Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Jerome Durand' _publ_contact_author_email DURAND@CHIMIE.UPS-TLSE.FR loop_ _publ_author_name J.Durand C.Carfagna B.Milani E.Zangrando data_2c _database_code_depnum_ccdc_archive 'CCDC 667850' _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis-[(S,S)-3,3-(2,3-butylenedioxy)]-2,2-bipyridine)-palladium(II) bis(hexafluorophosphate) ; _chemical_name_common ; bis-((S,S)-3,3-(2,3-butylenedioxy))-2,2-bipyridine)- palladium(ii) bis(hexafluorophosphate) ; _chemical_melting_point ? _chemical_formula_moiety 'C28 H28 N4 O4 Pd 2+, 2(P F6 1-)' _chemical_formula_sum 'C28 H28 F12 N4 O4 P2 Pd' _chemical_formula_weight 880.88 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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.438(3) _cell_length_b 10.834(4) _cell_length_c 16.503(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.89(3) _cell_angle_gamma 90.00 _cell_volume 1671.5(9) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour yellow _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.750 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 880 _exptl_absorpt_coefficient_mu 0.759 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.5881 _exptl_absorpt_correction_T_max 0.9134 _exptl_absorpt_process_details ; Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56 Cubic fit to sin(theta)/lambda - 24 parameters ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mok\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'image plate dip1030' _diffrn_measurement_method 'laser scanner' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17414 _diffrn_reflns_av_R_equivalents 0.0310 _diffrn_reflns_av_sigmaI/netI 0.0561 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 27.10 _reflns_number_total 6437 _reflns_number_gt 5558 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Xpress' _computing_cell_refinement 'Mosflm (Acta Cryst. D50, 760, 1994)' _computing_data_reduction 'Scala (Acta Cryst. D50, 760, 1994)' _computing_structure_solution 'SHELX97 (Sheldrick, 1998)' _computing_structure_refinement 'SHELX97 (Sheldrick, 1998)' _computing_molecular_graphics 'Ortep3/windows (Farrugia,1997)' _computing_publication_material 'Wingx 1.70.00 (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0479P)^2^+0.8580P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.03(3) _refine_ls_number_reflns 6437 _refine_ls_number_parameters 460 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0508 _refine_ls_R_factor_gt 0.0412 _refine_ls_wR_factor_ref 0.1140 _refine_ls_wR_factor_gt 0.1052 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd 0.49915(4) 0.40252(7) 0.25609(2) 0.04988(11) Uani 1 1 d . . . N1 N 0.3043(4) 0.4089(8) 0.2195(2) 0.0580(11) Uani 1 1 d . . . N2 N 0.4053(5) 0.2507(5) 0.3095(3) 0.0609(12) Uani 1 1 d . . . O1 O 0.0285(4) 0.1843(4) 0.1903(3) 0.0692(11) Uani 1 1 d . . . O2 O 0.1875(6) 0.0077(5) 0.2356(5) 0.112(2) Uani 1 1 d . . . C1 C 0.2424(9) 0.5085(8) 0.1964(5) 0.0624(19) Uani 1 1 d . . . H1 H 0.2920 0.5828 0.2018 0.075 Uiso 1 1 calc R . . C2 C 0.1124(8) 0.5061(9) 0.1658(5) 0.078(3) Uani 1 1 d . . . H2 H 0.0631 0.5778 0.1484 0.094 Uiso 1 1 calc R . . C3 C 0.0479(6) 0.3938(9) 0.1595(3) 0.0739(17) Uani 1 1 d . . . H3 H -0.0460 0.3909 0.1335 0.089 Uiso 1 1 calc R . . C4 C 0.1066(7) 0.2879(6) 0.1870(4) 0.0605(16) Uani 1 1 d . . . C5 C 0.2375(8) 0.2952(7) 0.2194(4) 0.0546(16) Uani 1 1 d . . . C6 C 0.3020(6) 0.2018(6) 0.2668(4) 0.0611(15) Uani 1 1 d . . . C7 C 0.2635(8) 0.0783(7) 0.2817(5) 0.084(2) Uani 1 1 d . . . C8 C 0.3073(9) 0.0191(8) 0.3497(6) 0.102(3) Uani 1 1 d . . . H8 H 0.2732 -0.0584 0.3616 0.123 Uiso 1 1 calc R . . C9 C 0.3959(9) 0.0741(9) 0.3956(6) 0.098(3) Uani 1 1 d . . . H9 H 0.4311 0.0400 0.4461 0.118 Uiso 1 1 calc R . . C10 C 0.4467(7) 0.1910(7) 0.3730(4) 0.0733(19) Uani 1 1 d . . . H10 H 0.5187 0.2269 0.4095 0.088 Uiso 1 1 calc R . . C21 C 0.0841(10) 0.1457(10) 0.0426(5) 0.119(3) Uani 1 1 d . . . H21A H 0.1710 0.1925 0.0455 0.178 Uiso 1 1 calc R . . H21B H 0.0039 0.1987 0.0257 0.178 Uiso 1 1 calc R . . H21C H 0.0857 0.0799 0.0038 0.178 Uiso 1 1 calc R . . C22 C 0.0703(8) 0.0899(8) 0.1297(4) 0.090(2) Uani 1 1 d . . . H22 H -0.0050 0.0270 0.1223 0.108 Uiso 1 1 calc R . . C23 C 0.2027(9) 0.0280(8) 0.1498(6) 0.098(3) Uani 1 1 d . . . H23 H 0.2820 0.0849 0.1456 0.118 Uiso 1 1 calc R . . C24 C 0.2297(12) -0.0977(10) 0.1073(8) 0.151(4) Uani 1 1 d . . . H24A H 0.1436 -0.1460 0.1012 0.227 Uiso 1 1 calc R . . H24B H 0.3046 -0.1421 0.1404 0.227 Uiso 1 1 calc R . . H24C H 0.2575 -0.0820 0.0545 0.227 Uiso 1 1 calc R . . N3 N 0.6963(4) 0.3974(7) 0.2940(2) 0.0520(10) Uani 1 1 d . . . N4 N 0.5919(5) 0.5553(4) 0.2032(2) 0.0512(11) Uani 1 1 d . . . O3 O 0.9043(4) 0.6360(4) 0.3792(3) 0.0735(13) Uani 1 1 d . . . O4 O 0.8898(4) 0.7520(4) 0.2388(2) 0.0603(10) Uani 1 1 d . . . C11 C 0.7586(9) 0.2978(7) 0.3216(5) 0.064(2) Uani 1 1 d . . . H11 H 0.7170 0.2205 0.3115 0.077 Uiso 1 1 calc R . . C12 C 0.8757(8) 0.3108(6) 0.3619(5) 0.0656(19) Uani 1 1 d . . . H12 H 0.9325 0.2431 0.3793 0.079 Uiso 1 1 calc R . . C13 C 0.9190(6) 0.4247(7) 0.3799(3) 0.0673(18) Uani 1 1 d . . . H13 H 1.0026 0.4327 0.4166 0.081 Uiso 1 1 calc R . . C14 C 0.8565(6) 0.5295(6) 0.3515(4) 0.0540(14) Uani 1 1 d . . . C15 C 0.7504(7) 0.5105(6) 0.3005(4) 0.0464(14) Uani 1 1 d . . . C16 C 0.7003(6) 0.6008(5) 0.2411(3) 0.0469(12) Uani 1 1 d . . . C17 C 0.7676(6) 0.7109(5) 0.2117(3) 0.0519(12) Uani 1 1 d . . . C18 C 0.7199(7) 0.7707(6) 0.1469(4) 0.0635(16) Uani 1 1 d . . . H18 H 0.7599 0.8434 0.1305 0.076 Uiso 1 1 calc R . . C19 C 0.6125(8) 0.7191(7) 0.1084(4) 0.0703(19) Uani 1 1 d . . . H19 H 0.5711 0.7527 0.0589 0.084 Uiso 1 1 calc R . . C20 C 0.5522(7) 0.6112(6) 0.1380(3) 0.0633(16) Uani 1 1 d . . . H20 H 0.4737 0.5782 0.1049 0.076 Uiso 1 1 calc R . . C25 C 0.8319(9) 0.8066(7) 0.4654(4) 0.090(2) Uani 1 1 d . . . H25A H 0.8193 0.7469 0.5068 0.136 Uiso 1 1 calc R . . H25B H 0.7621 0.8709 0.4657 0.136 Uiso 1 1 calc R . . H25C H 0.9262 0.8413 0.4762 0.136 Uiso 1 1 calc R . . C26 C 0.8137(7) 0.7461(6) 0.3848(4) 0.0652(16) Uani 1 1 d . . . H26 H 0.7129 0.7246 0.3688 0.078 Uiso 1 1 calc R . . C27 C 0.8713(7) 0.8273(6) 0.3126(4) 0.0678(16) Uani 1 1 d . . . H27 H 0.9672 0.8558 0.3351 0.081 Uiso 1 1 calc R . . C28 C 0.7786(11) 0.9401(6) 0.3046(5) 0.097(3) Uani 1 1 d . . . H28A H 0.7984 0.9877 0.2583 0.146 Uiso 1 1 calc R . . H28B H 0.7982 0.9890 0.3533 0.146 Uiso 1 1 calc R . . H28C H 0.6799 0.9159 0.2969 0.146 Uiso 1 1 calc R . . P1 P 0.6378(2) 0.1371(2) 0.07736(11) 0.0703(5) Uani 1 1 d . . . P2 P 0.3390(2) 0.65890(17) 0.42447(9) 0.0645(4) Uani 1 1 d . . . F1 F 0.5039(5) 0.2285(5) 0.0838(3) 0.1102(17) Uani 1 1 d . . . F2 F 0.5401(6) 0.0300(5) 0.0514(4) 0.125(2) Uani 1 1 d . . . F3 F 0.7685(5) 0.0449(5) 0.0722(3) 0.1016(15) Uani 1 1 d . . . F4 F 0.7334(7) 0.2465(6) 0.1013(4) 0.145(3) Uani 1 1 d . . . F5 F 0.5911(7) 0.1003(8) 0.1684(3) 0.154(3) Uani 1 1 d . . . F6 F 0.6791(5) 0.1696(5) -0.0162(3) 0.1031(15) Uani 1 1 d . . . F7 F 0.4779(6) 0.5747(6) 0.4171(3) 0.1105(17) Uani 1 1 d . . . F8 F 0.2556(6) 0.5467(5) 0.3932(3) 0.1033(15) Uani 1 1 d . . . F9 F 0.2050(5) 0.7452(5) 0.4284(3) 0.1041(16) Uani 1 1 d . . . F10 F 0.4266(6) 0.7712(5) 0.4554(3) 0.1131(18) Uani 1 1 d . . . F11 F 0.3870(6) 0.7014(5) 0.3328(3) 0.1109(17) Uani 1 1 d . . . F12 F 0.2984(5) 0.6164(4) 0.5159(2) 0.0907(13) 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 Pd 0.04870(19) 0.04183(17) 0.05152(18) -0.0026(2) -0.02027(12) -0.00352(16) N1 0.057(2) 0.053(3) 0.0557(19) 0.007(3) -0.0218(16) 0.011(4) N2 0.050(3) 0.054(3) 0.071(3) 0.004(2) -0.020(2) -0.006(2) O1 0.045(2) 0.084(3) 0.072(2) -0.011(2) -0.0158(17) -0.012(2) O2 0.073(4) 0.055(3) 0.192(7) -0.020(3) -0.047(4) -0.021(2) C1 0.060(4) 0.054(4) 0.068(4) 0.003(3) -0.013(3) -0.001(3) C2 0.056(4) 0.085(5) 0.086(5) 0.007(4) -0.018(3) 0.015(4) C3 0.048(3) 0.092(5) 0.073(3) 0.017(5) -0.021(2) -0.005(4) C4 0.049(4) 0.075(4) 0.052(3) -0.006(3) -0.011(3) -0.005(3) C5 0.047(3) 0.061(4) 0.051(3) -0.006(3) -0.011(3) -0.007(3) C6 0.043(3) 0.056(3) 0.077(4) -0.001(2) -0.019(3) -0.007(3) C7 0.054(4) 0.056(4) 0.129(6) 0.000(4) -0.029(4) -0.010(3) C8 0.069(5) 0.065(5) 0.162(8) 0.046(5) -0.025(5) -0.004(4) C9 0.078(6) 0.075(6) 0.129(7) 0.042(5) -0.033(5) -0.008(4) C10 0.064(4) 0.074(4) 0.072(4) 0.019(3) -0.024(3) -0.010(3) C21 0.121(6) 0.147(7) 0.085(5) -0.024(5) 0.000(4) -0.047(5) C22 0.074(5) 0.107(6) 0.085(5) -0.038(4) -0.009(4) -0.028(4) C23 0.067(4) 0.091(5) 0.131(6) -0.053(5) -0.006(4) -0.018(4) C24 0.127(7) 0.118(7) 0.200(8) -0.076(7) -0.006(6) -0.025(6) N3 0.052(2) 0.041(2) 0.0553(18) -0.008(3) -0.0203(15) -0.013(3) N4 0.057(3) 0.041(2) 0.048(2) 0.0011(16) -0.0206(19) 0.000(2) O3 0.063(3) 0.057(2) 0.084(3) -0.0108(19) -0.047(2) -0.0022(19) O4 0.052(2) 0.055(2) 0.067(2) -0.0037(16) -0.0136(17) -0.0119(18) C11 0.065(4) 0.046(4) 0.071(4) 0.015(3) -0.025(3) 0.001(3) C12 0.058(4) 0.053(4) 0.076(4) 0.012(3) -0.025(3) 0.005(3) C13 0.056(3) 0.075(5) 0.061(3) 0.011(3) -0.026(2) -0.001(3) C14 0.045(3) 0.053(3) 0.057(3) 0.000(2) -0.016(2) -0.003(2) C15 0.044(3) 0.040(3) 0.049(3) -0.001(2) -0.016(2) 0.000(2) C16 0.046(3) 0.044(3) 0.045(2) -0.0021(18) -0.015(2) 0.004(2) C17 0.054(3) 0.044(3) 0.053(3) 0.002(2) -0.009(2) -0.001(2) C18 0.072(4) 0.041(3) 0.071(4) 0.011(2) -0.015(3) -0.007(3) C19 0.065(4) 0.078(5) 0.060(4) 0.021(3) -0.017(3) 0.003(3) C20 0.064(4) 0.063(4) 0.053(3) 0.009(2) -0.024(3) -0.002(3) C25 0.114(6) 0.076(5) 0.069(4) -0.022(3) -0.031(4) -0.018(4) C26 0.066(4) 0.060(4) 0.062(3) -0.007(2) -0.021(3) -0.006(3) C27 0.068(4) 0.053(4) 0.074(4) -0.008(3) -0.020(3) -0.012(3) C28 0.152(8) 0.045(4) 0.085(5) -0.007(3) -0.018(5) 0.010(4) P1 0.0663(11) 0.0744(12) 0.0619(9) 0.0074(8) -0.0214(8) 0.0008(9) P2 0.0686(11) 0.0608(10) 0.0583(8) -0.0062(7) -0.0122(7) -0.0013(8) F1 0.093(3) 0.106(4) 0.118(4) -0.003(3) -0.032(3) 0.032(3) F2 0.085(3) 0.088(4) 0.187(6) 0.001(3) -0.032(3) -0.026(3) F3 0.086(3) 0.084(3) 0.122(4) 0.026(3) -0.033(3) 0.005(2) F4 0.117(4) 0.115(5) 0.175(6) -0.047(4) -0.078(4) -0.006(4) F5 0.151(5) 0.228(8) 0.078(3) 0.055(4) -0.006(3) 0.053(5) F6 0.121(4) 0.105(4) 0.073(2) 0.018(2) -0.021(2) 0.001(3) F7 0.095(3) 0.117(4) 0.109(4) -0.011(3) -0.025(3) 0.032(3) F8 0.112(4) 0.083(3) 0.102(3) -0.014(2) -0.033(3) -0.018(3) F9 0.081(3) 0.093(3) 0.127(4) -0.001(3) -0.024(3) 0.024(3) F10 0.128(4) 0.084(3) 0.109(3) -0.005(2) -0.049(3) -0.034(3) F11 0.143(4) 0.118(4) 0.066(2) 0.002(2) -0.006(3) -0.007(3) F12 0.126(4) 0.074(3) 0.068(2) 0.0041(18) -0.003(2) -0.004(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 Pd N1 1.856(4) . ? Pd N3 1.880(4) . ? Pd N2 2.116(5) . ? Pd N4 2.116(5) . ? N1 C1 1.261(11) . ? N1 C5 1.384(11) . ? N2 C6 1.241(7) . ? N2 C10 1.247(7) . ? O1 C4 1.348(8) . ? O1 C22 1.520(9) . ? O2 C7 1.237(8) . ? O2 C23 1.458(11) . ? C1 C2 1.261(11) . ? C2 C3 1.358(12) . ? C3 C4 1.327(10) . ? C4 C5 1.280(9) . ? C5 C6 1.369(9) . ? C6 C7 1.417(10) . ? C7 C8 1.309(11) . ? C8 C9 1.206(12) . ? C9 C10 1.422(11) . ? C21 C22 1.581(12) . ? C22 C23 1.418(11) . ? C23 C24 1.568(12) . ? N3 C11 1.283(10) . ? N3 C15 1.326(10) . ? N4 C16 1.227(6) . ? N4 C20 1.246(7) . ? O3 C14 1.300(7) . ? O3 C26 1.477(8) . ? O4 C17 1.260(6) . ? O4 C27 1.497(7) . ? C11 C12 1.217(10) . ? C12 C13 1.321(10) . ? C13 C14 1.335(9) . ? C14 C15 1.233(8) . ? C15 C16 1.420(8) . ? C16 C17 1.464(8) . ? C17 C18 1.278(8) . ? C18 C19 1.251(9) . ? C19 C20 1.416(9) . ? C25 C26 1.470(8) . ? C26 C27 1.633(9) . ? C27 C28 1.497(10) . ? P1 F2 1.507(5) . ? P1 F4 1.509(6) . ? P1 F3 1.598(5) . ? P1 F1 1.621(5) . ? P1 F5 1.671(6) . ? P1 F6 1.681(5) . ? P2 F8 1.501(5) . ? P2 F10 1.520(5) . ? P2 F9 1.581(5) . ? P2 F7 1.615(6) . ? P2 F12 1.672(5) . ? P2 F11 1.701(5) . ? 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 N1 Pd N3 179.4(4) . . ? N1 Pd N2 73.3(3) . . ? N3 Pd N2 106.8(2) . . ? N1 Pd N4 106.5(3) . . ? N3 Pd N4 73.4(2) . . ? N2 Pd N4 179.5(2) . . ? C1 N1 C5 124.7(5) . . ? C1 N1 Pd 121.9(7) . . ? C5 N1 Pd 113.5(5) . . ? C6 N2 C10 112.7(6) . . ? C6 N2 Pd 115.9(4) . . ? C10 N2 Pd 130.7(5) . . ? C4 O1 C22 109.9(5) . . ? C7 O2 C23 112.3(7) . . ? C2 C1 N1 119.3(9) . . ? C1 C2 C3 116.7(8) . . ? C4 C3 C2 125.9(5) . . ? C5 C4 C3 115.1(7) . . ? C5 C4 O1 122.4(7) . . ? C3 C4 O1 121.9(6) . . ? C4 C5 C6 121.4(7) . . ? C4 C5 N1 118.0(6) . . ? C6 C5 N1 119.4(6) . . ? N2 C6 C5 105.2(6) . . ? N2 C6 C7 120.3(6) . . ? C5 C6 C7 133.8(6) . . ? O2 C7 C8 108.3(8) . . ? O2 C7 C6 128.1(7) . . ? C8 C7 C6 123.6(7) . . ? C9 C8 C7 114.0(8) . . ? C8 C9 C10 120.3(8) . . ? N2 C10 C9 127.2(7) . . ? C23 C22 O1 117.7(5) . . ? C23 C22 C21 102.4(8) . . ? O1 C22 C21 113.7(8) . . ? C22 C23 O2 95.6(6) . . ? C22 C23 C24 119.9(7) . . ? O2 C23 C24 110.3(9) . . ? C11 N3 C15 126.6(5) . . ? C11 N3 Pd 121.9(6) . . ? C15 N3 Pd 110.6(5) . . ? C16 N4 C20 112.1(5) . . ? C16 N4 Pd 117.8(3) . . ? C20 N4 Pd 130.1(4) . . ? C14 O3 C26 124.3(4) . . ? C17 O4 C27 106.2(5) . . ? C12 C11 N3 115.7(7) . . ? C11 C12 C13 117.5(6) . . ? C12 C13 C14 127.4(5) . . ? C15 C14 O3 126.7(6) . . ? C15 C14 C13 112.1(6) . . ? O3 C14 C13 121.1(5) . . ? C14 C15 N3 118.5(6) . . ? C14 C15 C16 121.3(6) . . ? N3 C15 C16 119.5(5) . . ? N4 C16 C15 104.5(5) . . ? N4 C16 C17 121.8(4) . . ? C15 C16 C17 132.2(5) . . ? O4 C17 C18 108.5(6) . . ? O4 C17 C16 126.0(5) . . ? C18 C17 C16 124.8(5) . . ? C19 C18 C17 111.4(6) . . ? C18 C19 C20 122.0(6) . . ? N4 C20 C19 127.7(6) . . ? C25 C26 O3 114.8(5) . . ? C25 C26 C27 114.2(6) . . ? O3 C26 C27 97.8(5) . . ? O4 C27 C28 120.3(5) . . ? O4 C27 C26 112.8(5) . . ? C28 C27 C26 104.8(6) . . ? F2 P1 F4 178.4(4) . . ? F2 P1 F3 87.2(3) . . ? F4 P1 F3 93.8(3) . . ? F2 P1 F1 92.1(3) . . ? F4 P1 F1 86.9(3) . . ? F3 P1 F1 178.8(3) . . ? F2 P1 F5 81.1(4) . . ? F4 P1 F5 100.0(4) . . ? F3 P1 F5 101.5(3) . . ? F1 P1 F5 77.5(3) . . ? F2 P1 F6 96.4(3) . . ? F4 P1 F6 82.6(4) . . ? F3 P1 F6 78.7(3) . . ? F1 P1 F6 102.3(3) . . ? F5 P1 F6 177.4(4) . . ? F8 P2 F10 178.6(4) . . ? F8 P2 F9 96.3(3) . . ? F10 P2 F9 85.0(3) . . ? F8 P2 F7 84.8(3) . . ? F10 P2 F7 93.9(3) . . ? F9 P2 F7 177.4(3) . . ? F8 P2 F12 85.0(3) . . ? F10 P2 F12 95.7(3) . . ? F9 P2 F12 80.9(3) . . ? F7 P2 F12 101.6(3) . . ? F8 P2 F11 96.0(3) . . ? F10 P2 F11 83.3(3) . . ? F9 P2 F11 100.9(3) . . ? F7 P2 F11 76.6(3) . . ? F12 P2 F11 177.8(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Pd N1 C1 54(37) . . . . ? N2 Pd N1 C1 155.4(6) . . . . ? N4 Pd N1 C1 -24.2(6) . . . . ? N3 Pd N1 C5 -126(37) . . . . ? N2 Pd N1 C5 -25.4(4) . . . . ? N4 Pd N1 C5 155.0(4) . . . . ? N1 Pd N2 C6 34.6(5) . . . . ? N3 Pd N2 C6 -146.1(5) . . . . ? N4 Pd N2 C6 95(23) . . . . ? N1 Pd N2 C10 -155.8(8) . . . . ? N3 Pd N2 C10 23.6(8) . . . . ? N4 Pd N2 C10 -96(23) . . . . ? C5 N1 C1 C2 -4.9(11) . . . . ? Pd N1 C1 C2 174.2(6) . . . . ? N1 C1 C2 C3 -0.4(13) . . . . ? C1 C2 C3 C4 4.4(13) . . . . ? C2 C3 C4 C5 -2.7(12) . . . . ? C2 C3 C4 O1 168.9(8) . . . . ? C22 O1 C4 C5 -76.2(9) . . . . ? C22 O1 C4 C3 112.9(7) . . . . ? C3 C4 C5 C6 164.7(7) . . . . ? O1 C4 C5 C6 -6.8(12) . . . . ? C3 C4 C5 N1 -2.5(10) . . . . ? O1 C4 C5 N1 -174.0(6) . . . . ? C1 N1 C5 C4 6.6(10) . . . . ? Pd N1 C5 C4 -172.7(6) . . . . ? C1 N1 C5 C6 -160.9(7) . . . . ? Pd N1 C5 C6 19.9(8) . . . . ? C10 N2 C6 C5 157.9(7) . . . . ? Pd N2 C6 C5 -30.6(7) . . . . ? C10 N2 C6 C7 -13.9(11) . . . . ? Pd N2 C6 C7 157.6(6) . . . . ? C4 C5 C6 N2 -158.4(7) . . . . ? N1 C5 C6 N2 8.6(9) . . . . ? C4 C5 C6 C7 11.9(14) . . . . ? N1 C5 C6 C7 178.9(8) . . . . ? C23 O2 C7 C8 -145.6(8) . . . . ? C23 O2 C7 C6 33.6(12) . . . . ? N2 C6 C7 O2 -162.1(8) . . . . ? C5 C6 C7 O2 28.8(16) . . . . ? N2 C6 C7 C8 16.9(14) . . . . ? C5 C6 C7 C8 -152.2(9) . . . . ? O2 C7 C8 C9 171.7(10) . . . . ? C6 C7 C8 C9 -7.4(16) . . . . ? C7 C8 C9 C10 -1.8(17) . . . . ? C6 N2 C10 C9 5.2(13) . . . . ? Pd N2 C10 C9 -164.7(7) . . . . ? C8 C9 C10 N2 3.4(17) . . . . ? C4 O1 C22 C23 74.4(9) . . . . ? C4 O1 C22 C21 -45.2(7) . . . . ? O1 C22 C23 O2 42.3(8) . . . . ? C21 C22 C23 O2 167.8(6) . . . . ? O1 C22 C23 C24 159.6(9) . . . . ? C21 C22 C23 C24 -75.0(11) . . . . ? C7 O2 C23 C22 -104.6(7) . . . . ? C7 O2 C23 C24 130.6(8) . . . . ? N1 Pd N3 C11 122(37) . . . . ? N2 Pd N3 C11 21.4(6) . . . . ? N4 Pd N3 C11 -159.0(6) . . . . ? N1 Pd N3 C15 -47(37) . . . . ? N2 Pd N3 C15 -148.1(4) . . . . ? N4 Pd N3 C15 31.4(4) . . . . ? N1 Pd N4 C16 150.5(5) . . . . ? N3 Pd N4 C16 -28.8(4) . . . . ? N2 Pd N4 C16 91(23) . . . . ? N1 Pd N4 C20 -27.9(6) . . . . ? N3 Pd N4 C20 152.8(7) . . . . ? N2 Pd N4 C20 -88(23) . . . . ? C15 N3 C11 C12 4.8(11) . . . . ? Pd N3 C11 C12 -163.0(6) . . . . ? N3 C11 C12 C13 6.8(13) . . . . ? C11 C12 C13 C14 -8.2(13) . . . . ? C26 O3 C14 C15 28.5(12) . . . . ? C26 O3 C14 C13 -148.8(6) . . . . ? C12 C13 C14 C15 -3.2(11) . . . . ? C12 C13 C14 O3 174.5(8) . . . . ? O3 C14 C15 N3 -163.5(7) . . . . ? C13 C14 C15 N3 14.0(11) . . . . ? O3 C14 C15 C16 26.6(12) . . . . ? C13 C14 C15 C16 -155.9(6) . . . . ? C11 N3 C15 C14 -16.8(10) . . . . ? Pd N3 C15 C14 152.2(6) . . . . ? C11 N3 C15 C16 153.3(8) . . . . ? Pd N3 C15 C16 -37.7(7) . . . . ? C20 N4 C16 C15 -165.6(6) . . . . ? Pd N4 C16 C15 15.7(6) . . . . ? C20 N4 C16 C17 2.2(8) . . . . ? Pd N4 C16 C17 -176.5(4) . . . . ? C14 C15 C16 N4 -177.2(7) . . . . ? N3 C15 C16 N4 13.0(8) . . . . ? C14 C15 C16 C17 16.8(11) . . . . ? N3 C15 C16 C17 -153.0(6) . . . . ? C27 O4 C17 C18 105.9(6) . . . . ? C27 O4 C17 C16 -83.1(7) . . . . ? N4 C16 C17 O4 -167.8(6) . . . . ? C15 C16 C17 O4 -3.9(10) . . . . ? N4 C16 C17 C18 1.8(10) . . . . ? C15 C16 C17 C18 165.8(7) . . . . ? O4 C17 C18 C19 167.0(7) . . . . ? C16 C17 C18 C19 -4.1(11) . . . . ? C17 C18 C19 C20 2.8(12) . . . . ? C16 N4 C20 C19 -3.7(10) . . . . ? Pd N4 C20 C19 174.8(6) . . . . ? C18 C19 C20 N4 1.2(14) . . . . ? C14 O3 C26 C25 128.7(7) . . . . ? C14 O3 C26 C27 -110.0(6) . . . . ? C17 O4 C27 C28 -62.9(8) . . . . ? C17 O4 C27 C26 61.7(6) . . . . ? C25 C26 C27 O4 163.9(5) . . . . ? O3 C26 C27 O4 42.1(5) . . . . ? C25 C26 C27 C28 -63.5(7) . . . . ? O3 C26 C27 C28 174.8(4) . . . . ? _diffrn_measured_fraction_theta_max 0.935 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_full 0.935 _refine_diff_density_max 0.385 _refine_diff_density_min -0.645 _refine_diff_density_rms 0.062 #===END data_3b _database_code_depnum_ccdc_archive 'CCDC 667851' _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis-trifluoroacetate-(3,3-(ethylenedioxy)-2,2-bipyridine)-palladium(II) ; _chemical_name_common ;bis-trifluoroacetate-(3,3-(ethylenedioxy)-2,2-bipyridine)- palladium(ii) ; _chemical_melting_point ? _chemical_formula_moiety 'C16 H10 F6 N2 O6 Pd' _chemical_formula_sum 'C16 H10 F6 N2 O6 Pd' _chemical_formula_weight 546.66 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' Pd Pd -0.9988 1.0072 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.305(3) _cell_length_b 9.105(3) _cell_length_c 16.979(4) _cell_angle_alpha 90.00 _cell_angle_beta 110.17(3) _cell_angle_gamma 90.00 _cell_volume 1785.6(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour yellow _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.033 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1072 _exptl_absorpt_coefficient_mu 1.141 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.6231 _exptl_absorpt_correction_T_max 0.8144 _exptl_absorpt_process_details ; Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56 Cubic fit to sin(theta)/lambda - 24 parameters ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mok\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'image plate dip1030' _diffrn_measurement_method 'laser scanner' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20050 _diffrn_reflns_av_R_equivalents 0.0590 _diffrn_reflns_av_sigmaI/netI 0.0480 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3942 _reflns_number_gt 3432 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Xpress' _computing_cell_refinement 'Mosflm (Acta Cryst. D50, 760, 1994)' _computing_data_reduction 'Scala (Acta Cryst. D50, 760, 1994)' _computing_structure_solution 'SHELX97 (Sheldrick, 1998)' _computing_structure_refinement 'SHELX97 (Sheldrick, 1998)' _computing_molecular_graphics 'Ortep3/windows (Farrugia,1997)' _computing_publication_material 'Wingx 1.70.00 (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0465P)^2^+2.0493P] 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 3942 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0432 _refine_ls_R_factor_gt 0.0374 _refine_ls_wR_factor_ref 0.1065 _refine_ls_wR_factor_gt 0.1014 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd 0.45654(2) 0.62891(3) 0.057157(14) 0.03967(11) Uani 1 1 d . . . O1 O 0.8975(2) 0.7196(3) 0.1855(2) 0.0634(7) Uani 1 1 d . . . O2 O 0.8552(3) 0.7761(3) 0.0210(2) 0.0694(8) Uani 1 1 d . . . N1 N 0.6125(2) 0.5586(3) 0.12873(17) 0.0407(6) Uani 1 1 d . . . N2 N 0.5529(2) 0.7537(3) 0.01065(17) 0.0438(6) Uani 1 1 d . . . C1 C 0.6296(3) 0.4584(4) 0.1897(2) 0.0464(7) Uani 1 1 d . . . H1 H 0.5671 0.4039 0.1924 0.056 Uiso 1 1 calc R . . C2 C 0.7384(4) 0.4342(5) 0.2488(2) 0.0559(9) Uani 1 1 d . . . H2 H 0.7502 0.3608 0.2891 0.067 Uiso 1 1 calc R . . C3 C 0.8283(4) 0.5215(5) 0.2464(3) 0.0601(10) Uani 1 1 d . . . H3 H 0.9012 0.5113 0.2872 0.072 Uiso 1 1 calc R . . C4 C 0.8105(3) 0.6245(4) 0.1834(3) 0.0503(8) Uani 1 1 d . . . C5 C 0.7025(3) 0.6366(3) 0.1203(2) 0.0418(7) Uani 1 1 d . . . C6 C 0.6706(3) 0.7327(4) 0.0458(2) 0.0429(7) Uani 1 1 d . . . C7 C 0.7415(3) 0.7977(4) 0.0063(2) 0.0519(8) Uani 1 1 d . . . C8 C 0.6923(4) 0.8994(5) -0.0584(3) 0.0601(10) Uani 1 1 d . . . H8 H 0.7398 0.9503 -0.0813 0.072 Uiso 1 1 calc R . . C9 C 0.5764(4) 0.9245(5) -0.0880(3) 0.0623(10) Uani 1 1 d . . . H9 H 0.5443 0.9936 -0.1299 0.075 Uiso 1 1 calc R . . C10 C 0.5064(4) 0.8441(4) -0.0541(2) 0.0530(8) Uani 1 1 d . . . H10 H 0.4264 0.8538 -0.0769 0.064 Uiso 1 1 calc R . . C11 C 0.9751(4) 0.6608(6) 0.1470(4) 0.0773(14) Uani 1 1 d . . . H11A H 1.0056 0.5673 0.1725 0.093 Uiso 1 1 calc R . . H11B H 1.0396 0.7275 0.1552 0.093 Uiso 1 1 calc R . . C12 C 0.9105(4) 0.6402(5) 0.0547(4) 0.0693(13) Uani 1 1 d . . . H12A H 0.9637 0.6118 0.0265 0.083 Uiso 1 1 calc R . . H12B H 0.8530 0.5633 0.0461 0.083 Uiso 1 1 calc R . . O3 O 0.3057(2) 0.7102(3) -0.02360(16) 0.0549(6) Uani 1 1 d . . . O5 O 0.3678(2) 0.4940(3) 0.10773(15) 0.0462(5) Uani 1 1 d . . . C13 C 0.2200(3) 0.7502(4) -0.0037(2) 0.0473(7) Uani 1 1 d . . . C14 C 0.1186(3) 0.8040(5) -0.0813(3) 0.0586(9) Uani 1 1 d . . . F1 F 0.0613(4) 0.6986(4) -0.1237(3) 0.164(2) Uani 1 1 d . . . F2 F 0.0439(3) 0.8827(6) -0.0603(3) 0.138(2) Uani 1 1 d . . . F3 F 0.1492(4) 0.8907(6) -0.1282(3) 0.148(2) Uani 1 1 d . . . O4 O 0.2059(3) 0.7525(4) 0.0627(2) 0.0772(9) Uani 1 1 d . . . O6 O 0.4090(3) 0.6431(3) 0.22001(19) 0.0629(7) Uani 1 1 d . . . C15 C 0.3622(3) 0.5387(4) 0.1775(2) 0.0463(7) Uani 1 1 d . . . C16 C 0.2894(4) 0.4347(5) 0.2111(3) 0.0626(10) Uani 1 1 d . . . F4 F 0.2659(5) 0.4868(6) 0.2730(3) 0.158(2) Uani 1 1 d . . . F5 F 0.1915(3) 0.3992(5) 0.1547(3) 0.1277(16) Uani 1 1 d . . . F6 F 0.3437(4) 0.3114(5) 0.2336(4) 0.156(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 Pd 0.03804(15) 0.04418(16) 0.03573(15) -0.00107(9) 0.01136(11) -0.00091(9) O1 0.0476(14) 0.0633(17) 0.0732(19) -0.0192(14) 0.0128(13) -0.0114(12) O2 0.0583(16) 0.0637(18) 0.098(2) 0.0018(16) 0.0415(16) -0.0085(14) N1 0.0407(13) 0.0427(14) 0.0377(13) -0.0028(11) 0.0121(11) -0.0003(11) N2 0.0472(15) 0.0452(15) 0.0387(13) -0.0024(11) 0.0146(12) -0.0015(12) C1 0.0489(18) 0.0470(18) 0.0452(18) 0.0025(14) 0.0187(15) 0.0050(14) C2 0.057(2) 0.058(2) 0.049(2) 0.0065(16) 0.0140(17) 0.0108(17) C3 0.051(2) 0.064(2) 0.052(2) -0.0040(18) 0.0005(17) 0.0073(18) C4 0.0452(18) 0.052(2) 0.0491(19) -0.0109(15) 0.0102(15) -0.0014(15) C5 0.0409(16) 0.0408(16) 0.0444(17) -0.0089(13) 0.0156(14) -0.0016(12) C6 0.0443(17) 0.0411(16) 0.0434(17) -0.0090(13) 0.0152(14) -0.0055(13) C7 0.057(2) 0.0487(19) 0.055(2) -0.0091(16) 0.0257(17) -0.0110(16) C8 0.074(3) 0.056(2) 0.057(2) -0.0031(17) 0.030(2) -0.0167(19) C9 0.079(3) 0.059(2) 0.048(2) 0.0075(18) 0.022(2) -0.006(2) C10 0.060(2) 0.056(2) 0.0413(18) 0.0056(15) 0.0151(16) -0.0002(17) C11 0.045(2) 0.076(3) 0.108(4) -0.014(3) 0.022(2) -0.006(2) C12 0.058(2) 0.062(3) 0.101(4) -0.012(2) 0.044(3) -0.0010(19) O3 0.0444(13) 0.0680(17) 0.0473(13) 0.0069(12) 0.0094(11) 0.0067(12) O5 0.0464(12) 0.0487(13) 0.0464(13) -0.0022(10) 0.0195(10) -0.0043(10) C13 0.0434(17) 0.0474(18) 0.0476(18) 0.0012(14) 0.0113(14) -0.0014(14) C14 0.0461(19) 0.061(2) 0.060(2) 0.0077(19) 0.0076(17) -0.0006(17) F1 0.144(4) 0.086(2) 0.152(4) -0.005(2) -0.089(3) -0.004(2) F2 0.105(3) 0.185(5) 0.112(4) 0.019(3) 0.022(3) 0.085(3) F3 0.084(2) 0.209(5) 0.130(3) 0.116(4) 0.011(2) 0.004(3) O4 0.076(2) 0.100(3) 0.0564(17) 0.0106(17) 0.0248(16) 0.0285(19) O6 0.0683(18) 0.0706(19) 0.0490(15) -0.0124(13) 0.0191(14) -0.0116(14) C15 0.0396(16) 0.0540(19) 0.0445(17) 0.0020(15) 0.0134(14) 0.0015(14) C16 0.057(2) 0.075(3) 0.063(2) 0.000(2) 0.030(2) -0.004(2) F4 0.215(5) 0.178(4) 0.153(4) -0.070(3) 0.153(4) -0.092(4) F5 0.088(2) 0.182(4) 0.115(3) -0.004(3) 0.039(2) -0.068(3) F6 0.167(4) 0.119(3) 0.234(6) 0.106(4) 0.134(4) 0.046(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 Pd N1 1.990(3) . ? Pd N2 1.992(3) . ? Pd O5 2.022(2) . ? Pd O3 2.029(3) . ? O1 C4 1.369(5) . ? O1 C11 1.434(6) . ? O2 C7 1.349(5) . ? O2 C12 1.432(6) . ? N1 C1 1.341(4) . ? N1 C5 1.364(4) . ? N2 C10 1.334(5) . ? N2 C6 1.376(4) . ? C1 C2 1.386(5) . ? C2 C3 1.375(6) . ? C3 C4 1.381(6) . ? C4 C5 1.395(5) . ? C5 C6 1.476(5) . ? C6 C7 1.402(5) . ? C7 C8 1.404(6) . ? C8 C9 1.358(6) . ? C9 C10 1.396(6) . ? C11 C12 1.505(8) . ? O3 C13 1.267(5) . ? O5 C15 1.277(4) . ? C13 O4 1.199(5) . ? C13 C14 1.549(5) . ? C14 F1 1.259(5) . ? C14 F3 1.267(6) . ? C14 F2 1.309(6) . ? O6 C15 1.212(4) . ? C15 C16 1.541(6) . ? C16 F4 1.274(6) . ? C16 F6 1.295(6) . ? C16 F5 1.295(6) . ? 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 N1 Pd N2 81.08(12) . . ? N1 Pd O5 95.37(11) . . ? N2 Pd O5 176.30(11) . . ? N1 Pd O3 174.05(11) . . ? N2 Pd O3 93.15(11) . . ? O5 Pd O3 90.37(11) . . ? C4 O1 C11 113.0(3) . . ? C7 O2 C12 121.3(3) . . ? C1 N1 C5 121.2(3) . . ? C1 N1 Pd 123.5(2) . . ? C5 N1 Pd 114.5(2) . . ? C10 N2 C6 122.1(3) . . ? C10 N2 Pd 122.2(3) . . ? C6 N2 Pd 115.5(2) . . ? N1 C1 C2 121.5(4) . . ? C3 C2 C1 118.2(4) . . ? C2 C3 C4 120.1(4) . . ? O1 C4 C3 119.7(4) . . ? O1 C4 C5 119.9(4) . . ? C3 C4 C5 120.2(4) . . ? N1 C5 C4 118.1(3) . . ? N1 C5 C6 114.4(3) . . ? C4 C5 C6 127.4(3) . . ? N2 C6 C7 118.0(3) . . ? N2 C6 C5 112.5(3) . . ? C7 C6 C5 129.5(3) . . ? O2 C7 C6 128.8(4) . . ? O2 C7 C8 112.4(4) . . ? C6 C7 C8 118.8(4) . . ? C9 C8 C7 121.0(4) . . ? C8 C9 C10 118.5(4) . . ? N2 C10 C9 120.8(4) . . ? O1 C11 C12 109.0(4) . . ? O2 C12 C11 108.4(4) . . ? C13 O3 Pd 125.2(2) . . ? C15 O5 Pd 114.2(2) . . ? O4 C13 O3 131.2(4) . . ? O4 C13 C14 117.4(3) . . ? O3 C13 C14 111.4(3) . . ? F1 C14 F3 110.2(5) . . ? F1 C14 F2 105.4(5) . . ? F3 C14 F2 102.7(5) . . ? F1 C14 C13 111.9(4) . . ? F3 C14 C13 113.9(4) . . ? F2 C14 C13 112.1(4) . . ? O6 C15 O5 129.5(3) . . ? O6 C15 C16 118.6(4) . . ? O5 C15 C16 111.8(3) . . ? F4 C16 F6 108.7(5) . . ? F4 C16 F5 106.5(5) . . ? F6 C16 F5 104.8(5) . . ? F4 C16 C15 113.7(4) . . ? F6 C16 C15 109.6(4) . . ? F5 C16 C15 113.0(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 N2 Pd N1 C1 178.0(3) . . . . ? O5 Pd N1 C1 -3.0(3) . . . . ? O3 Pd N1 C1 -167.5(10) . . . . ? N2 Pd N1 C5 7.9(2) . . . . ? O5 Pd N1 C5 -173.1(2) . . . . ? O3 Pd N1 C5 22.4(12) . . . . ? N1 Pd N2 C10 176.4(3) . . . . ? O5 Pd N2 C10 160.1(15) . . . . ? O3 Pd N2 C10 -2.1(3) . . . . ? N1 Pd N2 C6 0.9(2) . . . . ? O5 Pd N2 C6 -15.4(17) . . . . ? O3 Pd N2 C6 -177.6(2) . . . . ? C5 N1 C1 C2 2.7(5) . . . . ? Pd N1 C1 C2 -166.7(3) . . . . ? N1 C1 C2 C3 3.5(6) . . . . ? C1 C2 C3 C4 -3.6(6) . . . . ? C11 O1 C4 C3 86.6(5) . . . . ? C11 O1 C4 C5 -96.7(4) . . . . ? C2 C3 C4 O1 174.3(4) . . . . ? C2 C3 C4 C5 -2.4(6) . . . . ? C1 N1 C5 C4 -8.6(5) . . . . ? Pd N1 C5 C4 161.7(2) . . . . ? C1 N1 C5 C6 174.9(3) . . . . ? Pd N1 C5 C6 -14.8(3) . . . . ? O1 C4 C5 N1 -168.3(3) . . . . ? C3 C4 C5 N1 8.4(5) . . . . ? O1 C4 C5 C6 7.7(5) . . . . ? C3 C4 C5 C6 -175.6(4) . . . . ? C10 N2 C6 C7 -6.5(5) . . . . ? Pd N2 C6 C7 169.1(2) . . . . ? C10 N2 C6 C5 175.8(3) . . . . ? Pd N2 C6 C5 -8.7(3) . . . . ? N1 C5 C6 N2 15.3(4) . . . . ? C4 C5 C6 N2 -160.8(3) . . . . ? N1 C5 C6 C7 -162.1(3) . . . . ? C4 C5 C6 C7 21.8(6) . . . . ? C12 O2 C7 C6 27.0(6) . . . . ? C12 O2 C7 C8 -152.5(4) . . . . ? N2 C6 C7 O2 -169.4(4) . . . . ? C5 C6 C7 O2 7.9(6) . . . . ? N2 C6 C7 C8 10.1(5) . . . . ? C5 C6 C7 C8 -172.6(3) . . . . ? O2 C7 C8 C9 173.3(4) . . . . ? C6 C7 C8 C9 -6.3(6) . . . . ? C7 C8 C9 C10 -1.5(7) . . . . ? C6 N2 C10 C9 -1.4(6) . . . . ? Pd N2 C10 C9 -176.6(3) . . . . ? C8 C9 C10 N2 5.5(7) . . . . ? C4 O1 C11 C12 65.6(5) . . . . ? C7 O2 C12 C11 -100.9(5) . . . . ? O1 C11 C12 O2 52.8(5) . . . . ? N1 Pd O3 C13 -149.0(10) . . . . ? N2 Pd O3 C13 -134.7(3) . . . . ? O5 Pd O3 C13 46.4(3) . . . . ? N1 Pd O5 C15 80.3(2) . . . . ? N2 Pd O5 C15 96.5(16) . . . . ? O3 Pd O5 C15 -101.3(2) . . . . ? Pd O3 C13 O4 0.8(6) . . . . ? Pd O3 C13 C14 -179.0(2) . . . . ? O4 C13 C14 F1 -100.1(6) . . . . ? O3 C13 C14 F1 79.7(5) . . . . ? O4 C13 C14 F3 134.1(5) . . . . ? O3 C13 C14 F3 -46.1(6) . . . . ? O4 C13 C14 F2 18.1(6) . . . . ? O3 C13 C14 F2 -162.1(4) . . . . ? Pd O5 C15 O6 -6.1(5) . . . . ? Pd O5 C15 C16 177.7(2) . . . . ? O6 C15 C16 F4 14.1(7) . . . . ? O5 C15 C16 F4 -169.2(5) . . . . ? O6 C15 C16 F6 -107.8(5) . . . . ? O5 C15 C16 F6 68.9(5) . . . . ? O6 C15 C16 F5 135.7(5) . . . . ? O5 C15 C16 F5 -47.6(5) . . . . ? _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 0.858 _refine_diff_density_min -0.657 _refine_diff_density_rms 0.097 #===END data_3c _database_code_depnum_ccdc_archive 'CCDC 667852' _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis(3,3-(ethylenedioxy)-2,2-bipyridine)-palladium(II) bis(hexafluorophosphate) ; _chemical_name_common ;bis(3,3-(ethylenedioxy)-2,2-bipyridine)-palladium(ii) bis(hexafluorophosphate) ; _chemical_melting_point ? _chemical_formula_moiety 'C24 H20 N4 O4 Pd 2+, 2(P F6 1-)' _chemical_formula_sum 'C24 H20 F12 N4 O4 P2 Pd' _chemical_formula_weight 824.78 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' P P 0.1023 0.0942 '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 7.862(3) _cell_length_b 9.272(3) _cell_length_c 10.358(4) _cell_angle_alpha 96.08(2) _cell_angle_beta 97.68(3) _cell_angle_gamma 107.75(2) _cell_volume 704.0(4) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour yellow _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.945 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 408 _exptl_absorpt_coefficient_mu 0.894 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.4615 _exptl_absorpt_correction_T_max 0.8798 _exptl_absorpt_process_details ; Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56 Cubic fit to sin(theta)/lambda - 24 parameters ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mok\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'image plate dip1030' _diffrn_measurement_method 'laser scanner' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7619 _diffrn_reflns_av_R_equivalents 0.0410 _diffrn_reflns_av_sigmaI/netI 0.0569 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.83 _diffrn_reflns_theta_max 29.00 _reflns_number_total 3397 _reflns_number_gt 3107 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Xpress' _computing_cell_refinement 'Mosflm (Acta Cryst. D50, 760, 1994)' _computing_data_reduction 'Scala (Acta Cryst. D50, 760, 1994)' _computing_structure_solution 'SHELX97 (Sheldrick, 1998)' _computing_structure_refinement 'SHELX97 (Sheldrick, 1998)' _computing_molecular_graphics 'Ortep3/windows (Farrugia,1997)' _computing_publication_material 'Wingx 1.70.00 (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0352P)^2^+0.6374P] 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 3397 _refine_ls_number_parameters 251 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0460 _refine_ls_R_factor_gt 0.0407 _refine_ls_wR_factor_ref 0.1118 _refine_ls_wR_factor_gt 0.1053 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.104 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd 1.0000 0.0000 0.0000 0.04139(13) Uani 1 2 d S . . N1 N 0.8157(4) 0.1055(3) 0.0335(3) 0.0445(6) Uani 1 1 d . . . N2 N 0.8688(4) -0.1268(3) 0.1285(3) 0.0440(6) Uani 1 1 d . . . O1 O 0.5194(4) 0.0895(3) 0.2761(3) 0.0580(6) Uani 1 1 d . . . O2 O 0.7534(5) 0.0017(4) 0.4422(3) 0.0656(8) Uani 1 1 d . . . C1 C 0.7513(5) 0.1878(4) -0.0471(3) 0.0503(8) Uani 1 1 d . . . H1 H 0.7956 0.2018 -0.1253 0.060 Uiso 1 1 calc R . . C2 C 0.6216(5) 0.2529(5) -0.0184(4) 0.0564(9) Uani 1 1 d . . . H2 H 0.5839 0.3142 -0.0738 0.068 Uiso 1 1 calc R . . C3 C 0.5497(5) 0.2251(5) 0.0935(4) 0.0550(8) Uani 1 1 d . . . H3 H 0.4622 0.2675 0.1149 0.066 Uiso 1 1 calc R . . C4 C 0.6081(5) 0.1331(4) 0.1750(3) 0.0487(7) Uani 1 1 d . . . C5 C 0.7474(4) 0.0773(4) 0.1461(3) 0.0433(7) Uani 1 1 d . . . C6 C 0.8027(4) -0.0393(4) 0.2125(3) 0.0434(7) Uani 1 1 d . . . C7 C 0.7762(5) -0.0824(5) 0.3353(3) 0.0520(8) Uani 1 1 d . . . C8 C 0.7748(6) -0.2299(5) 0.3549(4) 0.0627(10) Uani 1 1 d . . . H8 H 0.7467 -0.2646 0.4329 0.075 Uiso 1 1 calc R . . C9 C 0.8145(6) -0.3234(5) 0.2603(4) 0.0609(10) Uani 1 1 d . . . H9 H 0.8042 -0.4240 0.2703 0.073 Uiso 1 1 calc R . . C10 C 0.8702(5) -0.2655(4) 0.1495(4) 0.0521(8) Uani 1 1 d . . . H10 H 0.9090 -0.3244 0.0890 0.063 Uiso 1 1 calc R . . C11 C 0.6040(7) 0.1859(5) 0.4020(4) 0.0664(11) Uani 1 1 d . . . H11A H 0.5256 0.1593 0.4666 0.080 Uiso 1 1 calc R . . H11B H 0.6235 0.2926 0.3932 0.080 Uiso 1 1 calc R . . C12 C 0.7810(6) 0.1627(5) 0.4463(4) 0.0635(10) Uani 1 1 d . . . H12A H 0.8658 0.2043 0.3891 0.076 Uiso 1 1 calc R . . H12B H 0.8319 0.2160 0.5354 0.076 Uiso 1 1 calc R . . P1 P 0.21513(15) 0.45130(12) 0.28045(10) 0.0557(2) Uani 1 1 d . . . F5 F 0.1609(5) 0.2694(3) 0.2704(4) 0.0972(10) Uani 1 1 d . . . F6 F 0.2677(5) 0.6327(3) 0.2889(3) 0.0840(8) Uani 1 1 d . . . F1 F 0.1846(14) 0.4648(9) 0.4300(6) 0.095(2) Uani 0.54 1 d P . . F2 F 0.0077(10) 0.4170(9) 0.2326(11) 0.107(2) Uani 0.54 1 d P . . F3 F 0.2507(14) 0.4222(10) 0.1384(7) 0.100(3) Uani 0.54 1 d P . . F4 F 0.4195(11) 0.4649(12) 0.3349(11) 0.108(3) Uani 0.54 1 d P . . F2A F 0.0677(14) 0.4541(11) 0.1549(9) 0.101(3) Uani 0.46 1 d P . . F1A F 0.0819(16) 0.4629(12) 0.3768(12) 0.109(3) Uani 0.46 1 d P . . F4A F 0.3643(17) 0.4679(13) 0.3930(10) 0.109(4) Uani 0.46 1 d P . . F3A F 0.3515(13) 0.4607(11) 0.1757(11) 0.095(3) Uani 0.46 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd 0.0459(2) 0.0444(2) 0.03822(18) 0.00634(13) 0.01343(13) 0.01840(15) N1 0.0481(14) 0.0471(16) 0.0419(13) 0.0076(11) 0.0123(11) 0.0185(13) N2 0.0473(14) 0.0452(15) 0.0444(13) 0.0117(11) 0.0162(11) 0.0171(13) O1 0.0560(14) 0.0617(17) 0.0606(15) 0.0070(12) 0.0260(12) 0.0196(13) O2 0.087(2) 0.073(2) 0.0491(14) 0.0161(12) 0.0312(13) 0.0341(17) C1 0.0516(18) 0.054(2) 0.0485(17) 0.0112(14) 0.0107(14) 0.0198(17) C2 0.056(2) 0.055(2) 0.065(2) 0.0192(17) 0.0111(16) 0.0230(18) C3 0.0519(19) 0.051(2) 0.067(2) 0.0083(16) 0.0148(16) 0.0233(17) C4 0.0491(18) 0.0471(19) 0.0525(18) 0.0050(14) 0.0170(14) 0.0167(16) C5 0.0446(16) 0.0437(17) 0.0426(15) 0.0036(12) 0.0119(12) 0.0151(14) C6 0.0445(16) 0.0423(17) 0.0452(16) 0.0073(12) 0.0145(12) 0.0137(14) C7 0.0551(19) 0.060(2) 0.0488(17) 0.0138(15) 0.0206(14) 0.0233(18) C8 0.069(2) 0.070(3) 0.064(2) 0.0326(19) 0.0278(19) 0.030(2) C9 0.063(2) 0.052(2) 0.080(3) 0.0277(19) 0.0273(19) 0.025(2) C10 0.0524(19) 0.0476(19) 0.061(2) 0.0081(15) 0.0165(15) 0.0199(16) C11 0.084(3) 0.064(3) 0.058(2) 0.0009(18) 0.032(2) 0.028(2) C12 0.076(3) 0.064(2) 0.0490(19) 0.0014(17) 0.0219(18) 0.019(2) P1 0.0621(6) 0.0533(6) 0.0526(5) 0.0030(4) 0.0106(4) 0.0212(5) F5 0.103(2) 0.0552(16) 0.128(3) 0.0011(17) 0.021(2) 0.0222(17) F6 0.132(3) 0.0584(16) 0.0672(15) 0.0111(12) 0.0308(16) 0.0333(17) F1 0.142(6) 0.079(4) 0.063(3) 0.017(3) 0.033(4) 0.026(4) F2 0.070(4) 0.084(4) 0.163(7) -0.001(4) -0.011(4) 0.039(3) F3 0.153(7) 0.088(5) 0.058(3) 0.003(3) 0.038(4) 0.034(5) F4 0.064(3) 0.108(5) 0.144(7) 0.008(5) 0.003(4) 0.025(3) F2A 0.102(6) 0.084(5) 0.102(5) 0.009(4) -0.028(4) 0.029(4) F1A 0.128(6) 0.100(6) 0.125(7) 0.029(5) 0.079(5) 0.046(5) F4A 0.122(8) 0.100(6) 0.092(5) 0.021(5) -0.032(5) 0.035(6) F3A 0.106(6) 0.074(5) 0.130(7) 0.016(4) 0.060(5) 0.048(5) _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 Pd N1 2.026(3) 2_755 ? Pd N1 2.026(3) . ? Pd N2 2.044(3) 2_755 ? Pd N2 2.044(3) . ? N1 C1 1.339(5) . ? N1 C5 1.366(4) . ? N2 C10 1.330(5) . ? N2 C6 1.384(4) . ? O1 C4 1.364(4) . ? O1 C11 1.449(5) . ? O2 C7 1.350(4) . ? O2 C12 1.437(5) . ? C1 C2 1.382(5) . ? C2 C3 1.371(6) . ? C3 C4 1.392(5) . ? C4 C5 1.398(5) . ? C5 C6 1.481(5) . ? C6 C7 1.396(5) . ? C7 C8 1.400(6) . ? C8 C9 1.369(6) . ? C9 C10 1.385(5) . ? C11 C12 1.493(7) . ? P1 F4A 1.498(9) . ? P1 F3 1.545(7) . ? P1 F1A 1.559(8) . ? P1 F2 1.562(7) . ? P1 F4 1.592(8) . ? P1 F6 1.595(3) . ? P1 F1 1.597(7) . ? P1 F5 1.597(3) . ? P1 F3A 1.615(9) . ? P1 F2A 1.630(8) . ? F1 F1A 0.909(12) . ? F1 F4A 1.506(16) . ? F2 F2A 1.025(11) . ? F2 F1A 1.494(15) . ? F3 F3A 0.788(11) . ? F3 F2A 1.581(14) . ? F4 F4A 0.791(13) . ? F4 F3A 1.657(16) . ? 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 N1 Pd N1 180.00(19) 2_755 . ? N1 Pd N2 78.77(11) 2_755 2_755 ? N1 Pd N2 101.23(11) . 2_755 ? N1 Pd N2 101.23(11) 2_755 . ? N1 Pd N2 78.77(11) . . ? N2 Pd N2 180.0(3) 2_755 . ? C1 N1 C5 120.0(3) . . ? C1 N1 Pd 126.1(2) . . ? C5 N1 Pd 113.7(2) . . ? C10 N2 C6 121.2(3) . . ? C10 N2 Pd 126.8(2) . . ? C6 N2 Pd 111.1(2) . . ? C4 O1 C11 113.8(3) . . ? C7 O2 C12 120.8(3) . . ? N1 C1 C2 122.5(3) . . ? C3 C2 C1 118.4(3) . . ? C2 C3 C4 119.8(3) . . ? O1 C4 C3 119.3(3) . . ? O1 C4 C5 120.9(3) . . ? C3 C4 C5 119.6(3) . . ? N1 C5 C4 119.4(3) . . ? N1 C5 C6 114.6(3) . . ? C4 C5 C6 124.7(3) . . ? N2 C6 C7 118.4(3) . . ? N2 C6 C5 111.4(3) . . ? C7 C6 C5 129.7(3) . . ? O2 C7 C6 128.1(4) . . ? O2 C7 C8 113.8(3) . . ? C6 C7 C8 118.1(3) . . ? C9 C8 C7 120.6(4) . . ? C8 C9 C10 118.9(4) . . ? N2 C10 C9 120.9(3) . . ? O1 C11 C12 108.8(3) . . ? O2 C12 C11 109.4(4) . . ? F4A P1 F3 118.4(7) . . ? F4A P1 F1A 91.5(7) . . ? F3 P1 F1A 149.9(7) . . ? F4A P1 F2 147.3(7) . . ? F3 P1 F2 92.7(6) . . ? F1A P1 F2 57.2(6) . . ? F4A P1 F4 29.4(5) . . ? F3 P1 F4 89.1(5) . . ? F1A P1 F4 120.9(6) . . ? F2 P1 F4 172.6(5) . . ? F4A P1 F6 91.5(5) . . ? F3 P1 F6 95.5(3) . . ? F1A P1 F6 86.8(4) . . ? F2 P1 F6 95.5(3) . . ? F4 P1 F6 91.5(4) . . ? F4A P1 F1 58.1(6) . . ? F3 P1 F1 173.6(5) . . ? F1A P1 F1 33.4(4) . . ? F2 P1 F1 89.9(5) . . ? F4 P1 F1 87.6(5) . . ? F6 P1 F1 90.1(3) . . ? F4A P1 F5 89.2(5) . . ? F3 P1 F5 84.1(4) . . ? F1A P1 F5 93.3(4) . . ? F2 P1 F5 84.0(3) . . ? F4 P1 F5 89.0(4) . . ? F6 P1 F5 179.3(2) . . ? F1 P1 F5 90.3(3) . . ? F4A P1 F3A 91.6(7) . . ? F3 P1 F3A 28.8(4) . . ? F1A P1 F3A 172.4(5) . . ? F2 P1 F3A 120.7(6) . . ? F4 P1 F3A 62.2(5) . . ? F6 P1 F3A 86.1(4) . . ? F1 P1 F3A 149.4(6) . . ? F5 P1 F3A 93.7(4) . . ? F4A P1 F2A 172.9(6) . . ? F3 P1 F2A 59.7(6) . . ? F1A P1 F2A 91.2(6) . . ? F2 P1 F2A 37.4(4) . . ? F4 P1 F2A 147.0(6) . . ? F6 P1 F2A 82.1(3) . . ? F1 P1 F2A 124.5(6) . . ? F5 P1 F2A 97.3(4) . . ? F3A P1 F2A 85.1(6) . . ? F1A F1 F4A 128.5(10) . . ? F1A F1 P1 71.0(7) . . ? F4A F1 P1 57.7(4) . . ? F2A F2 F1A 128.5(10) . . ? F2A F2 P1 74.9(7) . . ? F1A F2 P1 61.3(5) . . ? F3A F3 P1 80.5(10) . . ? F3A F3 F2A 132.8(12) . . ? P1 F3 F2A 62.9(5) . . ? F4A F4 P1 68.7(10) . . ? F4A F4 F3A 128.1(14) . . ? P1 F4 F3A 59.6(4) . . ? F2 F2A F3 117.7(9) . . ? F2 F2A P1 67.7(6) . . ? F3 F2A P1 57.5(4) . . ? F1 F1A F2 135.1(11) . . ? F1 F1A P1 75.6(8) . . ? F2 F1A P1 61.5(5) . . ? F4 F4A P1 81.9(11) . . ? F4 F4A F1 146.1(14) . . ? P1 F4A F1 64.2(5) . . ? F3 F3A P1 70.7(9) . . ? F3 F3A F4 124.6(13) . . ? P1 F3A F4 58.2(5) . . ? 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 N1 Pd N1 C1 0(100) 2_755 . . . ? N2 Pd N1 C1 24.2(3) 2_755 . . . ? N2 Pd N1 C1 -155.8(3) . . . . ? N1 Pd N1 C5 0(100) 2_755 . . . ? N2 Pd N1 C5 -160.3(2) 2_755 . . . ? N2 Pd N1 C5 19.7(2) . . . . ? N1 Pd N2 C10 -17.7(3) 2_755 . . . ? N1 Pd N2 C10 162.3(3) . . . . ? N2 Pd N2 C10 -43(100) 2_755 . . . ? N1 Pd N2 C6 150.8(2) 2_755 . . . ? N1 Pd N2 C6 -29.2(2) . . . . ? N2 Pd N2 C6 125(100) 2_755 . . . ? C5 N1 C1 C2 2.9(6) . . . . ? Pd N1 C1 C2 178.2(3) . . . . ? N1 C1 C2 C3 -3.5(6) . . . . ? C1 C2 C3 C4 0.0(6) . . . . ? C11 O1 C4 C3 -96.2(4) . . . . ? C11 O1 C4 C5 88.7(4) . . . . ? C2 C3 C4 O1 -171.4(4) . . . . ? C2 C3 C4 C5 3.8(6) . . . . ? C1 N1 C5 C4 1.0(5) . . . . ? Pd N1 C5 C4 -174.8(2) . . . . ? C1 N1 C5 C6 168.5(3) . . . . ? Pd N1 C5 C6 -7.4(4) . . . . ? O1 C4 C5 N1 170.7(3) . . . . ? C3 C4 C5 N1 -4.3(5) . . . . ? O1 C4 C5 C6 4.7(5) . . . . ? C3 C4 C5 C6 -170.4(3) . . . . ? C10 N2 C6 C7 14.5(5) . . . . ? Pd N2 C6 C7 -154.7(3) . . . . ? C10 N2 C6 C5 -157.7(3) . . . . ? Pd N2 C6 C5 33.1(3) . . . . ? N1 C5 C6 N2 -17.2(4) . . . . ? C4 C5 C6 N2 149.4(3) . . . . ? N1 C5 C6 C7 171.7(4) . . . . ? C4 C5 C6 C7 -21.7(6) . . . . ? C12 O2 C7 C6 -9.3(6) . . . . ? C12 O2 C7 C8 169.7(4) . . . . ? N2 C6 C7 O2 163.6(4) . . . . ? C5 C6 C7 O2 -25.8(7) . . . . ? N2 C6 C7 C8 -15.3(5) . . . . ? C5 C6 C7 C8 155.3(4) . . . . ? O2 C7 C8 C9 -173.4(4) . . . . ? C6 C7 C8 C9 5.7(6) . . . . ? C7 C8 C9 C10 5.1(7) . . . . ? C6 N2 C10 C9 -3.6(6) . . . . ? Pd N2 C10 C9 163.9(3) . . . . ? C8 C9 C10 N2 -6.4(6) . . . . ? C4 O1 C11 C12 -68.3(4) . . . . ? C7 O2 C12 C11 94.2(4) . . . . ? O1 C11 C12 O2 -52.0(4) . . . . ? F4A P1 F1 F1A 175.8(12) . . . . ? F3 P1 F1 F1A -126(4) . . . . ? F2 P1 F1 F1A -11.4(10) . . . . ? F4 P1 F1 F1A 175.5(10) . . . . ? F6 P1 F1 F1A 84.1(10) . . . . ? F5 P1 F1 F1A -95.4(9) . . . . ? F3A P1 F1 F1A 166.7(10) . . . . ? F2A P1 F1 F1A 3.6(12) . . . . ? F3 P1 F1 F4A 59(5) . . . . ? F1A P1 F1 F4A -175.8(12) . . . . ? F2 P1 F1 F4A 172.8(6) . . . . ? F4 P1 F1 F4A -0.2(8) . . . . ? F6 P1 F1 F4A -91.7(6) . . . . ? F5 P1 F1 F4A 88.8(6) . . . . ? F3A P1 F1 F4A -9.1(11) . . . . ? F2A P1 F1 F4A -172.1(7) . . . . ? F4A P1 F2 F2A 170.7(10) . . . . ? F3 P1 F2 F2A -26.5(8) . . . . ? F1A P1 F2 F2A 151.9(10) . . . . ? F4 P1 F2 F2A -131(4) . . . . ? F6 P1 F2 F2A 69.3(8) . . . . ? F1 P1 F2 F2A 159.4(8) . . . . ? F5 P1 F2 F2A -110.3(8) . . . . ? F3A P1 F2 F2A -19.5(10) . . . . ? F4A P1 F2 F1A 18.8(11) . . . . ? F3 P1 F2 F1A -178.4(6) . . . . ? F4 P1 F2 F1A 77(4) . . . . ? F6 P1 F2 F1A -82.7(5) . . . . ? F1 P1 F2 F1A 7.5(6) . . . . ? F5 P1 F2 F1A 97.8(5) . . . . ? F3A P1 F2 F1A -171.4(6) . . . . ? F2A P1 F2 F1A -151.9(10) . . . . ? F4A P1 F3 F3A -23.0(14) . . . . ? F1A P1 F3 F3A 164.8(11) . . . . ? F2 P1 F3 F3A 167.5(12) . . . . ? F4 P1 F3 F3A -19.7(12) . . . . ? F6 P1 F3 F3A 71.7(12) . . . . ? F1 P1 F3 F3A -79(5) . . . . ? F5 P1 F3 F3A -108.8(12) . . . . ? F2A P1 F3 F3A 149.2(14) . . . . ? F4A P1 F3 F2A -172.2(6) . . . . ? F1A P1 F3 F2A 15.6(12) . . . . ? F2 P1 F3 F2A 18.3(6) . . . . ? F4 P1 F3 F2A -168.9(6) . . . . ? F6 P1 F3 F2A -77.5(5) . . . . ? F1 P1 F3 F2A 132(4) . . . . ? F5 P1 F3 F2A 102.0(5) . . . . ? F3A P1 F3 F2A -149.2(14) . . . . ? F3 P1 F4 F4A -174.1(15) . . . . ? F1A P1 F4 F4A 3.2(17) . . . . ? F2 P1 F4 F4A -70(5) . . . . ? F6 P1 F4 F4A 90.4(15) . . . . ? F1 P1 F4 F4A 0.4(15) . . . . ? F5 P1 F4 F4A -90.0(15) . . . . ? F3A P1 F4 F4A 175.3(17) . . . . ? F2A P1 F4 F4A 168.1(12) . . . . ? F4A P1 F4 F3A -175.3(17) . . . . ? F3 P1 F4 F3A 10.6(6) . . . . ? F1A P1 F4 F3A -172.1(6) . . . . ? F2 P1 F4 F3A 115(4) . . . . ? F6 P1 F4 F3A -84.9(4) . . . . ? F1 P1 F4 F3A -174.9(5) . . . . ? F5 P1 F4 F3A 94.7(4) . . . . ? F2A P1 F4 F3A -7.2(11) . . . . ? F1A F2 F2A F3 61.2(15) . . . . ? P1 F2 F2A F3 29.4(8) . . . . ? F1A F2 F2A P1 31.8(10) . . . . ? F3A F3 F2A F2 -76(2) . . . . ? P1 F3 F2A F2 -32.6(10) . . . . ? F3A F3 F2A P1 -43.5(18) . . . . ? F4A P1 F2A F2 -135(5) . . . . ? F3 P1 F2A F2 148.9(10) . . . . ? F1A P1 F2A F2 -23.3(8) . . . . ? F4 P1 F2A F2 169.7(8) . . . . ? F6 P1 F2A F2 -109.9(8) . . . . ? F1 P1 F2A F2 -25.3(10) . . . . ? F5 P1 F2A F2 70.1(8) . . . . ? F3A P1 F2A F2 163.3(8) . . . . ? F4A P1 F2A F3 76(5) . . . . ? F1A P1 F2A F3 -172.2(6) . . . . ? F2 P1 F2A F3 -148.9(10) . . . . ? F4 P1 F2A F3 20.7(11) . . . . ? F6 P1 F2A F3 101.1(5) . . . . ? F1 P1 F2A F3 -174.2(5) . . . . ? F5 P1 F2A F3 -78.8(5) . . . . ? F3A P1 F2A F3 14.3(6) . . . . ? F4A F1 F1A F2 22(3) . . . . ? P1 F1 F1A F2 17.0(14) . . . . ? F4A F1 F1A P1 4.6(13) . . . . ? F2A F2 F1A F1 -54(2) . . . . ? P1 F2 F1A F1 -18.8(16) . . . . ? F2A F2 F1A P1 -35.5(11) . . . . ? F4A P1 F1A F1 -3.6(10) . . . . ? F3 P1 F1A F1 169.5(9) . . . . ? F2 P1 F1A F1 166.4(12) . . . . ? F4 P1 F1A F1 -5.2(12) . . . . ? F6 P1 F1A F1 -95.0(9) . . . . ? F5 P1 F1A F1 85.6(9) . . . . ? F3A P1 F1A F1 -117(5) . . . . ? F2A P1 F1A F1 -177.0(10) . . . . ? F4A P1 F1A F2 -170.0(6) . . . . ? F3 P1 F1A F2 3.2(12) . . . . ? F4 P1 F1A F2 -171.6(6) . . . . ? F6 P1 F1A F2 98.6(4) . . . . ? F1 P1 F1A F2 -166.4(12) . . . . ? F5 P1 F1A F2 -80.7(5) . . . . ? F3A P1 F1A F2 76(5) . . . . ? F2A P1 F1A F2 16.6(6) . . . . ? F3A F4 F4A P1 5.2(18) . . . . ? P1 F4 F4A F1 -1(3) . . . . ? F3A F4 F4A F1 4(5) . . . . ? F3 P1 F4A F4 6.7(17) . . . . ? F1A P1 F4A F4 -177.2(15) . . . . ? F2 P1 F4A F4 167.1(10) . . . . ? F6 P1 F4A F4 -90.4(14) . . . . ? F1 P1 F4A F4 -179.6(17) . . . . ? F5 P1 F4A F4 89.5(14) . . . . ? F3A P1 F4A F4 -4.2(15) . . . . ? F2A P1 F4A F4 -65(6) . . . . ? F3 P1 F4A F1 -173.8(5) . . . . ? F1A P1 F4A F1 2.3(7) . . . . ? F2 P1 F4A F1 -13.4(12) . . . . ? F4 P1 F4A F1 179.6(17) . . . . ? F6 P1 F4A F1 89.2(5) . . . . ? F5 P1 F4A F1 -90.9(5) . . . . ? F3A P1 F4A F1 175.4(6) . . . . ? F2A P1 F4A F1 114(5) . . . . ? F1A F1 F4A F4 -4(4) . . . . ? P1 F1 F4A F4 1(3) . . . . ? F1A F1 F4A P1 -5.1(14) . . . . ? F2A F3 F3A P1 38.4(15) . . . . ? P1 F3 F3A F4 23.2(13) . . . . ? F2A F3 F3A F4 62(2) . . . . ? F4A P1 F3A F3 159.9(12) . . . . ? F1A P1 F3A F3 -87(5) . . . . ? F2 P1 F3A F3 -14.6(14) . . . . ? F4 P1 F3A F3 157.6(14) . . . . ? F6 P1 F3A F3 -108.7(12) . . . . ? F1 P1 F3A F3 167.6(9) . . . . ? F5 P1 F3A F3 70.6(12) . . . . ? F2A P1 F3A F3 -26.4(12) . . . . ? F4A P1 F3A F4 2.3(8) . . . . ? F3 P1 F3A F4 -157.6(14) . . . . ? F1A P1 F3A F4 116(5) . . . . ? F2 P1 F3A F4 -172.2(6) . . . . ? F6 P1 F3A F4 93.7(5) . . . . ? F1 P1 F3A F4 10.0(10) . . . . ? F5 P1 F3A F4 -86.9(5) . . . . ? F2A P1 F3A F4 176.1(6) . . . . ? F4A F4 F3A F3 -32(3) . . . . ? P1 F4 F3A F3 -25.9(15) . . . . ? F4A F4 F3A P1 -6(2) . . . . ? _diffrn_measured_fraction_theta_max 0.908 _diffrn_reflns_theta_full 29.00 _diffrn_measured_fraction_theta_full 0.908 _refine_diff_density_max 0.592 _refine_diff_density_min -1.228 _refine_diff_density_rms 0.080 #===END data_4c _database_code_depnum_ccdc_archive 'CCDC 667853' _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis(3,3-(propylenedioxy)-2,2-bipyridine)-palladium(II) bis(hexafluorophosphate) ; _chemical_name_common ;bis(3,3-(propylenedioxy)-2,2-bipyridine)-palladium(ii) bis(hexafluorophosphate) ; _chemical_melting_point ? _chemical_formula_moiety 'C26 H24 N4 O4 Pd 2+, 2(P F6 1-)' _chemical_formula_sum 'C26 H24 F12 N4 O4 P2 Pd' _chemical_formula_weight 852.83 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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.613(3) _cell_length_b 13.447(3) _cell_length_c 17.281(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.39(3) _cell_angle_gamma 90.00 _cell_volume 3137.1(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour yellow _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.806 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1696 _exptl_absorpt_coefficient_mu 0.806 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mok\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'image plate dip1030' _diffrn_measurement_method 'laser scanner' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29930 _diffrn_reflns_av_R_equivalents 0.0997 _diffrn_reflns_av_sigmaI/netI 0.1366 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 26.42 _reflns_number_total 6100 _reflns_number_gt 2573 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Xpress' _computing_cell_refinement 'Denzo (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELX97 (Sheldrick, 1998)' _computing_structure_refinement 'SHELX97 (Sheldrick, 1998)' _computing_molecular_graphics 'Ortep3/windows (Farrugia,1997)' _computing_publication_material 'Wingx 1.70.00 (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0345P)^2^] 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 6100 _refine_ls_number_parameters 442 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1355 _refine_ls_R_factor_gt 0.0449 _refine_ls_wR_factor_ref 0.1085 _refine_ls_wR_factor_gt 0.0856 _refine_ls_goodness_of_fit_ref 0.801 _refine_ls_restrained_S_all 0.801 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd 0.84314(3) 0.13085(3) 0.90360(3) 0.05420(16) Uani 1 1 d . . . N1 N 0.8348(3) 0.2738(3) 0.9441(3) 0.0550(12) Uani 1 1 d . . . N2 N 0.7754(3) 0.1012(3) 0.9999(3) 0.0571(13) Uani 1 1 d . . . N3 N 0.8902(3) -0.0076(3) 0.8792(3) 0.0564(13) Uani 1 1 d . . . N4 N 0.8660(3) 0.1540(3) 0.7902(3) 0.0538(12) Uani 1 1 d . . . O1 O 0.8158(3) 0.3364(3) 1.1425(2) 0.0625(11) Uani 1 1 d . . . O2 O 0.6341(3) 0.2778(3) 1.0966(2) 0.0631(11) Uani 1 1 d . . . O3 O 1.0188(3) -0.0842(3) 0.7213(3) 0.0648(11) Uani 1 1 d . . . O4 O 0.8512(3) -0.0363(3) 0.6432(2) 0.0679(12) Uani 1 1 d . . . C1 C 0.8797(4) 0.3546(4) 0.9185(4) 0.0660(17) Uani 1 1 d . . . H1 H 0.9037 0.3533 0.8705 0.079 Uiso 1 1 calc R . . C2 C 0.8896(5) 0.4391(4) 0.9639(4) 0.0683(18) Uani 1 1 d . . . H2 H 0.9126 0.4973 0.9435 0.082 Uiso 1 1 calc R . . C3 C 0.8662(4) 0.4387(4) 1.0384(4) 0.0647(17) Uani 1 1 d . . . H3 H 0.8775 0.4948 1.0699 0.078 Uiso 1 1 calc R . . C4 C 0.8257(4) 0.3544(4) 1.0663(4) 0.0557(15) Uani 1 1 d . . . C5 C 0.8026(4) 0.2750(4) 1.0149(4) 0.0507(14) Uani 1 1 d . . . C6 C 0.7492(4) 0.1873(4) 1.0358(3) 0.0526(15) Uani 1 1 d . . . C7 C 0.6724(5) 0.1876(5) 1.0801(3) 0.0596(17) Uani 1 1 d . . . C8 C 0.6318(5) 0.0990(5) 1.1000(4) 0.078(2) Uani 1 1 d . . . H8 H 0.5847 0.0975 1.1345 0.094 Uiso 1 1 calc R . . C9 C 0.6625(5) 0.0129(5) 1.0679(4) 0.083(2) Uani 1 1 d . . . H9 H 0.6371 -0.0480 1.0815 0.100 Uiso 1 1 calc R . . C10 C 0.7309(5) 0.0163(4) 1.0155(4) 0.0688(19) Uani 1 1 d . . . H10 H 0.7464 -0.0419 0.9906 0.083 Uiso 1 1 calc R . . C11 C 0.9154(4) -0.0798(4) 0.9313(4) 0.0620(17) Uani 1 1 d . . . H11 H 0.9011 -0.0725 0.9822 0.074 Uiso 1 1 calc R . . C12 C 0.9621(5) -0.1648(5) 0.9107(4) 0.0709(19) Uani 1 1 d . . . H12 H 0.9717 -0.2176 0.9456 0.085 Uiso 1 1 calc R . . C13 C 0.9946(4) -0.1724(4) 0.8391(4) 0.0643(17) Uani 1 1 d . . . H13 H 1.0288 -0.2284 0.8259 0.077 Uiso 1 1 calc R . . C14 C 0.9752(4) -0.0946(4) 0.7869(4) 0.0555(16) Uani 1 1 d . . . C15 C 0.9163(4) -0.0159(4) 0.8071(4) 0.0496(15) Uani 1 1 d . . . C16 C 0.8831(4) 0.0660(4) 0.7537(4) 0.0529(15) Uani 1 1 d . . . C17 C 0.8583(4) 0.0574(5) 0.6740(4) 0.0591(16) Uani 1 1 d . . . C18 C 0.8309(5) 0.1412(5) 0.6298(4) 0.0737(18) Uani 1 1 d . . . H18 H 0.8184 0.1373 0.5757 0.088 Uiso 1 1 calc R . . C19 C 0.8225(5) 0.2303(5) 0.6676(4) 0.0744(19) Uani 1 1 d . . . H19 H 0.8083 0.2884 0.6391 0.089 Uiso 1 1 calc R . . C20 C 0.8351(4) 0.2329(4) 0.7474(4) 0.0653(17) Uani 1 1 d . . . H20 H 0.8217 0.2916 0.7725 0.078 Uiso 1 1 calc R . . C21 C 0.7798(5) 0.4125(5) 1.1913(4) 0.088(2) Uani 1 1 d . . . H21A H 0.7989 0.4775 1.1741 0.105 Uiso 1 1 calc R . . H21B H 0.8099 0.4034 1.2448 0.105 Uiso 1 1 calc R . . C22 C 0.6712(6) 0.4077(6) 1.1877(4) 0.095(2) Uani 1 1 d . . . H22A H 0.6419 0.4489 1.1447 0.113 Uiso 1 1 calc R . . H22B H 0.6525 0.4357 1.2354 0.113 Uiso 1 1 calc R . . C23 C 0.6279(5) 0.3043(6) 1.1772(4) 0.089(2) Uani 1 1 d . . . H23A H 0.6655 0.2579 1.2123 0.107 Uiso 1 1 calc R . . H23B H 0.5596 0.3039 1.1875 0.107 Uiso 1 1 calc R . . C24 C 1.0257(6) -0.1675(5) 0.6695(4) 0.093(2) Uani 1 1 d . . . H24A H 1.0178 -0.2288 0.6976 0.112 Uiso 1 1 calc R . . H24B H 1.0911 -0.1681 0.6528 0.112 Uiso 1 1 calc R . . C25 C 0.9516(6) -0.1636(6) 0.6013(5) 0.119(3) Uani 1 1 d . . . H25A H 0.8983 -0.2086 0.6095 0.143 Uiso 1 1 calc R . . H25B H 0.9813 -0.1880 0.5569 0.143 Uiso 1 1 calc R . . C26 C 0.9079(6) -0.0629(6) 0.5812(4) 0.092(2) Uani 1 1 d . . . H26A H 0.9599 -0.0145 0.5774 0.110 Uiso 1 1 calc R . . H26B H 0.8654 -0.0652 0.5317 0.110 Uiso 1 1 calc R . . P1 P 1.19112(16) 0.27078(13) 0.91359(12) 0.0756(6) Uani 1 1 d . . . P2 P 0.58193(14) 0.03509(13) 0.77665(12) 0.0709(5) Uani 1 1 d . . . F1 F 1.1178(3) 0.1798(3) 0.8999(3) 0.1192(15) Uani 1 1 d . . . F2 F 1.1213(4) 0.3214(3) 0.9686(3) 0.1223(16) Uani 1 1 d . . . F3 F 1.2659(3) 0.3625(3) 0.9306(2) 0.0961(12) Uani 1 1 d . . . F4 F 1.2596(3) 0.2202(3) 0.8597(3) 0.1235(16) Uani 1 1 d . . . F5 F 1.1346(4) 0.3279(3) 0.8427(3) 0.1403(19) Uani 1 1 d . . . F6 F 1.2456(3) 0.2140(3) 0.9872(2) 0.1067(14) Uani 1 1 d . . . F7 F 0.4907(3) 0.0801(3) 0.8092(3) 0.143(2) Uani 1 1 d . . . F8 F 0.5447(5) 0.0777(5) 0.6968(3) 0.195(3) Uani 1 1 d . . . F9 F 0.6722(3) -0.0120(3) 0.7453(4) 0.154(2) Uani 1 1 d . . . F10 F 0.6181(5) -0.0091(5) 0.8564(3) 0.198(3) Uani 1 1 d . . . F11 F 0.6418(3) 0.1327(3) 0.7981(3) 0.1396(19) Uani 1 1 d . . . F12 F 0.5232(3) -0.0634(3) 0.7558(3) 0.1320(18) 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 Pd 0.0625(3) 0.0505(2) 0.0511(3) 0.0007(2) 0.0128(2) 0.0001(3) N1 0.059(3) 0.053(3) 0.055(3) 0.002(2) 0.017(3) -0.008(2) N2 0.063(3) 0.054(3) 0.056(3) 0.002(2) 0.015(3) -0.001(3) N3 0.061(3) 0.066(3) 0.045(3) 0.002(3) 0.019(3) 0.006(3) N4 0.065(3) 0.048(3) 0.048(3) 0.002(2) 0.006(3) 0.001(2) O1 0.068(3) 0.065(3) 0.054(3) -0.006(2) 0.005(2) 0.014(2) O2 0.058(3) 0.072(3) 0.061(3) 0.001(2) 0.013(2) 0.015(2) O3 0.062(3) 0.064(2) 0.071(3) -0.005(2) 0.020(2) 0.003(2) O4 0.065(3) 0.074(3) 0.064(3) -0.014(2) 0.010(2) -0.007(2) C1 0.073(4) 0.064(4) 0.063(4) 0.008(4) 0.013(3) -0.006(4) C2 0.075(5) 0.056(4) 0.074(5) 0.000(4) 0.011(4) -0.011(3) C3 0.072(5) 0.057(4) 0.066(5) -0.009(3) 0.013(4) 0.005(3) C4 0.053(4) 0.062(4) 0.053(4) 0.000(3) 0.009(3) 0.008(3) C5 0.047(4) 0.058(4) 0.050(4) 0.001(3) 0.014(3) 0.005(3) C6 0.052(4) 0.059(4) 0.047(4) 0.009(3) 0.009(3) 0.003(3) C7 0.059(4) 0.064(4) 0.057(4) 0.010(3) 0.011(3) 0.006(3) C8 0.078(5) 0.086(5) 0.079(5) 0.008(4) 0.042(4) 0.000(4) C9 0.093(6) 0.068(4) 0.095(6) 0.016(4) 0.032(5) -0.020(4) C10 0.087(5) 0.046(3) 0.077(5) 0.003(3) 0.023(4) -0.008(3) C11 0.071(5) 0.064(4) 0.051(4) 0.011(3) 0.007(3) 0.002(3) C12 0.079(5) 0.064(4) 0.071(5) 0.014(4) 0.014(4) 0.013(4) C13 0.067(4) 0.057(4) 0.069(5) 0.005(4) 0.008(4) 0.016(3) C14 0.048(4) 0.055(4) 0.066(4) -0.008(3) 0.018(3) -0.002(3) C15 0.051(4) 0.043(3) 0.054(4) 0.002(3) 0.007(3) -0.005(3) C16 0.050(4) 0.055(4) 0.055(4) -0.003(3) 0.007(3) 0.001(3) C17 0.061(4) 0.063(4) 0.053(4) -0.005(3) 0.008(3) -0.006(3) C18 0.092(5) 0.081(5) 0.048(4) 0.010(4) 0.008(4) -0.007(4) C19 0.098(5) 0.072(5) 0.053(5) 0.009(4) 0.009(4) 0.004(4) C20 0.074(5) 0.060(4) 0.060(5) 0.004(3) 0.005(4) 0.002(3) C21 0.104(6) 0.087(5) 0.074(5) -0.026(4) 0.021(5) 0.016(4) C22 0.098(6) 0.101(6) 0.086(6) -0.022(5) 0.018(5) 0.023(5) C23 0.076(5) 0.137(7) 0.057(5) -0.006(5) 0.022(4) 0.020(5) C24 0.123(7) 0.082(5) 0.083(6) -0.019(4) 0.041(5) 0.007(5) C25 0.123(7) 0.114(7) 0.115(8) -0.057(6) -0.001(6) 0.029(6) C26 0.108(6) 0.101(6) 0.069(5) -0.030(4) 0.024(5) -0.014(5) P1 0.0997(15) 0.0623(11) 0.0655(13) 0.0029(10) 0.0132(12) 0.0064(11) P2 0.0624(12) 0.0715(12) 0.0798(15) -0.0073(11) 0.0127(11) -0.0040(10) F1 0.138(4) 0.094(3) 0.119(4) -0.002(3) -0.007(3) -0.029(3) F2 0.149(4) 0.092(3) 0.141(4) -0.006(3) 0.074(3) 0.010(3) F3 0.118(3) 0.074(2) 0.099(3) 0.004(2) 0.026(3) -0.020(2) F4 0.149(4) 0.109(3) 0.124(4) -0.023(3) 0.062(3) 0.016(3) F5 0.195(5) 0.111(3) 0.103(4) 0.032(3) -0.029(3) 0.026(3) F6 0.160(4) 0.070(2) 0.080(3) 0.007(2) -0.019(3) -0.001(3) F7 0.093(3) 0.118(3) 0.231(6) -0.054(4) 0.074(4) -0.007(3) F8 0.255(7) 0.209(6) 0.111(5) 0.060(4) -0.008(5) 0.019(5) F9 0.087(3) 0.113(3) 0.279(7) -0.055(4) 0.084(4) -0.011(3) F10 0.273(8) 0.204(6) 0.098(5) 0.037(4) -0.048(5) 0.003(5) F11 0.090(3) 0.087(3) 0.245(6) -0.049(4) 0.036(3) -0.027(3) F12 0.089(3) 0.101(3) 0.209(5) -0.052(3) 0.032(3) -0.030(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 Pd N3 2.031(5) . ? Pd N2 2.043(5) . ? Pd N4 2.047(5) . ? Pd N1 2.054(4) . ? N1 C1 1.348(6) . ? N1 C5 1.352(6) . ? N2 C10 1.336(6) . ? N2 C6 1.383(6) . ? N3 C11 1.339(6) . ? N3 C15 1.342(7) . ? N4 C20 1.331(7) . ? N4 C16 1.375(6) . ? O1 C4 1.362(6) . ? O1 C21 1.451(6) . ? O2 C7 1.365(6) . ? O2 C23 1.451(7) . ? O3 C14 1.352(6) . ? O3 C24 1.445(7) . ? O4 C17 1.366(6) . ? O4 C26 1.443(7) . ? C1 C2 1.377(7) . ? C2 C3 1.366(8) . ? C3 C4 1.376(7) . ? C4 C5 1.398(7) . ? C5 C6 1.457(7) . ? C6 C7 1.372(7) . ? C7 C8 1.375(8) . ? C8 C9 1.373(8) . ? C9 C10 1.380(8) . ? C11 C12 1.377(7) . ? C12 C13 1.370(8) . ? C13 C14 1.384(7) . ? C14 C15 1.399(7) . ? C15 C16 1.471(7) . ? C16 C17 1.380(7) . ? C17 C18 1.385(8) . ? C18 C19 1.377(8) . ? C19 C20 1.368(8) . ? C21 C22 1.474(9) . ? C22 C23 1.511(9) . ? C24 C25 1.450(9) . ? C25 C26 1.502(9) . ? P1 F4 1.557(4) . ? P1 F5 1.561(4) . ? P1 F1 1.577(4) . ? P1 F2 1.582(4) . ? P1 F6 1.584(4) . ? P1 F3 1.603(4) . ? P2 F8 1.520(5) . ? P2 F10 1.523(5) . ? P2 F9 1.541(4) . ? P2 F7 1.551(4) . ? P2 F11 1.564(4) . ? P2 F12 1.565(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Pd N2 100.24(19) . . ? N3 Pd N4 81.35(18) . . ? N2 Pd N4 161.74(18) . . ? N3 Pd N1 164.06(19) . . ? N2 Pd N1 81.68(19) . . ? N4 Pd N1 101.84(18) . . ? C1 N1 C5 120.0(5) . . ? C1 N1 Pd 126.6(4) . . ? C5 N1 Pd 111.0(4) . . ? C10 N2 C6 118.3(5) . . ? C10 N2 Pd 126.6(4) . . ? C6 N2 Pd 111.9(4) . . ? C11 N3 C15 119.3(5) . . ? C11 N3 Pd 125.8(4) . . ? C15 N3 Pd 113.4(4) . . ? C20 N4 C16 119.4(5) . . ? C20 N4 Pd 125.3(4) . . ? C16 N4 Pd 111.4(4) . . ? C4 O1 C21 121.3(5) . . ? C7 O2 C23 119.3(5) . . ? C14 O3 C24 120.7(5) . . ? C17 O4 C26 119.9(5) . . ? N1 C1 C2 119.6(6) . . ? C3 C2 C1 121.1(6) . . ? C2 C3 C4 119.1(6) . . ? O1 C4 C3 125.4(6) . . ? O1 C4 C5 116.0(5) . . ? C3 C4 C5 118.3(6) . . ? N1 C5 C4 120.8(5) . . ? N1 C5 C6 116.5(5) . . ? C4 C5 C6 122.6(6) . . ? C7 C6 N2 120.9(5) . . ? C7 C6 C5 125.2(6) . . ? N2 C6 C5 113.6(5) . . ? O2 C7 C6 117.3(5) . . ? O2 C7 C8 122.7(5) . . ? C6 C7 C8 119.7(6) . . ? C9 C8 C7 118.4(6) . . ? C8 C9 C10 120.2(6) . . ? N2 C10 C9 121.5(6) . . ? N3 C11 C12 120.9(6) . . ? C13 C12 C11 120.6(6) . . ? C12 C13 C14 118.4(6) . . ? O3 C14 C13 123.9(5) . . ? O3 C14 C15 117.3(5) . . ? C13 C14 C15 118.4(6) . . ? N3 C15 C14 121.5(5) . . ? N3 C15 C16 115.1(5) . . ? C14 C15 C16 123.3(6) . . ? N4 C16 C17 119.8(5) . . ? N4 C16 C15 114.3(5) . . ? C17 C16 C15 125.4(5) . . ? O4 C17 C16 117.5(6) . . ? O4 C17 C18 122.4(6) . . ? C16 C17 C18 119.7(6) . . ? C19 C18 C17 118.6(6) . . ? C20 C19 C18 119.6(6) . . ? N4 C20 C19 122.0(6) . . ? O1 C21 C22 110.9(6) . . ? C21 C22 C23 114.8(6) . . ? O2 C23 C22 105.8(6) . . ? O3 C24 C25 112.4(6) . . ? C24 C25 C26 115.7(7) . . ? O4 C26 C25 106.5(6) . . ? F4 P1 F5 91.1(3) . . ? F4 P1 F1 89.3(3) . . ? F5 P1 F1 91.4(3) . . ? F4 P1 F2 179.5(3) . . ? F5 P1 F2 89.2(3) . . ? F1 P1 F2 90.4(3) . . ? F4 P1 F6 90.9(3) . . ? F5 P1 F6 178.0(3) . . ? F1 P1 F6 88.2(2) . . ? F2 P1 F6 88.8(3) . . ? F4 P1 F3 91.8(2) . . ? F5 P1 F3 90.1(2) . . ? F1 P1 F3 178.1(3) . . ? F2 P1 F3 88.6(2) . . ? F6 P1 F3 90.2(2) . . ? F8 P2 F10 179.1(4) . . ? F8 P2 F9 91.4(4) . . ? F10 P2 F9 88.7(4) . . ? F8 P2 F7 89.6(4) . . ? F10 P2 F7 90.3(4) . . ? F9 P2 F7 178.6(3) . . ? F8 P2 F11 90.1(3) . . ? F10 P2 F11 90.8(3) . . ? F9 P2 F11 90.8(2) . . ? F7 P2 F11 90.2(2) . . ? F8 P2 F12 90.5(3) . . ? F10 P2 F12 88.5(3) . . ? F9 P2 F12 88.7(2) . . ? F7 P2 F12 90.3(2) . . ? F11 P2 F12 179.2(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Pd N1 C1 71.4(9) . . . . ? N2 Pd N1 C1 169.5(5) . . . . ? N4 Pd N1 C1 -28.7(5) . . . . ? N3 Pd N1 C5 -90.6(8) . . . . ? N2 Pd N1 C5 7.5(4) . . . . ? N4 Pd N1 C5 169.3(4) . . . . ? N3 Pd N2 C10 -30.2(5) . . . . ? N4 Pd N2 C10 63.3(8) . . . . ? N1 Pd N2 C10 165.9(5) . . . . ? N3 Pd N2 C6 170.8(4) . . . . ? N4 Pd N2 C6 -95.8(6) . . . . ? N1 Pd N2 C6 6.9(4) . . . . ? N2 Pd N3 C11 -30.0(5) . . . . ? N4 Pd N3 C11 168.4(5) . . . . ? N1 Pd N3 C11 65.5(9) . . . . ? N2 Pd N3 C15 164.3(4) . . . . ? N4 Pd N3 C15 2.7(4) . . . . ? N1 Pd N3 C15 -100.2(8) . . . . ? N3 Pd N4 C20 167.5(5) . . . . ? N2 Pd N4 C20 71.0(8) . . . . ? N1 Pd N4 C20 -28.4(5) . . . . ? N3 Pd N4 C16 10.3(4) . . . . ? N2 Pd N4 C16 -86.2(7) . . . . ? N1 Pd N4 C16 174.4(4) . . . . ? C5 N1 C1 C2 -2.0(9) . . . . ? Pd N1 C1 C2 -162.5(4) . . . . ? N1 C1 C2 C3 8.3(10) . . . . ? C1 C2 C3 C4 -4.5(9) . . . . ? C21 O1 C4 C3 44.4(8) . . . . ? C21 O1 C4 C5 -143.2(6) . . . . ? C2 C3 C4 O1 167.1(5) . . . . ? C2 C3 C4 C5 -5.1(9) . . . . ? C1 N1 C5 C4 -7.8(8) . . . . ? Pd N1 C5 C4 155.5(4) . . . . ? C1 N1 C5 C6 176.0(5) . . . . ? Pd N1 C5 C6 -20.7(6) . . . . ? O1 C4 C5 N1 -161.5(5) . . . . ? C3 C4 C5 N1 11.4(8) . . . . ? O1 C4 C5 C6 14.4(8) . . . . ? C3 C4 C5 C6 -172.7(5) . . . . ? C10 N2 C6 C7 -6.6(8) . . . . ? Pd N2 C6 C7 154.4(5) . . . . ? C10 N2 C6 C5 179.7(5) . . . . ? Pd N2 C6 C5 -19.4(6) . . . . ? N1 C5 C6 C7 -146.0(6) . . . . ? C4 C5 C6 C7 38.0(9) . . . . ? N1 C5 C6 N2 27.4(7) . . . . ? C4 C5 C6 N2 -148.6(5) . . . . ? C23 O2 C7 C6 -125.9(6) . . . . ? C23 O2 C7 C8 59.9(8) . . . . ? N2 C6 C7 O2 -163.3(5) . . . . ? C5 C6 C7 O2 9.6(9) . . . . ? N2 C6 C7 C8 11.1(9) . . . . ? C5 C6 C7 C8 -175.9(6) . . . . ? O2 C7 C8 C9 167.2(6) . . . . ? C6 C7 C8 C9 -6.9(10) . . . . ? C7 C8 C9 C10 -1.4(10) . . . . ? C6 N2 C10 C9 -1.9(9) . . . . ? Pd N2 C10 C9 -159.8(5) . . . . ? C8 C9 C10 N2 5.9(11) . . . . ? C15 N3 C11 C12 -3.9(9) . . . . ? Pd N3 C11 C12 -168.9(4) . . . . ? N3 C11 C12 C13 7.9(9) . . . . ? C11 C12 C13 C14 -3.0(9) . . . . ? C24 O3 C14 C13 46.9(8) . . . . ? C24 O3 C14 C15 -140.8(6) . . . . ? C12 C13 C14 O3 166.9(5) . . . . ? C12 C13 C14 C15 -5.3(9) . . . . ? C11 N3 C15 C14 -4.7(8) . . . . ? Pd N3 C15 C14 162.0(4) . . . . ? C11 N3 C15 C16 178.6(5) . . . . ? Pd N3 C15 C16 -14.7(6) . . . . ? O3 C14 C15 N3 -163.3(5) . . . . ? C13 C14 C15 N3 9.4(8) . . . . ? O3 C14 C15 C16 13.1(8) . . . . ? C13 C14 C15 C16 -174.2(5) . . . . ? C20 N4 C16 C17 -6.8(8) . . . . ? Pd N4 C16 C17 152.0(5) . . . . ? C20 N4 C16 C15 -179.5(5) . . . . ? Pd N4 C16 C15 -20.8(6) . . . . ? N3 C15 C16 N4 24.1(7) . . . . ? C14 C15 C16 N4 -152.5(5) . . . . ? N3 C15 C16 C17 -148.2(6) . . . . ? C14 C15 C16 C17 35.2(9) . . . . ? C26 O4 C17 C16 -125.5(6) . . . . ? C26 O4 C17 C18 62.0(8) . . . . ? N4 C16 C17 O4 -162.8(5) . . . . ? C15 C16 C17 O4 9.2(9) . . . . ? N4 C16 C17 C18 9.9(9) . . . . ? C15 C16 C17 C18 -178.1(6) . . . . ? O4 C17 C18 C19 167.9(6) . . . . ? C16 C17 C18 C19 -4.4(9) . . . . ? C17 C18 C19 C20 -4.1(10) . . . . ? C16 N4 C20 C19 -2.0(9) . . . . ? Pd N4 C20 C19 -157.6(5) . . . . ? C18 C19 C20 N4 7.5(10) . . . . ? C4 O1 C21 C22 90.3(7) . . . . ? O1 C21 C22 C23 32.9(9) . . . . ? C7 O2 C23 C22 131.5(6) . . . . ? C21 C22 C23 O2 -73.8(7) . . . . ? C14 O3 C24 C25 101.3(8) . . . . ? O3 C24 C25 C26 21.1(10) . . . . ? C17 O4 C26 C25 135.6(6) . . . . ? C24 C25 C26 O4 -67.1(9) . . . . ? _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 26.42 _diffrn_measured_fraction_theta_full 0.947 _refine_diff_density_max 0.425 _refine_diff_density_min -0.494 _refine_diff_density_rms 0.076 #===END data_5 _database_code_depnum_ccdc_archive 'CCDC 667854' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 3,3-(butylenedioxy)-2,2-bipyridine methanol solvate ; _chemical_name_common '3,3-(butylenedioxy)-2,2-bipyridine methanol solvate' _chemical_melting_point ? _chemical_formula_moiety 'C14 H14 N2 O2, C H4 O' _chemical_formula_sum 'C15 H18 N2 O3' _chemical_formula_weight 274.31 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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P bcn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y, z-1/2' _cell_length_a 10.780(3) _cell_length_b 14.567(4) _cell_length_c 8.764(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1376.2(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour yellow _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.324 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 584 _exptl_absorpt_coefficient_mu 0.093 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mok\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'image plate dip1030' _diffrn_measurement_method 'laser scanner' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16043 _diffrn_reflns_av_R_equivalents 0.0561 _diffrn_reflns_av_sigmaI/netI 0.0301 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.80 _diffrn_reflns_theta_max 29.62 _reflns_number_total 1901 _reflns_number_gt 1410 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Xpress' _computing_cell_refinement 'Denzo (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELX97 (Sheldrick, 1998)' _computing_structure_refinement 'SHELX97 (Sheldrick, 1998)' _computing_molecular_graphics 'Ortep3/windows (Farrugia,1997)' _computing_publication_material 'Wingx 1.70.00 (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0970P)^2^+0.0035P] 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 1901 _refine_ls_number_parameters 96 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0570 _refine_ls_R_factor_gt 0.0455 _refine_ls_wR_factor_ref 0.1592 _refine_ls_wR_factor_gt 0.1511 _refine_ls_goodness_of_fit_ref 1.123 _refine_ls_restrained_S_all 1.271 _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 O1 O 0.11169(9) 0.06171(6) 0.68293(10) 0.0670(3) Uani 1 1 d . . . N1 N 0.08954(11) 0.28159(7) 0.86877(13) 0.0714(3) Uani 1 1 d . . . C1 C 0.19969(15) 0.28573(11) 0.93910(16) 0.0806(4) Uani 1 1 d . . . H1 H 0.2190 0.3381 0.9948 0.097 Uiso 1 1 calc R . . C2 C 0.28522(14) 0.21618(12) 0.93260(17) 0.0850(5) Uani 1 1 d . . . H2 H 0.3602 0.2212 0.9844 0.102 Uiso 1 1 calc R . . C3 C 0.25890(13) 0.13887(11) 0.84865(16) 0.0764(4) Uani 1 1 d . . . H3 H 0.3162 0.0913 0.8417 0.092 Uiso 1 1 calc R . . C4 C 0.14513(11) 0.13282(8) 0.77426(13) 0.0618(3) Uani 1 1 d . . . C5 C 0.06190(11) 0.20600(8) 0.78889(12) 0.0605(3) Uani 1 1 d . . . C6 C 0.15460(15) -0.02855(10) 0.72647(18) 0.0793(4) Uani 1 1 d . . . H6A H 0.1751 -0.0291 0.8342 0.095 Uiso 1 1 calc R . . H6B H 0.2288 -0.0440 0.6693 0.095 Uiso 1 1 calc R . . C7 C 0.05513(17) -0.09787(10) 0.69470(16) 0.0827(4) Uani 1 1 d . . . H7A H 0.0925 -0.1585 0.6960 0.099 Uiso 1 1 calc R . . H7B H 0.0238 -0.0873 0.5924 0.099 Uiso 1 1 calc R . . O2 O -0.0036(4) 0.4646(3) 0.9204(7) 0.1689(18) Uani 0.50 1 d PU . . C8 C 0.0000 0.4735(3) 0.7500 0.190(2) Uani 1 2 d SU . . 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 O1 0.0679(5) 0.0732(5) 0.0599(5) -0.0014(4) -0.0037(3) 0.0082(4) N1 0.0727(7) 0.0714(6) 0.0702(6) -0.0013(5) -0.0046(5) -0.0101(5) C1 0.0824(9) 0.0855(9) 0.0739(8) 0.0004(7) -0.0128(6) -0.0223(7) C2 0.0682(8) 0.1065(11) 0.0803(8) 0.0090(8) -0.0167(6) -0.0186(7) C3 0.0570(7) 0.0951(9) 0.0771(8) 0.0100(7) -0.0062(5) 0.0007(6) C4 0.0571(6) 0.0729(7) 0.0555(5) 0.0048(5) -0.0004(4) -0.0017(5) C5 0.0578(6) 0.0670(6) 0.0566(6) 0.0027(5) -0.0013(4) -0.0040(4) C6 0.0804(9) 0.0765(8) 0.0810(8) -0.0031(7) -0.0045(7) 0.0154(7) C7 0.1049(12) 0.0723(7) 0.0710(7) -0.0038(6) -0.0066(7) 0.0069(7) O2 0.150(3) 0.0972(19) 0.259(5) -0.012(3) 0.041(4) -0.0031(19) C8 0.136(3) 0.085(2) 0.350(8) 0.000 0.010(5) 0.000 _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 O1 C4 1.3578(15) . ? O1 C6 1.4450(17) . ? N1 C5 1.3384(17) . ? N1 C1 1.3392(18) . ? C1 C2 1.371(3) . ? C2 C3 1.375(2) . ? C3 C4 1.3918(18) . ? C4 C5 1.3991(17) . ? C5 C5 1.499(2) 4_556 ? C6 C7 1.499(2) . ? C7 C7 1.534(3) 4_556 ? O2 C8 1.500(7) . ? O2 O2 1.736(11) 5_567 ? C8 O2 1.500(7) 4_556 ? 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 C4 O1 C6 116.97(10) . . ? C5 N1 C1 118.37(12) . . ? N1 C1 C2 122.94(13) . . ? C1 C2 C3 119.26(13) . . ? C2 C3 C4 118.97(14) . . ? O1 C4 C3 123.94(12) . . ? O1 C4 C5 117.71(10) . . ? C3 C4 C5 118.29(12) . . ? N1 C5 C4 122.14(11) . . ? N1 C5 C5 115.86(8) . 4_556 ? C4 C5 C5 121.96(8) . 4_556 ? O1 C6 C7 109.57(12) . . ? C6 C7 C7 115.91(11) . 4_556 ? C8 O2 O2 138.4(5) . 5_567 ? O2 C8 O2 170.1(5) 4_556 . ? 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 C5 N1 C1 C2 0.1(2) . . . . ? N1 C1 C2 C3 1.0(2) . . . . ? C1 C2 C3 C4 -0.9(2) . . . . ? C6 O1 C4 C3 35.57(17) . . . . ? C6 O1 C4 C5 -147.21(12) . . . . ? C2 C3 C4 O1 176.93(12) . . . . ? C2 C3 C4 C5 -0.27(19) . . . . ? C1 N1 C5 C4 -1.41(18) . . . . ? C1 N1 C5 C5 -179.20(12) . . . 4_556 ? O1 C4 C5 N1 -175.89(10) . . . . ? C3 C4 C5 N1 1.49(18) . . . . ? O1 C4 C5 C5 1.77(18) . . . 4_556 ? C3 C4 C5 C5 179.14(12) . . . 4_556 ? C4 O1 C6 C7 141.96(12) . . . . ? O1 C6 C7 C7 -74.43(17) . . . 4_556 ? O2 O2 C8 O2 174.4(7) 5_567 . . 4_556 ? N1 C5 C5 N1 47.8(2) . . 4_556 4_556 ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 29.62 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.174 _refine_diff_density_min -0.130 _refine_diff_density_rms 0.025 #===END data_5c _database_code_depnum_ccdc_archive 'CCDC 667855' _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis(3,3-(butylenedioxy)-2,2-bipyridine)-palladium(II) bis(hexafluorophosphate) ; _chemical_name_common ;bis(3,3-(butylenedioxy)-2,2-bipyridine)-palladium(ii) bis(hexafluorophosphate) ; _chemical_melting_point ? _chemical_formula_moiety 'C28 H28 N4 O4 Pd 2+, 2(P F6 1-)' _chemical_formula_sum 'C28 H28 F12 N4 O4 P2 Pd' _chemical_formula_weight 880.88 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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.430(3) _cell_length_b 13.511(3) _cell_length_c 18.203(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.69(3) _cell_angle_gamma 90.00 _cell_volume 3301.5(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour yellow _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.772 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1760 _exptl_absorpt_coefficient_mu 0.769 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.4088 _exptl_absorpt_correction_T_max 0.9520 _exptl_absorpt_process_details ; Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56 Cubic fit to sin(theta)/lambda - 24 parameters ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mok\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'image plate dip1030' _diffrn_measurement_method 'laser scanner' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34816 _diffrn_reflns_av_R_equivalents 0.0741 _diffrn_reflns_av_sigmaI/netI 0.0918 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 26.37 _reflns_number_total 6587 _reflns_number_gt 3590 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Xpress' _computing_cell_refinement 'Mosflm (Acta Cryst. D50, 760, 1994)' _computing_data_reduction 'Scala (Acta Cryst. D50, 760, 1994)' _computing_structure_solution 'SHELX97 (Sheldrick, 1998)' _computing_structure_refinement 'SHELX97 (Sheldrick, 1998)' _computing_molecular_graphics 'Ortep3/windows (Farrugia,1997)' _computing_publication_material 'Wingx 1.70.00 (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0666P)^2^] 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 6587 _refine_ls_number_parameters 460 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1188 _refine_ls_R_factor_gt 0.0581 _refine_ls_wR_factor_ref 0.1582 _refine_ls_wR_factor_gt 0.1260 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd 0.14991(4) 0.13982(3) 0.60973(2) 0.05337(17) Uani 1 1 d . . . N1 N 0.2109(4) 0.1102(3) 0.5118(3) 0.0528(12) Uani 1 1 d . . . N2 N 0.1601(3) 0.2807(4) 0.5695(3) 0.0517(12) Uani 1 1 d . . . N3 N 0.1345(4) 0.1591(4) 0.7200(3) 0.0591(13) Uani 1 1 d . . . N4 N 0.0986(4) 0.0043(3) 0.6366(3) 0.0559(12) Uani 1 1 d . . . O1 O 0.3353(3) 0.2712(3) 0.3867(2) 0.0606(11) Uani 1 1 d . . . O2 O 0.1661(3) 0.3556(3) 0.3802(2) 0.0645(11) Uani 1 1 d . . . O3 O 0.1433(3) -0.0313(3) 0.8588(2) 0.0680(12) Uani 1 1 d . . . O4 O -0.0203(3) -0.0837(3) 0.7982(2) 0.0642(11) Uani 1 1 d . . . C1 C 0.2541(5) 0.0243(5) 0.4963(3) 0.0628(16) Uani 1 1 d . . . H1 H 0.2412 -0.0303 0.5256 0.075 Uiso 1 1 calc R . . C2 C 0.3167(5) 0.0129(5) 0.4387(4) 0.0684(18) Uani 1 1 d . . . H2 H 0.3419 -0.0491 0.4272 0.082 Uiso 1 1 calc R . . C3 C 0.3415(5) 0.0946(5) 0.3986(4) 0.0672(17) Uani 1 1 d . . . H3 H 0.3843 0.0886 0.3596 0.081 Uiso 1 1 calc R . . C4 C 0.3028(5) 0.1856(5) 0.4162(3) 0.0549(15) Uani 1 1 d . . . C5 C 0.2321(5) 0.1918(4) 0.4704(3) 0.0541(14) Uani 1 1 d . . . C6 C 0.1838(4) 0.2824(4) 0.4975(3) 0.0544(15) Uani 1 1 d . . . C7 C 0.1590(4) 0.3641(4) 0.4540(3) 0.0557(14) Uani 1 1 d . . . C8 C 0.1245(5) 0.4502(5) 0.4873(4) 0.0637(16) Uani 1 1 d . . . H8 H 0.1126 0.5074 0.4600 0.076 Uiso 1 1 calc R . . C9 C 0.1086(5) 0.4482(5) 0.5620(4) 0.0677(18) Uani 1 1 d . . . H9 H 0.0898 0.5055 0.5863 0.081 Uiso 1 1 calc R . . C10 C 0.1208(5) 0.3610(5) 0.6000(4) 0.0603(15) Uani 1 1 d . . . H10 H 0.1011 0.3578 0.6485 0.072 Uiso 1 1 calc R . . C11 C 0.1734(5) 0.2356(5) 0.7583(4) 0.0693(18) Uani 1 1 d . . . H11 H 0.1897 0.2933 0.7335 0.083 Uiso 1 1 calc R . . C12 C 0.1896(6) 0.2311(6) 0.8322(4) 0.082(2) Uani 1 1 d . . . H12 H 0.2088 0.2878 0.8579 0.098 Uiso 1 1 calc R . . C13 C 0.1779(6) 0.1434(6) 0.8697(4) 0.077(2) Uani 1 1 d . . . H13 H 0.1921 0.1394 0.9199 0.093 Uiso 1 1 calc R . . C14 C 0.1444(5) 0.0611(5) 0.8302(3) 0.0598(16) Uani 1 1 d . . . C15 C 0.1172(4) 0.0720(4) 0.7563(3) 0.0555(15) Uani 1 1 d . . . C16 C 0.0754(4) -0.0070(4) 0.7081(3) 0.0545(14) Uani 1 1 d . . . C17 C 0.0149(5) -0.0851(5) 0.7297(4) 0.0631(16) Uani 1 1 d . . . C18 C -0.0129(5) -0.1566(5) 0.6774(4) 0.0686(18) Uani 1 1 d . . . H18 H -0.0499 -0.2115 0.6909 0.082 Uiso 1 1 calc R . . C19 C 0.0147(5) -0.1450(5) 0.6067(4) 0.0712(18) Uani 1 1 d . . . H19 H -0.0014 -0.1933 0.5720 0.085 Uiso 1 1 calc R . . C20 C 0.0666(5) -0.0617(4) 0.5861(3) 0.0627(16) Uani 1 1 d . . . H20 H 0.0794 -0.0513 0.5368 0.075 Uiso 1 1 calc R . . C21 C 0.3583(6) 0.2698(5) 0.3087(4) 0.0752(19) Uani 1 1 d . . . H21A H 0.3124 0.2264 0.2821 0.090 Uiso 1 1 calc R . . H21B H 0.4255 0.2454 0.3024 0.090 Uiso 1 1 calc R . . C22 C 0.3491(6) 0.3733(5) 0.2798(4) 0.080(2) Uani 1 1 d . . . H22A H 0.3803 0.3760 0.2325 0.096 Uiso 1 1 calc R . . H22B H 0.3862 0.4169 0.3129 0.096 Uiso 1 1 calc R . . C23 C 0.2451(6) 0.4128(6) 0.2706(4) 0.082(2) Uani 1 1 d . . . H23A H 0.2048 0.3625 0.2459 0.099 Uiso 1 1 calc R . . H23B H 0.2471 0.4695 0.2381 0.099 Uiso 1 1 calc R . . C24 C 0.1923(6) 0.4437(5) 0.3392(4) 0.076(2) Uani 1 1 d . . . H24A H 0.2355 0.4859 0.3692 0.091 Uiso 1 1 calc R . . H24B H 0.1326 0.4808 0.3258 0.091 Uiso 1 1 calc R . . C25 C 0.1092(6) -0.0414(6) 0.9336(4) 0.081(2) Uani 1 1 d . . . H25A H 0.0558 0.0053 0.9418 0.097 Uiso 1 1 calc R . . H25B H 0.1635 -0.0267 0.9682 0.097 Uiso 1 1 calc R . . C26 C 0.0730(6) -0.1443(6) 0.9456(4) 0.087(2) Uani 1 1 d . . . H26A H 0.0735 -0.1571 0.9980 0.105 Uiso 1 1 calc R . . H26B H 0.1194 -0.1900 0.9239 0.105 Uiso 1 1 calc R . . C27 C -0.0309(6) -0.1657(6) 0.9139(4) 0.087(2) Uani 1 1 d . . . H27A H -0.0555 -0.2253 0.9369 0.104 Uiso 1 1 calc R . . H27B H -0.0744 -0.1118 0.9273 0.104 Uiso 1 1 calc R . . C28 C -0.0382(6) -0.1789(5) 0.8321(4) 0.079(2) Uani 1 1 d . . . H28A H 0.0108 -0.2267 0.8165 0.095 Uiso 1 1 calc R . . H28B H -0.1039 -0.2031 0.8175 0.095 Uiso 1 1 calc R . . P1 P 0.33608(14) 0.24253(14) 0.06597(10) 0.0678(5) Uani 1 1 d . . . F1 F 0.2813(3) 0.2927(3) -0.0025(2) 0.0871(13) Uani 1 1 d . . . F2 F 0.2586(3) 0.2907(3) 0.1188(2) 0.0949(13) Uani 1 1 d . . . F3 F 0.4060(4) 0.3379(3) 0.0754(2) 0.0975(14) Uani 1 1 d . . . F4 F 0.4147(3) 0.1944(3) 0.0130(2) 0.0960(13) Uani 1 1 d . . . F5 F 0.3913(4) 0.1905(4) 0.1338(3) 0.1095(16) Uani 1 1 d . . . F6 F 0.2663(3) 0.1473(3) 0.0555(3) 0.0897(12) Uani 1 1 d . . . P2 P 0.08104(14) 0.53183(15) 0.79604(12) 0.0748(5) Uani 1 1 d . . . F7 F 0.0697(7) 0.5869(6) 0.7217(4) 0.186(3) Uani 1 1 d . . . F8 F 0.1810(4) 0.4843(4) 0.7730(5) 0.177(3) Uani 1 1 d . . . F9 F -0.0205(3) 0.5770(4) 0.8201(3) 0.1176(18) Uani 1 1 d . . . F10 F 0.0902(6) 0.4747(5) 0.8698(3) 0.170(3) Uani 1 1 d . . . F11 F 0.0234(4) 0.4400(3) 0.7631(3) 0.1139(16) Uani 1 1 d . . . F12 F 0.1390(4) 0.6242(4) 0.8279(4) 0.137(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 Pd 0.0614(3) 0.0440(3) 0.0550(3) -0.0021(2) 0.0078(2) -0.0010(2) N1 0.062(3) 0.044(3) 0.052(3) -0.003(2) 0.002(2) 0.005(2) N2 0.053(3) 0.049(3) 0.054(3) -0.004(2) 0.001(2) -0.001(2) N3 0.067(3) 0.051(3) 0.059(3) -0.006(2) 0.006(3) 0.003(2) N4 0.065(3) 0.047(3) 0.056(3) -0.003(2) 0.013(2) 0.001(2) O1 0.068(3) 0.059(3) 0.055(2) -0.002(2) 0.009(2) -0.008(2) O2 0.078(3) 0.058(3) 0.057(2) 0.003(2) -0.005(2) -0.003(2) O3 0.072(3) 0.067(3) 0.065(3) 0.011(2) 0.004(2) 0.007(2) O4 0.069(3) 0.053(3) 0.071(3) 0.007(2) 0.015(2) 0.002(2) C1 0.071(4) 0.048(4) 0.070(4) 0.006(3) 0.018(3) 0.000(3) C2 0.078(5) 0.053(4) 0.075(4) -0.006(3) 0.014(4) 0.012(3) C3 0.075(4) 0.059(4) 0.069(4) -0.008(3) 0.018(4) 0.005(4) C4 0.063(4) 0.052(4) 0.050(3) -0.002(3) 0.000(3) -0.005(3) C5 0.061(4) 0.043(3) 0.059(3) -0.006(3) 0.003(3) 0.003(3) C6 0.055(4) 0.042(3) 0.066(4) -0.006(3) 0.005(3) -0.003(3) C7 0.053(3) 0.048(3) 0.067(4) 0.003(3) 0.001(3) -0.005(3) C8 0.066(4) 0.048(4) 0.077(4) 0.000(3) 0.005(3) 0.000(3) C9 0.070(4) 0.041(4) 0.093(5) -0.012(3) 0.018(4) 0.005(3) C10 0.063(4) 0.048(3) 0.070(4) -0.002(3) 0.005(3) 0.002(3) C11 0.086(5) 0.050(4) 0.072(4) -0.009(3) 0.004(4) -0.006(3) C12 0.114(6) 0.070(5) 0.061(4) -0.012(4) -0.005(4) -0.012(4) C13 0.090(5) 0.084(5) 0.057(4) -0.007(4) 0.000(4) 0.007(4) C14 0.065(4) 0.062(4) 0.054(3) -0.005(3) 0.009(3) 0.003(3) C15 0.055(3) 0.051(4) 0.061(4) -0.006(3) 0.010(3) -0.002(3) C16 0.051(3) 0.051(4) 0.062(4) -0.001(3) 0.008(3) 0.004(3) C17 0.070(4) 0.048(4) 0.072(4) 0.001(3) 0.013(3) 0.003(3) C18 0.072(4) 0.054(4) 0.080(5) -0.002(3) 0.013(4) -0.013(3) C19 0.084(5) 0.058(4) 0.071(4) -0.009(3) -0.001(4) -0.013(4) C20 0.077(4) 0.052(4) 0.060(4) -0.011(3) 0.006(3) 0.000(3) C21 0.090(5) 0.073(5) 0.064(4) 0.007(4) 0.011(4) -0.012(4) C22 0.097(6) 0.074(5) 0.069(4) 0.005(4) 0.015(4) -0.019(4) C23 0.101(6) 0.082(5) 0.065(4) 0.008(4) 0.005(4) -0.011(5) C24 0.103(6) 0.053(4) 0.072(4) 0.014(3) 0.004(4) -0.005(4) C25 0.070(5) 0.111(6) 0.061(4) 0.013(4) 0.000(4) 0.004(4) C26 0.087(5) 0.091(6) 0.084(5) 0.033(4) 0.006(4) 0.001(5) C27 0.085(5) 0.085(6) 0.091(5) 0.025(4) 0.022(4) -0.007(4) C28 0.090(5) 0.069(5) 0.079(5) 0.013(4) 0.014(4) -0.011(4) P1 0.0749(12) 0.0596(11) 0.0692(11) 0.0076(9) 0.0085(9) 0.0022(9) F1 0.110(3) 0.065(3) 0.085(3) 0.006(2) -0.025(2) 0.002(2) F2 0.106(3) 0.086(3) 0.095(3) -0.012(2) 0.030(3) 0.012(3) F3 0.107(3) 0.085(3) 0.100(3) -0.003(2) -0.005(3) -0.030(3) F4 0.095(3) 0.090(3) 0.105(3) 0.009(3) 0.031(3) 0.017(3) F5 0.112(4) 0.124(4) 0.092(3) 0.040(3) -0.008(3) 0.019(3) F6 0.093(3) 0.058(2) 0.119(3) 0.007(2) 0.017(2) -0.008(2) P2 0.0643(11) 0.0672(12) 0.0934(14) -0.0100(10) 0.0114(10) -0.0057(9) F7 0.290(10) 0.151(6) 0.118(5) 0.035(4) 0.024(5) -0.052(6) F8 0.085(4) 0.113(4) 0.337(10) -0.060(5) 0.082(5) -0.014(3) F9 0.079(3) 0.093(4) 0.182(5) -0.032(3) 0.035(3) 0.001(3) F10 0.223(8) 0.163(6) 0.121(4) 0.029(4) -0.050(5) 0.005(5) F11 0.109(4) 0.090(3) 0.143(4) -0.039(3) 0.012(3) -0.020(3) F12 0.085(3) 0.096(4) 0.229(7) -0.061(4) -0.004(4) -0.014(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 Pd N4 2.022(5) . ? Pd N1 2.023(5) . ? Pd N3 2.041(5) . ? Pd N2 2.046(5) . ? N1 C1 1.331(7) . ? N1 C5 1.371(7) . ? N2 C10 1.334(7) . ? N2 C6 1.359(7) . ? N3 C11 1.343(8) . ? N3 C15 1.373(8) . ? N4 C20 1.343(7) . ? N4 C16 1.356(7) . ? O1 C4 1.354(7) . ? O1 C21 1.462(7) . ? O2 C7 1.355(7) . ? O2 C24 1.455(7) . ? O3 C14 1.352(7) . ? O3 C25 1.456(8) . ? O4 C17 1.347(7) . ? O4 C28 1.450(8) . ? C1 C2 1.371(9) . ? C2 C3 1.370(9) . ? C3 C4 1.377(9) . ? C4 C5 1.392(8) . ? C5 C6 1.477(8) . ? C6 C7 1.393(8) . ? C7 C8 1.397(8) . ? C8 C9 1.382(9) . ? C9 C10 1.374(8) . ? C11 C12 1.358(9) . ? C12 C13 1.378(10) . ? C13 C14 1.391(9) . ? C14 C15 1.391(8) . ? C15 C16 1.482(8) . ? C16 C17 1.396(8) . ? C17 C18 1.398(9) . ? C18 C19 1.359(9) . ? C19 C20 1.380(9) . ? C21 C22 1.498(9) . ? C22 C23 1.499(10) . ? C23 C24 1.512(10) . ? C25 C26 1.491(10) . ? C26 C27 1.521(10) . ? C27 C28 1.501(10) . ? P1 F2 1.578(4) . ? P1 F1 1.581(4) . ? P1 F5 1.586(4) . ? P1 F4 1.590(5) . ? P1 F6 1.600(4) . ? P1 F3 1.601(4) . ? P2 F7 1.547(7) . ? P2 F10 1.551(6) . ? P2 F8 1.557(6) . ? P2 F9 1.568(5) . ? P2 F11 1.572(5) . ? P2 F12 1.573(5) . ? 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 N4 Pd N1 100.57(19) . . ? N4 Pd N3 80.4(2) . . ? N1 Pd N3 161.3(2) . . ? N4 Pd N2 163.03(19) . . ? N1 Pd N2 80.57(19) . . ? N3 Pd N2 104.04(19) . . ? C1 N1 C5 119.0(5) . . ? C1 N1 Pd 123.4(4) . . ? C5 N1 Pd 114.9(4) . . ? C10 N2 C6 119.6(5) . . ? C10 N2 Pd 125.2(4) . . ? C6 N2 Pd 112.4(4) . . ? C11 N3 C15 118.6(5) . . ? C11 N3 Pd 124.0(5) . . ? C15 N3 Pd 112.8(4) . . ? C20 N4 C16 120.3(5) . . ? C20 N4 Pd 122.7(4) . . ? C16 N4 Pd 115.1(4) . . ? C4 O1 C21 117.0(5) . . ? C7 O2 C24 117.7(5) . . ? C14 O3 C25 117.0(5) . . ? C17 O4 C28 116.6(5) . . ? N1 C1 C2 122.8(6) . . ? C3 C2 C1 118.8(6) . . ? C2 C3 C4 119.7(6) . . ? O1 C4 C3 122.8(6) . . ? O1 C4 C5 117.7(5) . . ? C3 C4 C5 119.3(6) . . ? N1 C5 C4 119.9(5) . . ? N1 C5 C6 112.5(5) . . ? C4 C5 C6 127.0(6) . . ? N2 C6 C7 120.2(5) . . ? N2 C6 C5 115.2(5) . . ? C7 C6 C5 124.6(6) . . ? O2 C7 C6 118.2(5) . . ? O2 C7 C8 122.4(6) . . ? C6 C7 C8 119.4(6) . . ? C9 C8 C7 118.2(6) . . ? C10 C9 C8 119.5(6) . . ? N2 C10 C9 122.0(6) . . ? N3 C11 C12 121.8(7) . . ? C11 C12 C13 120.8(7) . . ? C12 C13 C14 118.1(6) . . ? O3 C14 C15 117.7(5) . . ? O3 C14 C13 123.1(6) . . ? C15 C14 C13 119.1(6) . . ? N3 C15 C14 120.9(5) . . ? N3 C15 C16 113.6(5) . . ? C14 C15 C16 125.4(6) . . ? N4 C16 C17 120.5(6) . . ? N4 C16 C15 113.2(5) . . ? C17 C16 C15 126.3(6) . . ? O4 C17 C16 118.2(6) . . ? O4 C17 C18 123.1(6) . . ? C16 C17 C18 118.5(6) . . ? C19 C18 C17 119.3(6) . . ? C18 C19 C20 120.4(6) . . ? N4 C20 C19 120.6(6) . . ? O1 C21 C22 108.1(6) . . ? C21 C22 C23 116.0(6) . . ? C22 C23 C24 117.7(6) . . ? O2 C24 C23 108.9(6) . . ? O3 C25 C26 109.7(6) . . ? C25 C26 C27 114.9(6) . . ? C28 C27 C26 115.6(7) . . ? O4 C28 C27 108.1(6) . . ? F2 P1 F1 90.2(3) . . ? F2 P1 F5 90.6(3) . . ? F1 P1 F5 179.0(3) . . ? F2 P1 F4 179.6(3) . . ? F1 P1 F4 89.9(2) . . ? F5 P1 F4 89.3(3) . . ? F2 P1 F6 90.6(3) . . ? F1 P1 F6 89.6(2) . . ? F5 P1 F6 89.7(3) . . ? F4 P1 F6 89.7(3) . . ? F2 P1 F3 89.9(3) . . ? F1 P1 F3 89.8(2) . . ? F5 P1 F3 90.8(3) . . ? F4 P1 F3 89.8(3) . . ? F6 P1 F3 179.3(3) . . ? F7 P2 F10 178.5(4) . . ? F7 P2 F8 91.5(5) . . ? F10 P2 F8 88.9(4) . . ? F7 P2 F9 89.6(4) . . ? F10 P2 F9 90.0(4) . . ? F8 P2 F9 178.5(4) . . ? F7 P2 F11 90.6(4) . . ? F10 P2 F11 87.9(4) . . ? F8 P2 F11 89.4(3) . . ? F9 P2 F11 89.5(3) . . ? F7 P2 F12 88.6(4) . . ? F10 P2 F12 92.8(4) . . ? F8 P2 F12 90.3(3) . . ? F9 P2 F12 90.8(3) . . ? F11 P2 F12 179.2(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 N4 Pd N1 C1 -33.4(5) . . . . ? N3 Pd N1 C1 57.8(9) . . . . ? N2 Pd N1 C1 163.8(5) . . . . ? N4 Pd N1 C5 165.3(4) . . . . ? N3 Pd N1 C5 -103.5(7) . . . . ? N2 Pd N1 C5 2.5(4) . . . . ? N4 Pd N2 C10 76.1(8) . . . . ? N1 Pd N2 C10 171.4(5) . . . . ? N3 Pd N2 C10 -27.1(5) . . . . ? N4 Pd N2 C6 -84.9(8) . . . . ? N1 Pd N2 C6 10.5(4) . . . . ? N3 Pd N2 C6 172.0(4) . . . . ? N4 Pd N3 C11 166.6(6) . . . . ? N1 Pd N3 C11 72.1(8) . . . . ? N2 Pd N3 C11 -30.2(6) . . . . ? N4 Pd N3 C15 11.1(4) . . . . ? N1 Pd N3 C15 -83.4(7) . . . . ? N2 Pd N3 C15 174.4(4) . . . . ? N1 Pd N4 C20 -31.7(5) . . . . ? N3 Pd N4 C20 167.3(5) . . . . ? N2 Pd N4 C20 60.7(9) . . . . ? N1 Pd N4 C16 164.0(4) . . . . ? N3 Pd N4 C16 3.0(4) . . . . ? N2 Pd N4 C16 -103.6(7) . . . . ? C5 N1 C1 C2 -2.2(9) . . . . ? Pd N1 C1 C2 -162.8(5) . . . . ? N1 C1 C2 C3 4.7(10) . . . . ? C1 C2 C3 C4 -0.5(10) . . . . ? C21 O1 C4 C3 39.6(8) . . . . ? C21 O1 C4 C5 -145.0(6) . . . . ? C2 C3 C4 O1 169.7(6) . . . . ? C2 C3 C4 C5 -5.7(9) . . . . ? C1 N1 C5 C4 -4.2(8) . . . . ? Pd N1 C5 C4 157.9(4) . . . . ? C1 N1 C5 C6 -176.2(5) . . . . ? Pd N1 C5 C6 -14.0(6) . . . . ? O1 C4 C5 N1 -167.4(5) . . . . ? C3 C4 C5 N1 8.1(8) . . . . ? O1 C4 C5 C6 3.3(9) . . . . ? C3 C4 C5 C6 178.8(6) . . . . ? C10 N2 C6 C7 -5.8(8) . . . . ? Pd N2 C6 C7 156.3(4) . . . . ? C10 N2 C6 C5 176.6(5) . . . . ? Pd N2 C6 C5 -21.2(6) . . . . ? N1 C5 C6 N2 23.6(7) . . . . ? C4 C5 C6 N2 -147.7(6) . . . . ? N1 C5 C6 C7 -153.9(6) . . . . ? C4 C5 C6 C7 34.9(9) . . . . ? C24 O2 C7 C6 -148.3(6) . . . . ? C24 O2 C7 C8 34.0(8) . . . . ? N2 C6 C7 O2 -167.4(5) . . . . ? C5 C6 C7 O2 9.8(9) . . . . ? N2 C6 C7 C8 10.3(9) . . . . ? C5 C6 C7 C8 -172.4(6) . . . . ? O2 C7 C8 C9 172.5(6) . . . . ? C6 C7 C8 C9 -5.2(9) . . . . ? C7 C8 C9 C10 -4.1(10) . . . . ? C6 N2 C10 C9 -3.9(9) . . . . ? Pd N2 C10 C9 -163.6(5) . . . . ? C8 C9 C10 N2 8.9(10) . . . . ? C15 N3 C11 C12 -4.5(10) . . . . ? Pd N3 C11 C12 -158.6(6) . . . . ? N3 C11 C12 C13 7.9(12) . . . . ? C11 C12 C13 C14 -3.1(12) . . . . ? C25 O3 C14 C15 -142.1(6) . . . . ? C25 O3 C14 C13 42.6(9) . . . . ? C12 C13 C14 O3 170.6(6) . . . . ? C12 C13 C14 C15 -4.6(10) . . . . ? C11 N3 C15 C14 -3.5(9) . . . . ? Pd N3 C15 C14 153.4(5) . . . . ? C11 N3 C15 C16 -179.3(6) . . . . ? Pd N3 C15 C16 -22.4(6) . . . . ? O3 C14 C15 N3 -167.4(5) . . . . ? C13 C14 C15 N3 8.1(9) . . . . ? O3 C14 C15 C16 7.8(9) . . . . ? C13 C14 C15 C16 -176.7(6) . . . . ? C20 N4 C16 C17 -2.5(9) . . . . ? Pd N4 C16 C17 162.3(5) . . . . ? C20 N4 C16 C15 179.7(5) . . . . ? Pd N4 C16 C15 -15.6(6) . . . . ? N3 C15 C16 N4 25.2(7) . . . . ? C14 C15 C16 N4 -150.3(6) . . . . ? N3 C15 C16 C17 -152.5(6) . . . . ? C14 C15 C16 C17 32.0(10) . . . . ? C28 O4 C17 C16 -150.2(6) . . . . ? C28 O4 C17 C18 35.2(9) . . . . ? N4 C16 C17 O4 -168.5(5) . . . . ? C15 C16 C17 O4 9.0(9) . . . . ? N4 C16 C17 C18 6.3(9) . . . . ? C15 C16 C17 C18 -176.2(6) . . . . ? O4 C17 C18 C19 170.7(6) . . . . ? C16 C17 C18 C19 -3.9(10) . . . . ? C17 C18 C19 C20 -2.3(11) . . . . ? C16 N4 C20 C19 -3.9(9) . . . . ? Pd N4 C20 C19 -167.4(5) . . . . ? C18 C19 C20 N4 6.3(11) . . . . ? C4 O1 C21 C22 155.7(6) . . . . ? O1 C21 C22 C23 -72.6(8) . . . . ? C21 C22 C23 C24 75.5(9) . . . . ? C7 O2 C24 C23 152.1(6) . . . . ? C22 C23 C24 O2 -71.9(8) . . . . ? C14 O3 C25 C26 156.8(6) . . . . ? O3 C25 C26 C27 -78.6(8) . . . . ? C25 C26 C27 C28 75.6(9) . . . . ? C17 O4 C28 C27 154.5(6) . . . . ? C26 C27 C28 O4 -69.3(8) . . . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.667 _refine_diff_density_min -0.605 _refine_diff_density_rms 0.139 #===END