7) yes . . . C15 C16 C17 121.9(8) yes . . . C16 C17 C18 133.1(8) yes . . . C16 C17 C25 115.1(7) yes . . . C18 C17 C25 110.8(7) yes . . . C17 C18 C19 125.0(8) yes . . . C18 C19 C20 121.3(7) yes . . . C6 C20 C19 130.3(7) yes . . . C6 C20 C21 115.0(7) yes . . . C19 C20 C21 113.7(7) yes . . . C20 C21 C22 123.2(6) yes . . . C20 C21 C25 122.9(7) yes . . . C22 C21 C25 108.4(6) yes . . . C8 C22 C21 121.8(6) yes . . . C8 C22 C23 123.4(7) yes . . . C21 C22 C23 108.1(6) yes . . . C11 C23 C22 121.6(7) yes . . . C11 C23 C24 124.5(6) yes . . . C22 C23 C24 107.5(6) yes . . . C14 C24 C23 120.7(7) yes . . . C14 C24 C25 126.6(8) yes . . . C23 C24 C25 106.0(6) yes . . . C17 C25 C21 124.6(7) yes . . . C17 C25 C24 119.0(7) yes . . . C21 C25 C24 110.0(7) yes . . . N1 C1 H1 117.897 no . . . C2 C1 H1 117.893 no . . . C1 C2 H2 120.588 no . . . C3 C2 H2 120.592 no . . . C2 C3 H3 120.557 no . . . C4 C3 H3 120.540 no . . . C3 C4 H4 120.071 no . . . C5 C4 H4 120.071 no . . . C6 C7 H7 118.490 no . . . C8 C7 H7 118.480 no . . . C8 C9 H9 117.848 no . . . C10 C9 H9 117.857 no . . . C9 C10 H10 120.544 no . . . C11 C10 H10 120.545 no . . . C11 C12 H12 118.252 no . . . C13 C12 H12 118.249 no . . . C12 C13 H13 120.061 no . . . C14 C13 H13 120.058 no . . . C14 C15 H15 118.373 no . . . C16 C15 H15 118.372 no . . . C15 C16 H16 119.076 no . . . C17 C16 H16 119.073 no . . . C17 C18 H18 117.507 no . . . C19 C18 H18 117.505 no . . . C18 C19 H19 119.356 no . . . C20 C19 H19 119.365 no . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 C1 N1 C5 C4 -1.7(10) no . . . . C1 N1 C5 C6 173.5(6) no . . . . C5 N1 C1 C2 1.2(10) no . . . . N1 C1 C2 C3 0.4(11) no . . . . C1 C2 C3 C4 -1.4(10) no . . . . C2 C3 C4 C5 0.9(10) no . . . . C3 C4 C5 N1 0.7(10) no . . . . C3 C4 C5 C6 -174.2(6) no . . . . N1 C5 C6 C7 -30.0(9) no . . . . N1 C5 C6 C20 146.4(6) no . . . . C4 C5 C6 C7 145.1(6) no . . . . C4 C5 C6 C20 -38.4(10) no . . . . C5 C6 C7 C8 -179.5(6) no . . . . C5 C6 C20 C19 -22.4(11) no . . . . C5 C6 C20 C21 170.1(5) no . . . . C7 C6 C20 C19 153.9(6) no . . . . C7 C6 C20 C21 -13.5(9) no . . . . C20 C6 C7 C8 4.1(10) no . . . . C6 C7 C8 C9 -157.4(7) no . . . . C6 C7 C8 C22 8.7(9) no . . . . C7 C8 C9 C10 158.0(7) no . . . . C7 C8 C22 C21 -11.7(9) no . . . . C7 C8 C22 C23 -159.5(6) no . . . . C9 C8 C22 C21 157.0(6) no . . . . C9 C8 C22 C23 9.3(10) no . . . . C22 C8 C9 C10 -8.2(10) no . . . . C8 C9 C10 C11 -1.0(11) no . . . . C9 C10 C11 C12 -157.0(7) no . . . . C9 C10 C11 C23 9.8(10) no . . . . C10 C11 C12 C13 156.4(7) no . . . . C10 C11 C23 C22 -9.0(10) no . . . . C10 C11 C23 C24 -157.2(6) no . . . . C12 C11 C23 C22 159.9(6) no . . . . C12 C11 C23 C24 11.7(10) no . . . . C23 C11 C12 C13 -10.9(10) no . . . . C11 C12 C13 C14 0.4(11) no . . . . C12 C13 C14 C15 -154.4(7) no . . . . C12 C13 C14 C24 10.0(10) no . . . . C13 C14 C15 C16 156.7(7) no . . . . C13 C14 C24 C23 -9.5(10) no . . . . C13 C14 C24 C25 -156.8(6) no . . . . C15 C14 C24 C23 157.5(6) no . . . . C15 C14 C24 C25 10.1(10) no . . . . C24 C14 C15 C16 -8.3(10) no . . . . C14 C15 C16 C17 -1.8(11) no . . . . C15 C16 C17 C18 -156.9(7) no . . . . C15 C16 C17 C25 10.4(9) no . . . . C16 C17 C18 C19 157.0(7) no . . . . C16 C17 C25 C21 -157.9(6) no . . . . C16 C17 C25 C24 -8.7(9) no . . . . C18 C17 C25 C21 12.3(9) no . . . . C18 C17 C25 C24 161.4(6) no . . . . C25 C17 C18 C19 -10.8(9) no . . . . C17 C18 C19 C20 0.5(10) no . . . . C18 C19 C20 C6 -158.4(6) no . . . . C18 C19 C20 C21 9.2(9) no . . . . C6 C20 C21 C22 10.7(9) no . . . . C6 C20 C21 C25 161.7(6) no . . . . C19 C20 C21 C22 -158.8(6) no . . . . C19 C20 C21 C25 -7.9(9) no . . . . C20 C21 C22 C8 2.2(10) no . . . . C20 C21 C22 C23 154.3(6) no . . . . C20 C21 C25 C17 -3.3(10) no . . . . C20 C21 C25 C24 -154.7(6) no . . . . C22 C21 C25 C17 151.4(6) no . . . . C22 C21 C25 C24 -0.1(7) no . . . . C25 C21 C22 C8 -152.3(6) no . . . . C25 C21 C22 C23 -0.3(7) no . . . . C8 C22 C23 C11 -0.9(11) no . . . . C8 C22 C23 C24 152.0(6) no . . . . C21 C22 C23 C11 -152.4(6) no . . . . C21 C22 C23 C24 0.5(7) no . . . . C11 C23 C24 C14 -1.8(11) no . . . . C11 C23 C24 C25 151.4(7) no . . . . C22 C23 C24 C14 -153.7(6) no . . . . C22 C23 C24 C25 -0.5(7) no . . . . C14 C24 C25 C17 -1.8(10) no . . . . C14 C24 C25 C21 151.5(6) no . . . . C23 C24 C25 C17 -152.9(6) no . . . . C23 C24 C25 C21 0.4(7) no . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 N1 C3 2.791(9) no . . N1 C7 2.873(9) no . . C1 C4 2.685(9) no . . C2 C5 2.728(9) no . . C4 C19 3.189(10) no . . C4 C20 3.032(10) no . . C5 C19 3.094(10) no . . C6 C22 2.804(10) no . . C7 C21 2.769(9) no . . C8 C11 2.927(10) no . . C8 C20 2.956(11) no . . C8 C25 3.562(10) no . . C9 C23 2.768(10) no . . C10 C22 2.788(10) no . . C11 C14 2.949(12) no . . C11 C21 3.557(10) no . . C11 C25 3.573(10) no . . C12 C24 2.785(11) no . . C13 C23 2.783(10) no . . C14 C17 2.958(11) no . . C14 C21 3.568(9) no . . C14 C22 3.563(10) no . . C15 C25 2.808(11) no . . C16 C24 2.758(12) no . . C17 C20 2.969(10) no . . C18 C21 2.743(12) no . . C19 C25 2.748(10) no . . C20 C23 3.600(10) no . . C20 C24 3.594(10) no . . N1 C2 3.451(10) no . 2_654 C1 C3 3.494(11) no . 2_654 C2 N1 3.451(10) no . 2_655 C3 C1 3.494(11) no . 2_655 C9 C18 3.474(11) no . 1_554 C10 C16 3.599(10) no . 1_554 C16 C10 3.599(10) no . 1_556 C18 C9 3.474(11) no . 1_556 C18 C20 3.558(10) no . 4_675 C19 C21 3.551(10) no . 4_675 C20 C18 3.558(10) no . 4_674 C21 C19 3.551(10) no . 4_674 N1 H2 3.2586 no . . N1 H4 3.2455 no . . N1 H7 2.5785 no . . C1 H3 3.2180 no . . C2 H4 3.2136 no . . C3 H1 3.1971 no . . C4 H2 3.2218 no . . C4 H19 2.6721 no . . C5 H1 3.1538 no . . C5 H3 3.2607 no . . C5 H7 2.6891 no . . C5 H19 2.8687 no . . C6 H4 2.6890 no . . C6 H19 2.7937 no . . C7 H9 2.7820 no . . C8 H10 3.3598 no . . C9 H7 2.7968 no . . C10 H12 2.7843 no . . C11 H9 3.3152 no . . C11 H13 3.3786 no . . C12 H10 2.8132 no . . C13 H15 2.8055 no . . C14 H12 3.3317 no . . C14 H16 3.3499 no . . C15 H13 2.8324 no . . C16 H18 2.8190 no . . C17 H15 3.3272 no . . C17 H19 3.3395 no . . C18 H16 2.8521 no . . C19 H4 2.7672 no . . C20 H4 2.7895 no . . C20 H7 3.3301 no . . C20 H18 3.3178 no . . C21 H19 3.2506 no . . C22 H7 3.2527 no . . C22 H9 3.2292 no . . C23 H10 3.2670 no . . C23 H12 3.2176 no . . C24 H13 3.2641 no . . C24 H15 3.2226 no . . C25 H16 3.3006 no . . C25 H18 3.2147 no . . H1 H2 2.3093 no . . H2 H3 2.3161 no . . H3 H4 2.3432 no . . H4 H19 2.2771 no . . H7 H9 2.7147 no . . H9 H10 2.3951 no . . H10 H12 2.7259 no . . H12 H13 2.3883 no . . H13 H15 2.7493 no . . H15 H16 2.3404 no . . H16 H18 2.7803 no . . H18 H19 2.3530 no . . N1 H2 3.5025 no . 2_654 N1 H12 2.8355 no . 4_665 N1 H13 2.8689 no . 3_565 C1 H7 2.9522 no . 2_655 C1 H13 3.0251 no . 3_565 C2 H3 3.4867 no . 2_654 C2 H7 3.1658 no . 2_655 C3 H16 3.3368 no . 4_674 C4 H16 3.1085 no . 4_674 C4 H18 3.4214 no . 4_674 C5 H2 3.4424 no . 2_654 C5 H12 3.0464 no . 4_665 C6 H10 2.9997 no . 4_665 C6 H12 3.1488 no . 4_665 C6 H18 3.2707 no . 4_674 C7 H1 3.3250 no . 2_654 C7 H2 3.3623 no . 2_654 C7 H10 2.8687 no . 4_665 C8 H10 2.7736 no . 4_665 C8 H18 3.0925 no . 1_554 C9 H10 3.2818 no . 4_665 C9 H18 3.0210 no . 1_554 C10 H16 3.2265 no . 1_554 C10 H18 3.3708 no . 1_554 C11 H9 3.1113 no . 4_665 C11 H16 3.0000 no . 1_554 C12 H1 3.5202 no . 3_465 C12 H9 3.0160 no . 4_665 C12 H15 3.1716 no . 2_554 C12 H16 3.4961 no . 1_554 C13 H1 3.0736 no . 3_465 C13 H9 2.8846 no . 4_665 C13 H15 2.7314 no . 2_554 C14 H3 3.5748 no . 3_475 C14 H3 3.5992 no . 4_674 C14 H9 2.8151 no . 4_665 C14 H15 3.5008 no . 2_554 C15 H2 3.4207 no . 3_475 C15 H3 2.9626 no . 3_475 C15 H9 3.2511 no . 4_665 C15 H13 3.4123 no . 2_555 C16 H2 3.0494 no . 3_475 C16 H3 3.1725 no . 3_475 C16 H4 3.5495 no . 4_675 C16 H10 3.5323 no . 1_556 C17 H2 2.8782 no . 3_475 C18 H4 3.4998 no . 4_675 C18 H9 3.5761 no . 1_556 C19 H10 3.5500 no . 4_665 C19 H18 3.5686 no . 4_674 C20 H10 2.9416 no . 4_665 C20 H12 3.5804 no . 4_665 C20 H18 2.9975 no . 4_674 C21 H10 2.9432 no . 4_665 C21 H18 3.2899 no . 4_674 C21 H19 3.1584 no . 4_674 C22 H4 3.1229 no . 4_674 C22 H10 2.8911 no . 4_665 C22 H18 3.2610 no . 1_554 C22 H19 3.3840 no . 4_674 C23 H3 3.5543 no . 4_674 C23 H4 2.8965 no . 4_674 C23 H9 3.1656 no . 4_665 C23 H10 3.3629 no . 4_665 C23 H16 3.4627 no . 1_554 C23 H18 3.5853 no . 1_554 C24 H2 3.2082 no . 3_475 C24 H3 3.3585 no . 4_674 C24 H4 3.3334 no . 4_674 C24 H9 3.0348 no . 4_665 C25 H2 2.8617 no . 3_475 C25 H9 3.5065 no . 4_665 C25 H10 3.4213 no . 4_665 C25 H19 3.5686 no . 4_674 H1 C7 3.3250 no . 2_655 H1 C12 3.5202 no . 3_565 H1 C13 3.0736 no . 3_565 H1 H7 2.5100 no . 2_655 H1 H12 3.3319 no . 3_565 H1 H13 2.5247 no . 3_565 H1 H19 3.1526 no . 2_654 H2 N1 3.5025 no . 2_655 H2 C5 3.4424 no . 2_655 H2 C7 3.3623 no . 2_655 H2 C15 3.4207 no . 3_575 H2 C16 3.0494 no . 3_575 H2 C17 2.8782 no . 3_575 H2 C24 3.2082 no . 3_575 H2 C25 2.8617 no . 3_575 H2 H7 2.9412 no . 2_655 H2 H16 3.4695 no . 3_575 H3 C2 3.4867 no . 2_655 H3 C14 3.5748 no . 3_575 H3 C14 3.5992 no . 4_675 H3 C15 2.9626 no . 3_575 H3 C16 3.1725 no . 3_575 H3 C23 3.5543 no . 4_675 H3 C24 3.3585 no . 4_675 H3 H15 2.9704 no . 3_575 H3 H16 3.2873 no . 3_575 H3 H16 3.2895 no . 4_674 H4 C16 3.5495 no . 4_674 H4 C18 3.4998 no . 4_674 H4 C22 3.1229 no . 4_675 H4 C23 2.8965 no . 4_675 H4 C24 3.3334 no . 4_675 H4 H16 2.8705 no . 4_674 H4 H18 2.7809 no . 4_674 H7 C1 2.9522 no . 2_654 H7 C2 3.1658 no . 2_654 H7 H1 2.5100 no . 2_654 H7 H2 2.9412 no . 2_654 H7 H10 3.4451 no . 4_665 H7 H13 3.5772 no . 4_664 H7 H15 3.3880 no . 4_664 H9 C11 3.1113 no . 4_664 H9 C12 3.0160 no . 4_664 H9 C13 2.8846 no . 4_664 H9 C14 2.8151 no . 4_664 H9 C15 3.2511 no . 4_664 H9 C18 3.5761 no . 1_554 H9 C23 3.1656 no . 4_664 H9 C24 3.0348 no . 4_664 H9 C25 3.5065 no . 4_664 H9 H13 3.4225 no . 4_664 H9 H18 3.3251 no . 1_554 H10 C6 2.9997 no . 4_664 H10 C7 2.8687 no . 4_664 H10 C8 2.7736 no . 4_664 H10 C9 3.2818 no . 4_664 H10 C16 3.5323 no . 1_554 H10 C19 3.5500 no . 4_664 H10 C20 2.9416 no . 4_664 H10 C21 2.9432 no . 4_664 H10 C22 2.8911 no . 4_664 H10 C23 3.3629 no . 4_664 H10 C25 3.4213 no . 4_664 H10 H7 3.4451 no . 4_664 H10 H16 3.3417 no . 1_554 H12 N1 2.8355 no . 4_664 H12 C5 3.0464 no . 4_664 H12 C6 3.1488 no . 4_664 H12 C20 3.5804 no . 4_664 H12 H1 3.3319 no . 3_465 H12 H13 3.3228 no . 2_554 H12 H15 3.2139 no . 2_554 H12 H16 3.5965 no . 1_554 H13 N1 2.8689 no . 3_465 H13 C1 3.0251 no . 3_465 H13 C15 3.4123 no . 2_554 H13 H1 2.5247 no . 3_465 H13 H7 3.5772 no . 4_665 H13 H9 3.4225 no . 4_665 H13 H12 3.3228 no . 2_555 H13 H15 2.4879 no . 2_554 H15 C12 3.1716 no . 2_555 H15 C13 2.7314 no . 2_555 H15 C14 3.5008 no . 2_555 H15 H3 2.9704 no . 3_475 H15 H7 3.3880 no . 4_665 H15 H12 3.2139 no . 2_555 H15 H13 2.4879 no . 2_555 H16 C3 3.3368 no . 4_675 H16 C4 3.1085 no . 4_675 H16 C10 3.2265 no . 1_556 H16 C11 3.0000 no . 1_556 H16 C12 3.4961 no . 1_556 H16 C23 3.4627 no . 1_556 H16 H2 3.4695 no . 3_475 H16 H3 3.2873 no . 3_475 H16 H3 3.2895 no . 4_675 H16 H4 2.8705 no . 4_675 H16 H10 3.3417 no . 1_556 H16 H12 3.5965 no . 1_556 H18 C4 3.4214 no . 4_675 H18 C6 3.2707 no . 4_675 H18 C8 3.0925 no . 1_556 H18 C9 3.0210 no . 1_556 H18 C10 3.3708 no . 1_556 H18 C19 3.5686 no . 4_675 H18 C20 2.9975 no . 4_675 H18 C21 3.2899 no . 4_675 H18 C22 3.2610 no . 1_556 H18 C23 3.5853 no . 1_556 H18 H4 2.7809 no . 4_675 H18 H9 3.3251 no . 1_556 H19 C21 3.1584 no . 4_675 H19 C22 3.3840 no . 4_675 H19 C25 3.5686 no . 4_675 H19 H1 3.1526 no . 2_655 data_pbca _database_code_depnum_ccdc_archive 'CCDC 911819' #TrackingRef 'CCDC911819_revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H18 B F4 N3 Pd' _chemical_formula_weight 601.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'Pbca ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 20.102(3) _cell_length_b 7.2793(9) _cell_length_c 64.688(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9466(2) _cell_formula_units_Z 16 _cell_measurement_temperature 93 _cell_measurement_reflns_used 3711 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 22.89 _exptl_crystal_description plate _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.689 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4800 _exptl_absorpt_coefficient_mu 0.841 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9132 _exptl_absorpt_correction_T_max 0.9834 _exptl_absorpt_process_details ; SADABS Sheldrick 1996 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 93 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker TXS fine-focus rotating anode' _diffrn_radiation_monochromator 'Bruker Helios multilayer confocal mirror' _diffrn_measurement_device_type 'Bruker APEXII CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.333 _diffrn_reflns_number 47213 _diffrn_reflns_av_R_equivalents 0.1285 _diffrn_reflns_av_unetI/netI 0.0898 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -77 _diffrn_reflns_limit_l_max 76 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 25.03 _reflns_number_total 8373 _reflns_number_gt 5883 _reflns_threshold_expression >2sigma _computing_data_collection 'APEX2 ' _computing_cell_refinement 'APEX2 ' _computing_data_reduction 'SAINT (Bruker AXS, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSHEL (Bruker AXS,2002)' _computing_publication_material 'XCIF (Bruker AXS, 2001)' _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. SADI restraint was used for BF4 (all distance between B-F and F-F) and aromatic rings (all distance between neighbor C-C). SIMU and ISOR restraints were also used for disordered BF4 anions. ; _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^)+(0.0000P)^2^+163.5502P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8373 _refine_ls_number_parameters 717 _refine_ls_number_restraints 793 _refine_ls_R_factor_all 0.1475 _refine_ls_R_factor_gt 0.1025 _refine_ls_wR_factor_ref 0.1846 _refine_ls_wR_factor_gt 0.1702 _refine_ls_goodness_of_fit_ref 1.228 _refine_ls_restrained_S_all 1.224 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group B1 B 0.6044(5) 0.8887(14) 0.10368(16) 0.034(3) Uani 1 1 d D . . B2 B 0.4046(5) 0.5464(15) 0.14378(16) 0.043(4) Uani 1 1 d D . . C1 C 0.1363(6) 0.2772(17) 0.08819(18) 0.034(3) Uani 1 1 d . . . H1 H 0.1542 0.2311 0.1008 0.041 Uiso 1 1 calc R . . C2 C 0.0687(6) 0.3097(17) 0.08693(19) 0.035(3) Uani 1 1 d . . . H2 H 0.0402 0.2837 0.0983 0.042 Uiso 1 1 calc R . . C3 C 0.0431(6) 0.3817(16) 0.0686(2) 0.036(3) Uani 1 1 d . . . H3 H -0.0029 0.4108 0.0674 0.044 Uiso 1 1 calc R . . C4 C 0.0852(6) 0.4094(16) 0.05226(18) 0.032(3) Uani 1 1 d . . . H4 H 0.0676 0.4538 0.0396 0.039 Uiso 1 1 calc R . . C5 C 0.1530(5) 0.3743(14) 0.05381(18) 0.026(3) Uani 1 1 d . . . C6 C 0.2034(5) 0.4034(14) 0.03815(15) 0.0272(19) Uani 1 1 d DU . . C7 C 0.2701(5) 0.3887(14) 0.04507(15) 0.0253(18) Uani 1 1 d DU . . C8 C 0.3258(5) 0.4126(14) 0.03165(15) 0.0284(18) Uani 1 1 d DU . . C9 C 0.3930(5) 0.3547(17) 0.03221(17) 0.037(3) Uani 1 1 d D . . H9 H 0.4110 0.3184 0.0452 0.044 Uiso 1 1 calc R . . C10 C 0.4349(6) 0.3477(18) 0.01472(16) 0.038(3) Uani 1 1 d D . . H10 H 0.4796 0.3085 0.0164 0.046 Uiso 1 1 calc R . . C11 C 0.4120(5) 0.3973(15) -0.00517(16) 0.035(3) Uani 1 1 d D . . C12 C 0.4358(6) 0.3572(17) -0.02547(17) 0.044(3) Uani 1 1 d D . . H12 H 0.4808 0.3201 -0.0271 0.053 Uiso 1 1 calc R . . C13 C 0.3957(6) 0.3700(16) -0.04316(19) 0.046(4) Uani 1 1 d D . . H13 H 0.4144 0.3396 -0.0562 0.055 Uiso 1 1 calc R . . C14 C 0.3281(6) 0.4268(17) -0.04232(17) 0.046(4) Uani 1 1 d D . . C15 C 0.2735(6) 0.3938(16) -0.05607(18) 0.040(3) Uani 1 1 d D . . H15 H 0.2821 0.3621 -0.0701 0.048 Uiso 1 1 calc R . . C16 C 0.2075(6) 0.4078(17) -0.04912(17) 0.043(4) Uani 1 1 d D . . H16 H 0.1728 0.3818 -0.0587 0.052 Uiso 1 1 calc R . . C17 C 0.1896(6) 0.4587(15) -0.02859(16) 0.039(3) Uani 1 1 d D . . C18 C 0.1308(6) 0.4254(16) -0.01708(17) 0.039(3) Uani 1 1 d D . . H18 H 0.0903 0.4077 -0.0244 0.047 Uiso 1 1 calc R . . C19 C 0.1296(6) 0.4175(15) 0.00457(16) 0.034(3) Uani 1 1 d D . . H19 H 0.0886 0.3910 0.0112 0.040 Uiso 1 1 calc R . . C20 C 0.1871(5) 0.4473(13) 0.01710(14) 0.0273(18) Uani 1 1 d DU . . C21 C 0.2423(5) 0.5090(14) 0.00546(14) 0.0298(19) Uani 1 1 d DU . . C22 C 0.3082(5) 0.4940(14) 0.01266(14) 0.0291(19) Uani 1 1 d DU . . C23 C 0.3489(5) 0.4807(15) -0.00514(16) 0.036(3) Uani 1 1 d D . . C24 C 0.3094(5) 0.4980(15) -0.02304(16) 0.034(3) Uani 1 1 d D . . C25 C 0.2432(5) 0.5128(14) -0.01627(15) 0.034(3) Uani 1 1 d D . . C26 C 0.8223(6) 0.2132(15) 0.15838(16) 0.028(3) Uani 1 1 d . . . H26 H 0.8039 0.2707 0.1465 0.034 Uiso 1 1 calc R . . C27 C 0.8911(5) 0.1773(16) 0.15937(18) 0.031(3) Uani 1 1 d . . . H27 H 0.9194 0.2058 0.1480 0.037 Uiso 1 1 calc R . . C28 C 0.9166(5) 0.0998(14) 0.17719(17) 0.026(3) Uani 1 1 d . . . H28 H 0.9629 0.0753 0.1783 0.031 Uiso 1 1 calc R . . C29 C 0.8743(6) 0.0582(16) 0.19336(18) 0.030(3) Uani 1 1 d . . . H29 H 0.8918 0.0031 0.2055 0.036 Uiso 1 1 calc R . . C30 C 0.8075(5) 0.0953(14) 0.19208(15) 0.020(2) Uani 1 1 d . . . C31 C 0.7563(5) 0.0578(14) 0.20784(14) 0.021(2) Uani 1 1 d D . . C32 C 0.6894(4) 0.0900(14) 0.20153(14) 0.021(2) Uani 1 1 d D . . C33 C 0.6340(4) 0.0748(14) 0.21528(15) 0.026(3) Uani 1 1 d D . . C34 C 0.5692(5) 0.1564(16) 0.21499(17) 0.032(3) Uani 1 1 d D . . H34 H 0.5521 0.1997 0.2022 0.039 Uiso 1 1 calc R . . C35 C 0.5301(5) 0.1751(16) 0.23285(15) 0.034(3) Uani 1 1 d D . . H35 H 0.4868 0.2261 0.2315 0.041 Uiso 1 1 calc R . . C36 C 0.5521(5) 0.1214(16) 0.25265(16) 0.038(3) Uani 1 1 d D . . C37 C 0.5314(6) 0.1741(19) 0.27283(16) 0.044(3) Uani 1 1 d D . . H37 H 0.4882 0.2242 0.2747 0.053 Uiso 1 1 calc R . . C38 C 0.5732(5) 0.1540(18) 0.28999(18) 0.042(3) Uani 1 1 d D . . H38 H 0.5581 0.1981 0.3030 0.051 Uiso 1 1 calc R . . C39 C 0.6370(5) 0.0710(18) 0.28889(16) 0.043(3) Uani 1 1 d D . . C40 C 0.6928(6) 0.090(2) 0.30211(19) 0.054(4) Uani 1 1 d D . . H40 H 0.6858 0.1289 0.3160 0.065 Uiso 1 1 calc R . . C41 C 0.7583(7) 0.053(2) 0.29550(17) 0.051(4) Uani 1 1 d D . . H41 H 0.7936 0.0617 0.3052 0.061 Uiso 1 1 calc R . . C42 C 0.7733(5) 0.0042(17) 0.27469(15) 0.041(3) Uani 1 1 d D . . C43 C 0.8323(6) 0.0214(18) 0.26282(17) 0.040(3) Uani 1 1 d D . . H43 H 0.8737 0.0302 0.2698 0.048 Uiso 1 1 calc R . . C44 C 0.8318(5) 0.0259(16) 0.24108(17) 0.035(3) Uani 1 1 d D . . H44 H 0.8730 0.0401 0.2341 0.042 Uiso 1 1 calc R . . C45 C 0.7724(5) 0.0103(16) 0.22901(14) 0.031(3) Uani 1 1 d D . . C46 C 0.7166(5) -0.0328(14) 0.24096(14) 0.028(3) Uani 1 1 d D . . C47 C 0.6508(5) -0.0022(16) 0.23436(15) 0.033(3) Uani 1 1 d D . . C48 C 0.6107(5) 0.0193(15) 0.25213(16) 0.033(3) Uani 1 1 d D . . C49 C 0.6508(5) -0.0044(17) 0.26956(15) 0.036(3) Uani 1 1 d D . . C50 C 0.7168(5) -0.0340(16) 0.26286(15) 0.033(3) Uani 1 1 d D . . C51 C 0.2874(6) 0.0760(19) 0.1429(2) 0.046(4) Uani 1 1 d . . . H51A H 0.3133 0.1645 0.1510 0.069 Uiso 1 1 calc R . . H51B H 0.3099 -0.0434 0.1430 0.069 Uiso 1 1 calc R . . H51C H 0.2429 0.0633 0.1489 0.069 Uiso 1 1 calc R . . C52 C 0.2815(5) 0.1406(15) 0.1218(2) 0.028(3) Uani 1 1 d . . . C53 C 0.4957(6) 0.348(2) 0.0926(2) 0.052(4) Uani 1 1 d . . . H53A H 0.5228 0.4083 0.0819 0.078 Uiso 1 1 calc R . . H53B H 0.5139 0.2264 0.0956 0.078 Uiso 1 1 calc R . . H53C H 0.4961 0.4228 0.1052 0.078 Uiso 1 1 calc R . . C54 C 0.4283(6) 0.3302(19) 0.08525(19) 0.039(3) Uani 1 1 d . . . C55 C 0.6799(6) 0.3756(17) 0.10279(18) 0.037(3) Uani 1 1 d . . . H55A H 0.6528 0.4873 0.1020 0.056 Uiso 1 1 calc R . . H55B H 0.6606 0.2808 0.0938 0.056 Uiso 1 1 calc R . . H55C H 0.7253 0.4028 0.0983 0.056 Uiso 1 1 calc R . . C56 C 0.6811(5) 0.3101(15) 0.12401(18) 0.027(2) Uani 1 1 d . . . C57 C 0.4660(6) 0.054(2) 0.1542(2) 0.049(4) Uani 1 1 d . . . H57A H 0.4495 0.1569 0.1459 0.073 Uiso 1 1 calc R . . H57B H 0.4363 0.0341 0.1660 0.073 Uiso 1 1 calc R . . H57C H 0.4673 -0.0574 0.1457 0.073 Uiso 1 1 calc R . . C58 C 0.5328(5) 0.0957(16) 0.16169(18) 0.028(3) Uani 1 1 d . . . F1 F 0.6029(4) 1.0034(11) 0.08670(11) 0.060(2) Uani 1 1 d D . . F2 F 0.6670(3) 0.8742(10) 0.11124(11) 0.048(2) Uani 1 1 d D . . F3 F 0.5821(3) 0.7206(9) 0.09737(12) 0.052(2) Uani 1 1 d D . . F4 F 0.5618(3) 0.9604(11) 0.11813(10) 0.053(2) Uani 1 1 d D . . F5 F 0.3685(4) 0.7009(12) 0.1439(2) 0.133(5) Uani 1 1 d D A . F6A F 0.3809(7) 0.4317(17) 0.12919(19) 0.084(6) Uani 0.696(17) 1 d PDU A 1 F7A F 0.4129(10) 0.457(2) 0.16199(17) 0.116(8) Uani 0.696(17) 1 d PDU A 1 F8A F 0.4685(4) 0.592(2) 0.1373(2) 0.089(6) Uani 0.696(17) 1 d PDU A 1 F6B F 0.3643(9) 0.410(2) 0.1521(4) 0.041(8) Uani 0.304(17) 1 d PDU A 2 F7B F 0.4472(16) 0.605(5) 0.1579(4) 0.107(15) Uani 0.304(17) 1 d PDU A 2 F8B F 0.434(2) 0.513(5) 0.1255(4) 0.153(18) Uani 0.304(17) 1 d PDU A 2 N1 N 0.1777(5) 0.3088(14) 0.07224(14) 0.034(2) Uani 1 1 d . . . N2 N 0.7819(4) 0.1652(11) 0.17455(14) 0.025(2) Uani 1 1 d . . . N3 N 0.2755(5) 0.1952(15) 0.10526(15) 0.036(2) Uani 1 1 d . . . N4 N 0.3757(5) 0.3203(14) 0.07900(15) 0.037(3) Uani 1 1 d . . . N5 N 0.6828(4) 0.2606(12) 0.14080(14) 0.025(2) Uani 1 1 d . . . N6 N 0.5844(5) 0.1282(12) 0.16784(14) 0.025(2) Uani 1 1 d . . . Pd1 Pd 0.68310(4) 0.16780(11) 0.171791(13) 0.0225(2) Uani 1 1 d . . . Pd2 Pd 0.27599(4) 0.29929(12) 0.074603(13) 0.0274(2) 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 B1 0.024(7) 0.035(9) 0.044(9) 0.004(7) 0.000(7) -0.006(6) B2 0.041(9) 0.060(11) 0.028(8) 0.015(8) 0.004(8) 0.025(8) C1 0.031(6) 0.043(8) 0.029(6) -0.013(6) 0.004(5) -0.010(6) C2 0.028(6) 0.027(7) 0.049(8) -0.009(6) 0.015(6) -0.005(6) C3 0.030(7) 0.023(7) 0.056(9) -0.013(6) 0.005(6) 0.007(5) C4 0.037(7) 0.028(7) 0.032(7) -0.007(6) -0.005(6) -0.001(6) C5 0.026(6) 0.010(6) 0.044(7) -0.008(5) 0.003(5) -0.007(5) C6 0.038(4) 0.010(3) 0.034(4) -0.008(3) 0.002(4) 0.001(3) C7 0.036(4) 0.012(3) 0.028(4) -0.013(3) 0.004(4) -0.001(3) C8 0.040(4) 0.016(4) 0.029(4) -0.010(3) 0.005(4) -0.003(4) C9 0.033(7) 0.042(8) 0.036(7) -0.016(6) -0.004(6) -0.024(6) C10 0.028(6) 0.040(8) 0.047(8) -0.011(7) 0.009(6) -0.009(6) C11 0.037(7) 0.022(6) 0.048(8) -0.007(6) 0.014(6) -0.014(6) C12 0.046(8) 0.034(8) 0.052(8) -0.003(7) 0.015(7) -0.024(6) C13 0.061(9) 0.024(7) 0.052(9) -0.006(6) 0.028(8) -0.017(7) C14 0.076(11) 0.022(7) 0.041(8) 0.002(6) 0.011(8) -0.012(7) C15 0.065(9) 0.029(7) 0.027(6) 0.000(5) 0.007(7) -0.005(7) C16 0.064(10) 0.033(8) 0.033(7) 0.013(6) -0.002(7) -0.003(7) C17 0.066(9) 0.015(6) 0.037(7) 0.007(5) 0.000(7) 0.016(6) C18 0.049(8) 0.024(7) 0.044(8) 0.002(6) -0.005(7) 0.016(6) C19 0.042(7) 0.021(6) 0.037(7) -0.007(6) 0.001(6) 0.008(6) C20 0.041(4) 0.006(3) 0.035(4) -0.007(3) 0.002(4) 0.004(3) C21 0.044(4) 0.010(4) 0.036(4) -0.004(3) 0.004(4) 0.002(4) C22 0.042(4) 0.013(4) 0.032(4) -0.003(3) 0.007(4) -0.001(4) C23 0.057(8) 0.012(6) 0.040(8) -0.003(6) 0.010(7) -0.014(6) C24 0.050(8) 0.013(6) 0.037(7) -0.003(5) 0.014(7) -0.014(6) C25 0.059(9) 0.006(5) 0.038(7) -0.002(5) -0.002(7) 0.002(6) C26 0.036(6) 0.026(6) 0.022(6) -0.001(5) -0.003(5) -0.003(6) C27 0.030(6) 0.024(6) 0.038(7) 0.001(6) 0.011(5) -0.001(6) C28 0.025(6) 0.018(6) 0.035(7) -0.013(5) 0.002(5) 0.001(5) C29 0.033(7) 0.024(6) 0.033(7) -0.003(5) -0.007(6) -0.001(5) C30 0.022(6) 0.015(5) 0.022(6) 0.003(5) 0.001(5) 0.002(5) C31 0.019(5) 0.012(5) 0.031(6) -0.001(5) 0.001(5) 0.005(4) C32 0.031(6) 0.021(6) 0.012(5) -0.005(4) -0.004(5) 0.001(5) C33 0.026(6) 0.018(6) 0.034(7) 0.005(5) 0.009(5) -0.009(5) C34 0.024(6) 0.025(7) 0.048(7) -0.001(6) 0.011(5) -0.009(5) C35 0.027(6) 0.023(6) 0.051(8) -0.004(6) 0.010(6) 0.002(6) C36 0.026(6) 0.041(8) 0.047(8) 0.005(7) 0.014(6) -0.012(6) C37 0.042(7) 0.046(8) 0.045(8) 0.001(7) 0.017(7) -0.002(7) C38 0.048(8) 0.043(8) 0.037(7) 0.002(7) 0.019(6) -0.010(7) C39 0.044(8) 0.051(9) 0.033(7) 0.011(7) 0.014(7) -0.007(7) C40 0.070(10) 0.060(10) 0.032(7) 0.017(7) 0.008(8) 0.010(9) C41 0.054(10) 0.058(10) 0.041(8) 0.020(8) 0.008(7) 0.008(8) C42 0.053(8) 0.040(8) 0.029(7) 0.018(6) 0.006(7) 0.016(7) C43 0.037(8) 0.042(8) 0.040(8) 0.008(6) 0.000(6) 0.011(6) C44 0.033(7) 0.023(6) 0.048(8) 0.006(6) 0.005(6) 0.004(5) C45 0.023(6) 0.037(7) 0.033(6) 0.000(6) 0.002(5) 0.006(6) C46 0.042(7) 0.012(5) 0.030(6) -0.001(5) 0.001(6) -0.004(5) C47 0.029(7) 0.026(7) 0.044(8) 0.008(6) 0.014(6) -0.003(6) C48 0.044(7) 0.020(6) 0.036(7) 0.006(6) 0.006(6) 0.002(6) C49 0.048(8) 0.033(7) 0.028(7) 0.009(6) 0.010(6) -0.007(6) C50 0.041(7) 0.025(6) 0.034(7) 0.019(6) 0.010(6) 0.000(6) C51 0.027(7) 0.052(9) 0.059(9) 0.006(8) -0.006(7) -0.011(6) C52 0.019(6) 0.016(6) 0.050(8) -0.015(6) 0.003(6) 0.006(5) C53 0.038(7) 0.039(8) 0.079(10) 0.003(8) -0.012(7) 0.007(7) C54 0.039(7) 0.038(8) 0.040(7) -0.014(7) -0.004(6) 0.012(7) C55 0.032(7) 0.039(8) 0.040(7) 0.009(6) -0.003(6) 0.007(6) C56 0.024(6) 0.015(6) 0.041(7) -0.006(6) 0.001(6) 0.004(5) C57 0.023(7) 0.074(11) 0.049(9) -0.017(8) -0.007(6) 0.012(7) C58 0.015(6) 0.032(7) 0.036(7) -0.006(6) -0.008(5) 0.001(5) F1 0.049(5) 0.064(6) 0.066(5) 0.031(5) 0.001(4) -0.008(4) F2 0.023(4) 0.050(5) 0.070(5) -0.008(4) -0.014(3) 0.005(3) F3 0.038(4) 0.036(4) 0.083(6) -0.013(4) -0.014(4) 0.005(4) F4 0.040(4) 0.081(6) 0.039(4) -0.016(4) 0.007(4) 0.012(4) F5 0.054(6) 0.051(7) 0.294(17) 0.029(9) 0.016(8) 0.008(5) F6A 0.089(11) 0.105(12) 0.059(9) -0.027(8) -0.013(8) -0.060(9) F7A 0.20(2) 0.093(14) 0.056(9) 0.010(9) 0.020(12) 0.067(15) F8A 0.021(6) 0.137(14) 0.108(14) -0.066(11) -0.003(7) -0.007(7) F6B 0.018(12) 0.016(11) 0.09(2) 0.003(13) -0.007(12) -0.005(9) F7B 0.10(2) 0.15(3) 0.07(2) 0.06(2) -0.07(2) -0.07(2) F8B 0.18(4) 0.17(4) 0.11(3) -0.03(3) 0.06(3) -0.03(4) N1 0.034(5) 0.035(6) 0.032(5) -0.009(5) 0.005(5) -0.007(5) N2 0.026(5) 0.009(4) 0.039(5) -0.004(4) 0.014(4) 0.005(4) N3 0.033(5) 0.041(6) 0.032(5) -0.018(6) 0.003(5) -0.006(5) N4 0.038(6) 0.030(6) 0.043(6) 0.012(5) -0.001(5) 0.018(5) N5 0.024(5) 0.024(5) 0.027(5) -0.010(4) 0.000(4) 0.001(4) N6 0.029(5) 0.017(5) 0.029(5) -0.004(4) 0.007(4) 0.009(4) Pd1 0.0211(4) 0.0176(4) 0.0288(4) -0.0040(4) 0.0020(4) -0.0006(4) Pd2 0.0266(4) 0.0247(4) 0.0310(5) -0.0094(4) 0.0036(4) -0.0035(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag B1 F2 1.354(10) . ? B1 F3 1.366(10) . ? B1 F4 1.370(10) . ? B1 F1 1.380(10) . ? B2 F7B 1.324(13) . ? B2 F8B 1.338(13) . ? B2 F5 1.339(11) . ? B2 F6A 1.347(11) . ? B2 F7A 1.357(11) . ? B2 F6B 1.387(12) . ? B2 F8A 1.390(11) . ? C1 N1 1.345(14) . ? C1 C2 1.383(15) . ? C1 H1 0.9500 . ? C2 C3 1.397(17) . ? C2 H2 0.9500 . ? C3 C4 1.367(16) . ? C3 H3 0.9500 . ? C4 C5 1.391(15) . ? C4 H4 0.9500 . ? C5 N1 1.377(14) . ? C5 C6 1.448(15) . ? C6 C7 1.418(11) . ? C6 C20 1.437(10) . ? C7 C8 1.427(10) . ? C7 Pd2 2.022(10) . ? C8 C22 1.409(10) . ? C8 C9 1.415(11) . ? C9 C10 1.411(11) . ? C9 H9 0.9500 . ? C10 C11 1.413(11) . ? C10 H10 0.9500 . ? C11 C23 1.405(11) . ? C11 C12 1.428(11) . ? C12 C13 1.403(11) . ? C12 H12 0.9500 . ? C13 C14 1.421(11) . ? C13 H13 0.9500 . ? C14 C24 1.401(11) . ? C14 C15 1.432(11) . ? C15 C16 1.406(11) . ? C15 H15 0.9500 . ? C16 C17 1.425(11) . ? C16 H16 0.9500 . ? C17 C25 1.396(11) . ? C17 C18 1.419(11) . ? C18 C19 1.402(11) . ? C18 H18 0.9500 . ? C19 C20 1.428(11) . ? C19 H19 0.9500 . ? C20 C21 1.414(10) . ? C21 C25 1.406(10) . ? C21 C22 1.409(11) . ? C22 C23 1.416(11) . ? C23 C24 1.410(11) . ? C24 C25 1.407(11) . ? C26 N2 1.370(13) . ? C26 C27 1.409(15) . ? C26 H26 0.9500 . ? C27 C28 1.382(15) . ? C27 H27 0.9500 . ? C28 C29 1.381(15) . ? C28 H28 0.9500 . ? C29 C30 1.373(15) . ? C29 H29 0.9500 . ? C30 N2 1.346(13) . ? C30 C31 1.474(14) . ? C31 C32 1.425(10) . ? C31 C45 1.449(10) . ? C32 C33 1.430(10) . ? C32 Pd1 2.010(9) . ? C33 C47 1.397(10) . ? C33 C34 1.431(10) . ? C34 C35 1.405(10) . ? C34 H34 0.9500 . ? C35 C36 1.411(11) . ? C35 H35 0.9500 . ? C36 C48 1.392(11) . ? C36 C37 1.423(11) . ? C37 C38 1.399(11) . ? C37 H37 0.9500 . ? C38 C39 1.420(11) . ? C38 H38 0.9500 . ? C39 C49 1.393(11) . ? C39 C40 1.417(11) . ? C40 C41 1.411(12) . ? C40 H40 0.9500 . ? C41 C42 1.425(11) . ? C41 H41 0.9500 . ? C42 C50 1.398(11) . ? C42 C43 1.418(11) . ? C43 C44 1.407(11) . ? C43 H43 0.9500 . ? C44 C45 1.431(11) . ? C44 H44 0.9500 . ? C45 C46 1.398(10) . ? C46 C47 1.408(10) . ? C46 C50 1.417(10) . ? C47 C48 1.413(11) . ? C48 C49 1.398(11) . ? C49 C50 1.412(11) . ? C51 C52 1.447(17) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 N3 1.146(14) . ? C53 C54 1.441(17) . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 N4 1.133(14) . ? C55 C56 1.453(16) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 N5 1.145(13) . ? C57 C58 1.460(15) . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 N6 1.135(13) . ? N1 Pd2 1.982(9) . ? N2 Pd1 1.994(8) . ? N3 Pd2 2.123(10) . ? N4 Pd2 2.031(10) . ? N5 Pd1 2.115(9) . ? N6 Pd1 2.022(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F2 B1 F3 110.1(8) . . ? F2 B1 F4 111.3(9) . . ? F3 B1 F4 109.9(8) . . ? F2 B1 F1 110.7(8) . . ? F3 B1 F1 107.3(9) . . ? F4 B1 F1 107.4(8) . . ? F7B B2 F8B 112.7(15) . . ? F7B B2 F5 94(2) . . ? F8B B2 F5 113.0(14) . . ? F7B B2 F6A 156(2) . . ? F8B B2 F6A 55(2) . . ? F5 B2 F6A 109.3(10) . . ? F7B B2 F7A 58.4(12) . . ? F8B B2 F7A 128.7(17) . . ? F5 B2 F7A 117.9(12) . . ? F6A B2 F7A 110.7(10) . . ? F7B B2 F6B 110.0(12) . . ? F8B B2 F6B 118(2) . . ? F5 B2 F6B 106.3(10) . . ? F6A B2 F6B 67.7(13) . . ? F7A B2 F6B 52.7(10) . . ? F7B B2 F8A 62.3(15) . . ? F8B B2 F8A 51.3(19) . . ? F5 B2 F8A 107.6(9) . . ? F6A B2 F8A 105.3(11) . . ? F7A B2 F8A 105.2(10) . . ? F6B B2 F8A 145.7(12) . . ? N1 C1 C2 122.3(12) . . ? N1 C1 H1 118.9 . . ? C2 C1 H1 118.9 . . ? C1 C2 C3 118.5(11) . . ? C1 C2 H2 120.8 . . ? C3 C2 H2 120.8 . . ? C4 C3 C2 118.9(11) . . ? C4 C3 H3 120.5 . . ? C2 C3 H3 120.5 . . ? C3 C4 C5 121.6(12) . . ? C3 C4 H4 119.2 . . ? C5 C4 H4 119.2 . . ? N1 C5 C4 118.7(10) . . ? N1 C5 C6 113.8(9) . . ? C4 C5 C6 127.5(11) . . ? C7 C6 C20 122.1(10) . . ? C7 C6 C5 115.5(9) . . ? C20 C6 C5 122.4(9) . . ? C6 C7 C8 122.7(9) . . ? C6 C7 Pd2 112.2(7) . . ? C8 C7 Pd2 124.6(7) . . ? C22 C8 C9 112.7(9) . . ? C22 C8 C7 112.6(9) . . ? C9 C8 C7 134.2(9) . . ? C10 C9 C8 124.0(11) . . ? C10 C9 H9 118.0 . . ? C8 C9 H9 118.0 . . ? C9 C10 C11 121.7(10) . . ? C9 C10 H10 119.1 . . ? C11 C10 H10 119.1 . . ? C23 C11 C10 113.8(9) . . ? C23 C11 C12 113.1(10) . . ? C10 C11 C12 132.5(11) . . ? C13 C12 C11 122.9(12) . . ? C13 C12 H12 118.5 . . ? C11 C12 H12 118.5 . . ? C12 C13 C14 122.5(11) . . ? C12 C13 H13 118.7 . . ? C14 C13 H13 118.7 . . ? C24 C14 C13 113.4(10) . . ? C24 C14 C15 114.2(10) . . ? C13 C14 C15 131.3(11) . . ? C16 C15 C14 120.9(11) . . ? C16 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? C15 C16 C17 123.7(11) . . ? C15 C16 H16 118.2 . . ? C17 C16 H16 118.2 . . ? C25 C17 C18 113.0(10) . . ? C25 C17 C16 114.3(10) . . ? C18 C17 C16 130.9(11) . . ? C19 C18 C17 123.1(11) . . ? C19 C18 H18 118.5 . . ? C17 C18 H18 118.5 . . ? C18 C19 C20 123.2(11) . . ? C18 C19 H19 118.4 . . ? C20 C19 H19 118.4 . . ? C21 C20 C19 112.4(9) . . ? C21 C20 C6 113.3(9) . . ? C19 C20 C6 133.5(9) . . ? C25 C21 C22 108.7(9) . . ? C25 C21 C20 123.2(9) . . ? C22 C21 C20 122.5(9) . . ? C21 C22 C8 123.8(9) . . ? C21 C22 C23 106.3(9) . . ? C8 C22 C23 122.4(9) . . ? C11 C23 C24 123.1(10) . . ? C11 C23 C22 123.5(10) . . ? C24 C23 C22 109.7(9) . . ? C14 C24 C25 124.0(10) . . ? C14 C24 C23 123.2(10) . . ? C25 C24 C23 106.5(9) . . ? C17 C25 C21 123.8(10) . . ? C17 C25 C24 122.0(9) . . ? C21 C25 C24 108.7(9) . . ? N2 C26 C27 120.0(10) . . ? N2 C26 H26 120.0 . . ? C27 C26 H26 120.0 . . ? C28 C27 C26 118.5(10) . . ? C28 C27 H27 120.8 . . ? C26 C27 H27 120.8 . . ? C29 C28 C27 119.6(10) . . ? C29 C28 H28 120.2 . . ? C27 C28 H28 120.2 . . ? C30 C29 C28 120.9(11) . . ? C30 C29 H29 119.6 . . ? C28 C29 H29 119.6 . . ? N2 C30 C29 120.0(10) . . ? N2 C30 C31 112.7(8) . . ? C29 C30 C31 127.2(10) . . ? C32 C31 C45 121.4(9) . . ? C32 C31 C30 115.5(8) . . ? C45 C31 C30 122.8(8) . . ? C31 C32 C33 123.0(9) . . ? C31 C32 Pd1 112.3(6) . . ? C33 C32 Pd1 124.6(7) . . ? C47 C33 C32 113.1(8) . . ? C47 C33 C34 113.5(9) . . ? C32 C33 C34 131.9(9) . . ? C35 C34 C33 122.6(10) . . ? C35 C34 H34 118.7 . . ? C33 C34 H34 118.7 . . ? C34 C35 C36 122.9(10) . . ? C34 C35 H35 118.5 . . ? C36 C35 H35 118.5 . . ? C48 C36 C35 113.1(9) . . ? C48 C36 C37 114.4(10) . . ? C35 C36 C37 131.8(10) . . ? C38 C37 C36 121.6(11) . . ? C38 C37 H37 119.2 . . ? C36 C37 H37 119.2 . . ? C37 C38 C39 123.1(11) . . ? C37 C38 H38 118.4 . . ? C39 C38 H38 118.4 . . ? C49 C39 C40 115.0(10) . . ? C49 C39 C38 113.1(10) . . ? C40 C39 C38 130.1(11) . . ? C41 C40 C39 122.5(12) . . ? C41 C40 H40 118.7 . . ? C39 C40 H40 118.7 . . ? C40 C41 C42 122.1(12) . . ? C40 C41 H41 119.0 . . ? C42 C41 H41 119.0 . . ? C50 C42 C43 113.7(9) . . ? C50 C42 C41 113.3(10) . . ? C43 C42 C41 131.7(11) . . ? C44 C43 C42 122.5(11) . . ? C44 C43 H43 118.8 . . ? C42 C43 H43 118.8 . . ? C43 C44 C45 123.4(10) . . ? C43 C44 H44 118.3 . . ? C45 C44 H44 118.3 . . ? C46 C45 C44 112.7(9) . . ? C46 C45 C31 113.4(8) . . ? C44 C45 C31 133.1(9) . . ? C45 C46 C47 123.4(9) . . ? C45 C46 C50 123.6(9) . . ? C47 C46 C50 107.8(9) . . ? C33 C47 C46 124.0(9) . . ? C33 C47 C48 122.4(9) . . ? C46 C47 C48 107.9(9) . . ? C36 C48 C49 122.3(10) . . ? C36 C48 C47 124.2(9) . . ? C49 C48 C47 108.2(9) . . ? C39 C49 C48 124.1(10) . . ? C39 C49 C50 121.5(10) . . ? C48 C49 C50 108.3(9) . . ? C42 C50 C49 124.4(10) . . ? C42 C50 C46 123.2(9) . . ? C49 C50 C46 107.7(9) . . ? C52 C51 H51A 109.5 . . ? C52 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C52 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? N3 C52 C51 178.0(13) . . ? C54 C53 H53A 109.5 . . ? C54 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C54 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? N4 C54 C53 177.6(16) . . ? C56 C55 H55A 109.5 . . ? C56 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C56 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? N5 C56 C55 178.9(13) . . ? C58 C57 H57A 109.5 . . ? C58 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C58 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? N6 C58 C57 178.8(13) . . ? C1 N1 C5 120.0(10) . . ? C1 N1 Pd2 123.4(8) . . ? C5 N1 Pd2 116.0(7) . . ? C30 N2 C26 120.9(9) . . ? C30 N2 Pd1 117.4(7) . . ? C26 N2 Pd1 121.3(7) . . ? C52 N3 Pd2 173.6(10) . . ? C54 N4 Pd2 167.1(10) . . ? C56 N5 Pd1 178.5(9) . . ? C58 N6 Pd1 166.0(9) . . ? N2 Pd1 C32 81.3(4) . . ? N2 Pd1 N6 171.0(3) . . ? C32 Pd1 N6 98.2(4) . . ? N2 Pd1 N5 95.2(4) . . ? C32 Pd1 N5 175.9(4) . . ? N6 Pd1 N5 85.6(3) . . ? N1 Pd2 C7 81.8(4) . . ? N1 Pd2 N4 172.7(4) . . ? C7 Pd2 N4 99.5(4) . . ? N1 Pd2 N3 94.6(4) . . ? C7 Pd2 N3 175.8(4) . . ? N4 Pd2 N3 84.3(4) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.215 _refine_diff_density_min -2.764 _refine_diff_density_rms 0.153