Supplementary Material (ESI) for Chemical Communications This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _audit_creation_date 2006-08-17 _audit_creation_method 'by CrystalStructure 3.6.0' _audit_update_record ? #============================================================================== # SUBMISSION DETAILS _publ_contact_author_name 'Dr. H. L. Kwong' _publ_contact_author_email bhhoik@cityu.edu.hk _publ_contact_author_fax '(852) 2788 7406' _publ_contact_author_phone '(852) 2788-7304' _publ_contact_author_address ; Department of Biology and Chemistry, City University of Hong Kong, 83 Tat Chee Avenue, Kowloon Tong, Hong Kong ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_category ? # 'CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? #============================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; Stereoselective formation of a single-stranded helicate: Structure of a bis(Palladium-allyl)quaterpyridine complex and its use in catalytic enantioselective allylic substitution ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Hoi Lun Kwong' . ; Department of Biology and Chemistry, City University of Hong Kong, 83 Tat Chee Avenue, Kowloon Tong, Hong Kong ; 'Ho-Lun Yeung' . ; Department of Biology and Chemistry, City University of Hong Kong, 83 Tat Chee Avenue, Kowloon Tong, Hong Kong ; 'Wing-Sze Lee' . ; Department of Biology and Chemistry, City University of Hong Kong, 83 Tat Chee Avenue, Kowloon Tong, Hong Kong ; 'Wing-Tak Wong' . ; Department of Chemistry The University of Hong Kong Pokfulam Road, Pokfulam, Hong Kong SAR, P. R. CHINA ; _publ_section_references ; Beurskens, P.T., Admiraal, G., Beurskens, G., Bosman, W.P., de Gelder, R., Israel, R. and Smits, J.M.M. (1999). The DIRDIF-99 program system, Technical Report of the Crystallography Laboratory, University of Nijmegen, The Netherlands. Bruker AXS Inc. (1998). SMART version 5.054, Madison, Wisconsin, USA. Bruker AXS Inc. (1999). SAINT, version 6.02, Madison, Wisconsin, USA. Flack, H.D. (1983). Acta Cryst. A39, 876-881. Johnson, C. K. (1976). ORTEP-II, A FORTRAN Thermal-Ellipsoid Plot Program, Report ORNL-5138, Oak Ridge National Laboratory, Oak Ridge, Tennessee, USA. Rigaku/MSC & Rigaku Corporation. (2003). CrystalStructure. Single Crystal Structure Analysis Software. Version 3.5.1. Rigaku/MSC, 9009 New Trails Drive, The Woodlands, TX, USA 77381-5209. Rigaku, 3-9-12 Akishima, Tokyo 196-8666, Japan. Sheldrick, G.M. (1997). SADABS & SHELXS97. G\"ottingen University, G\"ottingen, Germany. Watkin, D.J., Prout, C.K. Carruthers, J.R. & Betteridge, P.W. (1996). CRYSTALS Issue 10, Chemical Crystallography Laboratory, Oxford, UK. ; _publ_section_exptl_refinement ; All of the non-H atoms were refined isotropically. The absolute configuration was determined based on the anomalous dispersions effects and with reference to the chirality of the starting ligand. The absolute configuration of C10, C12 and C13 were found to be R, R and S respectively. All H-atoms were placed at geometrical positions with C-H = 0.95\%A and refined using riding model, U~iso~(H) = 1.2U~eq~(C). ; #============================================================================== data__wt0787wc-OrthoP-HLKwong095 _database_code_depnum_ccdc_archive 'CCDC 610954' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C44 H50 Cl6 F12 N4 Pd2 Sb2 ' _chemical_formula_moiety 'C42 H48 N4 Pd2, 2(F6 Sb), 2(C H Cl3)' _chemical_formula_weight 1531.90 _chemical_melting_point ? _chemical_absolute_configuration rmad #'CHOOSE rm ad rmad syn or unk' #============================================================================== # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 2' _symmetry_space_group_name_Hall 'P 2 2ab' _symmetry_Int_Tables_number 18 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 1/2+X,1/2-Y,-Z 3 1/2-X,1/2+Y,-Z 4 -X,-Y,+Z #------------------------------------------------------------------------------ _cell_length_a 16.179(13) _cell_length_b 15.653(12) _cell_length_c 10.866(8) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2751.7(37) _cell_formula_units_Z 2 _cell_measurement_reflns_used 32129 _cell_measurement_theta_min 1.3 _cell_measurement_theta_max 28.5 _cell_measurement_temperature 298(1) #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.28 _exptl_crystal_density_diffrn 1.849 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1492.00 _exptl_absorpt_coefficient_mu 1.980 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.282 _exptl_absorpt_correction_T_max 0.574 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1997)' #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Bruker SMART CCD' _diffrn_measurement_method ' \w and \f scan' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 32129 _diffrn_reflns_av_R_equivalents 0.064 _diffrn_reflns_theta_max 28.55 _diffrn_measured_fraction_theta_max 0.9060 _diffrn_reflns_theta_full 28.55 _diffrn_measured_fraction_theta_full 0.9060 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement using all reflections. 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^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 6341 _reflns_number_gt 3239 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0400 _refine_ls_wR_factor_ref 0.0470 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 6341 _refine_ls_number_parameters 342 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0002Fo^2^ + 0.6\s(Fo^2^) + 0.0001]' _refine_ls_shift/su_max 0.0050 _refine_diff_density_max 1.54 _refine_diff_density_min -2.31 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack (1983). 2764 Friedel Pairs' _refine_ls_abs_structure_Flack 0.00(4) 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) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 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) ; F F 0.017 0.010 ; 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) ; Sb Sb -0.587 1.546 ; 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 Sb(2) Sb 0.39581(4) 0.25332(4) -0.03768(5) 0.0800(2) Uani 1.00 1 d . . . Pd(1) Pd 0.40617(4) 0.42009(3) 0.41587(5) 0.0541(2) Uani 1.00 1 d . . . Cl(1) Cl 0.2176(3) 0.3626(3) 0.2154(6) 0.258(3) Uani 1.00 1 d . . . Cl(2) Cl 0.1689(4) 0.2356(4) 0.3739(6) 0.309(4) Uani 1.00 1 d . . . Cl(3) Cl 0.0700(3) 0.3796(4) 0.3350(7) 0.339(4) Uani 1.00 1 d . . . F(1) F 0.2845(4) 0.2354(5) 0.0055(8) 0.184(3) Uani 1.00 1 d . . . F(2) F 0.4304(6) 0.2308(5) 0.1167(7) 0.216(4) Uani 1.00 1 d . . . F(4) F 0.5044(5) 0.2737(5) -0.0785(12) 0.265(5) Uani 1.00 1 d . . . F(5) F 0.3555(6) 0.2728(5) -0.1879(6) 0.200(4) Uani 1.00 1 d . . . F(6) F 0.3819(3) 0.3614(3) 0.0126(6) 0.134(2) Uani 1.00 1 d . . . F(7) F 0.4054(4) 0.1421(3) -0.0788(6) 0.137(2) Uani 1.00 1 d . . . N(1) N 0.4024(4) 0.5104(3) 0.2746(4) 0.048(2) Uani 1.00 1 d . . . N(2) N 0.3069(4) 0.5003(3) 0.4808(5) 0.051(2) Uani 1.00 1 d . . . C(1) C 0.4578(4) 0.5208(4) 0.1794(6) 0.048(2) Uani 1.00 1 d . . . C(2) C 0.4341(4) 0.5674(4) 0.0806(8) 0.063(2) Uani 1.00 1 d . . . C(3) C 0.3573(5) 0.6062(5) 0.0737(8) 0.065(3) Uani 1.00 1 d . . . C(4) C 0.3045(5) 0.5976(5) 0.1733(7) 0.068(3) Uani 1.00 1 d . . . C(5) C 0.3279(4) 0.5501(4) 0.2737(7) 0.052(2) Uani 1.00 1 d . . . C(6) C 0.2727(4) 0.5428(4) 0.3831(7) 0.054(2) Uani 1.00 1 d . . . C(7) C 0.1953(5) 0.5798(5) 0.3927(7) 0.071(3) Uani 1.00 1 d . . . C(8) C 0.1488(5) 0.5717(6) 0.5002(8) 0.079(3) Uani 1.00 1 d . . . C(9) C 0.1842(5) 0.5328(4) 0.6003(8) 0.063(3) Uani 1.00 1 d . . . C(10) C 0.1424(5) 0.5268(5) 0.7232(8) 0.071(3) Uani 1.00 1 d . . . C(11) C 0.2075(6) 0.5533(5) 0.8169(8) 0.081(3) Uani 1.00 1 d . . . C(12) C 0.2447(5) 0.4653(5) 0.8048(7) 0.066(3) Uani 1.00 1 d . . . C(13) C 0.3033(5) 0.4607(5) 0.6974(7) 0.058(2) Uani 1.00 1 d . . . C(14) C 0.2641(4) 0.4982(4) 0.5858(8) 0.050(2) Uani 1.00 1 d . . . C(15) C 0.1532(5) 0.4371(6) 0.7741(8) 0.079(3) Uani 1.00 1 d . . . C(16) C 0.1001(6) 0.4237(6) 0.8938(8) 0.123(4) Uani 1.00 1 d . . . C(17) C 0.1453(6) 0.3651(6) 0.6911(9) 0.099(4) Uani 1.00 1 d . . . C(18) C 0.3893(6) 0.4983(6) 0.7272(8) 0.099(4) Uani 1.00 1 d . . . C(19) C 0.4031(7) 0.3120(5) 0.5288(9) 0.113(4) Uani 1.00 1 d . . . C(20) C 0.4337(9) 0.2947(6) 0.4148(12) 0.154(6) Uani 1.00 1 d . . . C(21) C 0.4955(6) 0.3299(5) 0.3556(8) 0.081(3) Uani 1.00 1 d . . . C(22) C 0.1371(3) 0.3100(3) 0.2675(5) 0.196(8) Uani 1.00 1 d . . . H(1) H 0.4714 0.5737 0.0137 0.076 Uiso 1.00 1 c R . . H(2) H 0.3413 0.6377 0.0029 0.077 Uiso 1.00 1 c R . . H(3) H 0.2519 0.6246 0.1721 0.081 Uiso 1.00 1 c R . . H(4) H 0.1735 0.6110 0.3252 0.086 Uiso 1.00 1 c R . . H(5) H 0.0938 0.5928 0.5040 0.095 Uiso 1.00 1 c R . . H(6) H 0.0892 0.5520 0.7306 0.086 Uiso 1.00 1 c R . . H(7) H 0.2425 0.5984 0.7906 0.097 Uiso 1.00 1 c R . . H(8) H 0.1862 0.5660 0.8963 0.097 Uiso 1.00 1 c R . . H(9) H 0.2660 0.4424 0.8793 0.080 Uiso 1.00 1 c R . . H(10) H 0.3115 0.4018 0.6805 0.070 Uiso 1.00 1 c R . . H(11) H 0.1366 0.3977 0.9510 0.147 Uiso 1.00 1 c R . . H(12) H 0.0887 0.4806 0.9191 0.147 Uiso 1.00 1 c R . . H(13) H 0.0542 0.3880 0.8756 0.147 Uiso 1.00 1 c R . . H(14) H 0.0892 0.3474 0.6952 0.119 Uiso 1.00 1 c R . . H(15) H 0.1813 0.3206 0.7168 0.119 Uiso 1.00 1 c R . . H(16) H 0.1584 0.3809 0.6089 0.119 Uiso 1.00 1 c R . . H(17) H 0.3891 0.5570 0.7053 0.119 Uiso 1.00 1 c R . . H(18) H 0.4303 0.4686 0.6815 0.119 Uiso 1.00 1 c R . . H(19) H 0.3996 0.4928 0.8129 0.119 Uiso 1.00 1 c R . . H(20) H 0.4275 0.3556 0.5776 0.135 Uiso 1.00 1 c R . . H(21) H 0.3573 0.2805 0.5595 0.135 Uiso 1.00 1 c R . . H(22) H 0.4061 0.2503 0.3716 0.184 Uiso 1.00 1 c R . . H(23) H 0.5262 0.3747 0.3928 0.098 Uiso 1.00 1 c R . . H(24) H 0.5097 0.3105 0.2754 0.098 Uiso 1.00 1 c R . . H(25) H 0.1103 0.2819 0.2010 0.235 Uiso 1.00 1 c R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Sb(2) 0.0835(4) 0.0641(3) 0.0923(4) -0.0088(4) -0.0191(4) -0.0078(3) Pd(1) 0.0640(3) 0.0503(3) 0.0480(3) 0.0172(3) 0.0049(3) 0.0067(3) Cl(1) 0.197(6) 0.274(6) 0.304(7) -0.041(5) 0.074(5) -0.060(5) Cl(2) 0.403(10) 0.235(6) 0.289(8) 0.049(7) 0.095(7) -0.004(6) Cl(3) 0.236(7) 0.364(9) 0.416(10) 0.016(6) 0.025(6) -0.204(8) F(1) 0.138(6) 0.154(6) 0.260(9) -0.069(5) 0.025(6) -0.064(7) F(2) 0.329(12) 0.171(7) 0.149(6) 0.096(7) -0.140(8) -0.058(5) F(4) 0.126(6) 0.191(8) 0.48(2) -0.069(5) 0.120(8) -0.205(10) F(5) 0.344(13) 0.138(6) 0.116(5) -0.001(7) -0.048(6) 0.037(4) F(6) 0.110(5) 0.073(3) 0.219(7) -0.009(3) 0.012(5) -0.021(4) F(7) 0.170(5) 0.080(3) 0.160(5) -0.003(4) -0.014(6) -0.036(4) N(1) 0.062(4) 0.042(3) 0.040(3) -0.005(3) 0.002(4) 0.002(2) N(2) 0.055(4) 0.049(3) 0.049(4) 0.004(3) -0.004(3) 0.008(3) C(1) 0.062(5) 0.037(4) 0.045(4) -0.010(3) -0.013(4) 0.001(3) C(2) 0.075(5) 0.056(4) 0.058(4) -0.013(4) 0.002(4) -0.002(4) C(3) 0.072(5) 0.075(5) 0.047(5) 0.007(4) -0.007(4) 0.016(4) C(4) 0.061(5) 0.075(6) 0.068(5) 0.009(4) -0.005(4) 0.011(4) C(5) 0.046(5) 0.053(4) 0.059(5) 0.009(3) -0.005(4) 0.009(4) C(6) 0.052(5) 0.044(4) 0.065(5) 0.008(3) -0.005(4) 0.003(3) C(7) 0.064(5) 0.076(5) 0.074(6) 0.027(5) -0.005(5) 0.017(5) C(8) 0.055(5) 0.088(6) 0.095(7) 0.030(5) 0.012(5) 0.013(6) C(9) 0.065(5) 0.051(4) 0.073(6) 0.004(4) 0.006(5) -0.001(4) C(10) 0.060(6) 0.076(6) 0.079(6) 0.020(5) 0.030(5) 0.013(5) C(11) 0.081(6) 0.071(6) 0.090(7) 0.012(5) 0.017(5) -0.012(5) C(12) 0.061(5) 0.078(5) 0.061(5) -0.004(4) 0.004(4) -0.001(4) C(13) 0.048(5) 0.072(5) 0.055(5) 0.003(4) -0.001(4) 0.001(4) C(14) 0.043(4) 0.052(4) 0.056(4) 0.007(3) 0.005(4) 0.002(4) C(15) 0.076(6) 0.088(7) 0.074(6) -0.005(5) 0.013(5) -0.002(5) C(16) 0.080(6) 0.153(9) 0.134(8) 0.003(9) 0.033(8) 0.059(8) C(17) 0.096(8) 0.090(7) 0.111(8) -0.014(6) -0.007(6) 0.019(6) C(18) 0.077(7) 0.142(8) 0.077(6) -0.017(7) 0.022(6) 0.017(6) C(19) 0.188(11) 0.058(5) 0.093(7) 0.043(7) 0.057(9) 0.027(5) C(20) 0.24(2) 0.075(7) 0.144(10) 0.073(9) 0.081(12) 0.044(7) C(21) 0.128(8) 0.041(5) 0.075(6) 0.024(5) 0.044(6) 0.007(4) C(22) 0.15(2) 0.27(2) 0.17(2) -0.05(2) 0.038(12) -0.06(1) #============================================================================== _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1998)' _computing_data_reduction 'SAINT (Bruker, 1998); CrystalStructure (Rigaku/MSC & Rigaku Corporation, 2003)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'CRYSTALS (Watkin et al., 1996)' _computing_publication_material CrystalStructure _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' #============================================================================== # 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 Sb(2) F(1) 1.882(7) ? . . Sb(2) F(2) 1.803(8) ? . . Sb(2) F(4) 1.840(8) ? . . Sb(2) F(5) 1.784(7) ? . . Sb(2) F(6) 1.791(5) ? . . Sb(2) F(7) 1.804(5) ? . . Pd(1) N(1) 2.088(5) ? . . Pd(1) N(2) 2.157(5) ? . . Pd(1) C(19) 2.090(8) ? . . Pd(1) C(20) 2.01(1) ? . . Pd(1) C(21) 2.125(9) ? . . Cl(1) C(22) 1.642(7) ? . . Cl(2) C(22) 1.720(8) ? . . Cl(3) C(22) 1.704(8) ? . . N(1) C(1) 1.378(9) ? . . N(1) C(5) 1.357(9) ? . . N(2) C(6) 1.369(9) ? . . N(2) C(14) 1.34(1) ? . . C(1) C(1) 1.512(9) ? . 66504 C(1) C(2) 1.35(1) ? . . C(2) C(3) 1.38(1) ? . . C(2) H(1) 0.9500 ? . . C(3) C(4) 1.39(1) ? . . C(3) H(2) 0.9500 ? . . C(4) C(5) 1.37(1) ? . . C(4) H(3) 0.9500 ? . . C(5) C(6) 1.49(1) ? . . C(6) C(7) 1.38(1) ? . . C(7) C(8) 1.39(1) ? . . C(7) H(4) 0.9500 ? . . C(8) C(9) 1.37(1) ? . . C(8) H(5) 0.9500 ? . . C(9) C(10) 1.50(1) ? . . C(9) C(14) 1.41(1) ? . . C(10) C(11) 1.52(1) ? . . C(10) C(15) 1.52(1) ? . . C(10) H(6) 0.9500 ? . . C(11) C(12) 1.51(1) ? . . C(11) H(7) 0.9500 ? . . C(11) H(8) 0.9500 ? . . C(12) C(13) 1.51(1) ? . . C(12) C(15) 1.58(1) ? . . C(12) H(9) 0.9500 ? . . C(13) C(14) 1.49(1) ? . . C(13) C(18) 1.54(1) ? . . C(13) H(10) 0.9500 ? . . C(15) C(16) 1.57(1) ? . . C(15) C(17) 1.45(1) ? . . C(16) H(11) 0.9499 ? . . C(16) H(12) 0.9500 ? . . C(16) H(13) 0.9500 ? . . C(17) H(14) 0.9500 ? . . C(17) H(15) 0.9500 ? . . C(17) H(16) 0.9500 ? . . C(18) H(17) 0.9500 ? . . C(18) H(18) 0.9500 ? . . C(18) H(19) 0.9500 ? . . C(19) C(20) 1.36(2) ? . . C(19) H(20) 0.9500 ? . . C(19) H(21) 0.9500 ? . . C(20) C(21) 1.31(2) ? . . C(20) H(22) 0.9500 ? . . C(21) H(23) 0.9500 ? . . C(21) H(24) 0.9500 ? . . C(22) H(25) 0.9500 ? . . 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 F(2) Sb(2) F(1) 92.1(4) ? . . . F(4) Sb(2) F(1) 178.5(4) ? . . . F(5) Sb(2) F(1) 84.5(4) ? . . . F(6) Sb(2) F(1) 86.8(3) ? . . . F(7) Sb(2) F(1) 90.0(3) ? . . . F(4) Sb(2) F(2) 87.8(5) ? . . . F(5) Sb(2) F(2) 176.4(4) ? . . . F(6) Sb(2) F(2) 86.6(3) ? . . . F(7) Sb(2) F(2) 90.8(3) ? . . . F(5) Sb(2) F(4) 95.7(5) ? . . . F(6) Sb(2) F(4) 91.7(3) ? . . . F(7) Sb(2) F(4) 91.5(3) ? . . . F(6) Sb(2) F(5) 94.1(3) ? . . . F(7) Sb(2) F(5) 88.3(3) ? . . . F(7) Sb(2) F(6) 175.8(3) ? . . . N(2) Pd(1) N(1) 79.9(2) ? . . . Pd(1) N(1) C(1) 127.8(4) ? . . . Pd(1) N(1) C(5) 109.9(4) ? . . . C(19) Pd(1) N(1) 168.2(3) ? . . . C(20) Pd(1) N(1) 131.5(4) ? . . . C(21) Pd(1) N(1) 104.0(3) ? . . . Pd(1) N(2) C(6) 109.3(4) ? . . . Pd(1) N(2) C(14) 130.6(4) ? . . . C(19) Pd(1) N(2) 105.2(3) ? . . . C(20) Pd(1) N(2) 137.3(4) ? . . . C(21) Pd(1) N(2) 173.9(3) ? . . . Pd(1) C(19) C(20) 67.6(6) ? . . . C(20) Pd(1) C(19) 38.7(5) ? . . . C(21) Pd(1) C(19) 70.1(4) ? . . . Pd(1) C(19) H(20) 74.7412 ? . . . Pd(1) C(19) H(21) 130.1214 ? . . . Pd(1) C(20) C(19) 73.7(6) ? . . . Pd(1) C(20) C(21) 76.2(6) ? . . . C(21) Pd(1) C(20) 36.8(5) ? . . . Pd(1) C(20) H(22) 127.7065 ? . . . Pd(1) C(21) C(20) 67.0(6) ? . . . Pd(1) C(21) H(23) 74.5155 ? . . . Pd(1) C(21) H(24) 131.1811 ? . . . Cl(1) C(22) Cl(2) 109.5(4) ? . . . Cl(1) C(22) Cl(3) 109.5(4) ? . . . Cl(1) C(22) H(25) 109.4412 ? . . . Cl(2) C(22) Cl(3) 109.5(4) ? . . . Cl(2) C(22) H(25) 109.4414 ? . . . Cl(3) C(22) H(25) 109.4412 ? . . . N(1) C(1) C(1) 122.4(6) ? . . 66504 C(5) N(1) C(1) 121.2(5) ? . . . N(1) C(1) C(2) 118.3(6) ? . . . N(1) C(5) C(6) 119.4(6) ? . . . N(1) C(5) C(4) 119.9(6) ? . . . N(2) C(6) C(5) 114.4(6) ? . . . C(14) N(2) C(6) 117.7(6) ? . . . N(2) C(6) C(7) 120.7(7) ? . . . N(2) C(14) C(13) 119.0(6) ? . . . N(2) C(14) C(9) 124.1(7) ? . . . C(1) C(1) C(2) 119.2(6) ? . 66504 66504 C(2) C(1) C(1) 119.2(6) ? . . 66504 C(1) C(1) N(1) 122.4(6) ? . 66504 66504 C(1) C(2) C(3) 122.2(7) ? . . . C(1) C(2) H(1) 118.8790 ? . . . C(2) C(3) C(4) 117.9(7) ? . . . H(1) C(2) C(3) 118.8793 ? . . . C(2) C(3) H(2) 121.0333 ? . . . C(3) C(4) C(5) 120.2(7) ? . . . C(3) C(4) H(3) 119.9030 ? . . . H(2) C(3) C(4) 121.0345 ? . . . C(4) C(5) C(6) 120.6(6) ? . . . H(3) C(4) C(5) 119.9028 ? . . . C(5) C(6) C(7) 124.8(7) ? . . . C(6) C(7) C(8) 120.9(7) ? . . . C(6) C(7) H(4) 119.5505 ? . . . C(7) C(8) C(9) 118.6(7) ? . . . H(4) C(7) C(8) 119.5515 ? . . . C(7) C(8) H(5) 120.6779 ? . . . C(8) C(9) C(14) 117.7(7) ? . . . H(5) C(8) C(9) 120.6789 ? . . . C(8) C(9) C(10) 123.1(7) ? . . . C(14) C(9) C(10) 119.2(7) ? . . . C(9) C(10) C(11) 105.5(7) ? . . . C(9) C(10) H(6) 117.1925 ? . . . C(9) C(10) C(15) 109.3(7) ? . . . C(9) C(14) C(13) 116.8(7) ? . . . H(6) C(10) C(11) 117.1927 ? . . . C(10) C(11) H(7) 114.4851 ? . . . C(10) C(11) C(12) 88.3(6) ? . . . C(15) C(10) C(11) 85.9(6) ? . . . C(10) C(11) H(8) 114.4857 ? . . . H(6) C(10) C(15) 117.1926 ? . . . C(10) C(15) C(12) 85.8(6) ? . . . C(10) C(15) C(17) 118.9(8) ? . . . C(10) C(15) C(16) 111.2(7) ? . . . C(11) C(12) C(13) 111.2(7) ? . . . H(7) C(11) C(12) 114.4849 ? . . . C(11) C(12) C(15) 84.2(6) ? . . . H(8) C(11) C(12) 114.4851 ? . . . C(11) C(12) H(9) 114.4907 ? . . . H(8) C(11) H(7) 109.4598 ? . . . C(12) C(13) C(14) 110.1(6) ? . . . C(12) C(13) H(10) 106.5172 ? . . . C(12) C(13) C(18) 112.7(6) ? . . . C(15) C(12) C(13) 114.4(6) ? . . . H(9) C(12) C(13) 114.4909 ? . . . C(12) C(15) C(17) 115.6(7) ? . . . H(9) C(12) C(15) 114.4908 ? . . . C(12) C(15) C(16) 112.0(7) ? . . . H(10) C(13) C(14) 106.5170 ? . . . C(18) C(13) C(14) 113.9(6) ? . . . H(10) C(13) C(18) 106.5165 ? . . . C(13) C(18) H(18) 109.4701 ? . . . C(13) C(18) H(17) 108.2730 ? . . . C(13) C(18) H(19) 109.2386 ? . . . C(17) C(15) C(16) 111.2(8) ? . . . C(15) C(16) H(11) 104.9619 ? . . . C(15) C(16) H(12) 102.7212 ? . . . C(15) C(16) H(13) 109.4703 ? . . . C(15) C(17) H(16) 111.2295 ? . . . C(15) C(17) H(14) 106.3968 ? . . . C(15) C(17) H(15) 109.4696 ? . . . H(12) C(16) H(11) 109.4540 ? . . . H(13) C(16) H(11) 111.6766 ? . . . H(13) C(16) H(12) 117.4801 ? . . . H(16) C(17) H(14) 109.4698 ? . . . H(15) C(17) H(14) 110.9866 ? . . . H(16) C(17) H(15) 109.2696 ? . . . H(18) C(18) H(17) 110.0677 ? . . . H(19) C(18) H(17) 109.4760 ? . . . H(19) C(18) H(18) 110.2804 ? . . . C(19) C(20) C(21) 129(1) ? . . . H(20) C(19) C(20) 119.9998 ? . . . H(21) C(19) C(20) 120.0002 ? . . . C(19) C(20) H(22) 115.0663 ? . . . H(21) C(19) H(20) 120.0000 ? . . . H(22) C(20) C(21) 115.0668 ? . . . C(20) C(21) H(23) 119.9997 ? . . . C(20) C(21) H(24) 120.0004 ? . . . H(24) C(21) H(23) 119.9998 ? . . . 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 Sb(2) H(1) 3.5011 ? . 66504 Sb(2) H(3) 3.4508 ? . 54503 Sb(2) H(8) 3.5665 ? . 54603 Pd(1) C(1) 3.128(7) ? . . Pd(1) C(1) 3.508(7) ? . 66504 Pd(1) C(5) 2.852(7) ? . . Pd(1) C(6) 2.912(7) ? . . Pd(1) C(13) 3.540(7) ? . . Pd(1) C(14) 3.192(7) ? . . Pd(1) H(10) 3.2697 ? . . Pd(1) H(18) 3.0099 ? . . Pd(1) H(20) 2.0558 ? . . Pd(1) H(21) 2.7984 ? . . Pd(1) H(22) 2.7009 ? . . Pd(1) H(23) 2.0833 ? . . Pd(1) H(23) 3.4026 ? . 66504 Pd(1) H(24) 2.8419 ? . . Cl(1) Cl(2) 2.746(8) ? . . Cl(1) Cl(3) 2.733(8) ? . . Cl(1) F(1) 3.22(1) ? . . Cl(1) F(6) 3.452(8) ? . . Cl(1) C(5) 3.492(9) ? . . Cl(1) C(6) 3.474(9) ? . . Cl(1) H(11) 3.2051 ? . 55401 Cl(1) H(25) 2.1532 ? . . Cl(2) Cl(3) 2.797(8) ? . . Cl(2) H(7) 3.1401 ? . 54603 Cl(2) H(16) 3.4240 ? . . Cl(2) H(17) 3.0718 ? . 54603 Cl(2) H(25) 2.2250 ? . . Cl(3) H(5) 3.2525 ? . 56504 Cl(3) H(16) 3.3023 ? . . Cl(3) H(25) 2.2100 ? . . F(1) F(2) 2.65(1) ? . . F(1) F(5) 2.46(1) ? . . F(1) F(6) 2.525(8) ? . . F(1) F(7) 2.607(9) ? . . F(1) C(3) 3.18(1) ? . 54503 F(1) C(4) 3.24(1) ? . 54503 F(1) C(11) 3.45(1) ? . 54603 F(1) H(2) 2.5476 ? . 54503 F(1) H(3) 2.6617 ? . 54503 F(1) H(7) 3.1140 ? . 54603 F(1) H(8) 2.8983 ? . 54603 F(1) H(9) 3.5311 ? . 55401 F(1) H(11) 3.5393 ? . 55401 F(2) F(4) 2.53(1) ? . . F(2) F(5) 3.59(1) ? . . F(2) F(6) 2.464(9) ? . . F(2) F(7) 2.57(1) ? . . F(2) C(20) 3.39(2) ? . . F(2) C(21) 3.20(1) ? . . F(2) H(6) 3.2686 ? . 54603 F(2) H(8) 3.1993 ? . 54603 F(2) H(13) 2.7338 ? . 55602 F(2) H(14) 3.5030 ? . 55602 F(2) H(22) 2.8142 ? . . F(2) H(24) 2.4852 ? . . F(4) F(5) 2.69(1) ? . . F(4) F(6) 2.61(1) ? . . F(4) F(7) 2.61(1) ? . . F(4) C(2) 3.19(1) ? . 66504 F(4) C(3) 3.36(1) ? . 66504 F(4) C(22) 3.25(1) ? . 55502 F(4) H(1) 2.6186 ? . 66504 F(4) H(2) 2.9891 ? . 66504 F(4) H(13) 3.4527 ? . 55602 F(4) H(25) 2.3382 ? . 55502 F(5) F(6) 2.617(9) ? . . F(5) F(7) 2.499(9) ? . . F(5) C(12) 3.51(1) ? . 55401 F(5) C(13) 3.30(1) ? . 55401 F(5) C(19) 3.23(1) ? . 55401 F(5) H(3) 2.9041 ? . 54503 F(5) H(4) 2.9768 ? . 54503 F(5) H(9) 3.1112 ? . 55401 F(5) H(10) 2.5748 ? . 55401 F(5) H(15) 3.0947 ? . 55401 F(5) H(18) 3.5883 ? . 55401 F(5) H(19) 3.5168 ? . 55401 F(5) H(20) 3.0866 ? . 55401 F(5) H(21) 2.7481 ? . 55401 F(6) F(7) 3.593(7) ? . . F(6) C(1) 3.319(8) ? . . F(6) C(2) 3.414(8) ? . . F(6) C(2) 3.264(9) ? . 66504 F(6) C(12) 3.56(1) ? . 55401 F(6) H(1) 2.5820 ? . 66504 F(6) H(9) 2.6879 ? . 55401 F(6) H(19) 3.0038 ? . 55401 F(7) H(3) 2.7536 ? . 54503 F(7) H(4) 3.0061 ? . 54503 F(7) H(8) 2.7472 ? . 54603 F(7) H(12) 3.0675 ? . 54603 F(7) H(13) 3.3000 ? . 55602 N(1) N(1) 3.17(1) ? . 66504 N(1) N(2) 2.726(8) ? . . N(1) C(1) 2.534(9) ? . 66504 N(1) C(2) 2.346(9) ? . . N(1) C(2) 3.59(1) ? . 66504 N(1) C(3) 2.747(9) ? . . N(1) C(4) 2.36(1) ? . . N(1) C(6) 2.461(9) ? . . N(1) C(21) 3.321(9) ? . . N(1) C(21) 3.12(1) ? . 66504 N(1) H(1) 3.2036 ? . . N(1) H(3) 3.2197 ? . . N(1) H(23) 3.1888 ? . . N(1) H(23) 2.4937 ? . 66504 N(1) H(24) 3.5772 ? . . N(1) H(24) 3.1437 ? . 66504 N(2) C(5) 2.405(9) ? . . N(2) C(7) 2.39(1) ? . . N(2) C(8) 2.799(9) ? . . N(2) C(9) 2.43(1) ? . . N(2) C(13) 2.435(9) ? . . N(2) C(18) 2.99(1) ? . . N(2) C(19) 3.37(1) ? . . N(2) H(4) 3.2433 ? . . N(2) H(10) 2.6631 ? . . N(2) H(16) 3.3484 ? . . N(2) H(17) 2.9172 ? . . N(2) H(18) 2.9979 ? . . N(2) H(20) 3.1692 ? . . N(2) H(23) 3.4683 ? . 66504 C(1) Pd(1) 3.508(7) ? . 66504 C(1) N(1) 2.534(9) ? . 66504 C(1) C(2) 2.47(1) ? . 66504 C(1) C(3) 2.40(1) ? . . C(1) C(4) 2.76(1) ? . . C(1) C(5) 2.38(1) ? . . C(1) C(21) 3.12(1) ? . 66504 C(1) H(1) 1.9942 ? . . C(1) H(1) 2.5964 ? . 66504 C(1) H(2) 3.2528 ? . . C(1) H(23) 3.4394 ? . . C(1) H(23) 2.8500 ? . 66504 C(1) H(24) 3.5531 ? . . C(1) H(24) 2.8884 ? . 66504 C(2) F(4) 3.19(1) ? . 66504 C(2) F(6) 3.264(9) ? . 66504 C(2) N(1) 3.59(1) ? . 66504 C(2) C(1) 2.47(1) ? . 66504 C(2) C(2) 3.00(1) ? . 66504 C(2) C(4) 2.37(1) ? . . C(2) C(5) 2.72(1) ? . . C(2) C(21) 3.58(1) ? . 66504 C(2) H(1) 2.7836 ? . 66504 C(2) H(2) 2.0438 ? . . C(2) H(3) 3.2369 ? . . C(2) H(19) 3.1827 ? . 55401 C(2) H(23) 3.5696 ? . 66504 C(2) H(24) 2.9938 ? . 66504 C(3) F(1) 3.18(1) ? . 55503 C(3) F(4) 3.36(1) ? . 66504 C(3) C(5) 2.39(1) ? . . C(3) H(1) 2.0227 ? . . C(3) H(3) 2.0330 ? . . C(3) H(7) 3.5948 ? . 55401 C(3) H(8) 3.4309 ? . 55401 C(3) H(19) 3.4124 ? . 55401 C(3) H(24) 3.3371 ? . 66504 C(4) F(1) 3.24(1) ? . 55503 C(4) C(6) 2.49(1) ? . . C(4) C(7) 2.98(1) ? . . C(4) H(1) 3.2308 ? . . C(4) H(2) 2.0440 ? . . C(4) H(4) 2.6946 ? . . C(4) H(24) 3.5129 ? . 66504 C(5) C(7) 2.55(1) ? . . C(5) C(21) 3.53(1) ? . 66504 C(5) H(2) 3.2534 ? . . C(5) H(3) 2.0220 ? . . C(5) H(4) 2.7325 ? . . C(5) H(23) 2.9372 ? . 66504 C(5) H(24) 3.4150 ? . 66504 C(6) C(8) 2.42(1) ? . . C(6) C(9) 2.76(1) ? . . C(6) C(14) 2.31(1) ? . . C(6) H(3) 2.6471 ? . . C(6) H(4) 2.0285 ? . . C(6) H(5) 3.2736 ? . . C(6) H(23) 3.5011 ? . 66504 C(7) C(9) 2.38(1) ? . . C(7) C(14) 2.70(1) ? . . C(7) H(3) 2.6601 ? . . C(7) H(5) 2.0490 ? . . C(7) H(21) 3.2972 ? . 55603 C(8) C(10) 2.53(1) ? . . C(8) C(11) 3.58(1) ? . . C(8) C(14) 2.38(1) ? . . C(8) H(4) 2.0380 ? . . C(8) H(6) 2.7003 ? . . C(8) H(7) 3.5256 ? . . C(8) H(16) 3.2163 ? . . C(8) H(21) 3.3339 ? . 55603 C(8) H(22) 3.2470 ? . 55603 C(9) C(11) 2.40(1) ? . . C(9) C(12) 2.65(1) ? . . C(9) C(13) 2.47(1) ? . . C(9) C(15) 2.46(1) ? . . C(9) C(17) 2.87(1) ? . . C(9) H(4) 3.2345 ? . . C(9) H(5) 2.0277 ? . . C(9) H(6) 2.1104 ? . . C(9) H(7) 2.4946 ? . . C(9) H(8) 3.2583 ? . . C(9) H(9) 3.5983 ? . . C(9) H(10) 3.0350 ? . . C(9) H(14) 3.4426 ? . . C(9) H(15) 3.5557 ? . . C(9) H(16) 2.4167 ? . . C(9) H(17) 3.5275 ? . . C(10) C(12) 2.11(1) ? . . C(10) C(13) 2.81(1) ? . . C(10) C(14) 2.51(1) ? . . C(10) C(16) 2.55(1) ? . . C(10) C(17) 2.56(1) ? . . C(10) H(5) 2.7126 ? . . C(10) H(7) 2.1008 ? . . C(10) H(8) 2.1008 ? . . C(10) H(9) 2.9356 ? . . C(10) H(10) 3.3956 ? . . C(10) H(11) 3.1972 ? . . C(10) H(12) 2.4101 ? . . C(10) H(13) 3.0825 ? . . C(10) H(14) 2.9539 ? . . C(10) H(15) 3.2900 ? . . C(10) H(16) 2.6131 ? . . C(11) F(1) 3.45(1) ? . 55603 C(11) C(13) 2.49(1) ? . . C(11) C(14) 2.81(1) ? . . C(11) C(15) 2.07(1) ? . . C(11) C(16) 2.80(1) ? . . C(11) C(17) 3.40(1) ? . . C(11) C(18) 3.22(1) ? . . C(11) H(2) 3.2436 ? . 55601 C(11) H(6) 2.1298 ? . . C(11) H(9) 2.0899 ? . . C(11) H(10) 3.2642 ? . . C(11) H(11) 3.0613 ? . . C(11) H(12) 2.4937 ? . . C(11) H(17) 3.1803 ? . . C(11) H(19) 3.2494 ? . . C(12) F(5) 3.51(1) ? . 55601 C(12) F(6) 3.56(1) ? . 55601 C(12) C(14) 2.45(1) ? . . C(12) C(16) 2.61(1) ? . . C(12) C(17) 2.56(1) ? . . C(12) C(18) 2.54(1) ? . . C(12) H(6) 2.9695 ? . . C(12) H(7) 2.0899 ? . . C(12) H(8) 2.0899 ? . . C(12) H(10) 1.9956 ? . . C(12) H(11) 2.5895 ? . . C(12) H(12) 2.8232 ? . . C(12) H(13) 3.3995 ? . . C(12) H(14) 3.3404 ? . . C(12) H(15) 2.6650 ? . . C(12) H(16) 2.8683 ? . . C(12) H(17) 2.9480 ? . . C(12) H(18) 3.2883 ? . . C(12) H(19) 2.5437 ? . . C(13) F(5) 3.30(1) ? . 55601 C(13) C(15) 2.59(1) ? . . C(13) C(17) 2.96(1) ? . . C(13) C(19) 3.37(1) ? . . C(13) H(7) 2.5770 ? . . C(13) H(8) 3.3131 ? . . C(13) H(9) 2.0869 ? . . C(13) H(15) 2.9593 ? . . C(13) H(16) 2.8258 ? . . C(13) H(17) 2.0511 ? . . C(13) H(18) 2.0652 ? . . C(13) H(19) 2.0625 ? . . C(13) H(20) 2.9045 ? . . C(13) H(21) 3.3112 ? . . C(14) C(15) 2.88(1) ? . . C(14) C(17) 3.06(1) ? . . C(14) C(18) 2.54(1) ? . . C(14) H(5) 3.2514 ? . . C(14) H(6) 3.3446 ? . . C(14) H(7) 2.7454 ? . . C(14) H(9) 3.3064 ? . . C(14) H(10) 1.9804 ? . . C(14) H(15) 3.3983 ? . . C(14) H(16) 2.5218 ? . . C(14) H(17) 2.5744 ? . . C(14) H(18) 2.9198 ? . . C(14) H(19) 3.3018 ? . . C(14) H(20) 3.4607 ? . . C(15) H(6) 2.1282 ? . . C(15) H(7) 2.9145 ? . . C(15) H(8) 2.4732 ? . . C(15) H(9) 2.1549 ? . . C(15) H(10) 2.8107 ? . . C(15) H(11) 2.0371 ? . . C(15) H(12) 2.0091 ? . . C(15) H(13) 2.0916 ? . . C(15) H(14) 1.9447 ? . . C(15) H(15) 1.9805 ? . . C(15) H(16) 2.0004 ? . . C(16) C(17) 2.50(1) ? . . C(16) H(6) 2.6844 ? . . C(16) H(6) 3.5590 ? . 56504 C(16) H(8) 2.6270 ? . . C(16) H(9) 2.7054 ? . . C(16) H(12) 3.4121 ? . 56504 C(16) H(14) 2.4729 ? . . C(16) H(15) 2.8345 ? . . C(16) H(16) 3.3044 ? . . C(17) H(6) 3.0933 ? . . C(17) H(9) 3.0767 ? . . C(17) H(10) 2.7530 ? . . C(17) H(11) 2.8737 ? . . C(17) H(12) 3.2012 ? . . C(17) H(13) 2.5137 ? . . C(17) H(24) 3.5354 ? . 45602 C(18) C(18) 3.58(1) ? . 66504 C(18) H(1) 3.5841 ? . 55601 C(18) H(7) 2.9278 ? . . C(18) H(9) 2.7337 ? . . C(18) H(10) 2.0301 ? . . C(18) H(18) 3.0060 ? . 66504 C(18) H(19) 3.5435 ? . 66504 C(18) H(20) 2.8307 ? . . C(19) F(5) 3.23(1) ? . 55601 C(19) C(21) 2.42(1) ? . . C(19) H(5) 3.4507 ? . 54603 C(19) H(10) 2.6239 ? . . C(19) H(18) 2.9931 ? . . C(19) H(22) 1.9625 ? . . C(19) H(23) 2.6676 ? . . C(19) H(24) 3.2488 ? . . C(20) H(5) 3.3113 ? . 54603 C(20) H(14) 3.5635 ? . 55602 C(20) H(20) 2.0122 ? . . C(20) H(21) 2.0122 ? . . C(20) H(23) 1.9661 ? . . C(20) H(24) 1.9661 ? . . C(21) N(1) 3.12(1) ? . 66504 C(21) C(1) 3.12(1) ? . 66504 C(21) C(2) 3.58(1) ? . 66504 C(21) C(5) 3.53(1) ? . 66504 C(21) H(14) 3.2088 ? . 55602 C(21) H(20) 2.6828 ? . . C(21) H(21) 3.2416 ? . . C(21) H(22) 1.9172 ? . . C(22) F(4) 3.25(1) ? . 45502 H(1) Sb(2) 3.5011 ? . 66504 H(1) F(4) 2.6186 ? . 66504 H(1) F(6) 2.5820 ? . 66504 H(1) C(1) 2.5964 ? . 66504 H(1) C(2) 2.7836 ? . 66504 H(1) C(18) 3.5841 ? . 55401 H(2) F(1) 2.5476 ? . 55503 H(2) F(4) 2.9891 ? . 66504 H(2) C(11) 3.2436 ? . 55401 H(3) Sb(2) 3.4508 ? . 55503 H(3) F(1) 2.6617 ? . 55503 H(3) F(5) 2.9041 ? . 55503 H(3) F(7) 2.7536 ? . 55503 H(4) F(5) 2.9768 ? . 55503 H(4) F(7) 3.0061 ? . 55503 H(5) Cl(3) 3.2525 ? . 56504 H(5) C(19) 3.4507 ? . 55603 H(5) C(20) 3.3113 ? . 55603 H(6) F(2) 3.2686 ? . 55603 H(6) C(16) 3.5590 ? . 56504 H(7) Cl(2) 3.1401 ? . 55603 H(7) F(1) 3.1140 ? . 55603 H(7) C(3) 3.5948 ? . 55601 H(8) Sb(2) 3.5665 ? . 55603 H(8) F(1) 2.8983 ? . 55603 H(8) F(2) 3.1993 ? . 55603 H(8) F(7) 2.7472 ? . 55603 H(8) C(3) 3.4309 ? . 55601 H(9) F(1) 3.5311 ? . 55601 H(9) F(5) 3.1112 ? . 55601 H(9) F(6) 2.6879 ? . 55601 H(10) F(5) 2.5748 ? . 55601 H(11) Cl(1) 3.2051 ? . 55601 H(11) F(1) 3.5393 ? . 55601 H(12) F(7) 3.0675 ? . 55603 H(12) C(16) 3.4121 ? . 56504 H(13) F(2) 2.7338 ? . 45602 H(13) F(4) 3.4527 ? . 45602 H(13) F(7) 3.3000 ? . 45602 H(14) F(2) 3.5030 ? . 45602 H(14) C(20) 3.5635 ? . 45602 H(14) C(21) 3.2088 ? . 45602 H(15) F(5) 3.0947 ? . 55601 H(17) Cl(2) 3.0718 ? . 55603 H(18) F(5) 3.5883 ? . 55601 H(18) C(18) 3.0060 ? . 66504 H(19) F(5) 3.5168 ? . 55601 H(19) F(6) 3.0038 ? . 55601 H(19) C(2) 3.1827 ? . 55601 H(19) C(3) 3.4124 ? . 55601 H(19) C(18) 3.5435 ? . 66504 H(20) F(5) 3.0866 ? . 55601 H(21) F(5) 2.7481 ? . 55601 H(21) C(7) 3.2972 ? . 54603 H(21) C(8) 3.3339 ? . 54603 H(22) C(8) 3.2470 ? . 54603 H(23) Pd(1) 3.4026 ? . 66504 H(23) N(1) 2.4937 ? . 66504 H(23) N(2) 3.4683 ? . 66504 H(23) C(1) 2.8500 ? . 66504 H(23) C(2) 3.5696 ? . 66504 H(23) C(5) 2.9372 ? . 66504 H(23) C(6) 3.5011 ? . 66504 H(24) N(1) 3.1437 ? . 66504 H(24) C(1) 2.8884 ? . 66504 H(24) C(2) 2.9938 ? . 66504 H(24) C(3) 3.3371 ? . 66504 H(24) C(4) 3.5129 ? . 66504 H(24) C(5) 3.4150 ? . 66504 H(24) C(17) 3.5354 ? . 55602 H(25) F(4) 2.3382 ? . 45502 Pd(1) Pd(1) 3.9340(8) ? . 66504 loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag C(3) H(2) F(1) 3_555 0.95 2.55 3.177(11) 124 ? C(21) H(23) N(1) 4_665 0.95 2.49 3.123(10) 124 ? C(21) H(24) F(2) . 0.95 2.49 3.202(12) 132 ? C(22) H(25) F(4) 2_455 0.95 2.34 3.247(12) 160 ? # start Validation Reply Form _vrf_PLAT029__wt0787wc-OrthoP-HLKwong095 ; PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.91 RESPONSE: The data collection (exposure) time was not long enough leading to some weak high angle data. ; _vrf_PLAT241__wt0787wc-OrthoP-HLKwong095 ; PROBLEM: Check High Ueq as Compared to Neighbors for C20 RESPONSE: The atom C20 was showing high thermal motion, this may due to slight disorder of the allyl group in the molecules. However, as the disorder was not very serious, and thus the other partial atom site was not located. ; _vrf_PLAT410__wt0787wc-OrthoP-HLKwong095 ; PROBLEM: Short Intra H...H Contact H20 .. H21 .. 1.65 Ang. RESPONSE: H20 and H21 were vinylic hydrogens, similarly for H23 & H24. ; # end Validation Reply Form #============================================================================== # 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 #==============================================================================