# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _audit_creation_date 2004-06-17 _audit_creation_method 'by CrystalStructure v3.16' _audit_update_record ? _publ_contact_author_name 'Kohsuke Aikawa' _publ_contact_author_address ; Applied Chemistry Tokyo Institute of Technology Ookayama Meguro-ku Tokyo JAPAN ; _publ_contact_author_email kaikawa@o.cc.titech.ac.jp _publ_contact_author_fax (+81)3-5734-2776 _publ_contact_author_phone (+81)3-5734-2776 _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_category 'CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? _publ_section_title ; Dual Chirality Control of Palladium(II) Complexes Bearing Tropos Biphenyl Diamine Ligands ; _publ_section_references ; ENTER OTHER REFERENCES Rigaku/MSC and Rigaku Corporation. (2001). CrystalStructure. Single Crystal Structure Analysis Software. Version 3.16. Rigaku/MSC, 9009 New Trails Drive, The Woodlands, TX, USA 77381-5209. Rigaku, 3-9-12 Akishima, Tokyo 196-8666, Japan. Watkin, D.J., Prout, C.K. Carruthers, J.R. & Betteridge, P.W. (1996) CRYSTALS Issue 10, Chemical Crystallography Laboratory, Oxford, UK. ; loop_ _publ_author_name 'Koichi Mikami' 'Kohsuke Aikawa' #============================================================================== data_DB-DABP-PdCl2 _database_code_depnum_ccdc_archive 'CCDC 277174' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C27 H26 Cl4 N2 Pd ' _chemical_formula_moiety 'C27 H26 Cl4 N2 Pd ' _chemical_formula_weight 626.72 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 #------------------------------------------------------------------------------ _cell_length_a 14.333(5) _cell_length_b 10.700(4) _cell_length_c 17.692(6) _cell_angle_alpha 90 _cell_angle_beta 91.002(5) _cell_angle_gamma 90 _cell_volume 2712.8(16) _cell_formula_units_Z 4 _cell_measurement_reflns_used 9435 _cell_measurement_theta_min 2.7 _cell_measurement_theta_max 31.5 _cell_measurement_temperature 193.1 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.534 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1264.00 _exptl_absorpt_coefficient_mu 1.097 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.654 _exptl_absorpt_correction_T_max 0.779 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 24204 _diffrn_reflns_av_R_equivalents 0.054 _diffrn_reflns_theta_max 31.40 _diffrn_measured_fraction_theta_max 0.8720 _diffrn_reflns_theta_full 31.40 _diffrn_measured_fraction_theta_full 0.8720 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 0.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 7849 _reflns_number_gt 7736 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0930 _refine_ls_wR_factor_ref 0.1440 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 7849 _refine_ls_number_parameters 333 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0000Fo^2^ + 2.0000\s^2^(Fo) + 0.2210]/(4Fo^2^)' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 1.18 _refine_diff_density_min -1.33 _refine_ls_extinction_method none _refine_ls_extinction_coef ? 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 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Cl Cl 0.148 0.159 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Pd Pd -0.999 1.007 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd(1) Pd 0.31609(2) 0.34022(3) 0.27641(2) 0.02904(9) Uani 1.00 1 d . . . Cl(1) Cl 0.25562(9) 0.46894(13) 0.36812(8) 0.0412(3) Uani 1.00 1 d . . . Cl(2) Cl 0.17782(9) 0.23312(13) 0.26177(9) 0.0435(4) Uani 1.00 1 d . . . Cl(3) Cl 0.5709(2) 0.9109(3) 0.0828(2) 0.0977(9) Uani 1.00 1 d . . . Cl(4) Cl 0.4365(2) 0.7333(3) 0.0239(1) 0.1019(9) Uani 1.00 1 d . . . N(1) N 0.4393(3) 0.4395(4) 0.2940(2) 0.0315(10) Uani 1.00 1 d . . . N(2) N 0.3695(3) 0.2183(4) 0.1980(2) 0.0310(10) Uani 1.00 1 d . . . C(1) C 0.5113(4) 0.4464(5) 0.2367(3) 0.0366(13) Uani 1.00 1 d . . . C(2) C 0.5339(4) 0.5627(6) 0.2078(4) 0.047(2) Uani 1.00 1 d . . . C(3) C 0.6037(5) 0.5740(7) 0.1550(4) 0.060(2) Uani 1.00 1 d . . . C(4) C 0.6519(5) 0.4693(8) 0.1327(4) 0.063(2) Uani 1.00 1 d . . . C(5) C 0.6308(4) 0.3541(7) 0.1620(4) 0.052(2) Uani 1.00 1 d . . . C(6) C 0.5587(3) 0.3388(6) 0.2137(3) 0.0389(13) Uani 1.00 1 d . . . C(7) C 0.4502(3) 0.1538(5) 0.2340(3) 0.0338(11) Uani 1.00 1 d . . . C(8) C 0.4346(4) 0.0352(6) 0.2611(3) 0.044(2) Uani 1.00 1 d . . . C(9) C 0.5061(5) -0.0326(6) 0.2950(4) 0.064(2) Uani 1.00 1 d . . . C(10) C 0.5943(5) 0.0203(7) 0.3011(4) 0.062(2) Uani 1.00 1 d . . . C(11) C 0.6096(4) 0.1394(6) 0.2745(4) 0.052(2) Uani 1.00 1 d . . . C(12) C 0.5372(4) 0.2104(5) 0.2405(3) 0.039(1) Uani 1.00 1 d . . . C(13) C 0.4838(4) 0.4093(5) 0.3724(3) 0.041(1) Uani 1.00 1 d . . . C(14) C 0.3857(3) 0.2626(6) 0.1189(3) 0.0388(13) Uani 1.00 1 d . . . C(15) C 0.5491(4) 0.5096(5) 0.3963(3) 0.0377(13) Uani 1.00 1 d . . . C(16) C 0.5144(4) 0.6247(6) 0.4187(4) 0.052(2) Uani 1.00 1 d . . . C(17) C 0.5765(5) 0.7193(7) 0.4424(4) 0.064(2) Uani 1.00 1 d . . . C(18) C 0.6700(5) 0.6988(7) 0.4434(4) 0.059(2) Uani 1.00 1 d . . . C(19) C 0.7043(5) 0.5859(8) 0.4212(5) 0.066(2) Uani 1.00 1 d . . . C(20) C 0.6460(4) 0.4910(6) 0.3994(4) 0.054(2) Uani 1.00 1 d . . . C(21) C 0.3018(4) 0.3307(5) 0.0861(3) 0.0363(12) Uani 1.00 1 d . . . C(22) C 0.2869(5) 0.4551(6) 0.1035(4) 0.053(2) Uani 1.00 1 d . . . C(23) C 0.2114(5) 0.5190(7) 0.0741(4) 0.061(2) Uani 1.00 1 d . . . C(24) C 0.1492(5) 0.4581(7) 0.0249(5) 0.068(2) Uani 1.00 1 d . . . C(25) C 0.1645(4) 0.3356(7) 0.0052(4) 0.058(2) Uani 1.00 1 d . . . C(26) C 0.2411(4) 0.2713(6) 0.0374(3) 0.044(2) Uani 1.00 1 d . . . C(27) C 0.4539(6) 0.8595(9) 0.0828(5) 0.082(3) Uani 1.00 1 d . . . H(1) H 0.5018(4) 0.6347(6) 0.2251(4) 0.057(2) Uiso 1.00 1 c . . . H(2) H 0.6185(5) 0.6535(7) 0.1344(4) 0.072(2) Uiso 1.00 1 c . . . H(3) H 0.6999(5) 0.4773(8) 0.0967(4) 0.076(2) Uiso 1.00 1 c . . . H(4) H 0.6658(4) 0.2834(7) 0.1467(4) 0.062(2) Uiso 1.00 1 c . . . H(5) H 0.3741(4) -0.0007(6) 0.2566(3) 0.052(2) Uiso 1.00 1 c . . . H(6) H 0.4951(5) -0.1137(6) 0.3149(4) 0.076(2) Uiso 1.00 1 c . . . H(7) H 0.6445(5) -0.0258(7) 0.3232(4) 0.075(2) Uiso 1.00 1 c . . . H(8) H 0.6702(4) 0.1750(6) 0.2791(4) 0.062(2) Uiso 1.00 1 c . . . H(9) H 0.4357(4) 0.4021(5) 0.4084(3) 0.049(2) Uiso 1.00 1 c . . . H(10) H 0.5165(4) 0.3323(5) 0.3692(3) 0.049(2) Uiso 1.00 1 c . . . H(11) H 0.4373(3) 0.3184(6) 0.1200(3) 0.046(2) Uiso 1.00 1 c . . . H(12) H 0.3995(3) 0.1933(6) 0.0874(3) 0.046(2) Uiso 1.00 1 c . . . H(13) H 0.4489(4) 0.6382(6) 0.4188(4) 0.062(2) Uiso 1.00 1 c . . . H(14) H 0.5528(5) 0.7985(7) 0.4569(4) 0.077(2) Uiso 1.00 1 c . . . H(15) H 0.7118(5) 0.7627(7) 0.4594(4) 0.071(2) Uiso 1.00 1 c . . . H(16) H 0.7697(5) 0.5719(8) 0.4226(5) 0.079(3) Uiso 1.00 1 c . . . H(17) H 0.6709(4) 0.4124(6) 0.3849(4) 0.065(2) Uiso 1.00 1 c . . . H(18) H 0.3296(5) 0.4975(6) 0.1362(4) 0.064(2) Uiso 1.00 1 c . . . H(19) H 0.2006(5) 0.6038(7) 0.0872(4) 0.073(2) Uiso 1.00 1 c . . . H(20) H 0.0966(5) 0.5016(7) 0.0047(5) 0.082(3) Uiso 1.00 1 c . . . H(21) H 0.1231(4) 0.2949(7) -0.0294(4) 0.069(2) Uiso 1.00 1 c . . . H(22) H 0.2515(4) 0.1862(6) 0.0248(3) 0.053(2) Uiso 1.00 1 c . . . H(23) H 0.4627(6) 0.8284(9) 0.1327(5) 0.099(3) Uiso 1.00 1 c . . . H(24) H 0.3993(6) 0.9099(9) 0.0806(5) 0.099(3) Uiso 1.00 1 c . . . H(25) H 0.4194(3) 0.5237(4) 0.2990(2) 0.038(1) Uiso 1.00 1 c . . . H(26) H 0.3234(3) 0.1552(4) 0.1923(2) 0.037(1) Uiso 1.00 1 c . . . 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) 0.0244(2) 0.0303(2) 0.0324(2) -0.0003(1) 0.00054(11) 0.0012(2) Cl(1) 0.0388(7) 0.0418(7) 0.0431(7) 0.0006(5) 0.0055(5) -0.0057(5) Cl(2) 0.0306(6) 0.0388(7) 0.0613(8) -0.0058(5) 0.0078(6) -0.0084(6) Cl(3) 0.086(2) 0.093(2) 0.116(2) -0.0207(13) 0.019(1) 0.000(2) Cl(4) 0.079(2) 0.145(3) 0.082(2) -0.026(2) 0.0055(12) -0.012(2) N(1) 0.026(2) 0.035(2) 0.033(2) 0.001(2) -0.002(2) -0.001(2) N(2) 0.030(2) 0.031(2) 0.032(2) -0.001(2) -0.002(2) 0.002(2) C(1) 0.028(2) 0.041(3) 0.040(3) -0.005(2) -0.002(2) 0.004(2) C(2) 0.032(3) 0.045(3) 0.064(4) -0.004(2) 0.003(3) 0.014(3) C(3) 0.044(3) 0.066(4) 0.072(4) -0.008(3) 0.010(3) 0.024(4) C(4) 0.045(4) 0.079(5) 0.065(4) -0.006(3) 0.018(3) 0.010(4) C(5) 0.034(3) 0.062(4) 0.060(4) 0.003(3) 0.014(3) -0.004(3) C(6) 0.025(2) 0.043(3) 0.048(3) -0.001(2) -0.001(2) -0.001(3) C(7) 0.028(2) 0.035(2) 0.038(2) 0.006(2) -0.008(2) -0.001(2) C(8) 0.040(3) 0.043(3) 0.048(3) 0.001(2) -0.011(2) -0.000(2) C(9) 0.076(5) 0.040(3) 0.074(5) 0.014(3) -0.008(4) 0.009(3) C(10) 0.052(4) 0.057(4) 0.078(5) 0.011(3) -0.033(3) 0.003(4) C(11) 0.032(3) 0.057(4) 0.066(4) 0.005(3) -0.022(3) -0.005(3) C(12) 0.033(3) 0.040(3) 0.045(3) 0.003(2) 0.002(2) -0.005(2) C(13) 0.037(3) 0.044(3) 0.042(3) -0.004(2) -0.006(2) 0.002(2) C(14) 0.027(2) 0.057(3) 0.033(2) -0.002(2) -0.002(2) -0.001(2) C(15) 0.032(3) 0.045(3) 0.037(2) -0.006(2) -0.003(2) -0.001(2) C(16) 0.043(3) 0.056(4) 0.056(4) 0.001(3) -0.003(3) -0.017(3) C(17) 0.073(5) 0.053(4) 0.065(4) -0.013(4) 0.011(4) -0.018(3) C(18) 0.053(4) 0.066(4) 0.058(4) -0.026(3) -0.010(3) -0.006(3) C(19) 0.034(3) 0.080(5) 0.084(5) -0.011(3) -0.016(3) 0.003(4) C(20) 0.037(3) 0.051(4) 0.074(4) 0.001(3) -0.008(3) -0.000(3) C(21) 0.037(3) 0.040(3) 0.032(2) -0.005(2) 0.006(2) 0.005(2) C(22) 0.074(4) 0.041(3) 0.044(3) -0.002(3) 0.006(3) 0.001(3) C(23) 0.072(5) 0.053(4) 0.056(4) 0.016(3) 0.000(3) 0.012(3) C(24) 0.059(4) 0.067(5) 0.079(5) 0.018(4) 0.006(4) 0.035(4) C(25) 0.046(3) 0.066(4) 0.061(4) -0.013(3) -0.016(3) 0.017(4) C(26) 0.041(3) 0.045(3) 0.047(3) -0.007(2) -0.013(2) 0.003(3) C(27) 0.064(5) 0.112(7) 0.072(5) 0.015(5) 0.026(4) 0.001(5) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SIR92 _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure Ver. 3.16' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Pd(1) Cl(1) 2.309(1) yes . . Pd(1) Cl(2) 2.3000(13) yes . . Pd(1) N(1) 2.080(4) yes . . Pd(1) N(2) 2.062(4) yes . . Cl(3) C(27) 1.765(9) yes . . Cl(4) C(27) 1.721(10) yes . . N(1) C(1) 1.461(7) yes . . N(1) C(13) 1.550(7) yes . . N(1) H(25) 0.950(6) no . . N(2) C(7) 1.481(6) yes . . N(2) C(14) 1.500(6) yes . . N(2) H(26) 0.950(6) no . . C(1) C(2) 1.386(8) yes . . C(1) C(6) 1.401(8) yes . . C(2) C(3) 1.386(9) yes . . C(2) H(1) 0.950(9) no . . C(3) C(4) 1.377(11) yes . . C(3) H(2) 0.950(11) no . . C(4) C(5) 1.373(11) yes . . C(4) H(3) 0.950(10) no . . C(5) C(6) 1.401(8) yes . . C(5) H(4) 0.950(9) no . . C(6) C(12) 1.488(8) yes . . C(7) C(8) 1.376(8) yes . . C(7) C(12) 1.389(7) yes . . C(8) C(9) 1.384(9) yes . . C(8) H(5) 0.950(8) no . . C(9) C(10) 1.389(10) yes . . C(9) H(6) 0.950(10) no . . C(10) C(11) 1.377(10) yes . . C(10) H(7) 0.950(10) no . . C(11) C(12) 1.413(8) yes . . C(11) H(8) 0.950(8) no . . C(13) C(15) 1.481(8) yes . . C(13) H(9) 0.950(8) no . . C(13) H(10) 0.950(8) no . . C(14) C(21) 1.514(7) yes . . C(14) H(11) 0.950(8) no . . C(14) H(12) 0.950(8) no . . C(15) C(16) 1.389(9) yes . . C(15) C(20) 1.403(8) yes . . C(16) C(17) 1.407(10) yes . . C(16) H(13) 0.950(9) no . . C(17) C(18) 1.357(10) yes . . C(17) H(14) 0.950(11) no . . C(18) C(19) 1.364(11) yes . . C(18) H(15) 0.950(10) no . . C(19) C(20) 1.366(10) yes . . C(19) H(16) 0.950(9) no . . C(20) H(17) 0.950(10) no . . C(21) C(22) 1.383(8) yes . . C(21) C(26) 1.369(8) yes . . C(22) C(23) 1.374(10) yes . . C(22) H(18) 0.950(9) no . . C(23) C(24) 1.396(11) yes . . C(23) H(19) 0.950(10) no . . C(24) C(25) 1.375(11) yes . . C(24) H(20) 0.950(11) no . . C(25) C(26) 1.408(9) yes . . C(25) H(21) 0.950(10) no . . C(26) H(22) 0.950(9) no . . C(27) H(23) 0.950(12) no . . C(27) H(24) 0.950(12) no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Cl(1) Pd(1) Cl(2) 92.47(5) yes . . . Cl(1) Pd(1) N(1) 85.32(12) yes . . . Cl(1) Pd(1) N(2) 177.30(12) yes . . . Cl(2) Pd(1) N(1) 177.63(12) yes . . . Cl(2) Pd(1) N(2) 86.48(12) yes . . . N(1) Pd(1) N(2) 95.7(2) yes . . . C(1) N(1) C(13) 110.3(4) yes . . . C(1) N(1) H(25) 103.5(5) no . . . C(1) N(1) Pd(1) 122.0(3) yes . . . C(13) N(1) H(25) 103.5(4) no . . . C(13) N(1) Pd(1) 111.3(3) yes . . . H(25) N(1) Pd(1) 104.1(4) no . . . C(7) N(2) C(14) 114.6(4) yes . . . C(7) N(2) H(26) 104.6(4) no . . . C(7) N(2) Pd(1) 107.6(3) yes . . . C(14) N(2) H(26) 104.1(4) no . . . C(14) N(2) Pd(1) 119.6(3) yes . . . H(26) N(2) Pd(1) 104.8(4) no . . . C(2) C(1) C(6) 120.9(5) yes . . . C(2) C(1) N(1) 118.3(5) yes . . . C(6) C(1) N(1) 120.8(5) yes . . . C(3) C(2) H(1) 120.3(7) no . . . C(3) C(2) C(1) 120.2(6) yes . . . H(1) C(2) C(1) 119.4(7) no . . . C(4) C(3) H(2) 120.1(8) no . . . C(4) C(3) C(2) 119.6(7) yes . . . H(2) C(3) C(2) 120.3(8) no . . . C(5) C(4) H(3) 120.0(9) no . . . C(5) C(4) C(3) 120.5(7) yes . . . H(3) C(4) C(3) 119.5(9) no . . . C(6) C(5) H(4) 119.5(8) no . . . C(6) C(5) C(4) 121.4(6) yes . . . H(4) C(5) C(4) 119.1(7) no . . . C(12) C(6) C(1) 124.2(5) yes . . . C(12) C(6) C(5) 118.4(5) yes . . . C(1) C(6) C(5) 117.4(5) yes . . . C(8) C(7) C(12) 121.6(5) yes . . . C(8) C(7) N(2) 116.7(4) yes . . . C(12) C(7) N(2) 121.7(5) yes . . . C(9) C(8) H(5) 119.4(7) no . . . C(9) C(8) C(7) 120.8(6) yes . . . H(5) C(8) C(7) 119.9(7) no . . . C(10) C(9) H(6) 120.0(9) no . . . C(10) C(9) C(8) 119.1(6) yes . . . H(6) C(9) C(8) 120.9(9) no . . . C(11) C(10) H(7) 119.8(8) no . . . C(11) C(10) C(9) 120.1(6) yes . . . H(7) C(10) C(9) 120.1(8) no . . . C(12) C(11) H(8) 119.0(7) no . . . C(12) C(11) C(10) 121.5(6) yes . . . H(8) C(11) C(10) 119.5(7) no . . . C(6) C(12) C(7) 124.5(5) yes . . . C(6) C(12) C(11) 118.6(5) yes . . . C(7) C(12) C(11) 116.9(5) yes . . . C(15) C(13) H(9) 109.3(6) no . . . C(15) C(13) H(10) 109.6(6) no . . . C(15) C(13) N(1) 110.7(4) yes . . . H(9) C(13) H(10) 109.5(7) no . . . H(9) C(13) N(1) 109.0(6) no . . . H(10) C(13) N(1) 108.9(6) no . . . C(21) C(14) H(11) 108.5(6) no . . . C(21) C(14) H(12) 108.9(5) no . . . C(21) C(14) N(2) 112.0(4) yes . . . H(11) C(14) H(12) 109.5(7) no . . . H(11) C(14) N(2) 108.1(5) no . . . H(12) C(14) N(2) 109.8(6) no . . . C(16) C(15) C(20) 118.3(5) yes . . . C(16) C(15) C(13) 119.8(5) yes . . . C(20) C(15) C(13) 121.9(5) yes . . . C(17) C(16) H(13) 120.6(8) no . . . C(17) C(16) C(15) 119.7(6) yes . . . H(13) C(16) C(15) 119.6(7) no . . . C(18) C(17) H(14) 120.0(9) no . . . C(18) C(17) C(16) 120.4(7) yes . . . H(14) C(17) C(16) 119.6(9) no . . . C(19) C(18) H(15) 119.6(8) no . . . C(19) C(18) C(17) 120.1(7) yes . . . H(15) C(18) C(17) 120.3(9) no . . . C(20) C(19) H(16) 119.2(9) no . . . C(20) C(19) C(18) 121.2(6) yes . . . H(16) C(19) C(18) 119.5(9) no . . . H(17) C(20) C(15) 119.4(7) no . . . H(17) C(20) C(19) 120.3(7) no . . . C(15) C(20) C(19) 120.4(6) yes . . . C(22) C(21) C(26) 119.2(5) yes . . . C(22) C(21) C(14) 120.2(5) yes . . . C(26) C(21) C(14) 120.6(5) yes . . . C(23) C(22) H(18) 119.2(8) no . . . C(23) C(22) C(21) 121.2(6) yes . . . H(18) C(22) C(21) 119.6(8) no . . . C(24) C(23) H(19) 119.5(9) no . . . C(24) C(23) C(22) 119.6(7) yes . . . H(19) C(23) C(22) 120.9(8) no . . . C(25) C(24) H(20) 120.0(9) no . . . C(25) C(24) C(23) 120.0(7) yes . . . H(20) C(24) C(23) 120.0(9) no . . . C(26) C(25) H(21) 120.6(8) no . . . C(26) C(25) C(24) 119.3(6) yes . . . H(21) C(25) C(24) 120.1(8) no . . . H(22) C(26) C(21) 119.5(6) no . . . H(22) C(26) C(25) 119.8(7) no . . . C(21) C(26) C(25) 120.7(6) yes . . . H(23) C(27) H(24) 109.5(11) no . . . H(23) C(27) Cl(3) 89.8(8) no . . . H(23) C(27) Cl(4) 107.7(10) no . . . H(24) C(27) Cl(3) 127.2(10) no . . . H(24) C(27) Cl(4) 108.0(9) no . . . Cl(3) C(27) Cl(4) 111.9(5) 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 Cl(1) Pd(1) N(1) C(1) -157.2(4) yes . . . . Cl(1) Pd(1) N(1) C(13) 69.8(3) yes . . . . Cl(1) Pd(1) N(1) H(25) -41.1(4) no . . . . N(2) Pd(1) N(1) C(1) 25.3(4) yes . . . . N(2) Pd(1) N(1) C(13) -107.7(3) yes . . . . N(2) Pd(1) N(1) H(25) 141.4(4) no . . . . Cl(2) Pd(1) N(2) C(7) -121.7(3) yes . . . . Cl(2) Pd(1) N(2) C(14) 105.3(3) yes . . . . Cl(2) Pd(1) N(2) H(26) -10.8(4) no . . . . N(1) Pd(1) N(2) C(7) 57.4(3) yes . . . . N(1) Pd(1) N(2) C(14) -75.6(3) yes . . . . N(1) Pd(1) N(2) H(26) 168.3(4) no . . . . Pd(1) N(1) C(1) C(2) 118.4(5) yes . . . . Pd(1) N(1) C(1) C(6) -64.0(6) yes . . . . C(13) N(1) C(1) C(2) -108.2(5) yes . . . . C(13) N(1) C(1) C(6) 69.4(6) yes . . . . H(25) N(1) C(1) C(2) 2.0(7) no . . . . H(25) N(1) C(1) C(6) 179.6(5) no . . . . Pd(1) N(1) C(13) C(15) -159.3(4) yes . . . . Pd(1) N(1) C(13) H(9) -39.2(7) no . . . . Pd(1) N(1) C(13) H(10) 80.2(6) no . . . . C(1) N(1) C(13) C(15) 62.0(5) yes . . . . C(1) N(1) C(13) H(9) -177.8(6) no . . . . C(1) N(1) C(13) H(10) -58.5(7) no . . . . H(25) N(1) C(13) C(15) -48.1(6) no . . . . H(25) N(1) C(13) H(9) 72.1(7) no . . . . H(25) N(1) C(13) H(10) -168.6(6) no . . . . Pd(1) N(2) C(7) C(8) 100.1(5) yes . . . . Pd(1) N(2) C(7) C(12) -79.6(5) yes . . . . C(14) N(2) C(7) C(8) -124.3(5) yes . . . . C(14) N(2) C(7) C(12) 56.1(6) yes . . . . H(26) N(2) C(7) C(8) -10.9(6) no . . . . H(26) N(2) C(7) C(12) 169.4(5) no . . . . Pd(1) N(2) C(14) C(21) -48.5(5) yes . . . . Pd(1) N(2) C(14) H(11) 71.1(6) no . . . . Pd(1) N(2) C(14) H(12) -169.6(5) no . . . . C(7) N(2) C(14) C(21) -178.4(4) yes . . . . C(7) N(2) C(14) H(11) -58.9(7) no . . . . C(7) N(2) C(14) H(12) 60.5(6) no . . . . H(26) N(2) C(14) C(21) 68.0(6) no . . . . H(26) N(2) C(14) H(11) -172.5(6) no . . . . H(26) N(2) C(14) H(12) -53.1(7) no . . . . N(1) C(1) C(2) C(3) 178.0(6) yes . . . . N(1) C(1) C(2) H(1) -1.0(10) no . . . . C(6) C(1) C(2) C(3) 0.4(9) yes . . . . C(6) C(1) C(2) H(1) -178.6(7) no . . . . N(1) C(1) C(6) C(5) -176.1(5) yes . . . . N(1) C(1) C(6) C(12) 4.0(8) yes . . . . C(2) C(1) C(6) C(5) 1.4(8) yes . . . . C(2) C(1) C(6) C(12) -178.4(5) yes . . . . C(1) C(2) C(3) C(4) -1.3(10) yes . . . . C(1) C(2) C(3) H(2) 178.7(8) no . . . . H(1) C(2) C(3) C(4) 177.7(8) no . . . . H(1) C(2) C(3) H(2) -2.3(13) no . . . . C(2) C(3) C(4) C(5) 0.3(10) yes . . . . C(2) C(3) C(4) H(3) -179.7(36) no . . . . H(2) C(3) C(4) C(5) -179.8(51) no . . . . H(2) C(3) C(4) H(3) 0.3(13) no . . . . C(3) C(4) C(5) C(6) 1.6(10) yes . . . . C(3) C(4) C(5) H(4) -178.5(8) no . . . . H(3) C(4) C(5) C(6) -178.4(8) no . . . . H(3) C(4) C(5) H(4) 1.5(13) no . . . . C(4) C(5) C(6) C(1) -2.5(8) yes . . . . C(4) C(5) C(6) C(12) 177.4(5) yes . . . . H(4) C(5) C(6) C(1) 177.6(7) no . . . . H(4) C(5) C(6) C(12) -2.5(10) no . . . . C(1) C(6) C(12) C(7) 56.6(8) yes . . . . C(1) C(6) C(12) C(11) -124.0(6) yes . . . . C(5) C(6) C(12) C(7) -123.3(6) yes . . . . C(5) C(6) C(12) C(11) 56.1(7) yes . . . . N(2) C(7) C(8) C(9) 179.5(6) yes . . . . N(2) C(7) C(8) H(5) -0.8(9) no . . . . C(12) C(7) C(8) C(9) -0.9(9) yes . . . . C(12) C(7) C(8) H(5) 178.9(7) no . . . . N(2) C(7) C(12) C(6) 0.6(8) yes . . . . N(2) C(7) C(12) C(11) -178.8(5) yes . . . . C(8) C(7) C(12) C(6) -179.0(5) yes . . . . C(8) C(7) C(12) C(11) 1.6(8) yes . . . . C(7) C(8) C(9) C(10) -0.4(10) yes . . . . C(7) C(8) C(9) H(6) 178.5(8) no . . . . H(5) C(8) C(9) C(10) 179.8(51) no . . . . H(5) C(8) C(9) H(6) -1.3(13) no . . . . C(8) C(9) C(10) C(11) 0.9(11) yes . . . . C(8) C(9) C(10) H(7) -178.4(9) no . . . . H(6) C(9) C(10) C(11) -178.0(9) no . . . . H(6) C(9) C(10) H(7) 2.7(15) no . . . . C(9) C(10) C(11) C(12) -0.2(11) yes . . . . C(9) C(10) C(11) H(8) 179.8(51) no . . . . H(7) C(10) C(11) C(12) 179.2(8) no . . . . H(7) C(10) C(11) H(8) -0.8(14) no . . . . C(10) C(11) C(12) C(6) 179.5(6) yes . . . . C(10) C(11) C(12) C(7) -1.0(9) yes . . . . H(8) C(11) C(12) C(6) -0.5(10) no . . . . H(8) C(11) C(12) C(7) 179.0(7) no . . . . N(1) C(13) C(15) C(16) 72.2(7) yes . . . . N(1) C(13) C(15) C(20) -109.9(6) yes . . . . H(9) C(13) C(15) C(16) -47.8(8) no . . . . H(9) C(13) C(15) C(20) 130.1(7) no . . . . H(10) C(13) C(15) C(16) -167.7(6) no . . . . H(10) C(13) C(15) C(20) 10.2(9) no . . . . N(2) C(14) C(21) C(22) 81.4(7) yes . . . . N(2) C(14) C(21) C(26) -100.3(6) yes . . . . H(11) C(14) C(21) C(22) -37.9(8) no . . . . H(11) C(14) C(21) C(26) 140.4(6) no . . . . H(12) C(14) C(21) C(22) -157.0(6) no . . . . H(12) C(14) C(21) C(26) 21.3(8) no . . . . C(13) C(15) C(16) C(17) 179.1(6) yes . . . . C(13) C(15) C(16) H(13) 0.4(10) no . . . . C(20) C(15) C(16) C(17) 1.0(9) yes . . . . C(20) C(15) C(16) H(13) -177.6(7) no . . . . C(13) C(15) C(20) C(19) 179.5(6) yes . . . . C(13) C(15) C(20) H(17) 1.2(11) no . . . . C(16) C(15) C(20) C(19) -2.6(9) yes . . . . C(16) C(15) C(20) H(17) 179.2(8) no . . . . C(15) C(16) C(17) C(18) 0.2(10) yes . . . . C(15) C(16) C(17) H(14) 178.9(9) no . . . . H(13) C(16) C(17) C(18) 178.9(8) no . . . . H(13) C(16) C(17) H(14) -2.4(13) no . . . . C(16) C(17) C(18) C(19) 0.0(11) yes . . . . C(16) C(17) C(18) H(15) 180.0(88) no . . . . H(14) C(17) C(18) C(19) -178.7(9) no . . . . H(14) C(17) C(18) H(15) 1.3(14) no . . . . C(17) C(18) C(19) C(20) -1.6(12) yes . . . . C(17) C(18) C(19) H(16) -179.2(9) no . . . . H(15) C(18) C(19) C(20) 178.5(9) no . . . . H(15) C(18) C(19) H(16) 0.8(15) no . . . . C(18) C(19) C(20) C(15) 2.9(12) yes . . . . C(18) C(19) C(20) H(17) -178.9(9) no . . . . H(16) C(19) C(20) C(15) -179.5(36) no . . . . H(16) C(19) C(20) H(17) -1.3(15) no . . . . C(14) C(21) C(22) C(23) 179.7(6) yes . . . . C(14) C(21) C(22) H(18) -0.2(10) no . . . . C(26) C(21) C(22) C(23) 1.4(9) yes . . . . C(26) C(21) C(22) H(18) -178.5(7) no . . . . C(14) C(21) C(26) C(25) -178.2(5) yes . . . . C(14) C(21) C(26) H(22) 0.9(9) no . . . . C(22) C(21) C(26) C(25) 0.1(8) yes . . . . C(22) C(21) C(26) H(22) 179.2(7) no . . . . C(21) C(22) C(23) C(24) -1.0(11) yes . . . . C(21) C(22) C(23) H(19) 178.4(9) no . . . . H(18) C(22) C(23) C(24) 178.9(8) no . . . . H(18) C(22) C(23) H(19) -1.7(13) no . . . . C(22) C(23) C(24) C(25) -1.0(11) yes . . . . C(22) C(23) C(24) H(20) 179.6(36) no . . . . H(19) C(23) C(24) C(25) 179.6(9) no . . . . H(19) C(23) C(24) H(20) 0.2(15) no . . . . C(23) C(24) C(25) C(26) 2.5(11) yes . . . . C(23) C(24) C(25) H(21) -178.2(9) no . . . . H(20) C(24) C(25) C(26) -178.0(9) no . . . . H(20) C(24) C(25) H(21) 1.2(14) no . . . . C(24) C(25) C(26) C(21) -2.1(9) yes . . . . C(24) C(25) C(26) H(22) 178.9(7) no . . . . H(21) C(25) C(26) C(21) 178.6(8) no . . . . H(21) C(25) C(26) H(22) -0.4(12) no . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Pd(1) H(5) 3.258(6) no . 55502 Cl(1) N(2) 3.411(4) yes . 55502 Cl(1) C(8) 3.597(6) yes . 55502 Cl(1) H(5) 2.880(6) no . 55502 Cl(1) H(12) 3.375(6) no . 55502 Cl(1) H(22) 3.002(6) no . 55502 Cl(1) H(26) 2.520(4) no . 55502 Cl(2) H(5) 2.961(6) no . 55502 Cl(2) H(6) 3.248(8) no . 55502 Cl(3) H(12) 3.246(6) no . 66503 Cl(3) H(16) 2.864(8) no . 65502 Cl(3) H(22) 3.371(6) no . 66503 Cl(4) C(5) 3.537(7) yes . 66503 Cl(4) H(4) 3.338(7) no . 66503 Cl(4) H(11) 3.197(6) no . 66503 Cl(4) H(12) 3.190(6) no . 66503 C(2) Cl(2) 3.588(6) yes . 55502 C(3) H(8) 3.590(9) no . 65502 C(4) H(7) 3.009(10) no . 65502 C(5) Cl(4) 3.537(7) yes . 66503 C(5) H(7) 3.474(9) no . 65502 C(11) H(21) 3.542(9) no . 55504 C(13) H(21) 3.414(9) no . 55504 C(16) H(6) 3.356(10) no . 56501 C(16) H(21) 3.343(9) no . 55502 C(17) H(6) 3.091(10) no . 56501 C(17) H(7) 3.593(11) no . 56501 C(17) H(20) 3.194(11) no . 56504 C(17) H(21) 3.371(10) no . 55502 C(18) H(3) 3.592(11) no . 65502 C(18) H(4) 3.005(9) no . 65502 C(18) H(19) 3.331(10) no . 56504 C(18) H(20) 3.550(11) no . 56504 C(19) H(4) 3.075(10) no . 65502 C(19) H(22) 3.501(10) no . 55504 C(20) H(21) 3.326(10) no . 55504 C(20) H(22) 3.268(9) no . 55504 C(22) H(5) 3.446(9) no . 55502 C(23) H(3) 3.299(10) no . 66503 C(23) H(5) 3.262(9) no . 55502 C(24) H(3) 3.154(11) no . 66503 C(24) H(20) 3.579(11) no . 56503 C(25) H(3) 3.341(10) no . 66503 C(27) Cl(1) 3.352(8) yes . 55502 H(1) Cl(2) 2.795(6) no . 55502 H(3) C(10) 3.462(10) no . 65502 H(3) C(23) 3.299(10) no . 66503 H(3) C(24) 3.154(11) no . 66503 H(3) C(25) 3.341(10) no . 66503 H(4) Cl(4) 3.338(7) no . 66503 H(11) Cl(4) 3.197(6) no . 66503 H(12) Cl(3) 3.246(6) no . 66503 H(12) Cl(4) 3.190(6) no . 66503 H(13) C(25) 2.997(10) no . 55502 H(13) C(26) 3.181(9) no . 55502 H(14) C(9) 3.441(10) no . 56501 H(14) C(24) 3.381(11) no . 55502 H(14) C(24) 3.175(11) no . 56504 H(14) C(25) 3.221(10) no . 55502 H(15) Cl(4) 3.398(7) no . 56504 H(15) C(4) 3.387(10) no . 65502 H(15) C(5) 3.291(9) no . 65502 H(15) C(23) 3.095(10) no . 56504 H(15) C(24) 3.333(11) no . 56504 H(17) C(25) 3.404(10) no . 55504 H(17) C(26) 3.473(9) no . 55504 H(18) Cl(2) 3.104(6) no . 55502 H(19) Pd(1) 3.507(7) no . 55502 H(19) Cl(2) 3.453(7) no . 55502 H(19) C(8) 3.418(9) no . 55502 H(20) C(24) 3.579(11) no . 56503 H(22) Cl(3) 3.371(6) no . 66503 H(23) Cl(1) 3.472(9) no . 55502 H(23) Cl(2) 2.952(9) no . 55502 H(23) C(8) 3.201(11) no . 56501 H(23) C(9) 3.284(11) no . 56501 H(24) Cl(1) 2.496(8) no . 55502 H(24) Cl(2) 3.562(9) no . 55502 H(24) C(8) 3.492(10) no . 56501 H(25) Cl(2) 2.840(4) no . 55502 #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF data_DN-DABP-PdCl2 _database_code_depnum_ccdc_archive 'CCDC 277175' _audit_creation_date 2004-10-04 _audit_creation_method 'by CrystalStructure v3.16' _audit_update_record ? #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C34 H28 Cl2 N2 Pd ' _chemical_formula_moiety 'C34 H28 Cl2 N2 Pd ' _chemical_formula_weight 641.91 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 #------------------------------------------------------------------------------ _cell_length_a 8.376(3) _cell_length_b 14.977(6) _cell_length_c 22.767(9) _cell_angle_alpha 90 _cell_angle_beta 93.923(5) _cell_angle_gamma 90 _cell_volume 2849.4(19) _cell_formula_units_Z 4 _cell_measurement_reflns_used 11052 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 31.5 _cell_measurement_temperature 193.1 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.496 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1304.00 _exptl_absorpt_coefficient_mu 0.865 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.585 _exptl_absorpt_correction_T_max 0.841 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 25322 _diffrn_reflns_av_R_equivalents 0.042 _diffrn_reflns_theta_max 31.38 _diffrn_measured_fraction_theta_max 0.8872 _diffrn_reflns_theta_full 31.38 _diffrn_measured_fraction_theta_full 0.8872 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 32 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 0.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 8321 _reflns_number_gt 8292 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0700 _refine_ls_wR_factor_ref 0.1120 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 8321 _refine_ls_number_parameters 380 _refine_ls_goodness_of_fit_ref 0.770 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0000Fo^2^ + 2.0000\s^2^(Fo) + 0.3970]/(4Fo^2^)' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 0.58 _refine_diff_density_min -0.80 _refine_ls_extinction_method none _refine_ls_extinction_coef ? 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 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Cl Cl 0.148 0.159 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Pd Pd -0.999 1.007 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd(1) Pd 0.52049(3) 0.19131(2) 0.729700(10) 0.03037(6) Uani 1.00 1 d . . . Cl(1) Cl 0.3865(1) 0.25705(8) 0.80210(4) 0.0576(3) Uani 1.00 1 d . . . Cl(2) Cl 0.43170(12) 0.29503(6) 0.66120(4) 0.0452(2) Uani 1.00 1 d . . . N(1) N 0.5931(4) 0.0991(2) 0.79399(12) 0.0344(7) Uani 1.00 1 d . . . N(2) N 0.6411(3) 0.1340(2) 0.66253(11) 0.0300(6) Uani 1.00 1 d . . . C(1) C 0.5900(4) 0.0072(2) 0.7742(1) 0.0328(8) Uani 1.00 1 d . . . C(2) C 0.7045(4) -0.0263(2) 0.7380(1) 0.0331(8) Uani 1.00 1 d . . . C(3) C 0.6960(5) -0.1171(2) 0.7235(2) 0.0424(10) Uani 1.00 1 d . . . C(4) C 0.5753(6) -0.1708(3) 0.7416(2) 0.0516(12) Uani 1.00 1 d . . . C(5) C 0.4594(5) -0.1356(3) 0.7749(2) 0.0497(11) Uani 1.00 1 d . . . C(6) C 0.4687(4) -0.0473(3) 0.7920(2) 0.0406(9) Uani 1.00 1 d . . . C(7) C 0.8036(4) 0.1042(2) 0.67878(13) 0.0291(7) Uani 1.00 1 d . . . C(8) C 0.8340(4) 0.0288(2) 0.7144(1) 0.0327(8) Uani 1.00 1 d . . . C(9) C 0.9935(5) 0.0022(3) 0.7250(2) 0.0441(10) Uani 1.00 1 d . . . C(10) C 1.1168(5) 0.0503(3) 0.7034(2) 0.0530(12) Uani 1.00 1 d . . . C(11) C 1.0844(5) 0.1260(3) 0.6703(2) 0.0506(11) Uani 1.00 1 d . . . C(12) C 0.9279(4) 0.1519(3) 0.6572(2) 0.0391(9) Uani 1.00 1 d . . . C(13) C 0.7403(5) 0.1252(3) 0.8321(2) 0.0415(9) Uani 1.00 1 d . . . C(14) C 0.7608(5) 0.0705(3) 0.8878(2) 0.0416(9) Uani 1.00 1 d . . . C(15) C 0.8495(6) -0.0066(3) 0.8877(2) 0.0520(12) Uani 1.00 1 d . . . C(16) C 0.8692(7) -0.0610(3) 0.9375(2) 0.064(1) Uani 1.00 1 d . . . C(17) C 0.8049(7) -0.0374(4) 0.9882(2) 0.064(1) Uani 1.00 1 d . . . C(18) C 0.7157(6) 0.0421(3) 0.9914(2) 0.0510(11) Uani 1.00 1 d . . . C(19) C 0.6516(7) 0.0682(4) 1.0448(2) 0.069(2) Uani 1.00 1 d . . . C(20) C 0.5623(7) 0.1427(4) 1.0473(2) 0.075(2) Uani 1.00 1 d . . . C(21) C 0.5289(6) 0.1947(4) 0.9970(2) 0.065(2) Uani 1.00 1 d . . . C(22) C 0.5902(6) 0.1727(3) 0.9445(2) 0.0511(12) Uani 1.00 1 d . . . C(23) C 0.6877(5) 0.0960(3) 0.9403(2) 0.0403(9) Uani 1.00 1 d . . . C(24) C 0.5437(4) 0.0695(3) 0.6237(2) 0.0365(8) Uani 1.00 1 d . . . C(25) C 0.6270(4) 0.0454(3) 0.5691(2) 0.0363(8) Uani 1.00 1 d . . . C(26) C 0.7094(5) -0.0334(3) 0.5675(2) 0.0462(10) Uani 1.00 1 d . . . C(27) C 0.7942(5) -0.0569(4) 0.5186(2) 0.0592(13) Uani 1.00 1 d . . . C(28) C 0.7955(5) -0.0011(4) 0.4716(2) 0.060(1) Uani 1.00 1 d . . . C(29) C 0.7116(5) 0.0800(3) 0.4703(2) 0.0472(10) Uani 1.00 1 d . . . C(30) C 0.7070(7) 0.1377(4) 0.4210(2) 0.067(2) Uani 1.00 1 d . . . C(31) C 0.6213(7) 0.2142(4) 0.4196(2) 0.073(2) Uani 1.00 1 d . . . C(32) C 0.5367(6) 0.2388(3) 0.4680(2) 0.061(1) Uani 1.00 1 d . . . C(33) C 0.5390(5) 0.1861(3) 0.5172(2) 0.0464(10) Uani 1.00 1 d . . . C(34) C 0.6254(4) 0.1050(3) 0.5202(2) 0.0392(9) Uani 1.00 1 d . . . H(1) H 0.7761(5) -0.1424(2) 0.7010(2) 0.051(1) Uiso 1.00 1 c . . . H(2) H 0.5704(6) -0.2320(3) 0.7306(2) 0.062(2) Uiso 1.00 1 c . . . H(3) H 0.3741(5) -0.1720(3) 0.7864(2) 0.060(2) Uiso 1.00 1 c . . . H(4) H 0.3916(4) -0.0232(3) 0.8163(2) 0.049(1) Uiso 1.00 1 c . . . H(5) H 1.0169(5) -0.0496(3) 0.7481(2) 0.053(1) Uiso 1.00 1 c . . . H(6) H 1.2244(5) 0.0309(3) 0.7105(2) 0.064(2) Uiso 1.00 1 c . . . H(7) H 1.1695(5) 0.1611(3) 0.6571(2) 0.061(2) Uiso 1.00 1 c . . . H(8) H 0.9050(4) 0.2026(3) 0.6329(2) 0.047(1) Uiso 1.00 1 c . . . H(9) H 0.5103(4) 0.1012(2) 0.82045(12) 0.0417(12) Uiso 1.00 1 c . . . H(10) H 0.6561(3) 0.1828(2) 0.63679(11) 0.0364(12) Uiso 1.00 1 c . . . H(11) H 0.8316(5) 0.1176(3) 0.8101(2) 0.050(1) Uiso 1.00 1 c . . . H(12) H 0.7311(5) 0.1862(3) 0.8428(2) 0.050(1) Uiso 1.00 1 c . . . H(13) H 0.5282(4) 0.0165(3) 0.6455(2) 0.0438(13) Uiso 1.00 1 c . . . H(14) H 0.4429(4) 0.0955(3) 0.6123(2) 0.0437(13) Uiso 1.00 1 c . . . H(15) H 0.8999(6) -0.0225(3) 0.8530(2) 0.062(2) Uiso 1.00 1 c . . . H(16) H 0.9266(7) -0.1155(3) 0.9357(2) 0.076(2) Uiso 1.00 1 c . . . H(17) H 0.8189(7) -0.0744(4) 1.0220(2) 0.076(2) Uiso 1.00 1 c . . . H(18) H 0.6700(7) 0.0318(4) 1.0788(2) 0.083(2) Uiso 1.00 1 c . . . H(19) H 0.5243(7) 0.1611(4) 1.0838(2) 0.091(2) Uiso 1.00 1 c . . . H(20) H 0.4613(6) 0.2454(4) 0.9989(2) 0.079(2) Uiso 1.00 1 c . . . H(21) H 0.5684(6) 0.2092(3) 0.9108(2) 0.061(2) Uiso 1.00 1 c . . . H(22) H 0.7092(5) -0.0729(3) 0.6002(2) 0.055(2) Uiso 1.00 1 c . . . H(23) H 0.8498(5) -0.1121(4) 0.5179(2) 0.071(2) Uiso 1.00 1 c . . . H(24) H 0.8559(5) -0.0165(4) 0.4393(2) 0.073(2) Uiso 1.00 1 c . . . H(25) H 0.7662(7) 0.1221(4) 0.3883(2) 0.082(2) Uiso 1.00 1 c . . . H(26) H 0.6193(7) 0.2511(4) 0.3856(2) 0.088(2) Uiso 1.00 1 c . . . H(27) H 0.4777(6) 0.2930(3) 0.4665(2) 0.073(2) Uiso 1.00 1 c . . . H(28) H 0.4813(5) 0.2038(3) 0.5498(2) 0.055(1) Uiso 1.00 1 c . . . 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) 0.03183(12) 0.03122(12) 0.02875(11) 0.00282(10) 0.00712(8) 0.00054(10) Cl(1) 0.0692(7) 0.0635(7) 0.0423(5) 0.0284(5) 0.0205(5) 0.0011(5) Cl(2) 0.0523(5) 0.0419(5) 0.0423(5) 0.0107(4) 0.0107(4) 0.0099(4) N(1) 0.038(1) 0.037(2) 0.0295(13) 0.0028(12) 0.0071(11) 0.0020(11) N(2) 0.0315(13) 0.0316(13) 0.0273(12) -0.0012(10) 0.0058(10) -0.0002(10) C(1) 0.035(2) 0.034(2) 0.030(1) -0.0000(13) 0.0012(12) 0.0040(12) C(2) 0.035(2) 0.032(2) 0.032(2) -0.0001(13) 0.0013(12) 0.0013(12) C(3) 0.051(2) 0.033(2) 0.044(2) 0.003(2) 0.009(2) 0.001(1) C(4) 0.069(3) 0.033(2) 0.053(2) -0.010(2) 0.005(2) 0.003(2) C(5) 0.052(2) 0.047(2) 0.050(2) -0.016(2) 0.002(2) 0.014(2) C(6) 0.038(2) 0.047(2) 0.038(2) -0.002(2) 0.006(1) 0.010(2) C(7) 0.027(1) 0.033(2) 0.028(1) -0.0027(12) 0.0049(11) -0.0045(12) C(8) 0.031(2) 0.035(2) 0.033(2) -0.0010(13) 0.0060(12) -0.0031(12) C(9) 0.039(2) 0.052(2) 0.042(2) 0.008(2) 0.006(2) 0.002(2) C(10) 0.029(2) 0.073(3) 0.057(2) 0.005(2) 0.001(2) -0.005(2) C(11) 0.031(2) 0.062(3) 0.060(2) -0.013(2) 0.014(2) -0.010(2) C(12) 0.038(2) 0.041(2) 0.040(2) -0.008(1) 0.010(1) -0.004(1) C(13) 0.052(2) 0.040(2) 0.033(2) -0.003(2) 0.002(2) -0.003(1) C(14) 0.048(2) 0.044(2) 0.033(2) -0.001(2) -0.001(1) -0.005(1) C(15) 0.062(3) 0.058(3) 0.035(2) 0.014(2) -0.002(2) -0.006(2) C(16) 0.086(4) 0.059(3) 0.045(2) 0.027(3) -0.003(2) 0.002(2) C(17) 0.085(4) 0.067(3) 0.039(2) 0.021(3) -0.001(2) 0.009(2) C(18) 0.059(3) 0.059(3) 0.034(2) 0.003(2) 0.001(2) -0.001(2) C(19) 0.091(4) 0.080(4) 0.037(2) 0.016(3) 0.009(2) 0.004(2) C(20) 0.100(4) 0.089(4) 0.038(2) 0.021(3) 0.018(2) -0.007(2) C(21) 0.076(3) 0.061(3) 0.059(3) 0.012(3) 0.015(2) -0.012(2) C(22) 0.065(3) 0.049(2) 0.040(2) 0.006(2) 0.005(2) -0.002(2) C(23) 0.045(2) 0.043(2) 0.032(2) -0.002(2) -0.000(1) -0.004(1) C(24) 0.030(2) 0.045(2) 0.034(2) -0.003(1) 0.0031(12) -0.003(1) C(25) 0.032(2) 0.042(2) 0.035(2) -0.006(1) 0.0035(12) -0.008(1) C(26) 0.045(2) 0.046(2) 0.047(2) -0.001(2) -0.000(2) -0.011(2) C(27) 0.047(2) 0.067(3) 0.064(3) 0.006(2) 0.004(2) -0.026(2) C(28) 0.044(2) 0.083(3) 0.055(3) -0.009(2) 0.015(2) -0.032(3) C(29) 0.041(2) 0.064(3) 0.038(2) -0.021(2) 0.009(2) -0.014(2) C(30) 0.075(3) 0.089(4) 0.040(2) -0.032(3) 0.018(2) -0.008(2) C(31) 0.093(4) 0.082(4) 0.044(3) -0.030(3) 0.003(3) 0.010(2) C(32) 0.075(3) 0.056(3) 0.050(3) -0.007(2) -0.003(2) 0.008(2) C(33) 0.052(2) 0.051(2) 0.035(2) -0.004(2) 0.001(2) -0.004(2) C(34) 0.034(2) 0.052(2) 0.032(2) -0.011(2) 0.0027(13) -0.007(2) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SIR92 _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure Ver. 3.16' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Pd(1) Cl(1) 2.2802(11) yes . . Pd(1) Cl(2) 2.2890(9) yes . . Pd(1) N(1) 2.074(3) yes . . Pd(1) N(2) 2.075(3) yes . . N(1) C(1) 1.447(4) yes . . N(1) C(13) 1.510(5) yes . . N(1) H(9) 0.950(4) no . . N(2) C(7) 1.456(4) yes . . N(2) C(24) 1.511(4) yes . . N(2) H(10) 0.950(4) no . . C(1) C(2) 1.400(5) yes . . C(1) C(6) 1.384(5) yes . . C(2) C(3) 1.401(5) yes . . C(2) C(8) 1.492(5) yes . . C(3) C(4) 1.377(6) yes . . C(3) H(1) 0.950(6) no . . C(4) C(5) 1.377(6) yes . . C(4) H(2) 0.950(6) no . . C(5) C(6) 1.379(6) yes . . C(5) H(3) 0.950(6) no . . C(6) H(4) 0.950(5) no . . C(7) C(8) 1.404(5) yes . . C(7) C(12) 1.381(5) yes . . C(8) C(9) 1.399(5) yes . . C(9) C(10) 1.378(6) yes . . C(9) H(5) 0.950(6) no . . C(10) C(11) 1.378(7) yes . . C(10) H(6) 0.950(6) no . . C(11) C(12) 1.380(5) yes . . C(11) H(7) 0.950(6) no . . C(12) H(8) 0.950(5) no . . C(13) C(14) 1.510(5) yes . . C(13) H(11) 0.950(6) no . . C(13) H(12) 0.950(6) no . . C(14) C(15) 1.373(6) yes . . C(14) C(23) 1.432(5) yes . . C(15) C(16) 1.397(6) yes . . C(15) H(15) 0.950(6) no . . C(16) C(17) 1.353(7) yes . . C(16) H(16) 0.950(7) no . . C(17) C(18) 1.410(7) yes . . C(17) H(17) 0.950(7) no . . C(18) C(19) 1.417(7) yes . . C(18) C(23) 1.422(5) yes . . C(19) C(20) 1.348(9) yes . . C(19) H(18) 0.950(7) no . . C(20) C(21) 1.399(7) yes . . C(20) H(19) 0.950(7) no . . C(21) C(22) 1.372(7) yes . . C(21) H(20) 0.950(8) no . . C(22) C(23) 1.416(6) yes . . C(22) H(21) 0.950(6) no . . C(24) C(25) 1.509(5) yes . . C(24) H(13) 0.950(5) no . . C(24) H(14) 0.950(5) no . . C(25) C(26) 1.370(6) yes . . C(25) C(34) 1.425(5) yes . . C(26) C(27) 1.405(7) yes . . C(26) H(22) 0.950(6) no . . C(27) C(28) 1.358(7) yes . . C(27) H(23) 0.950(7) no . . C(28) C(29) 1.404(7) yes . . C(28) H(24) 0.950(7) no . . C(29) C(30) 1.415(7) yes . . C(29) C(34) 1.437(5) yes . . C(30) C(31) 1.351(9) yes . . C(30) H(25) 0.950(7) no . . C(31) C(32) 1.399(8) yes . . C(31) H(26) 0.950(8) no . . C(32) C(33) 1.370(6) yes . . C(32) H(27) 0.950(7) no . . C(33) C(34) 1.414(6) yes . . C(33) H(28) 0.950(6) no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Cl(1) Pd(1) Cl(2) 92.66(4) yes . . . Cl(1) Pd(1) N(1) 84.99(9) yes . . . Cl(1) Pd(1) N(2) 178.65(8) yes . . . Cl(2) Pd(1) N(1) 177.54(9) yes . . . Cl(2) Pd(1) N(2) 86.01(8) yes . . . N(1) Pd(1) N(2) 96.35(11) yes . . . C(1) N(1) C(13) 115.0(3) yes . . . C(1) N(1) H(9) 103.3(3) no . . . C(1) N(1) Pd(1) 114.6(2) yes . . . C(13) N(1) H(9) 103.3(3) no . . . C(13) N(1) Pd(1) 114.9(2) yes . . . H(9) N(1) Pd(1) 103.5(3) no . . . C(7) N(2) C(24) 114.2(3) yes . . . C(7) N(2) H(10) 103.4(3) no . . . C(7) N(2) Pd(1) 115.7(2) yes . . . C(24) N(2) H(10) 102.7(3) no . . . C(24) N(2) Pd(1) 115.2(2) yes . . . H(10) N(2) Pd(1) 103.2(3) no . . . C(2) C(1) C(6) 120.5(3) yes . . . C(2) C(1) N(1) 121.6(3) yes . . . C(6) C(1) N(1) 117.9(3) yes . . . C(3) C(2) C(8) 118.5(3) yes . . . C(3) C(2) C(1) 117.4(3) yes . . . C(8) C(2) C(1) 124.0(3) yes . . . C(4) C(3) H(1) 119.3(4) no . . . C(4) C(3) C(2) 121.5(4) yes . . . H(1) C(3) C(2) 119.2(4) no . . . C(5) C(4) H(2) 119.8(5) no . . . C(5) C(4) C(3) 120.0(4) yes . . . H(2) C(4) C(3) 120.2(5) no . . . C(6) C(5) H(3) 120.2(5) no . . . C(6) C(5) C(4) 119.7(4) yes . . . H(3) C(5) C(4) 120.2(5) no . . . H(4) C(6) C(1) 119.2(4) no . . . H(4) C(6) C(5) 120.1(5) no . . . C(1) C(6) C(5) 120.7(4) yes . . . C(8) C(7) C(12) 120.7(3) yes . . . C(8) C(7) N(2) 121.6(3) yes . . . C(12) C(7) N(2) 117.7(3) yes . . . C(9) C(8) C(2) 119.3(3) yes . . . C(9) C(8) C(7) 117.5(3) yes . . . C(2) C(8) C(7) 123.0(3) yes . . . C(10) C(9) H(5) 119.5(4) no . . . C(10) C(9) C(8) 121.3(4) yes . . . H(5) C(9) C(8) 119.1(4) no . . . C(11) C(10) H(6) 119.6(5) no . . . C(11) C(10) C(9) 120.1(4) yes . . . H(6) C(10) C(9) 120.3(5) no . . . C(12) C(11) H(7) 119.9(5) no . . . C(12) C(11) C(10) 119.9(4) yes . . . H(7) C(11) C(10) 120.2(5) no . . . H(8) C(12) C(7) 119.6(4) no . . . H(8) C(12) C(11) 120.1(4) no . . . C(7) C(12) C(11) 120.4(4) yes . . . C(14) C(13) H(11) 109.2(4) no . . . C(14) C(13) H(12) 108.2(4) no . . . C(14) C(13) N(1) 112.5(3) yes . . . H(11) C(13) H(12) 109.5(5) no . . . H(11) C(13) N(1) 108.7(4) no . . . H(12) C(13) N(1) 108.7(4) no . . . C(15) C(14) C(23) 119.2(4) yes . . . C(15) C(14) C(13) 119.1(4) yes . . . C(23) C(14) C(13) 121.7(3) yes . . . C(16) C(15) H(15) 119.6(5) no . . . C(16) C(15) C(14) 121.5(4) yes . . . H(15) C(15) C(14) 118.8(5) no . . . C(17) C(16) H(16) 119.7(6) no . . . C(17) C(16) C(15) 120.5(5) yes . . . H(16) C(16) C(15) 119.8(5) no . . . C(18) C(17) H(17) 119.1(6) no . . . C(18) C(17) C(16) 120.6(4) yes . . . H(17) C(17) C(16) 120.3(6) no . . . C(19) C(18) C(23) 119.6(4) yes . . . C(19) C(18) C(17) 120.7(4) yes . . . C(23) C(18) C(17) 119.7(4) yes . . . C(20) C(19) H(18) 120.0(6) no . . . C(20) C(19) C(18) 120.6(5) yes . . . H(18) C(19) C(18) 119.4(6) no . . . C(21) C(20) H(19) 119.6(7) no . . . C(21) C(20) C(19) 120.5(5) yes . . . H(19) C(20) C(19) 119.9(6) no . . . C(22) C(21) H(20) 119.6(6) no . . . C(22) C(21) C(20) 120.9(5) yes . . . H(20) C(21) C(20) 119.5(6) no . . . C(23) C(22) H(21) 119.5(5) no . . . C(23) C(22) C(21) 120.4(4) yes . . . H(21) C(22) C(21) 120.1(5) no . . . C(14) C(23) C(18) 118.4(4) yes . . . C(14) C(23) C(22) 123.7(3) yes . . . C(18) C(23) C(22) 118.0(4) yes . . . C(25) C(24) H(13) 108.7(4) no . . . C(25) C(24) H(14) 109.1(4) no . . . C(25) C(24) N(2) 111.9(3) yes . . . H(13) C(24) H(14) 109.5(4) no . . . H(13) C(24) N(2) 108.4(4) no . . . H(14) C(24) N(2) 109.3(4) no . . . C(26) C(25) C(34) 119.8(3) yes . . . C(26) C(25) C(24) 119.3(3) yes . . . C(34) C(25) C(24) 120.9(3) yes . . . C(27) C(26) H(22) 119.5(5) no . . . C(27) C(26) C(25) 121.3(4) yes . . . H(22) C(26) C(25) 119.2(5) no . . . C(28) C(27) H(23) 119.5(6) no . . . C(28) C(27) C(26) 120.2(5) yes . . . H(23) C(27) C(26) 120.4(6) no . . . C(29) C(28) H(24) 119.0(6) no . . . C(29) C(28) C(27) 121.2(4) yes . . . H(24) C(28) C(27) 119.7(6) no . . . C(30) C(29) C(34) 118.7(4) yes . . . C(30) C(29) C(28) 122.2(4) yes . . . C(34) C(29) C(28) 119.1(4) yes . . . C(31) C(30) H(25) 119.7(6) no . . . C(31) C(30) C(29) 121.4(5) yes . . . H(25) C(30) C(29) 118.9(7) no . . . C(32) C(31) H(26) 120.5(7) no . . . C(32) C(31) C(30) 120.1(5) yes . . . H(26) C(31) C(30) 119.4(7) no . . . C(33) C(32) H(27) 119.9(6) no . . . C(33) C(32) C(31) 120.9(5) yes . . . H(27) C(32) C(31) 119.2(6) no . . . C(34) C(33) H(28) 119.2(5) no . . . C(34) C(33) C(32) 120.9(4) yes . . . H(28) C(33) C(32) 120.0(5) no . . . C(25) C(34) C(29) 118.4(4) yes . . . C(25) C(34) C(33) 123.6(3) yes . . . C(29) C(34) C(33) 118.0(3) 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 Cl(1) Pd(1) N(1) C(1) 137.9(2) yes . . . . Cl(1) Pd(1) N(1) C(13) -85.7(2) yes . . . . Cl(1) Pd(1) N(1) H(9) 26.1(3) no . . . . N(2) Pd(1) N(1) C(1) -42.3(2) yes . . . . N(2) Pd(1) N(1) C(13) 94.1(2) yes . . . . N(2) Pd(1) N(1) H(9) -154.1(3) no . . . . Cl(2) Pd(1) N(2) C(7) 137.8(2) yes . . . . Cl(2) Pd(1) N(2) C(24) -85.4(2) yes . . . . Cl(2) Pd(1) N(2) H(10) 25.7(2) no . . . . N(1) Pd(1) N(2) C(7) -42.9(2) yes . . . . N(1) Pd(1) N(2) C(24) 93.9(2) yes . . . . N(1) Pd(1) N(2) H(10) -155.1(2) no . . . . Pd(1) N(1) C(1) C(2) 73.8(4) yes . . . . Pd(1) N(1) C(1) C(6) -105.8(3) yes . . . . C(13) N(1) C(1) C(2) -62.6(4) yes . . . . C(13) N(1) C(1) C(6) 117.8(3) yes . . . . H(9) N(1) C(1) C(2) -174.3(3) no . . . . H(9) N(1) C(1) C(6) 6.1(4) no . . . . Pd(1) N(1) C(13) C(14) 163.7(3) yes . . . . Pd(1) N(1) C(13) H(11) -75.2(4) no . . . . Pd(1) N(1) C(13) H(12) 43.9(5) no . . . . C(1) N(1) C(13) C(14) -60.0(4) yes . . . . C(1) N(1) C(13) H(11) 61.1(5) no . . . . C(1) N(1) C(13) H(12) -179.8(36) no . . . . H(9) N(1) C(13) C(14) 51.8(4) no . . . . H(9) N(1) C(13) H(11) 172.9(4) no . . . . H(9) N(1) C(13) H(12) -68.0(5) no . . . . Pd(1) N(2) C(7) C(8) 71.7(3) yes . . . . Pd(1) N(2) C(7) C(12) -109.3(3) yes . . . . C(24) N(2) C(7) C(8) -65.5(4) yes . . . . C(24) N(2) C(7) C(12) 113.5(3) yes . . . . H(10) N(2) C(7) C(8) -176.3(3) no . . . . H(10) N(2) C(7) C(12) 2.7(4) no . . . . Pd(1) N(2) C(24) C(25) 168.2(2) yes . . . . Pd(1) N(2) C(24) H(13) -71.9(4) no . . . . Pd(1) N(2) C(24) H(14) 47.3(4) no . . . . C(7) N(2) C(24) C(25) -54.3(4) yes . . . . C(7) N(2) C(24) H(13) 65.5(4) no . . . . C(7) N(2) C(24) H(14) -175.3(4) no . . . . H(10) N(2) C(24) C(25) 56.9(4) no . . . . H(10) N(2) C(24) H(13) 176.7(4) no . . . . H(10) N(2) C(24) H(14) -64.1(5) no . . . . N(1) C(1) C(2) C(3) 177.1(3) yes . . . . N(1) C(1) C(2) C(8) -2.8(5) yes . . . . C(6) C(1) C(2) C(3) -3.3(5) yes . . . . C(6) C(1) C(2) C(8) 176.8(3) yes . . . . N(1) C(1) C(6) C(5) -179.7(3) yes . . . . N(1) C(1) C(6) H(4) 0.2(6) no . . . . C(2) C(1) C(6) C(5) 0.7(5) yes . . . . C(2) C(1) C(6) H(4) -179.5(4) no . . . . C(1) C(2) C(3) C(4) 3.1(5) yes . . . . C(1) C(2) C(3) H(1) -176.1(4) no . . . . C(8) C(2) C(3) C(4) -177.0(3) yes . . . . C(8) C(2) C(3) H(1) 3.8(6) no . . . . C(1) C(2) C(8) C(7) -59.0(5) yes . . . . C(1) C(2) C(8) C(9) 124.7(4) yes . . . . C(3) C(2) C(8) C(7) 121.1(4) yes . . . . C(3) C(2) C(8) C(9) -55.2(4) yes . . . . C(2) C(3) C(4) C(5) -0.1(6) yes . . . . C(2) C(3) C(4) H(2) 178.7(5) no . . . . H(1) C(3) C(4) C(5) 179.0(5) no . . . . H(1) C(3) C(4) H(2) -2.1(8) no . . . . C(3) C(4) C(5) C(6) -2.6(6) yes . . . . C(3) C(4) C(5) H(3) 177.9(5) no . . . . H(2) C(4) C(5) C(6) 178.5(5) no . . . . H(2) C(4) C(5) H(3) -0.9(8) no . . . . C(4) C(5) C(6) C(1) 2.4(6) yes . . . . C(4) C(5) C(6) H(4) -177.5(5) no . . . . H(3) C(5) C(6) C(1) -178.2(5) no . . . . H(3) C(5) C(6) H(4) 1.9(7) no . . . . N(2) C(7) C(8) C(2) 0.1(5) yes . . . . N(2) C(7) C(8) C(9) 176.5(3) yes . . . . C(12) C(7) C(8) C(2) -178.9(3) yes . . . . C(12) C(7) C(8) C(9) -2.5(5) yes . . . . N(2) C(7) C(12) C(11) -178.9(3) yes . . . . N(2) C(7) C(12) H(8) 0.5(6) no . . . . C(8) C(7) C(12) C(11) 0.1(5) yes . . . . C(8) C(7) C(12) H(8) 179.6(4) no . . . . C(2) C(8) C(9) C(10) 179.2(4) yes . . . . C(2) C(8) C(9) H(5) -1.9(6) no . . . . C(7) C(8) C(9) C(10) 2.7(6) yes . . . . C(7) C(8) C(9) H(5) -178.4(5) no . . . . C(8) C(9) C(10) C(11) -0.4(7) yes . . . . C(8) C(9) C(10) H(6) -179.1(5) no . . . . H(5) C(9) C(10) C(11) -179.4(5) no . . . . H(5) C(9) C(10) H(6) 1.9(8) no . . . . C(9) C(10) C(11) C(12) -2.1(7) yes . . . . C(9) C(10) C(11) H(7) 176.6(5) no . . . . H(6) C(10) C(11) C(12) 176.6(5) no . . . . H(6) C(10) C(11) H(7) -4.7(9) no . . . . C(10) C(11) C(12) C(7) 2.3(6) yes . . . . C(10) C(11) C(12) H(8) -177.2(5) no . . . . H(7) C(11) C(12) C(7) -176.4(5) no . . . . H(7) C(11) C(12) H(8) 4.1(8) no . . . . N(1) C(13) C(14) C(15) 91.1(5) yes . . . . N(1) C(13) C(14) C(23) -87.7(4) yes . . . . H(11) C(13) C(14) C(15) -29.7(6) no . . . . H(11) C(13) C(14) C(23) 151.5(4) no . . . . H(12) C(13) C(14) C(15) -148.8(5) no . . . . H(12) C(13) C(14) C(23) 32.4(6) no . . . . C(13) C(14) C(15) C(16) -178.4(4) yes . . . . C(13) C(14) C(15) H(15) 2.7(7) no . . . . C(23) C(14) C(15) C(16) 0.4(6) yes . . . . C(23) C(14) C(15) H(15) -178.5(5) no . . . . C(13) C(14) C(23) C(18) -178.5(4) yes . . . . C(13) C(14) C(23) C(22) 0.7(6) yes . . . . C(15) C(14) C(23) C(18) 2.6(6) yes . . . . C(15) C(14) C(23) C(22) -178.1(4) yes . . . . C(14) C(15) C(16) C(17) -2.1(8) yes . . . . C(14) C(15) C(16) H(16) 176.8(6) no . . . . H(15) C(15) C(16) C(17) 176.8(6) no . . . . H(15) C(15) C(16) H(16) -4.4(9) no . . . . C(15) C(16) C(17) C(18) 0.5(8) yes . . . . C(15) C(16) C(17) H(17) -179.8(36) no . . . . H(16) C(16) C(17) C(18) -178.3(6) no . . . . H(16) C(16) C(17) H(17) 1.4(10) no . . . . C(16) C(17) C(18) C(19) -178.4(5) yes . . . . C(16) C(17) C(18) C(23) 2.6(7) yes . . . . H(17) C(17) C(18) C(19) 1.9(9) no . . . . H(17) C(17) C(18) C(23) -177.1(6) no . . . . C(17) C(18) C(19) C(20) -178.0(5) yes . . . . C(17) C(18) C(19) H(18) 0.5(9) no . . . . C(23) C(18) C(19) C(20) 1.1(8) yes . . . . C(23) C(18) C(19) H(18) 179.6(6) no . . . . C(17) C(18) C(23) C(14) -4.1(6) yes . . . . C(17) C(18) C(23) C(22) 176.6(4) yes . . . . C(19) C(18) C(23) C(14) 176.8(4) yes . . . . C(19) C(18) C(23) C(22) -2.5(6) yes . . . . C(18) C(19) C(20) C(21) 1.2(9) yes . . . . C(18) C(19) C(20) H(19) -177.0(7) no . . . . H(18) C(19) C(20) C(21) -177.3(7) no . . . . H(18) C(19) C(20) H(19) 4.6(11) no . . . . C(19) C(20) C(21) C(22) -2.1(9) yes . . . . C(19) C(20) C(21) H(20) 176.8(7) no . . . . H(19) C(20) C(21) C(22) 176.1(7) no . . . . H(19) C(20) C(21) H(20) -5.0(11) no . . . . C(20) C(21) C(22) C(23) 0.6(7) yes . . . . C(20) C(21) C(22) H(21) -178.8(6) no . . . . H(20) C(21) C(22) C(23) -178.3(6) no . . . . H(20) C(21) C(22) H(21) 2.3(9) no . . . . C(21) C(22) C(23) C(14) -177.6(4) yes . . . . C(21) C(22) C(23) C(18) 1.6(6) yes . . . . H(21) C(22) C(23) C(14) 1.8(7) no . . . . H(21) C(22) C(23) C(18) -179.0(5) no . . . . N(2) C(24) C(25) C(26) 99.4(4) yes . . . . N(2) C(24) C(25) C(34) -78.5(4) yes . . . . H(13) C(24) C(25) C(26) -20.3(5) no . . . . H(13) C(24) C(25) C(34) 161.9(4) no . . . . H(14) C(24) C(25) C(26) -139.5(4) no . . . . H(14) C(24) C(25) C(34) 42.6(5) no . . . . C(24) C(25) C(26) C(27) -177.3(4) yes . . . . C(24) C(25) C(26) H(22) 2.5(6) no . . . . C(34) C(25) C(26) C(27) 0.6(6) yes . . . . C(34) C(25) C(26) H(22) -179.6(4) no . . . . C(24) C(25) C(34) C(29) 177.8(3) yes . . . . C(24) C(25) C(34) C(33) -4.5(5) yes . . . . C(26) C(25) C(34) C(29) -0.1(5) yes . . . . C(26) C(25) C(34) C(33) 177.6(4) yes . . . . C(25) C(26) C(27) C(28) -0.2(7) yes . . . . C(25) C(26) C(27) H(23) -179.3(5) no . . . . H(22) C(26) C(27) C(28) -179.9(88) no . . . . H(22) C(26) C(27) H(23) 0.9(8) no . . . . C(26) C(27) C(28) C(29) -0.8(7) yes . . . . C(26) C(27) C(28) H(24) 178.0(6) no . . . . H(23) C(27) C(28) C(29) 178.4(5) no . . . . H(23) C(27) C(28) H(24) -2.8(9) no . . . . C(27) C(28) C(29) C(30) -177.9(5) yes . . . . C(27) C(28) C(29) C(34) 1.3(6) yes . . . . H(24) C(28) C(29) C(30) 3.3(8) no . . . . H(24) C(28) C(29) C(34) -177.5(5) no . . . . C(28) C(29) C(30) C(31) 177.8(5) yes . . . . C(28) C(29) C(30) H(25) -2.5(9) no . . . . C(34) C(29) C(30) C(31) -1.3(7) yes . . . . C(34) C(29) C(30) H(25) 178.4(6) no . . . . C(28) C(29) C(34) C(25) -0.8(5) yes . . . . C(28) C(29) C(34) C(33) -178.7(4) yes . . . . C(30) C(29) C(34) C(25) 178.3(3) yes . . . . C(30) C(29) C(34) C(33) 0.5(5) yes . . . . C(29) C(30) C(31) C(32) 1.2(9) yes . . . . C(29) C(30) C(31) H(26) -179.0(7) no . . . . H(25) C(30) C(31) C(32) -178.5(7) no . . . . H(25) C(30) C(31) H(26) 1.3(11) no . . . . C(30) C(31) C(32) C(33) -0.2(8) yes . . . . C(30) C(31) C(32) H(27) 179.5(7) no . . . . H(26) C(31) C(32) C(33) -180.0(88) no . . . . H(26) C(31) C(32) H(27) -0.3(11) no . . . . C(31) C(32) C(33) C(34) -0.7(7) yes . . . . C(31) C(32) C(33) H(28) 179.8(36) no . . . . H(27) C(32) C(33) C(34) 179.7(6) no . . . . H(27) C(32) C(33) H(28) 0.1(9) no . . . . C(32) C(33) C(34) C(25) -177.3(4) yes . . . . C(32) C(33) C(34) C(29) 0.5(6) yes . . . . H(28) C(33) C(34) C(25) 2.3(7) no . . . . H(28) C(33) C(34) C(29) -180.0(88) no . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 C(10) H(4) 3.508(6) no . 65501 C(11) H(14) 3.392(5) no . 65501 C(14) H(27) 3.201(6) no . 55504 C(18) H(27) 3.377(7) no . 55504 C(22) H(27) 3.290(7) no . 55504 C(23) H(27) 2.970(6) no . 55504 H(6) Pd(1) 3.459(4) no . 65501 H(6) C(1) 3.317(5) no . 65501 H(6) C(5) 3.442(6) no . 65501 H(6) C(6) 2.913(6) no . 65501 H(6) C(24) 3.481(6) no . 65501 H(7) Pd(1) 3.304(4) no . 65501 H(7) Cl(2) 2.971(4) no . 65501 H(7) C(24) 3.552(5) no . 65501 #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== data_43 _database_code_depnum_ccdc_archive 'CCDC 277176' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common DB-DABP-Pt-DABNTf _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H19 Cl1.50 F3 N2 O3 Pd0.50 S' _chemical_formula_weight 590.86 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' Cl Cl 0.1484 0.1585 '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' 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4(3)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y+1/2, x+1/2, z+3/4' '-x, -y, z+1/2' 'y+1/2, -x+1/2, z+1/4' 'x+1/2, -y+1/2, -z+1/4' 'y, x, -z' '-x+1/2, y+1/2, -z+3/4' '-y, -x, -z+1/2' _cell_length_a 12.3252(5) _cell_length_b 12.3252(5) _cell_length_c 33.675(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5115.6(5) _cell_formula_units_Z 8 _cell_measurement_temperature 90 _cell_measurement_reflns_used 9015 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 27.83 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.534 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2388 _exptl_absorpt_coefficient_mu 0.676 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8129 _exptl_absorpt_correction_T_max 0.8881 _exptl_absorpt_process_details ; SADABS Sheldrick 1996 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 90 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.333 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 51634 _diffrn_reflns_av_R_equivalents 0.0628 _diffrn_reflns_av_sigmaI/netI 0.0271 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 25.34 _reflns_number_total 4678 _reflns_number_gt 4638 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0677P)^2^+51.5569P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.06(7) _refine_ls_number_reflns 4678 _refine_ls_number_parameters 323 _refine_ls_number_restraints 277 _refine_ls_R_factor_all 0.0750 _refine_ls_R_factor_gt 0.0745 _refine_ls_wR_factor_ref 0.1864 _refine_ls_wR_factor_gt 0.1860 _refine_ls_goodness_of_fit_ref 1.179 _refine_ls_restrained_S_all 1.204 _refine_ls_shift/su_max 0.003 _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 C1 C 0.7930(7) 0.5826(7) 0.2351(2) 0.0205(11) Uani 1 1 d U . . C2 C 0.6828(6) 0.3389(6) 0.2956(2) 0.0150(10) Uani 1 1 d U . . C3 C 0.7193(6) 0.2576(6) 0.2715(2) 0.0143(11) Uani 1 1 d U . . C4 C 0.7304(6) 0.1502(7) 0.2874(2) 0.0168(10) Uani 1 1 d U . . C5 C 0.7622(6) 0.0600(7) 0.2634(3) 0.0189(12) Uani 1 1 d U . . H5 H 0.7775 0.0706 0.2361 0.023 Uiso 1 1 calc R . . C6 C 0.7709(7) -0.0409(7) 0.2794(3) 0.0215(12) Uani 1 1 d U . . H6 H 0.7949 -0.0997 0.2635 0.026 Uiso 1 1 calc R . . C7 C 0.7441(7) -0.0588(7) 0.3200(3) 0.0238(12) Uani 1 1 d U . . H7 H 0.7477 -0.1300 0.3307 0.029 Uiso 1 1 calc R . . C8 C 0.7133(7) 0.0252(8) 0.3434(3) 0.0227(12) Uani 1 1 d U . . H8 H 0.6969 0.0124 0.3706 0.027 Uiso 1 1 calc R . . C9 C 0.7053(7) 0.1319(7) 0.3280(2) 0.0191(10) Uani 1 1 d U . . C10 C 0.6712(7) 0.2192(7) 0.3518(2) 0.0196(12) Uani 1 1 d U . . H10 H 0.6562 0.2073 0.3792 0.024 Uiso 1 1 calc R . . C11 C 0.6595(6) 0.3204(6) 0.3362(2) 0.0177(11) Uani 1 1 d U . . H11 H 0.6356 0.3785 0.3526 0.021 Uiso 1 1 calc R . . C12 C 0.4165(8) 0.5704(7) 0.1789(3) 0.0257(12) Uani 1 1 d U . . H12 H 0.4830 0.5393 0.1669 0.031 Uiso 1 1 calc R . . H13 H 0.4328 0.6459 0.1869 0.031 Uiso 1 1 calc R . . C1A C 0.3274(5) 0.5714(5) 0.1483(2) 0.0372(13) Uani 1 1 d GU . . C2A C 0.3025(6) 0.4754(5) 0.1286(2) 0.0376(14) Uani 1 1 d GU . . H2A H 0.3456 0.4125 0.1328 0.045 Uiso 1 1 calc R . . C3A C 0.2146(6) 0.4714(5) 0.1028(2) 0.0462(16) Uani 1 1 d GU . . H3A H 0.1976 0.4058 0.0894 0.055 Uiso 1 1 calc R . . C4A C 0.1516(6) 0.5634(6) 0.0966(2) 0.0572(17) Uani 1 1 d GU . . H4A H 0.0916 0.5607 0.0790 0.069 Uiso 1 1 calc R . . C5A C 0.1766(7) 0.6594(5) 0.1163(3) 0.0603(17) Uani 1 1 d GU . . H5A H 0.1335 0.7223 0.1121 0.072 Uiso 1 1 calc R . . C6A C 0.2645(7) 0.6634(5) 0.1421(2) 0.0527(16) Uani 1 1 d GU . . H6A H 0.2815 0.7290 0.1555 0.063 Uiso 1 1 calc R . . C1B C 0.2858(3) 0.5397(4) 0.23420(16) 0.0188(10) Uani 1 1 d GU . . C2B C 0.2021(4) 0.4642(3) 0.23594(13) 0.0209(12) Uani 1 1 d GU . . H2B H 0.2115 0.3942 0.2246 0.025 Uiso 1 1 calc R . . C3B C 0.1047(3) 0.4911(3) 0.25425(17) 0.0225(12) Uani 1 1 d GU . . H3B H 0.0475 0.4395 0.2554 0.027 Uiso 1 1 calc R . . C4B C 0.0909(3) 0.5935(4) 0.27081(14) 0.0224(12) Uani 1 1 d GU . . H4B H 0.0243 0.6118 0.2833 0.027 Uiso 1 1 calc R . . C5B C 0.1745(4) 0.6689(3) 0.26907(9) 0.0220(12) Uani 1 1 d GU . . H5B H 0.1651 0.7389 0.2804 0.026 Uiso 1 1 calc R . . C6B C 0.2720(3) 0.6421(3) 0.25076(16) 0.0199(12) Uani 1 1 d GU . . C1S C 0.0477(10) 0.9942(4) 0.30281(12) 0.113(3) Uani 0.695(8) 1 d PGDU A 1 H1SA H 0.1106 1.0428 0.3071 0.135 Uiso 0.695(8) 1 calc PR A 1 H1SB H -0.0186 1.0377 0.3076 0.135 Uiso 0.695(8) 1 calc PR A 1 C2S C 0.163(3) 1.0051(19) 0.2835(6) 0.113(3) Uani 0.305(8) 1 d PDU A 2 H2SA H 0.2335 1.0144 0.2698 0.135 Uiso 0.305(8) 1 calc PR A 2 H2SB H 0.1316 1.0784 0.2872 0.135 Uiso 0.305(8) 1 calc PR A 2 Cl1S Cl 0.0479(5) 0.9521(5) 0.2500 0.113(3) Uani 0.695(8) 2 d SPDU A 1 Cl2S Cl 0.0531(6) 0.8857(7) 0.34083(19) 0.104(2) Uani 0.695(8) 1 d PDU A 1 Cl3S Cl 0.1898(14) 0.9472(16) 0.3333(3) 0.113(3) Uani 0.305(8) 1 d PDU A 2 Cl4S Cl 0.0720(13) 0.9280(13) 0.2500 0.114(3) Uani 0.305(8) 2 d SPDU A 2 F1 F 0.7052(4) 0.6061(5) 0.21394(16) 0.0315(12) Uani 1 1 d U . . F2 F 0.8522(4) 0.6720(4) 0.23773(15) 0.0255(11) Uani 1 1 d U . . F3 F 0.8492(4) 0.5090(4) 0.21505(14) 0.0267(11) Uani 1 1 d U . . N1 N 0.3865(5) 0.5055(5) 0.2150(2) 0.0172(9) Uani 1 1 d U . . N2 N 0.6647(5) 0.4480(5) 0.28037(19) 0.0132(9) Uani 1 1 d U . . O1 O 0.7182(5) 0.6335(5) 0.30245(17) 0.0191(12) Uani 1 1 d U . . O2 O 0.8550(4) 0.4889(5) 0.30086(16) 0.0197(11) Uani 1 1 d U . . O1S O 0.943(3) 0.630(3) 0.1302(9) 0.32(2) Uani 1 1 d . . . Pd1 Pd 0.52146(4) 0.47854(4) 0.2500 0.0116(2) Uani 1 2 d SU . . S1 S 0.75766(15) 0.53426(16) 0.28519(5) 0.0144(4) Uani 1 1 d U . . 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 C1 0.021(2) 0.019(2) 0.021(2) 0.001(2) 0.001(2) -0.005(2) C2 0.011(2) 0.017(2) 0.0169(19) 0.0006(18) -0.0038(17) -0.0037(18) C3 0.009(2) 0.016(2) 0.018(2) 0.000(2) -0.0047(19) -0.0043(19) C4 0.013(2) 0.018(2) 0.019(2) 0.0008(19) -0.0060(19) -0.0033(18) C5 0.015(2) 0.020(2) 0.023(2) 0.002(2) -0.006(2) -0.001(2) C6 0.017(2) 0.020(3) 0.027(3) 0.002(2) -0.008(2) 0.000(2) C7 0.020(2) 0.022(2) 0.029(3) 0.006(2) -0.010(2) -0.002(2) C8 0.020(2) 0.023(2) 0.025(2) 0.005(2) -0.009(2) -0.004(2) C9 0.015(2) 0.020(2) 0.021(2) 0.0023(19) -0.0078(19) -0.0052(19) C10 0.015(2) 0.023(2) 0.020(2) 0.001(2) -0.005(2) -0.005(2) C11 0.015(2) 0.020(2) 0.018(2) -0.001(2) -0.003(2) -0.005(2) C12 0.032(3) 0.020(2) 0.026(2) -0.003(2) -0.007(2) -0.001(2) C1A 0.048(3) 0.028(2) 0.036(3) -0.004(2) -0.016(2) 0.005(2) C2A 0.048(3) 0.029(3) 0.036(3) -0.006(3) -0.016(3) 0.004(3) C3A 0.057(3) 0.037(3) 0.044(3) -0.008(3) -0.023(3) 0.006(3) C4A 0.069(4) 0.047(3) 0.055(3) -0.010(3) -0.029(3) 0.009(3) C5A 0.073(4) 0.048(3) 0.059(3) -0.009(3) -0.030(3) 0.011(3) C6A 0.066(3) 0.040(3) 0.052(3) -0.007(3) -0.026(3) 0.009(3) C1B 0.017(2) 0.016(2) 0.024(2) 0.0019(19) -0.0020(19) -0.0027(19) C2B 0.017(2) 0.018(2) 0.028(2) 0.001(2) -0.001(2) -0.006(2) C3B 0.017(2) 0.018(3) 0.032(3) 0.001(2) 0.000(2) -0.004(2) C4B 0.017(2) 0.017(2) 0.033(3) -0.001(2) -0.001(2) -0.003(2) C5B 0.017(2) 0.017(2) 0.032(3) -0.002(2) -0.003(2) -0.002(2) C6B 0.015(2) 0.016(2) 0.028(2) 0.001(2) -0.005(2) -0.002(2) C1S 0.117(4) 0.119(4) 0.101(4) 0.026(3) 0.028(3) 0.074(4) C2S 0.117(4) 0.119(4) 0.102(4) 0.026(3) 0.028(3) 0.075(5) Cl1S 0.118(4) 0.118(4) 0.103(4) 0.030(3) 0.030(3) 0.078(4) Cl2S 0.111(4) 0.123(4) 0.077(3) -0.001(3) 0.019(3) 0.061(4) Cl3S 0.117(5) 0.125(5) 0.096(5) 0.009(5) 0.019(5) 0.065(5) Cl4S 0.119(4) 0.119(4) 0.103(4) 0.029(3) 0.029(3) 0.075(5) F1 0.026(3) 0.038(3) 0.030(3) 0.015(2) -0.010(2) -0.010(2) F2 0.030(3) 0.016(2) 0.031(3) 0.0028(19) 0.003(2) -0.009(2) F3 0.036(3) 0.021(3) 0.023(2) -0.003(2) 0.009(2) -0.005(2) N1 0.0174(18) 0.0148(19) 0.0195(18) -0.0003(17) -0.0035(16) -0.0019(16) N2 0.0115(16) 0.0134(17) 0.0146(16) 0.0008(15) -0.0021(15) -0.0007(15) O1 0.015(3) 0.018(3) 0.024(3) -0.005(2) -0.003(2) -0.006(2) O2 0.017(2) 0.019(3) 0.024(3) -0.001(2) -0.002(2) -0.003(2) O1S 0.29(3) 0.38(4) 0.30(3) 0.25(3) 0.18(3) 0.16(3) Pd1 0.0110(2) 0.0110(2) 0.0127(3) -0.0019(2) -0.0019(2) -0.0020(3) S1 0.0138(8) 0.0142(9) 0.0151(8) -0.0004(7) -0.0003(7) -0.0023(7) _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 C1 F2 1.324(9) . ? C1 F3 1.327(10) . ? C1 F1 1.328(10) . ? C1 S1 1.840(9) . ? C2 C3 1.367(11) . ? C2 C11 1.415(11) . ? C2 N2 1.457(10) . ? C3 C4 1.433(11) . ? C3 C3 1.505(15) 8_665 ? C4 C9 1.419(12) . ? C4 C5 1.429(12) . ? C5 C6 1.359(12) . ? C5 H5 0.9500 . ? C6 C7 1.422(13) . ? C6 H6 0.9500 . ? C7 C8 1.356(13) . ? C7 H7 0.9500 . ? C8 C9 1.418(13) . ? C8 H8 0.9500 . ? C9 C10 1.406(12) . ? C10 C11 1.361(12) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 N1 1.504(11) . ? C12 C1A 1.506(10) . ? C12 H12 0.9900 . ? C12 H13 0.9900 . ? C1A C2A 1.3900 . ? C1A C6A 1.3900 . ? C2A C3A 1.3900 . ? C2A H2A 0.9500 . ? C3A C4A 1.3900 . ? C3A H3A 0.9500 . ? C4A C5A 1.3900 . ? C4A H4A 0.9500 . ? C5A C6A 1.3900 . ? C5A H5A 0.9500 . ? C6A H6A 0.9500 . ? C1B C2B 1.3900 . ? C1B C6B 1.3900 . ? C1B N1 1.461(7) . ? C2B C3B 1.3900 . ? C2B H2B 0.9500 . ? C3B C4B 1.3900 . ? C3B H3B 0.9500 . ? C4B C5B 1.3900 . ? C4B H4B 0.9500 . ? C5B C6B 1.3900 . ? C5B H5B 0.9500 . ? C6B C6B 1.499(6) 8_665 ? C1S Cl2S 1.853(4) . ? C1S Cl1S 1.853(4) . ? C1S H1SA 0.9900 . ? C1S H1SB 0.9900 . ? C2S Cl3S 1.852(4) . ? C2S Cl4S 1.853(4) . ? C2S H2SA 0.9900 . ? C2S H2SB 0.9900 . ? Cl1S C1S 1.853(5) 8_665 ? Cl4S C2S 1.852(5) 8_665 ? N1 Pd1 2.065(6) . ? N2 S1 1.571(7) . ? N2 Pd1 2.075(6) . ? O1 S1 1.439(6) . ? O2 S1 1.425(6) . ? Pd1 N1 2.065(6) 8_665 ? Pd1 N2 2.075(6) 8_665 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F2 C1 F3 108.4(7) . . ? F2 C1 F1 107.7(7) . . ? F3 C1 F1 107.5(7) . . ? F2 C1 S1 109.8(6) . . ? F3 C1 S1 111.6(6) . . ? F1 C1 S1 111.7(6) . . ? C3 C2 C11 121.5(7) . . ? C3 C2 N2 121.2(7) . . ? C11 C2 N2 117.3(7) . . ? C2 C3 C4 119.1(7) . . ? C2 C3 C3 119.7(6) . 8_665 ? C4 C3 C3 121.1(6) . 8_665 ? C9 C4 C5 118.7(8) . . ? C9 C4 C3 119.0(7) . . ? C5 C4 C3 122.3(7) . . ? C6 C5 C4 120.7(8) . . ? C6 C5 H5 119.7 . . ? C4 C5 H5 119.7 . . ? C5 C6 C7 120.3(8) . . ? C5 C6 H6 119.9 . . ? C7 C6 H6 119.9 . . ? C8 C7 C6 120.4(8) . . ? C8 C7 H7 119.8 . . ? C6 C7 H7 119.8 . . ? C7 C8 C9 120.9(8) . . ? C7 C8 H8 119.5 . . ? C9 C8 H8 119.5 . . ? C10 C9 C8 121.4(8) . . ? C10 C9 C4 119.6(8) . . ? C8 C9 C4 119.1(8) . . ? C11 C10 C9 120.8(8) . . ? C11 C10 H10 119.6 . . ? C9 C10 H10 119.6 . . ? C10 C11 C2 120.0(8) . . ? C10 C11 H11 120.0 . . ? C2 C11 H11 120.0 . . ? N1 C12 C1A 112.3(7) . . ? N1 C12 H12 109.1 . . ? C1A C12 H12 109.1 . . ? N1 C12 H13 109.1 . . ? C1A C12 H13 109.1 . . ? H12 C12 H13 107.9 . . ? C2A C1A C6A 120.0 . . ? C2A C1A C12 118.7(5) . . ? C6A C1A C12 121.1(5) . . ? C1A C2A C3A 120.0 . . ? C1A C2A H2A 120.0 . . ? C3A C2A H2A 120.0 . . ? C4A C3A C2A 120.0 . . ? C4A C3A H3A 120.0 . . ? C2A C3A H3A 120.0 . . ? C3A C4A C5A 120.0 . . ? C3A C4A H4A 120.0 . . ? C5A C4A H4A 120.0 . . ? C6A C5A C4A 120.0 . . ? C6A C5A H5A 120.0 . . ? C4A C5A H5A 120.0 . . ? C5A C6A C1A 120.0 . . ? C5A C6A H6A 120.0 . . ? C1A C6A H6A 120.0 . . ? C2B C1B C6B 120.0 . . ? C2B C1B N1 117.1(4) . . ? C6B C1B N1 122.9(4) . . ? C3B C2B C1B 120.0 . . ? C3B C2B H2B 120.0 . . ? C1B C2B H2B 120.0 . . ? C2B C3B C4B 120.0 . . ? C2B C3B H3B 120.0 . . ? C4B C3B H3B 120.0 . . ? C5B C4B C3B 120.0 . . ? C5B C4B H4B 120.0 . . ? C3B C4B H4B 120.0 . . ? C6B C5B C4B 120.0 . . ? C6B C5B H5B 120.0 . . ? C4B C5B H5B 120.0 . . ? C5B C6B C1B 120.0 . . ? C5B C6B C6B 117.2(3) . 8_665 ? C1B C6B C6B 122.8(4) . 8_665 ? Cl2S C1S Cl1S 117.4(4) . . ? Cl2S C1S H1SA 107.9 . . ? Cl1S C1S H1SA 107.9 . . ? Cl2S C1S H1SB 107.9 . . ? Cl1S C1S H1SB 107.9 . . ? H1SA C1S H1SB 107.2 . . ? Cl3S C2S Cl4S 117.5(4) . . ? Cl3S C2S H2SA 107.9 . . ? Cl4S C2S H2SA 107.9 . . ? Cl3S C2S H2SB 107.9 . . ? Cl4S C2S H2SB 107.9 . . ? H2SA C2S H2SB 107.2 . . ? C1S Cl1S C1S 157.0(7) . 8_665 ? C2S Cl4S C2S 173(3) 8_665 . ? C1B N1 C12 114.4(6) . . ? C1B N1 Pd1 118.6(4) . . ? C12 N1 Pd1 110.4(5) . . ? C2 N2 S1 118.4(5) . . ? C2 N2 Pd1 118.2(5) . . ? S1 N2 Pd1 123.3(4) . . ? N1 Pd1 N1 93.8(4) . 8_665 ? N1 Pd1 N2 90.1(3) . 8_665 ? N1 Pd1 N2 174.7(3) 8_665 8_665 ? N1 Pd1 N2 174.7(3) . . ? N1 Pd1 N2 90.1(3) 8_665 . ? N2 Pd1 N2 86.2(4) 8_665 . ? O2 S1 O1 118.0(3) . . ? O2 S1 N2 112.7(3) . . ? O1 S1 N2 111.7(3) . . ? O2 S1 C1 105.5(4) . . ? O1 S1 C1 100.1(4) . . ? N2 S1 C1 107.3(4) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.34 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.730 _refine_diff_density_min -1.733 _refine_diff_density_rms 0.162