Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_General _audit_creation_date 'Mon Jul 9 12:50:46 2001' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ _journal_coden_Cambridge 186 #------------------------------------------------------------------------------ # SUBMISSION DETAILS _publ_contact_author_name 'Prof Makoto Fujita' _publ_contact_author_address ; Department of Applied Chemistry, School of Engineering, Nagoya University, CREST, Japan Science and Technology Corporation (JST), Chikusa-ku, Nagoya 464-8603, Japan ; _publ_contact_author_email 'MFUJITA@APCHEM.NAGOYA-U.AC.JP' _publ_requested_journal ' Dalton Transactions' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? #------------------------------------------------------------------------------ # TITLE AND AUTHOR LIST loop_ _publ_author_name 'Fujita, Makoto' 'Yamaguchi, Kentaro' 'Yu, Shu-Yan' _publ_section_title ; A dimer-to-dimer metal-metal linear aggregate from a (u-1,3-NO3)2 double-bridged cis-(2,2'-bipyridine)palladium(II) cofacial dimer ; #------------------------------------------------------------------------------ # TEXT _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (1999). teXsan. Single Crystal Structure Analysis Software. Version 1.10. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. Zachariasen, W. H. (1967). Acta Cryst. 23, 558-564. ; #------------------------------------------------------------------------------ data_Dimer_2 _database_code_CSD 170480 #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C24 H26 F6 N9 O11 P Pd2 ' _chemical_formula_moiety '?' _chemical_formula_weight 974.29 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 13.18(1) _cell_length_b 13.64(1) _cell_length_c 11.68(1) _cell_angle_alpha 113.32(6) _cell_angle_beta 97.29(4) _cell_angle_gamma 69.43(3) _cell_volume 1805(3) _cell_formula_units_Z 2 _cell_measurement_reflns_used 3 _cell_measurement_theta_min ? _cell_measurement_theta_max 14.0 _cell_measurement_temperature 110.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'prism' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.150 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.792 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 1.137 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-II Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 0.010000 _diffrn_reflns_number 5388 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_theta_max 26.33 _diffrn_measured_fraction_theta_max 0.7413 _diffrn_reflns_theta_full 26.33 _diffrn_measured_fraction_theta_full 0.7413 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 3.5 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 4.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 5388 _reflns_number_gt 4415 _reflns_threshold_expression F^2^>4.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0717 _refine_ls_wR_factor_ref 0.0919 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 4415 _refine_ls_number_parameters 479 _refine_ls_goodness_of_fit_ref 2.880 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00051|Fo|^2^]' _refine_ls_shift/su_max 2.5443 _refine_diff_density_max 1.30 _refine_diff_density_min -1.29 _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.017(2) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Pd' 'Pd' -0.999 1.007 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'P' 'P' 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'F' 'F' 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd(1) Pd 0.12507(5) 0.46721(6) 0.48802(6) 0.0436(2) Uani 1.00 d . . . Pd(2) Pd 0.35539(6) 0.40141(6) 0.48602(7) 0.0495(2) Uani 1.00 d . . . P(1) P -0.1261(3) 0.8583(2) 0.0690(3) 0.0614(8) Uani 1.00 d . . . F(1) F -0.0957(6) 0.9449(5) 0.0304(6) 0.081(2) Uani 1.00 d . . . F(2) F -0.1543(6) 0.7694(5) 0.1061(6) 0.079(2) Uani 1.00 d . . . F(3) F -0.0320(5) 0.7541(5) -0.0246(6) 0.072(2) Uani 1.00 d . . . F(4) F -0.2173(7) 0.9606(6) 0.1621(7) 0.091(3) Uani 1.00 d . . . F(5) F -0.0425(6) 0.8691(5) 0.1810(6) 0.080(2) Uani 1.00 d . . . F(6) F -0.2089(7) 0.8427(6) -0.0435(7) 0.091(3) Uani 1.00 d . . . O(1) O 0.3427(6) 0.2476(6) 0.4035(8) 0.069(2) Uani 1.00 d . . . O(2) O 0.1558(5) 0.3012(5) 0.3801(6) 0.048(2) Uani 1.00 d . . . O(3) O 0.2550(10) 0.1025(8) 0.2938(10) 0.110(4) Uani 1.00 d . . . O(4) O 0.3304(7) 0.3992(7) 0.6518(8) 0.078(3) Uani 1.00 d . . . O(5) O 0.1442(5) 0.4313(5) 0.6410(6) 0.051(2) Uani 1.00 d . . . O(6) O 0.235(1) 0.3936(10) 0.8181(10) 0.116(4) Uani 1.00 d . . . O(7) O 0.5101(9) 0.299(1) -0.196(1) 0.129(5) Uani 1.00 d . . . O(8) O 0.561(1) 0.154(1) -0.350(2) 0.198(8) Uani 1.00 d . . . O(9) O 0.531(1) 0.059(1) 0.397(3) 0.26(1) Uani 1.00 d . . . O(10) O 0.515(2) -0.152(1) 0.210(2) 0.190(7) Uani 1.00 d . . . O(11) O 0.534(2) 0.030(2) 0.108(7) 0.60(4) Uani 1.00 d . . . N(1) N 0.2509(8) 0.2264(8) 0.3649(9) 0.064(3) Uani 1.00 d . . . N(2) N 0.2374(9) 0.4086(8) 0.6950(9) 0.071(3) Uani 1.00 d . . . N(3) N 0.3833(7) 0.4097(8) 0.3232(9) 0.058(3) Uani 1.00 d . . . N(4) N 0.3602(6) 0.5611(7) 0.5540(8) 0.052(2) Uani 1.00 d . . . N(5) N 0.1040(6) 0.5151(6) 0.3454(8) 0.045(2) Uani 1.00 d . . . N(6) N 0.0868(6) 0.6354(6) 0.5832(7) 0.044(2) Uani 1.00 d . . . N(7) N 0.8427(9) 0.0572(10) 0.556(1) 0.079(4) Uani 1.00 d . . . N(8) N 0.720(1) 0.358(1) 0.048(1) 0.093(4) Uani 1.00 d . . . N(9) N 0.4850(9) -0.197(1) 0.258(1) 0.092(5) Uani 1.00 d . . . C(1) C 0.3860(8) 0.5118(9) 0.337(1) 0.057(3) Uani 1.00 d . . . C(2) C 0.4009(9) 0.530(1) 0.227(1) 0.072(4) Uani 1.00 d . . . C(3) C 0.4177(10) 0.444(1) 0.114(1) 0.084(5) Uani 1.00 d . . . C(4) C 0.4141(9) 0.340(1) 0.105(1) 0.073(4) Uani 1.00 d . . . C(5) C 0.3983(9) 0.324(1) 0.208(1) 0.067(4) Uani 1.00 d . . . C(6) C 0.3724(8) 0.5987(10) 0.461(1) 0.062(3) Uani 1.00 d . . . C(7) C 0.3699(9) 0.7072(9) 0.495(1) 0.063(4) Uani 1.00 d . . . C(8) C 0.3514(9) 0.781(1) 0.618(2) 0.077(4) Uani 1.00 d . . . C(9) C 0.3406(9) 0.7466(8) 0.711(1) 0.062(3) Uani 1.00 d . . . C(10) C 0.3472(9) 0.6342(10) 0.673(1) 0.063(3) Uani 1.00 d . . . C(11) C 0.0872(7) 0.6262(8) 0.3756(9) 0.046(3) Uani 1.00 d . . . C(12) C 0.0794(8) 0.6718(9) 0.2830(9) 0.055(3) Uani 1.00 d . . . C(13) C 0.0880(9) 0.5987(9) 0.1591(10) 0.058(3) Uani 1.00 d . . . C(14) C 0.1044(9) 0.4856(9) 0.1283(10) 0.059(3) Uani 1.00 d . . . C(15) C 0.1133(8) 0.4441(9) 0.2216(9) 0.055(3) Uani 1.00 d . . . C(16) C 0.0755(8) 0.6957(9) 0.5108(10) 0.055(3) Uani 1.00 d . . . C(17) C 0.0570(8) 0.8105(8) 0.5642(10) 0.053(3) Uani 1.00 d . . . C(18) C 0.0442(8) 0.8649(8) 0.6935(10) 0.054(3) Uani 1.00 d . . . C(19) C 0.0536(8) 0.8040(9) 0.7613(10) 0.057(3) Uani 1.00 d . . . C(20) C 0.0751(8) 0.6882(8) 0.7065(9) 0.050(3) Uani 1.00 d . . . C(21) C 0.225(1) 0.108(1) 0.588(1) 0.096(5) Uani 1.00 d . . . C(22) C 0.188(1) 0.016(1) 0.509(1) 0.073(4) Uani 1.00 d . . . C(23) C 0.782(1) 0.151(1) 0.886(1) 0.103(5) Uani 1.00 d . . . C(24) C 0.749(1) 0.265(1) 0.977(1) 0.075(4) Uani 1.00 d . . . H(1) H 0.3997 0.6036 0.2342 0.0878 Uiso 1.00 calc . . . H(2) H 0.4273 0.4593 0.0419 0.0950 Uiso 1.00 calc . . . H(3) H 0.4238 0.2775 0.0229 0.0897 Uiso 1.00 calc . . . H(4) H 0.3946 0.2519 0.2012 0.0800 Uiso 1.00 calc . . . H(5) H 0.3802 0.7328 0.4339 0.0700 Uiso 1.00 calc . . . H(6) H 0.3473 0.8585 0.6375 0.0988 Uiso 1.00 calc . . . H(7) H 0.3318 0.7953 0.7975 0.0728 Uiso 1.00 calc . . . H(8) H 0.3372 0.6101 0.7353 0.0748 Uiso 1.00 calc . . . H(9) H 0.0637 0.7537 0.3045 0.0638 Uiso 1.00 calc . . . H(10) H 0.0851 0.6261 0.0963 0.0709 Uiso 1.00 calc . . . H(11) H 0.1102 0.4363 0.0394 0.0721 Uiso 1.00 calc . . . H(12) H 0.1259 0.3631 0.2031 0.0639 Uiso 1.00 calc . . . H(13) H 0.0528 0.8518 0.5148 0.0584 Uiso 1.00 calc . . . H(14) H 0.0308 0.9456 0.7320 0.0653 Uiso 1.00 calc . . . H(15) H 0.0445 0.8415 0.8523 0.0663 Uiso 1.00 calc . . . H(16) H 0.0829 0.6448 0.7589 0.0601 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Pd(1) 0.0476(4) 0.0404(4) 0.0407(4) -0.0178(3) -0.0007(3) 0.0106(3) Pd(2) 0.0475(5) 0.0476(4) 0.0554(5) -0.0190(3) -0.0022(3) 0.0190(4) P(1) 0.090(2) 0.048(1) 0.045(1) -0.027(1) 0.001(1) 0.012(1) F(1) 0.132(6) 0.051(3) 0.066(4) -0.030(4) 0.014(4) 0.024(3) F(2) 0.123(6) 0.064(4) 0.063(4) -0.048(4) 0.005(4) 0.020(3) F(3) 0.093(5) 0.061(4) 0.059(4) -0.031(3) 0.013(3) 0.011(3) F(4) 0.118(6) 0.068(4) 0.067(5) -0.012(4) 0.023(4) 0.013(4) F(5) 0.125(6) 0.053(4) 0.062(4) -0.040(4) -0.028(4) 0.021(3) F(6) 0.114(6) 0.084(5) 0.065(5) -0.031(4) -0.021(4) 0.026(4) O(1) 0.070(5) 0.057(4) 0.080(6) -0.024(4) 0.004(4) 0.022(4) O(2) 0.050(4) 0.037(3) 0.048(4) -0.017(3) -0.005(3) 0.005(3) O(3) 0.156(10) 0.078(6) 0.087(7) -0.049(7) 0.027(7) 0.006(6) O(4) 0.088(6) 0.085(6) 0.080(6) -0.049(5) -0.007(4) 0.034(5) O(5) 0.053(4) 0.049(4) 0.053(4) -0.016(3) 0.000(3) 0.022(3) O(6) 0.18(1) 0.116(8) 0.081(7) -0.083(8) -0.015(7) 0.042(7) O(7) 0.108(8) 0.123(9) 0.21(1) -0.081(8) -0.076(9) 0.10(1) O(8) 0.21(2) 0.16(1) 0.24(2) 0.02(1) 0.13(2) 0.11(1) O(9) 0.073(8) 0.082(9) 0.58(4) -0.018(7) 0.03(2) 0.09(2) O(10) 0.29(2) 0.098(9) 0.20(2) -0.07(1) 0.15(1) 0.018(9) O(11) 0.20(2) 0.18(2) 1.0(2) 0.01(2) -0.17(5) -0.06(5) N(1) 0.076(6) 0.063(6) 0.060(6) -0.031(5) 0.002(5) 0.022(5) N(2) 0.095(8) 0.058(5) 0.060(6) -0.034(5) 0.009(5) 0.013(5) N(3) 0.048(5) 0.064(5) 0.064(6) -0.028(4) -0.006(4) 0.020(5) N(4) 0.049(5) 0.052(5) 0.055(5) -0.023(4) -0.001(4) 0.015(4) N(5) 0.042(4) 0.037(4) 0.058(5) -0.013(3) -0.008(3) 0.021(4) N(6) 0.053(4) 0.042(4) 0.045(4) -0.021(3) -0.003(3) 0.021(4) N(7) 0.090(8) 0.079(7) 0.080(8) -0.037(6) -0.008(6) 0.036(7) N(8) 0.13(1) 0.075(8) 0.068(7) -0.046(7) -0.004(7) 0.012(6) N(9) 0.076(7) 0.13(1) 0.11(1) -0.039(7) -0.006(7) 0.077(10) C(1) 0.047(5) 0.065(6) 0.062(7) -0.023(5) -0.007(5) 0.026(6) C(2) 0.058(7) 0.108(10) 0.082(9) -0.035(6) -0.015(6) 0.063(9) C(3) 0.059(7) 0.14(1) 0.066(8) -0.033(8) -0.003(6) 0.055(9) C(4) 0.062(7) 0.096(9) 0.064(7) -0.024(6) -0.004(5) 0.036(7) C(5) 0.056(6) 0.076(8) 0.068(8) -0.025(6) -0.002(5) 0.023(7) C(6) 0.043(5) 0.069(7) 0.088(9) -0.017(5) -0.008(5) 0.046(7) C(7) 0.062(6) 0.041(5) 0.096(9) -0.020(5) -0.013(6) 0.035(7) C(8) 0.053(6) 0.054(7) 0.13(1) -0.021(5) -0.008(7) 0.035(8) C(9) 0.059(6) 0.043(5) 0.088(8) -0.021(5) -0.015(5) 0.030(6) C(10) 0.051(6) 0.057(6) 0.084(9) -0.022(5) -0.004(5) 0.027(7) C(11) 0.042(5) 0.048(5) 0.046(5) -0.013(4) -0.011(4) 0.021(5) C(12) 0.070(6) 0.064(6) 0.045(6) -0.029(5) 0.001(5) 0.028(5) C(13) 0.071(7) 0.058(6) 0.047(6) -0.027(5) -0.006(5) 0.018(5) C(14) 0.074(7) 0.059(6) 0.047(6) -0.027(5) -0.008(5) 0.022(5) C(15) 0.045(5) 0.059(6) 0.045(6) -0.017(5) -0.005(4) 0.006(5) C(16) 0.052(6) 0.055(6) 0.050(6) -0.024(5) 0.002(4) 0.007(5) C(17) 0.053(6) 0.042(5) 0.056(6) -0.016(4) 0.000(5) 0.011(5) C(18) 0.062(6) 0.042(5) 0.057(6) -0.017(4) 0.001(5) 0.018(5) C(19) 0.051(6) 0.056(6) 0.053(6) -0.028(5) 0.000(5) 0.000(5) C(20) 0.056(6) 0.048(5) 0.044(6) -0.018(4) 0.001(4) 0.014(5) C(21) 0.15(1) 0.11(1) 0.069(9) -0.09(1) -0.031(9) 0.047(9) C(22) 0.074(8) 0.089(9) 0.066(8) -0.022(7) -0.004(6) 0.043(8) C(23) 0.14(1) 0.061(8) 0.08(1) -0.019(8) -0.016(9) 0.009(8) C(24) 0.108(10) 0.056(7) 0.065(8) -0.038(7) -0.014(7) 0.022(7) #------------------------------------------------------------------------------ _computing_data_collection 'PROCESS' _computing_cell_refinement 'PROCESS' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution SAPI91 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd(1) Pd(2) 2.848(3) . . yes Pd(1) O(2) 2.027(6) . . yes Pd(1) O(5) 1.998(6) . . yes Pd(1) N(5) 1.974(7) . . yes Pd(1) N(6) 2.016(8) . . yes Pd(2) O(1) 1.991(8) . . yes Pd(2) O(4) 2.019(8) . . yes Pd(2) N(3) 2.035(9) . . yes Pd(2) N(4) 2.023(8) . . yes P(1) F(1) 1.600(6) . . yes P(1) F(2) 1.604(6) . . yes P(1) F(3) 1.621(7) . . yes P(1) F(4) 1.590(8) . . yes P(1) F(5) 1.594(7) . . yes P(1) F(6) 1.594(8) . . yes O(1) N(1) 1.33(1) . . yes O(2) N(1) 1.29(1) . . yes O(3) N(1) 1.54(1) . . yes O(4) N(2) 1.33(1) . . yes O(5) N(2) 1.30(1) . . yes O(6) N(2) 1.54(1) . . yes O(7) N(9) 1.27(2) . 2_655 yes O(8) N(9) 1.14(2) . 2_655 yes O(10) N(9) 1.16(1) . . yes N(3) C(1) 1.35(1) . . yes N(3) C(5) 1.36(2) . . yes N(4) C(6) 1.42(1) . . yes N(4) C(10) 1.34(2) . . yes N(5) C(11) 1.35(1) . . yes N(5) C(15) 1.38(1) . . yes N(6) C(16) 1.36(1) . . yes N(6) C(20) 1.33(1) . . yes N(7) C(22) 1.16(2) . 2_656 yes N(8) C(24) 1.16(2) . 1_554 yes C(1) C(2) 1.45(1) . . yes C(1) C(6) 1.45(2) . . yes C(2) C(3) 1.36(2) . . yes C(3) C(4) 1.39(2) . . yes C(4) C(5) 1.36(2) . . yes C(6) C(7) 1.36(1) . . yes C(7) C(8) 1.38(2) . . yes C(8) C(9) 1.38(2) . . yes C(9) C(10) 1.39(1) . . yes C(11) C(12) 1.42(1) . . yes C(11) C(16) 1.48(1) . . yes C(12) C(13) 1.39(1) . . yes C(13) C(14) 1.38(1) . . yes C(14) C(15) 1.39(1) . . yes C(16) C(17) 1.38(1) . . yes C(17) C(18) 1.40(1) . . yes C(18) C(19) 1.33(1) . . yes C(19) C(20) 1.38(1) . . yes C(21) C(22) 1.44(2) . . yes C(23) C(24) 1.45(2) . . yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Pd(2) Pd(1) O(2) 82.4(2) . 1_555 1_555 yes Pd(2) Pd(1) O(5) 84.9(2) . 1_555 1_555 yes Pd(2) Pd(1) N(5) 95.6(2) . 1_555 1_555 yes Pd(2) Pd(1) N(6) 100.3(2) . 1_555 1_555 yes O(2) Pd(1) O(5) 90.1(3) . 1_555 1_555 yes O(2) Pd(1) N(5) 94.4(3) . 1_555 1_555 yes O(2) Pd(1) N(6) 175.1(3) . 1_555 1_555 yes O(5) Pd(1) N(5) 175.6(3) . 1_555 1_555 yes O(5) Pd(1) N(6) 94.3(3) . 1_555 1_555 yes N(5) Pd(1) N(6) 81.3(3) . 1_555 1_555 yes Pd(1) Pd(2) O(1) 82.1(2) . 1_555 1_555 yes Pd(1) Pd(2) O(4) 79.9(2) . 1_555 1_555 yes Pd(1) Pd(2) N(3) 101.2(2) . 1_555 1_555 yes Pd(1) Pd(2) N(4) 95.2(2) . 1_555 1_555 yes O(1) Pd(2) O(4) 88.7(3) . 1_555 1_555 yes O(1) Pd(2) N(3) 93.9(3) . 1_555 1_555 yes O(1) Pd(2) N(4) 173.9(3) . 1_555 1_555 yes O(4) Pd(2) N(3) 177.4(3) . 1_555 1_555 yes O(4) Pd(2) N(4) 96.2(3) . 1_555 1_555 yes N(3) Pd(2) N(4) 81.3(4) . 1_555 1_555 yes F(1) P(1) F(2) 178.8(4) . 1_555 1_555 yes F(1) P(1) F(3) 89.8(4) . 1_555 1_555 yes F(1) P(1) F(4) 90.2(4) . 1_555 1_555 yes F(1) P(1) F(5) 91.9(4) . 1_555 1_555 yes F(1) P(1) F(6) 89.9(4) . 1_555 1_555 yes F(2) P(1) F(3) 89.0(4) . 1_555 1_555 yes F(2) P(1) F(4) 91.0(4) . 1_555 1_555 yes F(2) P(1) F(5) 87.9(4) . 1_555 1_555 yes F(2) P(1) F(6) 90.2(4) . 1_555 1_555 yes F(3) P(1) F(4) 179.3(5) . 1_555 1_555 yes F(3) P(1) F(5) 90.3(4) . 1_555 1_555 yes F(3) P(1) F(6) 88.7(4) . 1_555 1_555 yes F(4) P(1) F(5) 89.0(4) . 1_555 1_555 yes F(4) P(1) F(6) 92.0(5) . 1_555 1_555 yes F(5) P(1) F(6) 177.9(4) . 1_555 1_555 yes Pd(2) O(1) N(1) 124.9(6) . 1_555 1_555 yes Pd(1) O(2) N(1) 123.5(6) . 1_555 1_555 yes Pd(2) O(4) N(2) 126.7(7) . 1_555 1_555 yes Pd(1) O(5) N(2) 122.4(6) . 1_555 1_555 yes O(1) N(1) O(2) 125.6(9) . 1_555 1_555 yes O(1) N(1) O(3) 118.9(9) . 1_555 1_555 yes O(2) N(1) O(3) 115.5(9) . 1_555 1_555 yes O(4) N(2) O(5) 124.9(9) . 1_555 1_555 yes O(4) N(2) O(6) 119.9(10) . 1_555 1_555 yes O(5) N(2) O(6) 115.3(9) . 1_555 1_555 yes Pd(2) N(3) C(1) 113.3(7) . 1_555 1_555 yes Pd(2) N(3) C(5) 126.4(7) . 1_555 1_555 yes C(1) N(3) C(5) 120.3(9) . 1_555 1_555 yes Pd(2) N(4) C(6) 114.0(7) . 1_555 1_555 yes Pd(2) N(4) C(10) 127.6(7) . 1_555 1_555 yes C(6) N(4) C(10) 118.3(9) . 1_555 1_555 yes Pd(1) N(5) C(11) 115.2(6) . 1_555 1_555 yes Pd(1) N(5) C(15) 125.4(6) . 1_555 1_555 yes C(11) N(5) C(15) 119.2(8) . 1_555 1_555 yes Pd(1) N(6) C(16) 114.3(6) . 1_555 1_555 yes Pd(1) N(6) C(20) 125.7(6) . 1_555 1_555 yes C(16) N(6) C(20) 119.9(8) . 1_555 1_555 yes O(7) N(9) O(8) 115(1) . 2_655 2_655 yes O(7) N(9) O(10) 117(1) . 2_655 1_555 yes O(8) N(9) O(10) 125(1) . 2_655 1_555 yes N(3) C(1) C(2) 118(1) . 1_555 1_555 yes N(3) C(1) C(6) 118.3(9) . 1_555 1_555 yes C(2) C(1) C(6) 122(1) . 1_555 1_555 yes C(1) C(2) C(3) 119(1) . 1_555 1_555 yes C(2) C(3) C(4) 118(1) . 1_555 1_555 yes C(3) C(4) C(5) 120(1) . 1_555 1_555 yes N(3) C(5) C(4) 121(1) . 1_555 1_555 yes N(4) C(6) C(1) 112.9(9) . 1_555 1_555 yes N(4) C(6) C(7) 119(1) . 1_555 1_555 yes C(1) C(6) C(7) 127.8(10) . 1_555 1_555 yes C(6) C(7) C(8) 120(1) . 1_555 1_555 yes C(7) C(8) C(9) 121(1) . 1_555 1_555 yes C(8) C(9) C(10) 116(1) . 1_555 1_555 yes N(4) C(10) C(9) 124(1) . 1_555 1_555 yes N(5) C(11) C(12) 121.8(9) . 1_555 1_555 yes N(5) C(11) C(16) 114.9(8) . 1_555 1_555 yes C(12) C(11) C(16) 123.2(9) . 1_555 1_555 yes C(11) C(12) C(13) 117.8(9) . 1_555 1_555 yes C(12) C(13) C(14) 120.3(9) . 1_555 1_555 yes C(13) C(14) C(15) 120.1(10) . 1_555 1_555 yes N(5) C(15) C(14) 120.8(9) . 1_555 1_555 yes N(6) C(16) C(11) 113.8(8) . 1_555 1_555 yes N(6) C(16) C(17) 120.5(9) . 1_555 1_555 yes C(11) C(16) C(17) 125.7(9) . 1_555 1_555 yes C(16) C(17) C(18) 118.9(9) . 1_555 1_555 yes C(17) C(18) C(19) 119.0(9) . 1_555 1_555 yes C(18) C(19) C(20) 121.4(10) . 1_555 1_555 yes N(6) C(20) C(19) 120.2(8) . 1_555 1_555 yes N(7) C(22) C(21) 179(1) . 2_656 1_555 yes N(8) C(24) C(23) 178(1) . 1_556 1_555 yes #------------------------------------------------------------------------------ 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 Pd(1) Pd(2) O(1) N(1) 9.0(7) 1_555 1_555 1_555 1_555 yes Pd(1) Pd(2) O(4) N(2) 9.7(8) 1_555 1_555 1_555 1_555 yes Pd(1) Pd(2) N(3) C(1) 90.7(6) 1_555 1_555 1_555 1_555 yes Pd(1) Pd(2) N(3) C(5) -89.2(9) 1_555 1_555 1_555 1_555 yes Pd(1) Pd(2) N(4) C(6) -96.9(6) 1_555 1_555 1_555 1_555 yes Pd(1) Pd(2) N(4) C(10) 79.0(8) 1_555 1_555 1_555 1_555 yes Pd(1) O(2) N(1) O(1) -8(1) 1_555 1_555 1_555 1_555 yes Pd(1) O(2) N(1) O(3) 172.1(6) 1_555 1_555 1_555 1_555 yes Pd(1) O(5) N(2) O(4) -4(1) 1_555 1_555 1_555 1_555 yes Pd(1) O(5) N(2) O(6) 174.7(6) 1_555 1_555 1_555 1_555 yes Pd(1) N(5) C(11) C(12) 174.8(7) 1_555 1_555 1_555 1_555 yes Pd(1) N(5) C(11) C(16) -6.3(10) 1_555 1_555 1_555 1_555 yes Pd(1) N(5) C(15) C(14) -175.4(7) 1_555 1_555 1_555 1_555 yes Pd(1) N(6) C(16) C(11) 3(1) 1_555 1_555 1_555 1_555 yes Pd(1) N(6) C(16) C(17) -175.4(7) 1_555 1_555 1_555 1_555 yes Pd(1) N(6) C(20) C(19) 177.0(7) 1_555 1_555 1_555 1_555 yes Pd(2) Pd(1) O(2) N(1) 11.1(6) 1_555 1_555 1_555 1_555 yes Pd(2) Pd(1) O(5) N(2) 8.7(7) 1_555 1_555 1_555 1_555 yes Pd(2) Pd(1) N(5) C(11) -93.2(6) 1_555 1_555 1_555 1_555 yes Pd(2) Pd(1) N(5) C(15) 81.7(7) 1_555 1_555 1_555 1_555 yes Pd(2) Pd(1) N(6) C(16) 88.9(6) 1_555 1_555 1_555 1_555 yes Pd(2) Pd(1) N(6) C(20) -89.5(8) 1_555 1_555 1_555 1_555 yes Pd(2) O(1) N(1) O(2) -3(1) 1_555 1_555 1_555 1_555 yes Pd(2) O(1) N(1) O(3) 175.6(6) 1_555 1_555 1_555 1_555 yes Pd(2) O(4) N(2) O(5) -6(1) 1_555 1_555 1_555 1_555 yes Pd(2) O(4) N(2) O(6) 174.1(7) 1_555 1_555 1_555 1_555 yes Pd(2) N(3) C(1) C(2) -177.6(7) 1_555 1_555 1_555 1_555 yes Pd(2) N(3) C(1) C(6) 1(1) 1_555 1_555 1_555 1_555 yes Pd(2) N(3) C(5) C(4) 178.6(8) 1_555 1_555 1_555 1_555 yes Pd(2) N(4) C(6) C(1) -3(1) 1_555 1_555 1_555 1_555 yes Pd(2) N(4) C(6) C(7) 176.0(7) 1_555 1_555 1_555 1_555 yes Pd(2) N(4) C(10) C(9) -173.2(8) 1_555 1_555 1_555 1_555 yes O(1) Pd(2) Pd(1) O(2) -8.4(3) 1_555 1_555 1_555 1_555 yes O(1) Pd(2) Pd(1) O(5) 82.4(3) 1_555 1_555 1_555 1_555 yes O(1) Pd(2) Pd(1) N(5) -102.0(3) 1_555 1_555 1_555 1_555 yes O(1) Pd(2) Pd(1) N(6) 175.9(3) 1_555 1_555 1_555 1_555 yes O(1) Pd(2) O(4) N(2) -72.5(9) 1_555 1_555 1_555 1_555 yes O(1) Pd(2) N(3) C(1) 173.4(7) 1_555 1_555 1_555 1_555 yes O(1) Pd(2) N(3) C(5) -6.5(9) 1_555 1_555 1_555 1_555 yes O(1) Pd(2) N(4) C(6) -33(3) 1_555 1_555 1_555 1_555 yes O(1) Pd(2) N(4) C(10) 142(2) 1_555 1_555 1_555 1_555 yes O(2) Pd(1) Pd(2) O(4) -98.4(3) 1_555 1_555 1_555 1_555 yes O(2) Pd(1) Pd(2) N(3) 84.0(3) 1_555 1_555 1_555 1_555 yes O(2) Pd(1) Pd(2) N(4) 166.2(3) 1_555 1_555 1_555 1_555 yes O(2) Pd(1) O(5) N(2) 91.0(7) 1_555 1_555 1_555 1_555 yes O(2) Pd(1) N(5) C(11) -175.9(6) 1_555 1_555 1_555 1_555 yes O(2) Pd(1) N(5) C(15) -1.0(8) 1_555 1_555 1_555 1_555 yes O(2) Pd(1) N(6) C(16) -32(3) 1_555 1_555 1_555 1_555 yes O(2) Pd(1) N(6) C(20) 148(2) 1_555 1_555 1_555 1_555 yes O(4) Pd(2) Pd(1) O(5) -7.6(3) 1_555 1_555 1_555 1_555 yes O(4) Pd(2) Pd(1) N(5) 167.9(3) 1_555 1_555 1_555 1_555 yes O(4) Pd(2) Pd(1) N(6) 85.8(3) 1_555 1_555 1_555 1_555 yes O(4) Pd(2) O(1) N(1) 89.0(8) 1_555 1_555 1_555 1_555 yes O(4) Pd(2) N(3) C(1) -23(7) 1_555 1_555 1_555 1_555 yes O(4) Pd(2) N(3) C(5) 156(7) 1_555 1_555 1_555 1_555 yes O(4) Pd(2) N(4) C(6) -177.3(6) 1_555 1_555 1_555 1_555 yes O(4) Pd(2) N(4) C(10) -1.3(9) 1_555 1_555 1_555 1_555 yes O(5) Pd(1) Pd(2) N(3) 174.8(3) 1_555 1_555 1_555 1_555 yes O(5) Pd(1) Pd(2) N(4) -103.1(3) 1_555 1_555 1_555 1_555 yes O(5) Pd(1) O(2) N(1) -73.7(7) 1_555 1_555 1_555 1_555 yes O(5) Pd(1) N(5) C(11) 3(3) 1_555 1_555 1_555 1_555 yes O(5) Pd(1) N(5) C(15) 178(3) 1_555 1_555 1_555 1_555 yes O(5) Pd(1) N(6) C(16) 174.5(7) 1_555 1_555 1_555 1_555 yes O(5) Pd(1) N(6) C(20) -3.9(8) 1_555 1_555 1_555 1_555 yes N(1) O(1) Pd(2) N(3) -91.8(8) 1_555 1_555 1_555 1_555 yes N(1) O(1) Pd(2) N(4) -54(3) 1_555 1_555 1_555 1_555 yes N(1) O(2) Pd(1) N(5) 106.2(7) 1_555 1_555 1_555 1_555 yes N(1) O(2) Pd(1) N(6) 133(2) 1_555 1_555 1_555 1_555 yes N(2) O(4) Pd(2) N(3) 124(7) 1_555 1_555 1_555 1_555 yes N(2) O(4) Pd(2) N(4) 103.9(9) 1_555 1_555 1_555 1_555 yes N(2) O(5) Pd(1) N(5) -88(3) 1_555 1_555 1_555 1_555 yes N(2) O(5) Pd(1) N(6) -91.3(7) 1_555 1_555 1_555 1_555 yes N(3) Pd(2) Pd(1) N(5) -9.6(3) 1_555 1_555 1_555 1_555 yes N(3) Pd(2) Pd(1) N(6) -91.7(3) 1_555 1_555 1_555 1_555 yes N(3) Pd(2) N(4) C(6) 3.7(6) 1_555 1_555 1_555 1_555 yes N(3) Pd(2) N(4) C(10) 179.6(9) 1_555 1_555 1_555 1_555 yes N(3) C(1) C(2) C(3) -3(1) 1_555 1_555 1_555 1_555 yes N(3) C(1) C(6) N(4) 1(1) 1_555 1_555 1_555 1_555 yes N(3) C(1) C(6) C(7) -178.3(10) 1_555 1_555 1_555 1_555 yes N(3) C(5) C(4) C(3) 1(1) 1_555 1_555 1_555 1_555 yes N(4) Pd(2) Pd(1) N(5) 72.5(3) 1_555 1_555 1_555 1_555 yes N(4) Pd(2) Pd(1) N(6) -9.6(3) 1_555 1_555 1_555 1_555 yes N(4) Pd(2) N(3) C(1) -2.9(6) 1_555 1_555 1_555 1_555 yes N(4) Pd(2) N(3) C(5) 177.2(9) 1_555 1_555 1_555 1_555 yes N(4) C(6) C(1) C(2) -179.4(9) 1_555 1_555 1_555 1_555 yes N(4) C(6) C(7) C(8) -2(1) 1_555 1_555 1_555 1_555 yes N(4) C(10) C(9) C(8) -1(1) 1_555 1_555 1_555 1_555 yes N(5) Pd(1) N(6) C(16) -5.3(6) 1_555 1_555 1_555 1_555 yes N(5) Pd(1) N(6) C(20) 176.3(8) 1_555 1_555 1_555 1_555 yes N(5) C(11) C(12) C(13) 0(1) 1_555 1_555 1_555 1_555 yes N(5) C(11) C(16) N(6) 1(1) 1_555 1_555 1_555 1_555 yes N(5) C(11) C(16) C(17) -179.5(9) 1_555 1_555 1_555 1_555 yes N(5) C(15) C(14) C(13) 1(1) 1_555 1_555 1_555 1_555 yes N(6) Pd(1) N(5) C(11) 6.3(6) 1_555 1_555 1_555 1_555 yes N(6) Pd(1) N(5) C(15) -178.7(8) 1_555 1_555 1_555 1_555 yes N(6) C(16) C(11) C(12) -179.3(9) 1_555 1_555 1_555 1_555 yes N(6) C(16) C(17) C(18) -3(1) 1_555 1_555 1_555 1_555 yes N(6) C(20) C(19) C(18) 0(1) 1_555 1_555 1_555 1_555 yes C(1) N(3) C(5) C(4) -1(1) 1_555 1_555 1_555 1_555 yes C(1) C(2) C(3) C(4) 3(1) 1_555 1_555 1_555 1_555 yes C(1) C(6) N(4) C(10) 179.8(9) 1_555 1_555 1_555 1_555 yes C(1) C(6) C(7) C(8) 177(1) 1_555 1_555 1_555 1_555 yes C(2) C(1) N(3) C(5) 2(1) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(6) C(7) 0(1) 1_555 1_555 1_555 1_555 yes C(2) C(3) C(4) C(5) -2(1) 1_555 1_555 1_555 1_555 yes C(3) C(2) C(1) C(6) 177(1) 1_555 1_555 1_555 1_555 yes C(5) N(3) C(1) C(6) -178.5(9) 1_555 1_555 1_555 1_555 yes C(6) N(4) C(10) C(9) 2(1) 1_555 1_555 1_555 1_555 yes C(6) C(7) C(8) C(9) 3(1) 1_555 1_555 1_555 1_555 yes C(7) C(6) N(4) C(10) 0(1) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(9) C(10) -1(1) 1_555 1_555 1_555 1_555 yes C(11) N(5) C(15) C(14) 0(1) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(13) C(14) 0(1) 1_555 1_555 1_555 1_555 yes C(11) C(16) N(6) C(20) -178.1(8) 1_555 1_555 1_555 1_555 yes C(11) C(16) C(17) C(18) 177.8(9) 1_555 1_555 1_555 1_555 yes C(12) C(11) N(5) C(15) 0(1) 1_555 1_555 1_555 1_555 yes C(12) C(11) C(16) C(17) 0(1) 1_555 1_555 1_555 1_555 yes C(12) C(13) C(14) C(15) 0(1) 1_555 1_555 1_555 1_555 yes C(13) C(12) C(11) C(16) -177.8(9) 1_555 1_555 1_555 1_555 yes C(15) N(5) C(11) C(16) 178.4(8) 1_555 1_555 1_555 1_555 yes C(16) N(6) C(20) C(19) -1(1) 1_555 1_555 1_555 1_555 yes C(16) C(17) C(18) C(19) 2(1) 1_555 1_555 1_555 1_555 yes C(17) C(16) N(6) C(20) 3(1) 1_555 1_555 1_555 1_555 yes C(17) C(18) C(19) C(20) 0(1) 1_555 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Pd(1) Pd(2) 2.848(3) . . ? Pd(1) Pd(1) 3.117(3) . 2_566 ? Pd(1) N(6) 3.419(8) . 2_566 ? Pd(2) C(7) 3.41(1) . 2_666 ? Pd(2) C(6) 3.56(1) . 2_666 ? F(1) C(19) 3.40(1) . 1_554 ? F(1) C(18) 3.41(1) . 2_576 ? F(1) C(19) 3.51(1) . 2_576 ? F(2) O(6) 3.21(1) . 2_566 ? F(2) C(14) 3.37(1) . 2_565 ? F(2) C(13) 3.38(1) . . ? F(2) C(21) 3.38(2) . 2_566 ? F(3) C(15) 3.20(1) . 2_565 ? F(3) C(19) 3.26(1) . 1_554 ? F(3) C(20) 3.27(1) . 1_554 ? F(3) C(14) 3.44(1) . 2_565 ? F(3) C(13) 3.46(1) . . ? F(4) O(11) 3.13(3) . 1_465 ? F(4) C(21) 3.42(1) . 2_566 ? F(4) C(8) 3.43(2) . 2_576 ? F(4) C(9) 3.49(1) . 2_576 ? F(5) C(12) 3.20(1) . . ? F(5) C(18) 3.32(1) . 2_576 ? F(5) C(13) 3.40(1) . . ? F(5) C(23) 3.51(2) . 2_666 ? F(6) O(3) 3.23(1) . 2_565 ? F(6) C(15) 3.46(1) . 2_565 ? F(6) N(1) 3.51(1) . 2_565 ? O(1) O(9) 2.86(2) . . ? O(2) N(6) 3.045(10) . 2_566 ? O(2) C(20) 3.06(1) . 2_566 ? O(2) C(16) 3.43(1) . 2_566 ? O(2) C(19) 3.49(1) . 2_566 ? O(3) C(23) 3.43(2) . 2_656 ? O(3) C(21) 3.48(2) . . ? O(3) C(22) 3.49(2) . . ? O(4) O(7) 3.04(1) . 1_556 ? O(4) N(9) 3.41(1) . 2_656 ? O(5) N(5) 3.103(10) . 2_566 ? O(5) C(11) 3.37(1) . 2_566 ? O(5) C(15) 3.49(1) . 2_566 ? O(6) N(8) 3.35(2) . 2_666 ? O(6) O(7) 3.40(2) . 1_556 ? O(7) C(2) 3.11(1) . 2_665 ? O(7) C(3) 3.50(2) . . ? O(7) C(24) 3.51(2) . 1_554 ? O(8) O(9) 2.76(4) . 1_554 ? O(8) O(9) 3.36(2) . 2_655 ? O(8) C(7) 3.38(2) . 2_665 ? O(8) C(22) 3.54(2) . 2_655 ? O(9) O(10) 2.90(3) . . ? O(9) C(8) 3.15(2) . 2_666 ? O(9) O(11) 3.25(8) . . ? O(9) C(21) 3.26(2) . 2_656 ? O(9) N(9) 3.45(2) . . ? O(9) C(7) 3.58(2) . 2_666 ? O(10) O(11) 3.24(7) . . ? O(10) C(4) 3.57(2) . 2_655 ? O(11) C(5) 3.53(3) . . ? N(2) N(8) 3.57(2) . 2_666 ? N(3) C(10) 3.39(1) . 2_666 ? N(3) C(9) 3.49(1) . 2_666 ? N(3) N(4) 3.59(1) . 2_666 ? N(4) C(1) 3.37(1) . 2_666 ? N(4) C(6) 3.42(1) . 2_666 ? N(7) C(21) 2.59(2) . 2_656 ? N(7) C(17) 3.33(1) . 2_666 ? N(7) C(17) 3.58(1) . 1_645 ? N(8) C(23) 2.61(2) . 1_554 ? N(8) C(10) 3.44(2) . 2_666 ? C(1) C(10) 3.37(1) . 2_666 ? C(5) C(9) 3.35(2) . 2_666 ? C(17) C(22) 3.50(2) . 2_566 ? #------------------------------------------------------------------------------