# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2001 X-Sun-Charset: iso-8859-1 X-Sun-Content-Lines: 765 data_first_block _journal_coden_Cambridge 440 _journal_volume ? _journal_year ? _journal_page_first ? _publ_contact_author_name 'Ana Rodriguez Fernández-Pacheco' _publ_contact_author_email amrodrig@qino-cr.uclm.es _publ_section_title ; New Complexes with Pyrazole-containing Ligands and Different Metallic Centres. Comparative Study of their Fluxional Behaviour Involving M-N Bond Rupture. ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Elguero, J.' ; Instituto de Quimica Medica CSIC Juan de la Cierva, 3 28006, Madrid Spain ; 'Guerrero, A.' ; Departamento de Quimica Inorganica, Organica y Bioquimica Facultad de Quimicas Avda. C.J. Cela, 10 13071, Ciudad Real Spain ; 'Gomez de la Torre, F.' ; Departamento de Quimica Inorganica, Organica y Bioquimica Facultad de Quimicas Avda. C.J. Cela, 10 13071, Ciudad Real Spain ; 'de la Hoz, A.' ; Departamento de Quimica Inorganica, Organica y Bioquimica Facultad de Quimicas Avda. C.J. Cela, 10 13071, Ciudad Real Spain ; 'Jalon, F.A.' ; Departamento de Quimica Inorganica, Organica y Bioquimica Facultad de Quimicas Avda. C.J. Cela, 10 13071, Ciudad Real Spain ; 'Manzano, B.R.' ; Departamento de Quimica Inorganica, Organica y Bioquimica Facultad de Quimicas Avda. C.J. Cela, 10 13071, Ciudad Real Spain ; 'Rodriguez, A.' ; Escuela Tecnica Superior de Ingenieros Industriales Avda. C.J. Cela, 3 13071, Ciudad Real Spain ; #=========================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ? _journal_techeditor_code ? _journal_techeditor_notes ? #=========================================================================== data_8 _database_code_CSD 160795 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C9 H9 Cl N4 O Pd' _chemical_formula_weight 331.05 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.729(8) _cell_length_b 10.712(2) _cell_length_c 13.985(4) _cell_angle_alpha 90.00 _cell_angle_beta 101.65(4) _cell_angle_gamma 90.00 _cell_volume 1134.0(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.939 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 648 _exptl_absorpt_coefficient_mu 1.855 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'four circle diffractometer Nonius-Mach' _diffrn_measurement_method '\w/2\q scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% ? _diffrn_reflns_number 2841 _diffrn_reflns_av_R_equivalents 0.0355 _diffrn_reflns_av_sigmaI/netI 0.0461 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 28.02 _reflns_number_total 2738 _reflns_number_gt 1874 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius (control program)' _computing_cell_refinement 'Nonius (control program)' _computing_data_reduction 'XRAY80 (Stewart, 1976)' _computing_structure_solution 'SIR92 (Altomare, 1994)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0668P)^2^+2.6747P] 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_number_reflns 2738 _refine_ls_number_parameters 145 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0819 _refine_ls_R_factor_gt 0.0435 _refine_ls_wR_factor_ref 0.1199 _refine_ls_wR_factor_gt 0.1026 _refine_ls_goodness_of_fit_ref 0.883 _refine_ls_restrained_S_all 0.883 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.25006(6) 0.15346(4) 0.53892(3) 0.04522(15) Uani 1 1 d . . . Cl1 Cl 0.1604(3) 0.16360(16) 0.68653(12) 0.0697(4) Uani 1 1 d . . . O1 O 0.2403(8) 0.3877(5) 0.4579(4) 0.0932(18) Uani 1 1 d . . . N1 N 0.2201(6) -0.0509(4) 0.5264(3) 0.0461(10) Uani 1 1 d . . . N2 N 0.2784(7) -0.2155(4) 0.4229(4) 0.0530(12) Uani 1 1 d . . . N3 N 0.3223(6) 0.1143(4) 0.4080(3) 0.0461(10) Uani 1 1 d . . . N4 N 0.3209(6) -0.0093(4) 0.3854(3) 0.0438(10) Uani 1 1 d . . . C1 C 0.2932(9) 0.3339(6) 0.5328(6) 0.0649(18) Uani 1 1 d . . . C2 C 0.3907(11) 0.3966(6) 0.6246(6) 0.080(2) Uani 1 1 d . . . H2A H 0.4202 0.3357 0.6757 0.120 Uiso 1 1 calc . . . H2B H 0.3169 0.4598 0.6442 0.120 Uiso 1 1 calc . . . H2C H 0.4969 0.4342 0.6125 0.120 Uiso 1 1 calc . . . C3 C 0.3746(9) 0.1726(5) 0.3349(5) 0.0562(15) Uani 1 1 d . . . H3 H 0.3869 0.2586 0.3306 0.067 Uiso 1 1 calc . . . C4 C 0.4088(9) 0.0871(7) 0.2652(4) 0.0632(16) Uani 1 1 d . . . H4 H 0.4482 0.1050 0.2081 0.076 Uiso 1 1 calc . . . C5 C 0.3728(8) -0.0268(6) 0.2980(4) 0.0566(14) Uani 1 1 d . . . H5 H 0.3814 -0.1028 0.2672 0.068 Uiso 1 1 calc . . . C6 C 0.2699(7) -0.0975(5) 0.4481(4) 0.0411(11) Uani 1 1 d . . . C7 C 0.2285(9) -0.2951(6) 0.4844(5) 0.0626(17) Uani 1 1 d . . . H7 H 0.2318 -0.3800 0.4708 0.075 Uiso 1 1 calc . . . C8 C 0.1723(9) -0.2594(6) 0.5671(5) 0.0610(16) Uani 1 1 d . . . H8 H 0.1361 -0.3177 0.6083 0.073 Uiso 1 1 calc . . . C9 C 0.1717(8) -0.1327(5) 0.5865(4) 0.0547(14) Uani 1 1 d . . . H9 H 0.1367 -0.1049 0.6427 0.066 Uiso 1 1 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0498(2) 0.0317(2) 0.0531(3) -0.00506(18) 0.00768(17) 0.00488(19) Cl1 0.0830(11) 0.0701(10) 0.0591(8) -0.0104(8) 0.0214(8) 0.0163(9) O1 0.139(5) 0.039(2) 0.094(4) 0.005(3) 0.007(4) -0.003(3) N1 0.058(3) 0.032(2) 0.047(2) 0.0020(18) 0.007(2) -0.0011(19) N2 0.065(3) 0.031(2) 0.061(3) -0.006(2) 0.007(2) 0.000(2) N3 0.050(3) 0.0316(19) 0.055(3) 0.0016(18) 0.007(2) 0.0024(18) N4 0.049(2) 0.035(2) 0.047(2) 0.0011(18) 0.008(2) 0.0009(18) C1 0.071(4) 0.035(3) 0.088(5) -0.011(3) 0.016(4) 0.006(3) C2 0.086(5) 0.047(3) 0.104(6) -0.027(4) 0.013(4) -0.002(4) C3 0.062(4) 0.045(3) 0.060(3) 0.013(3) 0.011(3) -0.001(3) C4 0.070(4) 0.070(4) 0.051(3) 0.014(3) 0.016(3) -0.003(3) C5 0.063(4) 0.058(3) 0.051(3) -0.003(3) 0.014(3) 0.000(3) C6 0.039(3) 0.034(2) 0.048(3) -0.001(2) 0.003(2) -0.002(2) C7 0.069(4) 0.033(3) 0.078(4) 0.002(3) -0.002(3) -0.004(3) C8 0.075(4) 0.047(3) 0.058(4) 0.015(3) 0.007(3) -0.010(3) C9 0.059(3) 0.049(3) 0.054(3) 0.003(2) 0.008(3) -0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C1 1.967(6) . ? Pd1 N3 2.063(5) . ? Pd1 N1 2.204(4) . ? Pd1 Cl1 2.3090(19) . ? O1 C1 1.192(8) . ? N1 C9 1.320(7) . ? N1 C6 1.330(7) . ? N2 C7 1.322(8) . ? N2 C6 1.317(7) . ? N3 C3 1.329(8) . ? N3 N4 1.360(6) . ? N4 C5 1.374(7) . ? N4 C6 1.399(7) . ? C1 C2 1.510(10) . ? C3 C4 1.400(9) . ? C4 C5 1.353(9) . ? C7 C8 1.369(10) . ? C8 C9 1.385(8) . ? 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 C1 Pd1 N3 94.7(2) . . ? C1 Pd1 N1 171.4(2) . . ? N3 Pd1 N1 76.74(17) . . ? C1 Pd1 Cl1 94.4(2) . . ? N3 Pd1 Cl1 170.85(13) . . ? N1 Pd1 Cl1 94.11(12) . . ? C9 N1 C6 116.2(5) . . ? C9 N1 Pd1 130.4(4) . . ? C6 N1 Pd1 113.3(3) . . ? C7 N2 C6 114.1(5) . . ? C3 N3 N4 105.6(5) . . ? C3 N3 Pd1 140.0(4) . . ? N4 N3 Pd1 114.4(3) . . ? N3 N4 C5 110.5(4) . . ? N3 N4 C6 120.2(4) . . ? C5 N4 C6 129.4(5) . . ? O1 C1 C2 123.8(6) . . ? O1 C1 Pd1 118.8(5) . . ? C2 C1 Pd1 117.4(5) . . ? N3 C3 C4 111.0(5) . . ? C5 C4 C3 105.8(5) . . ? C4 C5 N4 107.2(5) . . ? N2 C6 N1 128.2(5) . . ? N2 C6 N4 116.5(5) . . ? N1 C6 N4 115.3(4) . . ? N2 C7 C8 123.5(6) . . ? C7 C8 C9 117.0(5) . . ? N1 C9 C8 120.9(6) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.02 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.561 _refine_diff_density_min -1.365 _refine_diff_density_rms 0.201 #==========================================END data_20 _database_code_CSD 160796 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H11 F3 N4 O3 Pd S' _chemical_formula_weight 454.71 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' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.623(4) _cell_length_b 10.1347(8) _cell_length_c 11.9270(10) _cell_angle_alpha 66.511(8) _cell_angle_beta 79.73(2) _cell_angle_gamma 81.53(2) _cell_volume 828.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.823 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 448 _exptl_absorpt_coefficient_mu 1.296 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'four circle diffractometer Nonius-Mach3' _diffrn_measurement_method '\w/2\q scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% ? _diffrn_reflns_number 3989 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0348 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 27.96 _reflns_number_total 3989 _reflns_number_gt 3029 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius (control program)' _computing_cell_refinement 'Nonius (control program)' _computing_data_reduction 'XRAY80 (Stewart, 1976)' _computing_structure_solution 'SIR92 (Altomare, 1994)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _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 w==1/[\s^2^(Fo^2^)+(0.1405P)^2^+0.4788P] 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_number_reflns 3989 _refine_ls_number_parameters 213 _refine_ls_number_restraints 29 _refine_ls_R_factor_all 0.0768 _refine_ls_R_factor_gt 0.0595 _refine_ls_wR_factor_ref 0.2064 _refine_ls_wR_factor_gt 0.1762 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.178 _refine_ls_shift/su_mean 0.009 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd -0.00422(6) 0.17599(5) 0.69744(4) 0.0534(2) Uani 1 d . . . N1 N 0.1118(8) -0.0131(6) 0.8274(6) 0.0564(12) Uani 1 d . . . N2 N 0.2772(9) -0.0900(7) 0.9956(6) 0.0691(15) Uani 1 d . . . N3 N 0.1304(8) 0.2571(6) 0.7911(5) 0.0576(12) Uani 1 d . . . N4 N 0.2077(7) 0.1536(6) 0.8845(5) 0.0530(11) Uani 1 d . . . C1 C 0.1002(10) -0.1533(8) 0.8468(8) 0.0683(18) Uani 1 d . . . H1 H 0.0405 -0.1749 0.7954 0.082 Uiso 1 calc . . . C2 C 0.1756(11) -0.2634(8) 0.9412(9) 0.075(2) Uani 1 d . . . H2 H 0.1672 -0.3596 0.9556 0.090 Uiso 1 calc . . . C3 C 0.2610(12) -0.2271(8) 1.0111(8) 0.075(2) Uani 1 d . . . H3 H 0.3130 -0.3011 1.0750 0.090 Uiso 1 calc . . . C4 C 0.2006(8) 0.0065(7) 0.9046(6) 0.0519(13) Uani 1 d . . . C5 C 0.2893(9) 0.2093(8) 0.9456(7) 0.0628(16) Uani 1 d . . . H5 H 0.3495 0.1572 1.0135 0.075 Uiso 1 calc . . . C6 C 0.2679(11) 0.3512(9) 0.8910(8) 0.0691(18) Uani 1 d . . . H6 H 0.3131 0.4181 0.9111 0.083 Uiso 1 calc . . . C7 C 0.1615(11) 0.3818(7) 0.7950(8) 0.0674(18) Uani 1 d . . . H7 H 0.1204 0.4734 0.7436 0.081 Uiso 1 calc . . . C8 C -0.1302(12) 0.1101(9) 0.5861(8) 0.0705(19) Uani 1 d . . . H8 H -0.1239 0.0428 0.5503 0.085 Uiso 1 calc . . . C9 C -0.2277(11) 0.2300(9) 0.6002(7) 0.0695(19) Uani 1 d . . . C10 C -0.1228(13) 0.3503(9) 0.5589(8) 0.076(2) Uani 1 d . . . H10 H -0.1131 0.4458 0.5047 0.092 Uiso 1 calc . . . C11 C -0.4093(12) 0.2260(16) 0.6725(10) 0.105(4) Uani 1 d . . . H11A H -0.4512 0.3207 0.6708 0.157 Uiso 1 calc . . . H11B H -0.4035 0.1600 0.7562 0.157 Uiso 1 calc . . . H11C H -0.4902 0.1945 0.6368 0.157 Uiso 1 calc . . . C12 C 0.5658(13) -0.2639(10) 0.6381(9) 0.095(3) Uani 1 d D . . S2 S 0.6937(3) -0.3169(2) 0.76071(18) 0.0760(6) Uani 1 d D . . O1 O 0.8705(16) -0.2804(17) 0.7033(14) 0.088(4) Uiso 0.50 d PDU A 1 O2 O 0.613(3) -0.2021(18) 0.8076(19) 0.109(6) Uiso 0.50 d PDU A 1 O3 O 0.668(3) -0.4594(15) 0.8301(19) 0.137(7) Uiso 0.50 d PDU A 1 O11 O 0.868(2) -0.339(2) 0.716(2) 0.141(8) Uiso 0.50 d PDU A 2 O21 O 0.666(3) -0.1767(18) 0.786(2) 0.133(8) Uiso 0.50 d PDU A 2 O31 O 0.6048(18) -0.4197(14) 0.8692(12) 0.092(4) Uiso 0.50 d PDU A 2 F1 F 0.559(2) -0.1300(15) 0.5622(17) 0.151(7) Uiso 0.50 d PDU B 1 F2 F 0.4011(17) -0.3019(16) 0.6765(13) 0.112(4) Uiso 0.50 d PDU B 1 F3 F 0.644(2) -0.3384(18) 0.5644(16) 0.139(6) Uiso 0.50 d PD B 1 F11 F 0.6358(16) -0.1618(12) 0.5361(10) 0.089(3) Uiso 0.50 d PDU B 2 F21 F 0.3996(15) -0.2232(16) 0.6551(13) 0.106(4) Uiso 0.50 d PDU B 2 F31 F 0.566(2) -0.3840(14) 0.6121(15) 0.121(5) Uiso 0.50 d PD B 2 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 Pd1 0.0547(3) 0.0536(3) 0.0547(3) -0.0250(2) -0.0027(2) -0.0061(2) N1 0.056(3) 0.047(3) 0.064(3) -0.023(2) 0.000(2) -0.003(2) N2 0.069(4) 0.064(3) 0.072(4) -0.024(3) -0.010(3) -0.002(3) N3 0.056(3) 0.053(3) 0.064(3) -0.021(2) -0.010(2) -0.004(2) N4 0.047(3) 0.055(3) 0.060(3) -0.026(2) -0.006(2) -0.001(2) C1 0.059(4) 0.058(4) 0.091(5) -0.032(4) -0.012(4) -0.005(3) C2 0.079(5) 0.046(3) 0.092(5) -0.024(4) -0.002(4) 0.001(3) C3 0.075(5) 0.054(4) 0.084(5) -0.017(4) -0.009(4) 0.004(3) C4 0.043(3) 0.053(3) 0.061(3) -0.026(3) 0.004(2) -0.007(2) C5 0.054(4) 0.076(4) 0.069(4) -0.039(4) -0.007(3) -0.003(3) C6 0.066(4) 0.072(4) 0.083(5) -0.044(4) -0.007(4) -0.009(3) C7 0.077(5) 0.051(3) 0.081(5) -0.031(3) -0.009(4) -0.007(3) C8 0.080(5) 0.079(5) 0.069(4) -0.044(4) -0.013(4) -0.006(4) C9 0.070(4) 0.088(5) 0.054(4) -0.025(4) -0.018(3) -0.012(4) C10 0.091(6) 0.058(4) 0.072(5) -0.015(3) -0.024(4) 0.005(4) C11 0.056(5) 0.179(12) 0.098(7) -0.074(8) -0.010(4) -0.006(6) C12 0.089(7) 0.091(6) 0.102(7) -0.033(6) -0.023(6) 0.003(5) S2 0.0760(12) 0.0833(13) 0.0577(10) -0.0079(9) -0.0160(9) -0.0206(10) _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 Pd1 N3 2.089(6) . ? Pd1 C10 2.099(8) . ? Pd1 N1 2.116(6) . ? Pd1 C9 2.114(7) . ? Pd1 C8 2.117(7) . ? N1 C4 1.324(9) . ? N1 C1 1.360(9) . ? N2 C4 1.299(9) . ? N2 C3 1.348(10) . ? N3 N4 1.345(8) . ? N3 C7 1.340(9) . ? N4 C5 1.353(9) . ? N4 C4 1.421(8) . ? C1 C2 1.373(11) . ? C2 C3 1.328(13) . ? C5 C6 1.320(11) . ? C6 C7 1.427(12) . ? C8 C9 1.382(12) . ? C9 C10 1.427(12) . ? C9 C11 1.492(12) . ? C12 F21 1.280(13) . ? C12 F1 1.296(14) . ? C12 F11 1.327(12) . ? C12 F2 1.316(13) . ? C12 F31 1.369(14) . ? C12 F3 1.381(14) . ? C12 S2 1.763(10) . ? S2 O11 1.363(14) . ? S2 O3 1.372(13) . ? S2 O1 1.428(11) . ? S2 O31 1.428(11) . ? S2 O2 1.493(13) . ? S2 O21 1.543(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Pd1 C10 108.6(3) . . ? N3 Pd1 N1 77.0(2) . . ? C10 Pd1 N1 174.1(3) . . ? N3 Pd1 C9 140.4(3) . . ? C10 Pd1 C9 39.6(3) . . ? N1 Pd1 C9 136.2(3) . . ? N3 Pd1 C8 174.3(3) . . ? C10 Pd1 C8 67.2(3) . . ? N1 Pd1 C8 107.1(3) . . ? C9 Pd1 C8 38.1(3) . . ? C4 N1 C1 115.1(6) . . ? C4 N1 Pd1 116.1(4) . . ? C1 N1 Pd1 128.7(5) . . ? C4 N2 C3 113.8(7) . . ? N4 N3 C7 105.0(6) . . ? N4 N3 Pd1 113.5(4) . . ? C7 N3 Pd1 141.4(5) . . ? N3 N4 C5 112.1(6) . . ? N3 N4 C4 119.1(5) . . ? C5 N4 C4 128.7(6) . . ? N1 C1 C2 120.7(7) . . ? C3 C2 C1 117.4(7) . . ? C2 C3 N2 124.3(7) . . ? N2 C4 N1 128.7(6) . . ? N2 C4 N4 117.1(6) . . ? N1 C4 N4 114.2(6) . . ? C6 C5 N4 107.3(7) . . ? C5 C6 C7 106.6(6) . . ? N3 C7 C6 108.9(7) . . ? C9 C8 Pd1 70.8(4) . . ? C8 C9 C10 112.3(8) . . ? C8 C9 C11 123.5(9) . . ? C10 C9 C11 123.2(9) . . ? C8 C9 Pd1 71.0(5) . . ? C10 C9 Pd1 69.6(4) . . ? C11 C9 Pd1 117.7(6) . . ? C9 C10 Pd1 70.8(4) . . ? F21 C12 F1 77.8(11) . . ? F21 C12 F11 106.4(10) . . ? F1 C12 F11 31.4(9) . . ? F21 C12 F2 32.8(8) . . ? F1 C12 F2 108.2(11) . . ? F11 C12 F2 131.4(11) . . ? F21 C12 F31 103.9(11) . . ? F1 C12 F31 127.8(13) . . ? F11 C12 F31 107.5(11) . . ? F2 C12 F31 75.8(10) . . ? F21 C12 F3 126.5(13) . . ? F1 C12 F3 103.8(12) . . ? F11 C12 F3 76.6(10) . . ? F2 C12 F3 106.3(11) . . ? F31 C12 F3 33.7(8) . . ? F21 C12 S2 119.1(9) . . ? F1 C12 S2 118.6(11) . . ? F11 C12 S2 113.0(8) . . ? F2 C12 S2 112.1(9) . . ? F31 C12 S2 106.0(9) . . ? F3 C12 S2 106.9(10) . . ? O11 S2 O3 96.4(12) . . ? O11 S2 O1 22.7(11) . . ? O3 S2 O1 118.2(10) . . ? O11 S2 O31 123.0(11) . . ? O3 S2 O31 32.7(9) . . ? O1 S2 O31 139.9(9) . . ? O11 S2 O2 127.2(13) . . ? O3 S2 O2 120.8(10) . . ? O1 S2 O2 106.6(9) . . ? O31 S2 O2 88.3(9) . . ? O11 S2 O21 109.8(11) . . ? O3 S2 O21 135.3(12) . . ? O1 S2 O21 88.5(10) . . ? O31 S2 O21 104.0(9) . . ? O2 S2 O21 18.2(11) . . ? O11 S2 C12 108.0(11) . . ? O3 S2 C12 106.2(10) . . ? O1 S2 C12 105.1(7) . . ? O31 S2 C12 110.0(7) . . ? O2 S2 C12 96.7(9) . . ? O21 S2 C12 99.4(11) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.96 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.322 _refine_diff_density_min -1.048 _refine_diff_density_rms 0.137