# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email litwin@chem.uw.edu.pl _publ_contact_author_name 'Agnieszka Krogul' loop_ _publ_author_name 'Agnieszka Krogul' 'Grzegorz Litwinienko' 'Jadwiga Skupinska' 'Katarzyna Wiktorska' 'Wojciech Oziminski' 'Jakub Cedrowski' data_vvv _database_code_depnum_ccdc_archive 'CCDC 837204' #TrackingRef '- PdCl2(2ClPy)2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H8 Cl4 N2 Pd' _chemical_formula_weight 404.38 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' 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.2008(18) _cell_length_b 8.5307(18) _cell_length_c 10.512(2) _cell_angle_alpha 91.866(17) _cell_angle_beta 91.018(17) _cell_angle_gamma 115.73(2) _cell_volume 661.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.030 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 392 _exptl_absorpt_coefficient_mu 2.186 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.46 _exptl_absorpt_correction_T_max 0.69 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.28cycle4 beta (release 11-11-2005 CrysAlis171 .NET) (compiled Nov 11 2005,15:50:43) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'KM4 CCD' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean 8.6479 _diffrn_standards_number '1 frame' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12182 _diffrn_reflns_av_R_equivalents 0.0350 _diffrn_reflns_av_sigmaI/netI 0.0462 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.65 _diffrn_reflns_theta_max 28.54 _reflns_number_total 3166 _reflns_number_gt 2321 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.28cycle4 beta (release 11-11-2005 CrysAlis171 .NET) (compiled Nov 11 2005,15:50:43) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.28cycle4 beta (release 11-11-2005 CrysAlis171 .NET) (compiled Nov 11 2005,15:50:43) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.28cycle4 beta (release 11-11-2005 CrysAlis171 .NET) (compiled Nov 11 2005,15:50:43) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Diamond _computing_publication_material SHELXTL-97 _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^)+(0.0394P)^2^+0.0042P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3166 _refine_ls_number_parameters 154 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0561 _refine_ls_R_factor_gt 0.0337 _refine_ls_wR_factor_ref 0.0761 _refine_ls_wR_factor_gt 0.0712 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.86622(4) 0.23709(3) 0.27830(3) 0.01657(10) Uani 1 1 d . . . Cl2 Cl 0.60934(12) 0.25330(11) 0.20136(10) 0.0259(2) Uani 1 1 d . . . Cl1 Cl 1.11628(12) 0.22129(11) 0.36875(9) 0.0236(2) Uani 1 1 d . . . N1A N 1.0109(4) 0.4966(4) 0.2546(3) 0.0195(7) Uani 1 1 d . . . C1A C 1.1290(5) 0.5619(5) 0.1636(4) 0.0218(8) Uani 1 1 d . . . Cl1A Cl 1.16422(14) 0.41427(12) 0.06608(10) 0.0286(2) Uani 1 1 d . . . C2A C 1.2231(5) 0.7404(5) 0.1436(4) 0.0240(9) Uani 1 1 d . . . H2A H 1.3056 0.7824 0.0767 0.029 Uiso 1 1 calc R . . C3A C 1.1904(5) 0.8524(5) 0.2256(4) 0.0242(9) Uani 1 1 d . . . H3A H 1.2528 0.9746 0.2164 0.029 Uiso 1 1 calc R . . C4A C 1.0675(5) 0.7882(5) 0.3211(4) 0.0261(9) Uani 1 1 d . . . H4A H 1.0439 0.8665 0.3755 0.031 Uiso 1 1 calc R . . C5A C 0.9792(5) 0.6120(4) 0.3377(4) 0.0265(9) Uani 1 1 d . . . H5A H 0.8975 0.5686 0.4048 0.032 Uiso 1 1 calc R . . N1B N 0.7190(4) -0.0211(4) 0.3047(3) 0.0178(7) Uani 1 1 d . . . C1B C 0.6959(5) -0.1433(5) 0.2139(4) 0.0207(8) Uani 1 1 d . . . Cl1B Cl 0.79695(14) -0.07178(12) 0.07103(10) 0.0305(2) Uani 1 1 d . . . C2B C 0.5959(5) -0.3202(5) 0.2305(4) 0.0252(9) Uani 1 1 d . . . H2B H 0.5845 -0.4034 0.1644 0.030 Uiso 1 1 calc R . . C3B C 0.5131(5) -0.3729(5) 0.3455(4) 0.0282(10) Uani 1 1 d . . . H3B H 0.4424 -0.4929 0.3593 0.034 Uiso 1 1 calc R . . C4B C 0.5354(5) -0.2475(5) 0.4394(4) 0.0288(10) Uani 1 1 d . . . H4B H 0.4794 -0.2807 0.5188 0.035 Uiso 1 1 calc R . . C5B C 0.6390(5) -0.0740(5) 0.4177(4) 0.0227(8) Uani 1 1 d . . . H5B H 0.6551 0.0109 0.4835 0.027 Uiso 1 1 calc 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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.01431(15) 0.00684(13) 0.02693(17) 0.00074(10) 0.00178(11) 0.00304(10) Cl2 0.0161(5) 0.0147(4) 0.0461(7) 0.0043(4) -0.0024(4) 0.0057(4) Cl1 0.0160(5) 0.0133(4) 0.0397(6) 0.0049(4) -0.0033(4) 0.0046(3) N1A 0.0153(16) 0.0114(14) 0.0282(18) 0.0029(13) -0.0023(14) 0.0024(12) C1A 0.0188(19) 0.0195(18) 0.028(2) -0.0017(16) -0.0025(17) 0.0098(16) Cl1A 0.0306(5) 0.0217(5) 0.0318(6) -0.0022(4) 0.0052(4) 0.0099(4) C2A 0.020(2) 0.0198(19) 0.031(2) 0.0025(17) -0.0021(17) 0.0080(16) C3A 0.0166(19) 0.0179(19) 0.033(2) 0.0054(17) -0.0020(17) 0.0027(15) C4A 0.028(2) 0.0174(19) 0.034(2) -0.0021(17) -0.0035(19) 0.0109(17) C5A 0.0165(19) 0.0092(16) 0.053(3) 0.0054(17) -0.0102(18) 0.0051(14) N1B 0.0135(15) 0.0111(14) 0.0297(18) 0.0023(13) -0.0015(13) 0.0060(12) C1B 0.0178(19) 0.0166(18) 0.029(2) 0.0015(16) 0.0008(16) 0.0088(15) Cl1B 0.0369(6) 0.0191(5) 0.0336(6) -0.0020(4) 0.0102(5) 0.0104(4) C2B 0.022(2) 0.0115(17) 0.040(3) -0.0010(17) -0.0057(19) 0.0064(15) C3B 0.018(2) 0.0142(18) 0.052(3) 0.0069(19) -0.0079(19) 0.0058(16) C4B 0.019(2) 0.029(2) 0.037(2) 0.0166(19) 0.0016(18) 0.0073(17) C5B 0.0172(19) 0.0194(19) 0.030(2) 0.0038(16) -0.0016(17) 0.0068(15) _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 N1B 2.032(3) . ? Pd1 N1A 2.034(3) . ? Pd1 Cl1 2.3036(11) . ? Pd1 Cl2 2.3045(11) . ? N1A C1A 1.328(5) . ? N1A C5A 1.405(5) . ? C1A C2A 1.402(5) . ? C1A Cl1A 1.721(4) . ? C2A C3A 1.380(5) . ? C2A H2A 0.9500 . ? C3A C4A 1.384(5) . ? C3A H3A 0.9500 . ? C4A C5A 1.375(5) . ? C4A H4A 0.9500 . ? C5A H5A 0.9500 . ? N1B C1B 1.338(4) . ? N1B C5B 1.360(5) . ? C1B C2B 1.388(5) . ? C1B Cl1B 1.726(4) . ? C2B C3B 1.387(6) . ? C2B H2B 0.9500 . ? C3B C4B 1.381(6) . ? C3B H3B 0.9500 . ? C4B C5B 1.379(5) . ? C4B H4B 0.9500 . ? C5B H5B 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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1B Pd1 N1A 178.88(12) . . ? N1B Pd1 Cl1 89.32(9) . . ? N1A Pd1 Cl1 91.02(9) . . ? N1B Pd1 Cl2 89.93(9) . . ? N1A Pd1 Cl2 89.65(9) . . ? Cl1 Pd1 Cl2 176.17(4) . . ? C1A N1A C5A 118.7(3) . . ? C1A N1A Pd1 123.8(2) . . ? C5A N1A Pd1 117.6(2) . . ? N1A C1A C2A 123.9(3) . . ? N1A C1A Cl1A 116.5(3) . . ? C2A C1A Cl1A 119.6(3) . . ? C3A C2A C1A 116.9(4) . . ? C3A C2A H2A 121.6 . . ? C1A C2A H2A 121.6 . . ? C2A C3A C4A 120.5(3) . . ? C2A C3A H3A 119.7 . . ? C4A C3A H3A 119.7 . . ? C5A C4A C3A 120.5(4) . . ? C5A C4A H4A 119.7 . . ? C3A C4A H4A 119.7 . . ? C4A C5A N1A 119.5(4) . . ? C4A C5A H5A 120.3 . . ? N1A C5A H5A 120.3 . . ? C1B N1B C5B 118.0(3) . . ? C1B N1B Pd1 122.3(2) . . ? C5B N1B Pd1 119.7(2) . . ? N1B C1B C2B 123.1(4) . . ? N1B C1B Cl1B 116.8(3) . . ? C2B C1B Cl1B 120.1(3) . . ? C3B C2B C1B 118.6(4) . . ? C3B C2B H2B 120.7 . . ? C1B C2B H2B 120.7 . . ? C4B C3B C2B 118.7(3) . . ? C4B C3B H3B 120.7 . . ? C2B C3B H3B 120.7 . . ? C5B C4B C3B 119.8(4) . . ? C5B C4B H4B 120.1 . . ? C3B C4B H4B 120.1 . . ? N1B C5B C4B 121.8(4) . . ? N1B C5B H5B 119.1 . . ? C4B C5B H5B 119.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1B Pd1 N1A C1A -175(6) . . . . ? Cl1 Pd1 N1A C1A 76.6(3) . . . . ? Cl2 Pd1 N1A C1A -107.1(3) . . . . ? N1B Pd1 N1A C5A 3(6) . . . . ? Cl1 Pd1 N1A C5A -105.2(2) . . . . ? Cl2 Pd1 N1A C5A 71.0(2) . . . . ? C5A N1A C1A C2A -1.0(5) . . . . ? Pd1 N1A C1A C2A 177.1(3) . . . . ? C5A N1A C1A Cl1A 179.2(3) . . . . ? Pd1 N1A C1A Cl1A -2.7(4) . . . . ? N1A C1A C2A C3A 0.8(6) . . . . ? Cl1A C1A C2A C3A -179.4(3) . . . . ? C1A C2A C3A C4A -1.0(5) . . . . ? C2A C3A C4A C5A 1.6(6) . . . . ? C3A C4A C5A N1A -1.8(6) . . . . ? C1A N1A C5A C4A 1.4(5) . . . . ? Pd1 N1A C5A C4A -176.8(3) . . . . ? N1A Pd1 N1B C1B 158(6) . . . . ? Cl1 Pd1 N1B C1B -94.2(3) . . . . ? Cl2 Pd1 N1B C1B 89.5(3) . . . . ? N1A Pd1 N1B C5B -22(6) . . . . ? Cl1 Pd1 N1B C5B 86.3(3) . . . . ? Cl2 Pd1 N1B C5B -90.0(3) . . . . ? C5B N1B C1B C2B -0.5(5) . . . . ? Pd1 N1B C1B C2B 179.9(3) . . . . ? C5B N1B C1B Cl1B 179.3(3) . . . . ? Pd1 N1B C1B Cl1B -0.2(4) . . . . ? N1B C1B C2B C3B 1.3(6) . . . . ? Cl1B C1B C2B C3B -178.5(3) . . . . ? C1B C2B C3B C4B -0.9(5) . . . . ? C2B C3B C4B C5B -0.3(6) . . . . ? C1B N1B C5B C4B -0.6(5) . . . . ? Pd1 N1B C5B C4B 178.9(3) . . . . ? C3B C4B C5B N1B 1.0(6) . . . . ? _diffrn_measured_fraction_theta_max 0.945 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.746 _refine_diff_density_min -0.945 _refine_diff_density_rms 0.133 # Attachment '- PdCl2(3MePy)2.CIF' data_xxx _database_code_depnum_ccdc_archive 'CCDC 837205' #TrackingRef '- PdCl2(3MePy)2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H14 Cl2 N2 Pd' _chemical_formula_weight 363.55 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' 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.7438(5) _cell_length_b 7.2880(8) _cell_length_c 8.4654(9) _cell_angle_alpha 69.081(10) _cell_angle_beta 79.744(8) _cell_angle_gamma 83.763(8) _cell_volume 325.33(6) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.856 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 180 _exptl_absorpt_coefficient_mu 1.814 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6700 _exptl_absorpt_correction_T_max 0.9148 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.28cycle4 beta (release 11-11-2005 CrysAlis171 .NET) (compiled Nov 11 2005,15:50:43) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 KM4CCD _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean 8.6479 _diffrn_standards_number '1 frame' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2 _diffrn_reflns_number 6242 _diffrn_reflns_av_R_equivalents 0.0130 _diffrn_reflns_av_sigmaI/netI 0.0121 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 28.60 _reflns_number_total 1581 _reflns_number_gt 1533 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.28cycle4 beta (release 11-11-2005 CrysAlis171 .NET) (compiled Nov 11 2005,15:50:43) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.28cycle4 beta (release 11-11-2005 CrysAlis171 .NET) (compiled Nov 11 2005,15:50:43) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.28cycle4 beta (release 11-11-2005 CrysAlis171 .NET) (compiled Nov 11 2005,15:50:43) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Diamond _computing_publication_material SHELXTL-97 _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^)+(0.0206P)^2^+0.0808P] 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 1581 _refine_ls_number_parameters 107 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0134 _refine_ls_R_factor_gt 0.0127 _refine_ls_wR_factor_ref 0.0337 _refine_ls_wR_factor_gt 0.0336 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.086 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.5000 0.5000 0.5000 0.01038(5) Uani 1 2 d S . . Cl1 Cl 0.57046(5) 0.80323(4) 0.29250(4) 0.01526(7) Uani 1 1 d . . . N1 N 0.24004(19) 0.62671(16) 0.62705(14) 0.0119(2) Uani 1 1 d . . . C1 C 0.2688(2) 0.63491(19) 0.77857(17) 0.0128(2) Uani 1 1 d . . . C2 C 0.1051(2) 0.72972(18) 0.86942(17) 0.0126(2) Uani 1 1 d . . . C3 C -0.1001(2) 0.81304(19) 0.80035(18) 0.0143(3) Uani 1 1 d . . . C4 C -0.1325(2) 0.80248(19) 0.64523(18) 0.0142(3) Uani 1 1 d . . . C5 C 0.0420(2) 0.71003(19) 0.56018(17) 0.0128(2) Uani 1 1 d . . . C6 C 0.1563(3) 0.7414(2) 1.03339(18) 0.0165(3) Uani 1 1 d . . . H1 H 0.409(3) 0.575(2) 0.821(2) 0.016(4) Uiso 1 1 d . . . H3 H -0.214(3) 0.877(3) 0.855(2) 0.021(4) Uiso 1 1 d . . . H4 H -0.270(3) 0.861(3) 0.593(2) 0.018(4) Uiso 1 1 d . . . H5 H 0.025(3) 0.704(2) 0.452(2) 0.011(4) Uiso 1 1 d . . . H6A H 0.283(4) 0.827(3) 1.013(3) 0.037(6) Uiso 1 1 d . . . H6B H 0.202(4) 0.622(3) 1.104(3) 0.034(5) Uiso 1 1 d . . . H6C H 0.022(4) 0.786(3) 1.091(3) 0.041(6) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.00916(7) 0.01114(8) 0.01030(7) -0.00431(5) -0.00048(5) 0.00230(5) Cl1 0.01489(15) 0.01302(16) 0.01452(16) -0.00241(13) 0.00004(12) 0.00156(12) N1 0.0108(5) 0.0118(5) 0.0122(5) -0.0043(4) 0.0002(4) 0.0004(4) C1 0.0110(6) 0.0133(6) 0.0131(6) -0.0039(5) -0.0015(5) 0.0006(5) C2 0.0135(6) 0.0100(6) 0.0132(6) -0.0035(5) 0.0007(5) -0.0021(5) C3 0.0125(6) 0.0112(6) 0.0183(6) -0.0061(5) 0.0015(5) 0.0004(5) C4 0.0113(6) 0.0119(6) 0.0181(6) -0.0037(5) -0.0027(5) 0.0014(5) C5 0.0128(6) 0.0118(6) 0.0128(6) -0.0033(5) -0.0017(5) 0.0000(5) C6 0.0175(7) 0.0174(7) 0.0155(6) -0.0076(6) -0.0018(5) 0.0007(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N1 2.0191(11) 2_666 ? Pd1 N1 2.0191(11) . ? Pd1 Cl1 2.3027(5) 2_666 ? Pd1 Cl1 2.3027(5) . ? N1 C1 1.3448(17) . ? N1 C5 1.3477(17) . ? C1 C2 1.3907(18) . ? C1 H1 0.936(18) . ? C2 C3 1.3916(19) . ? C2 C6 1.5019(18) . ? C3 C4 1.3883(19) . ? C3 H3 0.919(18) . ? C4 C5 1.3857(18) . ? C4 H4 0.956(18) . ? C5 H5 0.957(17) . ? C6 H6A 0.96(2) . ? C6 H6B 0.90(2) . ? C6 H6C 0.93(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pd1 N1 180.0 2_666 . ? N1 Pd1 Cl1 89.47(3) 2_666 2_666 ? N1 Pd1 Cl1 90.53(3) . 2_666 ? N1 Pd1 Cl1 90.53(3) 2_666 . ? N1 Pd1 Cl1 89.47(3) . . ? Cl1 Pd1 Cl1 180.000(11) 2_666 . ? C1 N1 C5 119.21(11) . . ? C1 N1 Pd1 119.36(9) . . ? C5 N1 Pd1 121.38(9) . . ? N1 C1 C2 123.04(12) . . ? N1 C1 H1 116.5(10) . . ? C2 C1 H1 120.5(10) . . ? C1 C2 C3 117.27(12) . . ? C1 C2 C6 119.76(12) . . ? C3 C2 C6 122.96(12) . . ? C4 C3 C2 119.95(12) . . ? C4 C3 H3 119.2(11) . . ? C2 C3 H3 120.8(11) . . ? C5 C4 C3 119.29(12) . . ? C5 C4 H4 118.8(10) . . ? C3 C4 H4 121.9(10) . . ? N1 C5 C4 121.21(12) . . ? N1 C5 H5 118.1(10) . . ? C4 C5 H5 120.7(10) . . ? C2 C6 H6A 111.3(13) . . ? C2 C6 H6B 110.9(13) . . ? H6A C6 H6B 106.9(18) . . ? C2 C6 H6C 110.5(13) . . ? H6A C6 H6C 109.5(18) . . ? H6B C6 H6C 107.6(18) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Pd1 N1 C1 95(100) 2_666 . . . ? Cl1 Pd1 N1 C1 68.01(10) 2_666 . . . ? Cl1 Pd1 N1 C1 -111.99(10) . . . . ? N1 Pd1 N1 C5 -88(100) 2_666 . . . ? Cl1 Pd1 N1 C5 -114.58(10) 2_666 . . . ? Cl1 Pd1 N1 C5 65.42(10) . . . . ? C5 N1 C1 C2 -1.42(19) . . . . ? Pd1 N1 C1 C2 176.05(10) . . . . ? N1 C1 C2 C3 2.2(2) . . . . ? N1 C1 C2 C6 -176.80(12) . . . . ? C1 C2 C3 C4 -1.16(19) . . . . ? C6 C2 C3 C4 177.82(12) . . . . ? C2 C3 C4 C5 -0.6(2) . . . . ? C1 N1 C5 C4 -0.46(19) . . . . ? Pd1 N1 C5 C4 -177.87(10) . . . . ? C3 C4 C5 N1 1.4(2) . . . . ? _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.393 _refine_diff_density_min -0.617 _refine_diff_density_rms 0.057 # Attachment '- PdCl2(4MePy)2.CIF' data_zzz _database_code_depnum_ccdc_archive 'CCDC 837206' #TrackingRef '- PdCl2(4MePy)2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H14 Cl2 N2 Pd' _chemical_formula_weight 363.55 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' 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 10.4617(5) _cell_length_b 3.9801(2) _cell_length_c 15.9063(9) _cell_angle_alpha 90.00 _cell_angle_beta 98.734(4) _cell_angle_gamma 90.00 _cell_volume 654.64(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.844 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 360 _exptl_absorpt_coefficient_mu 1.803 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.82 _exptl_absorpt_correction_T_max 0.93 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.28cycle4 beta (release 11-11-2005 CrysAlis171 .NET) (compiled Nov 11 2005,15:50:43) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'KM4 CCD' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean 8.6479 _diffrn_standards_number '1 frame' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7405 _diffrn_reflns_av_R_equivalents 0.0163 _diffrn_reflns_av_sigmaI/netI 0.0196 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 28.76 _reflns_number_total 1603 _reflns_number_gt 1356 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.28cycle4 beta (release 11-11-2005 CrysAlis171 .NET) (compiled Nov 11 2005,15:50:43) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.28cycle4 beta (release 11-11-2005 CrysAlis171 .NET) (compiled Nov 11 2005,15:50:43) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.28cycle4 beta (release 11-11-2005 CrysAlis171 .NET) (compiled Nov 11 2005,15:50:43) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Diamond _computing_publication_material SHELXTL-97 _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^)+(0.0216P)^2^+0.0000P] 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 SHELXL _refine_ls_extinction_coef 0.0036(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1603 _refine_ls_number_parameters 105 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0186 _refine_ls_R_factor_gt 0.0140 _refine_ls_wR_factor_ref 0.0342 _refine_ls_wR_factor_gt 0.0338 _refine_ls_goodness_of_fit_ref 0.965 _refine_ls_restrained_S_all 0.965 _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 0.5000 0.0000 0.0000 0.01034(6) Uani 1 2 d S . . Cl1 Cl 0.70433(3) 0.23173(10) 0.01995(2) 0.01519(9) Uani 1 1 d . . . N1 N 0.49672(11) 0.0351(3) 0.12596(7) 0.0114(2) Uani 1 1 d . . . C1 C 0.59194(14) -0.0996(4) 0.18243(9) 0.0128(3) Uani 1 1 d . . . C2 C 0.59407(14) -0.0730(4) 0.26892(9) 0.0136(3) Uani 1 1 d . . . C3 C 0.49538(14) 0.0993(4) 0.30081(9) 0.0131(3) Uani 1 1 d . . . C4 C 0.39797(14) 0.2342(4) 0.24160(9) 0.0141(3) Uani 1 1 d . . . C5 C 0.40056(14) 0.1982(4) 0.15550(9) 0.0133(3) Uani 1 1 d . . . C6 C 0.49513(17) 0.1349(5) 0.39438(10) 0.0194(3) Uani 1 1 d . . . H1 H 0.6538(15) -0.205(4) 0.1594(9) 0.011(4) Uiso 1 1 d . . . H2 H 0.6551(15) -0.169(4) 0.3054(10) 0.010(4) Uiso 1 1 d . . . H4 H 0.3327(15) 0.354(4) 0.2582(10) 0.018(4) Uiso 1 1 d . . . H5 H 0.3397(15) 0.288(4) 0.1148(10) 0.015(4) Uiso 1 1 d . . . H6A H 0.4217(16) 0.236(5) 0.4062(10) 0.023 Uiso 1 1 d . . . H6B H 0.5599(16) 0.250(5) 0.4167(10) 0.023 Uiso 1 1 d . . . H6C H 0.4968(17) -0.073(5) 0.4189(11) 0.023 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.00988(8) 0.01342(9) 0.00735(8) 0.00104(7) 0.00008(5) -0.00095(7) Cl1 0.01234(16) 0.01990(19) 0.01276(15) 0.00147(14) 0.00004(12) -0.00379(15) N1 0.0117(6) 0.0125(7) 0.0096(5) 0.0008(5) 0.0008(4) -0.0022(5) C1 0.0104(7) 0.0135(8) 0.0144(7) 0.0005(6) 0.0019(6) -0.0005(6) C2 0.0122(7) 0.0155(9) 0.0120(7) 0.0027(6) -0.0017(5) -0.0009(6) C3 0.0148(7) 0.0114(7) 0.0131(7) -0.0001(5) 0.0026(5) -0.0043(6) C4 0.0128(7) 0.0137(8) 0.0165(7) -0.0009(6) 0.0046(5) -0.0002(6) C5 0.0117(7) 0.0134(8) 0.0143(7) 0.0017(6) -0.0002(5) 0.0000(6) C6 0.0222(9) 0.0232(9) 0.0131(7) -0.0004(7) 0.0032(6) 0.0016(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 Pd1 N1 2.0139(11) . ? Pd1 N1 2.0139(11) 3_655 ? Pd1 Cl1 2.3054(3) . ? Pd1 Cl1 2.3054(3) 3_655 ? N1 C5 1.3408(18) . ? N1 C1 1.3472(19) . ? C1 C2 1.377(2) . ? C1 H1 0.894(16) . ? C2 C3 1.397(2) . ? C2 H2 0.881(16) . ? C3 C4 1.386(2) . ? C3 C6 1.495(2) . ? C4 C5 1.3813(19) . ? C4 H4 0.905(16) . ? C5 H5 0.909(15) . ? C6 H6A 0.912(17) . ? C6 H6B 0.849(17) . ? C6 H6C 0.915(19) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pd1 N1 180.00(6) . 3_655 ? N1 Pd1 Cl1 89.48(3) . . ? N1 Pd1 Cl1 90.52(3) 3_655 . ? N1 Pd1 Cl1 90.52(3) . 3_655 ? N1 Pd1 Cl1 89.48(3) 3_655 3_655 ? Cl1 Pd1 Cl1 180.0 . 3_655 ? C5 N1 C1 118.50(12) . . ? C5 N1 Pd1 120.62(9) . . ? C1 N1 Pd1 120.87(10) . . ? N1 C1 C2 122.27(14) . . ? N1 C1 H1 114.9(9) . . ? C2 C1 H1 122.8(9) . . ? C1 C2 C3 119.99(14) . . ? C1 C2 H2 121.6(10) . . ? C3 C2 H2 118.3(10) . . ? C4 C3 C2 116.79(13) . . ? C4 C3 C6 121.82(14) . . ? C2 C3 C6 121.39(13) . . ? C5 C4 C3 120.68(14) . . ? C5 C4 H4 118.2(10) . . ? C3 C4 H4 121.0(10) . . ? N1 C5 C4 121.76(13) . . ? N1 C5 H5 115.0(10) . . ? C4 C5 H5 123.3(10) . . ? C3 C6 H6A 112.1(10) . . ? C3 C6 H6B 110.1(11) . . ? H6A C6 H6B 108.6(16) . . ? C3 C6 H6C 109.6(11) . . ? H6A C6 H6C 106.0(16) . . ? H6B C6 H6C 110.4(17) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Pd1 N1 C5 79(19) 3_655 . . . ? Cl1 Pd1 N1 C5 124.87(11) . . . . ? Cl1 Pd1 N1 C5 -55.13(11) 3_655 . . . ? N1 Pd1 N1 C1 -100(19) 3_655 . . . ? Cl1 Pd1 N1 C1 -54.02(11) . . . . ? Cl1 Pd1 N1 C1 125.98(11) 3_655 . . . ? C5 N1 C1 C2 -0.5(2) . . . . ? Pd1 N1 C1 C2 178.44(11) . . . . ? N1 C1 C2 C3 -0.2(2) . . . . ? C1 C2 C3 C4 0.6(2) . . . . ? C1 C2 C3 C6 -179.60(15) . . . . ? C2 C3 C4 C5 -0.3(2) . . . . ? C6 C3 C4 C5 179.91(15) . . . . ? C1 N1 C5 C4 0.8(2) . . . . ? Pd1 N1 C5 C4 -178.12(12) . . . . ? C3 C4 C5 N1 -0.4(2) . . . . ? _diffrn_measured_fraction_theta_max 0.940 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.380 _refine_diff_density_min -0.402 _refine_diff_density_rms 0.064