# Electronic Supplementary Material (ESI) for Polymer Chemistry # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_3 _audit_creation_date 2012-08-28 _audit_creation_method ; Olex2 1.1 (compiled Nov 1 2011 20:42:30, GUI svn.r3906) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C11.5 H9.5 N3.5' _chemical_formula_sum 'C11.50 H9.50 N3.50' _chemical_formula_weight 196.73 _chemical_absolute_configuration unk _chemical_melting_point ? 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' _space_group_crystal_system tetragonal _space_group_IT_number 96 _space_group_name_H-M_alt 'P 43 21 2' _space_group_name_Hall 'P 4nw 2abw' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-y+1/2, x+1/2, z+3/4' 3 '-x, -y, z+1/2' 4 'y+1/2, -x+1/2, z+1/4' 5 'x+1/2, -y+1/2, -z+1/4' 6 '-x+1/2, y+1/2, -z+3/4' 7 'y, x, -z' 8 '-y, -x, -z+1/2' _cell_length_a 6.1133(9) _cell_length_b 6.1133(9) _cell_length_c 52.627(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1966.8(6) _cell_formula_units_Z 8 _cell_measurement_reflns_used 5144 _cell_measurement_temperature 200(2) _cell_measurement_theta_max 24.59 _cell_measurement_theta_min 1.55 _exptl_absorpt_coefficient_mu 0.08 _exptl_absorpt_correction_T_max 0.9838 _exptl_absorpt_correction_T_min 0.9748 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details ? _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.329 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 824 _exptl_crystal_size_max 0.398 _exptl_crystal_size_mid 0.311 _exptl_crystal_size_min 0.194 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0418 _diffrn_reflns_av_unetI/netI 0.0474 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 58 _diffrn_reflns_limit_l_min -65 _diffrn_reflns_number 10517 _diffrn_reflns_theta_full 26.79 _diffrn_reflns_theta_max 26.80 _diffrn_reflns_theta_min 1.55 _diffrn_ambient_temperature 200.15 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.988 _diffrn_measured_fraction_theta_max 0.988 _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 1339 _reflns_number_total 2082 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ? _computing_data_collection ? _computing_data_reduction ? _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; SHELXL, G.M. Sheldrick, Acta Cryst. 2008). A64, 112-122 ; _computing_structure_solution ; SHELXS, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _refine_diff_density_max 0.082 _refine_diff_density_min -0.134 _refine_diff_density_rms 0.026 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -1(3) _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.899 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 138 _refine_ls_number_reflns 2082 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0775 _refine_ls_R_factor_gt 0.0375 _refine_ls_restrained_S_all 0.899 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0336P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0648 _refine_ls_wR_factor_ref 0.0742 _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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 N1 N 0.4195(2) 0.8093(2) 0.05544(3) 0.0539(4) Uani 1 1 d . . . N2 N -0.0675(2) 0.9325(2) 0.0000 0.0559(5) Uani 1 2 d S . . N3 N 0.3721(3) 0.5930(3) 0.05778(3) 0.0664(4) Uani 1 1 d . . . N4 N 0.2008(3) 0.5554(3) 0.04345(3) 0.0681(5) Uani 1 1 d . . . C5 C -0.2061(3) 0.5876(3) 0.01490(4) 0.0639(5) Uani 1 1 d . . . H5 H -0.1852 0.4606 0.0250 0.077 Uiso 1 1 calc R . . C6 C 0.6052(3) 0.8971(3) 0.06839(3) 0.0513(4) Uani 1 1 d . . . C7 C 0.2772(3) 0.9056(3) 0.03935(4) 0.0545(5) Uani 1 1 d . . . H7 H 0.2747 1.0548 0.0343 0.065 Uiso 1 1 calc R . . C8 C -0.3899(3) 0.6101(3) 0.0000 0.0658(7) Uani 1 2 d S . . H8 H -0.4998 0.5002 0.0000 0.079 Uiso 1 2 calc SR . . C9 C 0.6796(3) 1.1035(3) 0.06267(4) 0.0642(5) Uani 1 1 d . . . H9 H 0.6059 1.1899 0.0504 0.077 Uiso 1 1 calc R . . C10 C -0.0520(3) 0.7540(3) 0.01483(4) 0.0559(5) Uani 1 1 d . . . C11 C 0.8953(3) 0.8576(3) 0.09829(4) 0.0713(6) Uani 1 1 d . . . H11 H 0.9689 0.7709 0.1106 0.086 Uiso 1 1 calc R . . C12 C 0.1380(3) 0.7444(3) 0.03185(4) 0.0556(5) Uani 1 1 d . . . C13 C 0.7133(3) 0.7740(3) 0.08627(4) 0.0677(5) Uani 1 1 d . . . H13 H 0.6626 0.6313 0.0903 0.081 Uiso 1 1 calc R . . C14 C 0.9731(3) 1.0643(3) 0.09288(4) 0.0572(5) Uani 1 1 d . . . C15 C 1.1709(3) 1.1579(3) 0.10631(4) 0.0735(6) Uani 1 1 d . . . H15A H 1.1248 1.2279 0.1222 0.110 Uiso 1 1 calc R . . H15B H 1.2416 1.2665 0.0953 0.110 Uiso 1 1 calc R . . H15C H 1.2746 1.0400 0.1101 0.110 Uiso 1 1 calc R . . C16 C 0.8621(3) 1.1845(3) 0.07493(4) 0.0650(5) Uani 1 1 d . . . H16 H 0.9125 1.3272 0.0709 0.078 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 N1 0.0589(9) 0.0467(8) 0.0561(10) 0.0084(7) 0.0049(8) 0.0003(7) N2 0.0565(8) 0.0565(8) 0.0545(14) -0.0043(8) 0.0043(8) -0.0041(10) N3 0.0686(11) 0.0524(10) 0.0781(12) 0.0166(8) 0.0034(9) -0.0046(8) N4 0.0663(10) 0.0590(10) 0.0789(13) 0.0099(9) 0.0055(10) -0.0090(8) C5 0.0680(12) 0.0643(12) 0.0594(13) -0.0029(11) 0.0096(10) -0.0079(10) C6 0.0554(11) 0.0479(10) 0.0507(12) 0.0052(9) 0.0072(9) 0.0065(9) C7 0.0610(11) 0.0488(10) 0.0536(12) 0.0074(9) 0.0073(10) 0.0018(9) C8 0.0675(10) 0.0675(10) 0.062(2) -0.0142(12) 0.0142(12) -0.0176(14) C9 0.0651(12) 0.0567(12) 0.0708(14) 0.0204(11) -0.0021(10) 0.0015(9) C10 0.0589(11) 0.0572(11) 0.0517(12) -0.0061(9) 0.0124(10) -0.0044(9) C11 0.0842(14) 0.0633(13) 0.0663(15) 0.0141(11) -0.0137(12) 0.0044(11) C12 0.0594(11) 0.0526(11) 0.0548(12) 0.0058(9) 0.0113(9) -0.0009(9) C13 0.0858(15) 0.0518(11) 0.0656(14) 0.0137(10) -0.0081(12) -0.0051(10) C14 0.0576(11) 0.0630(12) 0.0509(13) 0.0022(10) 0.0057(9) 0.0065(9) C15 0.0669(13) 0.0835(15) 0.0702(15) 0.0022(11) -0.0008(11) -0.0002(10) C16 0.0631(13) 0.0559(11) 0.0761(15) 0.0127(11) 0.0011(11) -0.0042(9) _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 N1 N3 1.3591(19) . ? N1 C6 1.429(2) . ? N1 C7 1.349(2) . ? N2 C10 1.3449(19) 7_465 ? N2 C10 1.3448(19) . ? N3 N4 1.311(2) . ? N4 C12 1.362(2) . ? C5 C8 1.377(2) . ? C5 C10 1.387(2) . ? C6 C9 1.374(2) . ? C6 C13 1.374(2) . ? C7 C12 1.361(2) . ? C8 C5 1.377(2) 7_465 ? C9 C16 1.381(3) . ? C10 C12 1.468(3) . ? C11 C13 1.379(3) . ? C11 C14 1.380(2) . ? C14 C15 1.513(3) . ? C14 C16 1.376(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 N3 N1 C6 119.44(14) . . ? C7 N1 N3 110.12(15) . . ? C7 N1 C6 130.37(14) . . ? C10 N2 C10 116.8(2) . 7_465 ? N4 N3 N1 106.79(15) . . ? N3 N4 C12 109.52(15) . . ? C8 C5 C10 118.6(2) . . ? C9 C6 N1 120.22(16) . . ? C13 C6 N1 120.19(15) . . ? C13 C6 C9 119.58(18) . . ? N1 C7 C12 105.61(16) . . ? C5 C8 C5 119.2(3) . 7_465 ? C6 C9 C16 119.63(18) . . ? N2 C10 C5 123.30(18) . . ? N2 C10 C12 116.27(14) . . ? C5 C10 C12 120.42(17) . . ? C13 C11 C14 121.57(19) . . ? N4 C12 C10 122.05(16) . . ? C7 C12 N4 107.95(17) . . ? C7 C12 C10 129.99(17) . . ? C6 C13 C11 119.94(18) . . ? C11 C14 C15 121.72(18) . . ? C16 C14 C11 117.42(19) . . ? C16 C14 C15 120.85(18) . . ? C14 C16 C9 121.86(18) . . ? _database_code_depnum_ccdc_archive 'CCDC 939314' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_4 _audit_creation_date 2013-05-15 _audit_creation_method ; Olex2 1.2 (compiled Apr 23 2013 17:59:47, GUI svn.r4466) ; #============================================================================== _chemical_formula_moiety 'C23 H19 Cl N7 Pd, C2 H6 Cl3 O Pd S, 2(C2 H6 O S)' _chemical_formula_sum 'C29 H37 Cl4 N7 O3 Pd2 S3' _chemical_formula_weight 982.43 _chemical_melting_point ? 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' 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' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.6458(17) _cell_length_b 13.837(3) _cell_length_c 17.394(4) _cell_angle_alpha 109.67(3) _cell_angle_beta 102.90(3) _cell_angle_gamma 95.46(3) _cell_volume 1876.9(8) _cell_formula_units_Z 2 _cell_measurement_reflns_used 11365 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 29.14 _cell_measurement_theta_min 1.59 _exptl_absorpt_coefficient_mu 1.451 _exptl_absorpt_correction_T_max 0.9506 _exptl_absorpt_correction_T_min 0.7627 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details 'STOE X-RED & X-SHAPE' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.738 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description needle _exptl_crystal_F_000 984 _exptl_crystal_size_max 0.434 _exptl_crystal_size_mid 0.182 _exptl_crystal_size_min 0.041 _exptl_special_details ; ? ; _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.1020 _diffrn_reflns_av_unetI/netI 0.1040 _diffrn_reflns_Laue_measured_fraction_full 0.962 _diffrn_reflns_Laue_measured_fraction_max 0.962 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 12065 _diffrn_reflns_point_group_measured_fraction_full 0.962 _diffrn_reflns_point_group_measured_fraction_max 0.962 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.251 _diffrn_reflns_theta_min 1.591 _diffrn_ambient_temperature 150.15 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.962 _diffrn_measured_fraction_theta_max 0.962 _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_measurement_method 'rotation method' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source ? _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 4222 _reflns_number_total 6552 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; SHELXL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ? _refine_diff_density_max 2.679 _refine_diff_density_min -1.951 _refine_diff_density_rms 0.237 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.952 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 461 _refine_ls_number_reflns 6552 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.1137 _refine_ls_R_factor_gt 0.0797 _refine_ls_restrained_S_all 0.952 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.1347P)^2^] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1915 _refine_ls_wR_factor_ref 0.2102 _refine_special_details ; ? ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2. Uiso/Uaniso restraints and constraints Uanis(S3B) = Uanis(O3B) = Uanis(C28B) = Uanis(C29B) 3. Same fragment restrains {S2, O2, C26, C27} as {S3A, O3A, C28A, C29A} {S2, O2, C26, C27} as {S3B, O3B, C28B, C29B} 4. Others Fixed Sof: S3A(0.75) O3A(0.75) C28A(0.75) H28A(0.75) H28B(0.75) H28C(0.75) C29A(0.75) H29A(0.75) H29B(0.75) H29C(0.75) S3B(0.25) O3B(0.25) C28B(0.25) H28D(0.25) H28E(0.25) H28F(0.25) C29B(0.25) H29D(0.25) H29E(0.25) H29F(0.25) 5.a Aromatic/amide H refined with riding coordinates: C1(H1), C2(H2), C5(H5), C7(H7), C8(H8), C10(H10), C11(H11), C13(H13), C16(H16), C18(H18), C19(H19), C21(H21), C22(H22) 5.b Idealised Me refined as rotating group: C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C12(H12A,H12B,H12C), C23(H23A,H23B, H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C28A(H28A,H28B,H28C), C29A(H29A,H29B,H29C), C28B(H28D,H28E,H28F), C29B(H29D,H29E,H29F) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary ? _atom_sites_solution_secondary ? 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.31429(9) 0.97514(6) 0.93793(5) 0.0326(2) Uani 1 1 d . . . . . Pd2 Pd 0.89989(9) 0.68687(6) 0.19001(5) 0.0339(2) Uani 1 1 d . . . . . Cl1 Cl 0.3483(3) 1.14924(19) 0.96153(17) 0.0411(6) Uani 1 1 d . . . . . Cl2 Cl 0.9656(3) 0.7631(2) 0.33564(16) 0.0443(6) Uani 1 1 d . . . . . Cl3 Cl 1.1679(3) 0.7177(2) 0.19130(18) 0.0436(6) Uani 1 1 d . . . . . Cl4 Cl 0.8326(3) 0.6071(2) 0.04556(17) 0.0456(6) Uani 1 1 d . . . . . S1 S 0.6414(3) 0.6652(2) 0.19459(17) 0.0399(6) Uani 1 1 d . . . . . S2 S 0.7841(5) 0.5642(3) 0.7306(2) 0.0643(9) Uani 1 1 d D . . . . O2 O 0.6517(17) 0.6142(9) 0.6977(7) 0.098(4) Uani 1 1 d D . . . . C26 C 0.7282(18) 0.4293(9) 0.6716(9) 0.065(4) Uani 1 1 d D . . . . H26A H 0.6263 0.4025 0.6796 0.098 Uiso 1 1 calc R U . . . H26B H 0.8126 0.3937 0.6909 0.098 Uiso 1 1 calc R U . . . H26C H 0.7144 0.4166 0.6113 0.098 Uiso 1 1 calc R U . . . C27 C 0.7663(16) 0.5611(13) 0.8297(8) 0.066(4) Uani 1 1 d D . . . . H27A H 0.8033 0.6314 0.8733 0.099 Uiso 1 1 calc R U . . . H27B H 0.8326 0.5135 0.8455 0.099 Uiso 1 1 calc R U . . . H27C H 0.6531 0.5366 0.8248 0.099 Uiso 1 1 calc R U . . . O1 O 0.6026(10) 0.5946(7) 0.2363(6) 0.057(2) Uani 1 1 d . . . . . N1 N 0.2775(10) 0.8242(6) 0.9153(5) 0.0336(17) Uani 1 1 d . . . . . N2 N 0.4072(10) 0.9237(6) 0.8387(5) 0.0369(19) Uani 1 1 d . . . . . N3 N 0.4625(11) 0.9665(7) 0.7911(5) 0.040(2) Uani 1 1 d . . . . . N4 N 0.4990(11) 0.8867(7) 0.7323(6) 0.041(2) Uani 1 1 d . . . . . N5 N 0.2034(10) 0.9741(6) 1.0275(5) 0.0334(17) Uani 1 1 d . . . . . N6 N 0.1624(10) 1.0436(7) 1.0883(5) 0.0373(19) Uani 1 1 d . . . . . N7 N 0.0881(10) 0.9888(6) 1.1250(5) 0.0353(18) Uani 1 1 d . . . . . C1 C 0.2394(14) 0.6177(8) 0.8895(7) 0.043(2) Uani 1 1 d . . . . . H1 H 0.2252 0.5452 0.8797 0.052 Uiso 1 1 calc R U . . . C2 C 0.3173(13) 0.6560(8) 0.8415(7) 0.043(2) Uani 1 1 d . . . . . H2 H 0.3586 0.6104 0.7998 0.051 Uiso 1 1 calc R U . . . C3 C 0.3344(12) 0.7605(8) 0.8547(6) 0.037(2) Uani 1 1 d . . . . . C4 C 0.4026(13) 0.8175(8) 0.8107(7) 0.040(2) Uani 1 1 d . . . . . C5 C 0.4650(14) 0.7954(8) 0.7406(7) 0.040(2) Uani 1 1 d . . . . . H5 H 0.4801 0.7293 0.7061 0.048 Uiso 1 1 calc R U . . . C6 C 0.5566(14) 0.9089(8) 0.6664(7) 0.045(3) Uani 1 1 d . . . . . C7 C 0.5295(18) 0.8290(9) 0.5884(8) 0.057(3) Uani 1 1 d . . . . . H7 H 0.4725 0.7612 0.5765 0.068 Uiso 1 1 calc R U . . . C8 C 0.5909(16) 0.8537(9) 0.5279(8) 0.050(3) Uani 1 1 d . . . . . H8 H 0.5743 0.8011 0.4735 0.060 Uiso 1 1 calc R U . . . C9 C 0.6743(13) 0.9515(9) 0.5449(7) 0.044(3) Uani 1 1 d . . . . . C10 C 0.6953(12) 1.0293(9) 0.6233(7) 0.042(2) Uani 1 1 d . . . . . H10 H 0.7514 1.0973 0.6351 0.050 Uiso 1 1 calc R U . . . C11 C 0.6351(12) 1.0088(8) 0.6849(7) 0.040(2) Uani 1 1 d . . . . . H11 H 0.6477 1.0622 0.7385 0.048 Uiso 1 1 calc R U . . . C12 C 0.7481(16) 0.9753(11) 0.4795(8) 0.054(3) Uani 1 1 d . . . . . H12A H 0.6660 0.9930 0.4402 0.082 Uiso 1 1 calc R U . . . H12B H 0.7868 0.9138 0.4478 0.082 Uiso 1 1 calc R U . . . H12C H 0.8387 1.0343 0.5087 0.082 Uiso 1 1 calc R U . . . C13 C 0.1812(13) 0.6847(8) 0.9524(7) 0.040(2) Uani 1 1 d . . . . . H13 H 0.1284 0.6591 0.9860 0.048 Uiso 1 1 calc R U . . . C14 C 0.2031(12) 0.7886(8) 0.9638(6) 0.038(2) Uani 1 1 d . . . . . C15 C 0.1589(11) 0.8739(8) 1.0251(6) 0.034(2) Uani 1 1 d . . . . . C16 C 0.0821(12) 0.8840(8) 1.0884(6) 0.038(2) Uani 1 1 d . . . . . H16 H 0.0356 0.8300 1.1030 0.045 Uiso 1 1 calc R U . . . C17 C 0.0347(12) 1.0437(8) 1.1990(6) 0.037(2) Uani 1 1 d . . . . . C18 C -0.0355(14) 0.9865(9) 1.2370(7) 0.043(2) Uani 1 1 d . . . . . H18 H -0.0551 0.9123 1.2140 0.052 Uiso 1 1 calc R U . . . C19 C -0.0769(13) 1.0400(8) 1.3096(7) 0.045(3) Uani 1 1 d . . . . . H19 H -0.1261 1.0012 1.3365 0.054 Uiso 1 1 calc R U . . . C20 C -0.0497(14) 1.1484(9) 1.3452(7) 0.043(2) Uani 1 1 d . . . . . C21 C 0.0174(18) 1.2021(10) 1.3019(9) 0.061(3) Uani 1 1 d . . . . . H21 H 0.0358 1.2763 1.3237 0.073 Uiso 1 1 calc R U . . . C22 C 0.0582(15) 1.1499(9) 1.2275(7) 0.048(3) Uani 1 1 d . . . . . H22 H 0.1010 1.1872 1.1976 0.057 Uiso 1 1 calc R U . . . C23 C -0.0901(18) 1.2052(10) 1.4256(8) 0.059(3) Uani 1 1 d . . . . . H23A H -0.1877 1.1656 1.4283 0.088 Uiso 1 1 calc R U . . . H23B H -0.1090 1.2745 1.4272 0.088 Uiso 1 1 calc R U . . . H23C H -0.0001 1.2128 1.4741 0.088 Uiso 1 1 calc R U . . . C24 C 0.5992(13) 0.7897(9) 0.2459(8) 0.048(3) Uani 1 1 d . . . . . H24A H 0.6710 0.8212 0.3036 0.072 Uiso 1 1 calc R U . . . H24B H 0.4867 0.7824 0.2482 0.072 Uiso 1 1 calc R U . . . H24C H 0.6165 0.8345 0.2142 0.072 Uiso 1 1 calc R U . . . C25 C 0.4927(12) 0.6256(9) 0.0944(7) 0.047(3) Uani 1 1 d . . . . . H25A H 0.5268 0.6630 0.0604 0.071 Uiso 1 1 calc R U . . . H25B H 0.3889 0.6418 0.1038 0.071 Uiso 1 1 calc R U . . . H25C H 0.4810 0.5502 0.0642 0.071 Uiso 1 1 calc R U . . . S3A S 0.2015(7) 0.4893(4) 0.5188(4) 0.0709(13) Uani 0.75 1 d D . P A 1 O3A O 0.296(3) 0.5959(13) 0.5417(19) 0.117(8) Uani 0.75 1 d D . P A 1 C28A C 0.338(3) 0.4056(16) 0.5018(16) 0.089(8) Uani 0.75 1 d D . P A 1 H28A H 0.3485 0.3889 0.4441 0.133 Uiso 0.75 1 calc R U P A 1 H28B H 0.2986 0.3412 0.5090 0.133 Uiso 0.75 1 calc R U P A 1 H28C H 0.4429 0.4394 0.5428 0.133 Uiso 0.75 1 calc R U P A 1 C29A C 0.171(3) 0.485(2) 0.6150(12) 0.099(9) Uani 0.75 1 d D . P A 1 H29A H 0.2445 0.4443 0.6360 0.149 Uiso 0.75 1 calc R U P A 1 H29B H 0.0591 0.4524 0.6051 0.149 Uiso 0.75 1 calc R U P A 1 H29C H 0.1926 0.5563 0.6571 0.149 Uiso 0.75 1 calc R U P A 1 S3B S 0.2967(17) 0.5231(11) 0.6050(9) 0.063(3) Uani 0.25 1 d D . P B 2 O3B O 0.277(7) 0.591(3) 0.554(3) 0.063(3) Uani 0.25 1 d D . P B 2 C28B C 0.328(7) 0.404(3) 0.540(3) 0.063(3) Uani 0.25 1 d D . P B 2 H28D H 0.2577 0.3849 0.4821 0.095 Uiso 0.25 1 calc R U P B 2 H28E H 0.3024 0.3497 0.5619 0.095 Uiso 0.25 1 calc R U P B 2 H28F H 0.4410 0.4101 0.5383 0.095 Uiso 0.25 1 calc R U P B 2 C29B C 0.104(5) 0.482(4) 0.614(4) 0.063(3) Uani 0.25 1 d D . P B 2 H29D H 0.0894 0.5281 0.6672 0.095 Uiso 0.25 1 calc R U P B 2 H29E H 0.0947 0.4102 0.6124 0.095 Uiso 0.25 1 calc R U P B 2 H29F H 0.0209 0.4843 0.5660 0.095 Uiso 0.25 1 calc R U P 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 0.0267(4) 0.0344(4) 0.0433(4) 0.0179(3) 0.0136(3) 0.0125(3) Pd2 0.0243(4) 0.0360(4) 0.0448(4) 0.0148(3) 0.0152(3) 0.0076(3) Cl1 0.0386(13) 0.0344(12) 0.0544(14) 0.0189(11) 0.0151(11) 0.0106(10) Cl2 0.0299(12) 0.0542(15) 0.0474(14) 0.0157(12) 0.0131(10) 0.0065(11) Cl3 0.0240(11) 0.0553(15) 0.0638(16) 0.0295(13) 0.0205(11) 0.0159(10) Cl4 0.0381(14) 0.0534(15) 0.0473(14) 0.0162(12) 0.0198(11) 0.0075(11) S1 0.0325(13) 0.0411(13) 0.0452(13) 0.0138(11) 0.0116(11) 0.0078(10) S2 0.057(2) 0.069(2) 0.079(2) 0.0385(18) 0.0237(17) 0.0156(16) O2 0.133(11) 0.083(7) 0.082(7) 0.031(6) 0.017(7) 0.070(7) C26 0.067(9) 0.063(8) 0.089(10) 0.045(7) 0.029(7) 0.036(7) C27 0.040(7) 0.100(11) 0.068(8) 0.041(8) 0.022(6) 0.008(7) O1 0.040(4) 0.067(5) 0.071(5) 0.034(4) 0.019(4) 0.006(4) N1 0.032(4) 0.035(4) 0.037(4) 0.014(3) 0.011(3) 0.013(3) N2 0.038(5) 0.035(4) 0.048(5) 0.026(4) 0.014(4) 0.013(4) N3 0.040(5) 0.047(5) 0.041(4) 0.020(4) 0.016(4) 0.018(4) N4 0.037(5) 0.040(5) 0.055(5) 0.019(4) 0.025(4) 0.021(4) N5 0.027(4) 0.038(4) 0.042(4) 0.018(3) 0.012(3) 0.018(3) N6 0.032(4) 0.047(5) 0.041(4) 0.024(4) 0.012(4) 0.014(4) N7 0.033(4) 0.043(5) 0.040(4) 0.023(4) 0.016(4) 0.013(4) C1 0.043(6) 0.038(5) 0.054(6) 0.021(5) 0.016(5) 0.015(5) C2 0.037(6) 0.044(6) 0.046(6) 0.015(5) 0.009(5) 0.015(5) C3 0.031(5) 0.037(5) 0.048(6) 0.017(4) 0.013(4) 0.014(4) C4 0.042(6) 0.039(5) 0.044(5) 0.020(4) 0.010(4) 0.017(5) C5 0.051(6) 0.034(5) 0.049(6) 0.020(4) 0.026(5) 0.024(5) C6 0.052(7) 0.042(6) 0.059(7) 0.025(5) 0.033(5) 0.026(5) C7 0.081(9) 0.040(6) 0.066(8) 0.025(6) 0.041(7) 0.022(6) C8 0.062(8) 0.044(6) 0.059(7) 0.019(5) 0.039(6) 0.021(5) C9 0.035(6) 0.055(6) 0.050(6) 0.020(5) 0.020(5) 0.015(5) C10 0.023(5) 0.059(6) 0.050(6) 0.026(5) 0.012(4) 0.007(4) C11 0.029(5) 0.048(6) 0.044(5) 0.017(5) 0.012(4) 0.007(4) C12 0.055(8) 0.068(8) 0.061(7) 0.034(6) 0.034(6) 0.024(6) C13 0.033(5) 0.039(5) 0.050(6) 0.020(5) 0.012(4) 0.007(4) C14 0.035(5) 0.047(6) 0.040(5) 0.022(4) 0.015(4) 0.010(4) C15 0.023(5) 0.040(5) 0.047(5) 0.022(4) 0.013(4) 0.012(4) C16 0.029(5) 0.045(6) 0.047(6) 0.023(5) 0.015(4) 0.006(4) C17 0.036(5) 0.046(6) 0.036(5) 0.021(4) 0.011(4) 0.017(4) C18 0.040(6) 0.042(6) 0.050(6) 0.015(5) 0.021(5) 0.011(5) C19 0.031(5) 0.045(6) 0.065(7) 0.025(5) 0.020(5) 0.011(5) C20 0.045(6) 0.047(6) 0.044(6) 0.022(5) 0.016(5) 0.021(5) C21 0.079(9) 0.039(6) 0.074(8) 0.021(6) 0.035(7) 0.020(6) C22 0.053(7) 0.047(6) 0.058(7) 0.027(5) 0.027(5) 0.021(5) C23 0.071(9) 0.052(7) 0.062(7) 0.019(6) 0.038(7) 0.014(6) C24 0.031(5) 0.044(6) 0.062(7) 0.005(5) 0.019(5) 0.013(5) C25 0.023(5) 0.058(7) 0.050(6) 0.011(5) 0.003(4) 0.008(5) S3A 0.065(3) 0.073(3) 0.085(3) 0.036(3) 0.026(3) 0.023(2) O3A 0.118(18) 0.068(10) 0.17(2) 0.031(11) 0.075(15) 0.021(10) C28A 0.13(2) 0.067(13) 0.094(17) 0.044(12) 0.043(16) 0.032(14) C29A 0.079(18) 0.16(3) 0.055(12) 0.020(14) 0.023(13) 0.040(19) S3B 0.043(7) 0.064(7) 0.077(8) 0.033(6) 0.004(6) -0.009(6) O3B 0.043(7) 0.064(7) 0.077(8) 0.033(6) 0.004(6) -0.009(6) C28B 0.043(7) 0.064(7) 0.077(8) 0.033(6) 0.004(6) -0.009(6) C29B 0.043(7) 0.064(7) 0.077(8) 0.033(6) 0.004(6) -0.009(6) _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 Cl1 2.281(3) . ? Pd1 N1 1.971(8) . ? Pd1 N2 2.008(8) . ? Pd1 N5 2.006(8) . ? Pd2 Cl2 2.301(3) . ? Pd2 Cl3 2.310(3) . ? Pd2 Cl4 2.286(3) . ? Pd2 S1 2.249(3) . ? S1 O1 1.455(9) . ? S1 C24 1.768(10) . ? S1 C25 1.793(11) . ? S2 O2 1.498(10) . ? S2 C26 1.757(13) . ? S2 C27 1.778(12) . ? N1 C3 1.348(12) . ? N1 C14 1.352(14) . ? N2 N3 1.310(12) . ? N2 C4 1.378(13) . ? N3 N4 1.347(11) . ? N4 C5 1.332(14) . ? N4 C6 1.456(14) . ? N5 N6 1.311(11) . ? N5 C15 1.386(13) . ? N6 N7 1.345(12) . ? N7 C16 1.365(13) . ? N7 C17 1.456(12) . ? C1 C2 1.382(17) . ? C1 C13 1.400(15) . ? C2 C3 1.373(15) . ? C3 C4 1.441(16) . ? C4 C5 1.395(15) . ? C6 C7 1.385(16) . ? C6 C11 1.378(16) . ? C7 C8 1.400(17) . ? C8 C9 1.375(17) . ? C9 C10 1.384(15) . ? C9 C12 1.530(16) . ? C10 C11 1.388(15) . ? C13 C14 1.372(15) . ? C14 C15 1.448(14) . ? C15 C16 1.383(14) . ? C17 C18 1.369(16) . ? C17 C22 1.362(15) . ? C18 C19 1.376(15) . ? C19 C20 1.390(15) . ? C20 C21 1.395(18) . ? C20 C23 1.493(15) . ? C21 C22 1.394(17) . ? S3A O3A 1.493(17) . ? S3A C28A 1.732(17) . ? S3A C29A 1.770(17) . ? S3B O3B 1.49(2) . ? S3B C28B 1.75(2) . ? S3B C29B 1.76(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 Cl1 178.1(2) . . ? N1 Pd1 N2 80.0(3) . . ? N1 Pd1 N5 80.5(3) . . ? N2 Pd1 Cl1 100.2(2) . . ? N5 Pd1 Cl1 99.2(2) . . ? N5 Pd1 N2 160.4(3) . . ? Cl2 Pd2 Cl3 91.25(10) . . ? Cl4 Pd2 Cl2 178.53(11) . . ? Cl4 Pd2 Cl3 89.30(10) . . ? S1 Pd2 Cl2 86.28(10) . . ? S1 Pd2 Cl3 176.90(10) . . ? S1 Pd2 Cl4 93.21(10) . . ? O1 S1 Pd2 114.4(4) . . ? O1 S1 C24 110.3(6) . . ? O1 S1 C25 107.8(6) . . ? C24 S1 Pd2 107.9(4) . . ? C24 S1 C25 100.0(6) . . ? C25 S1 Pd2 115.5(4) . . ? O2 S2 C26 106.9(7) . . ? O2 S2 C27 108.0(7) . . ? C26 S2 C27 97.8(7) . . ? C3 N1 Pd1 118.9(7) . . ? C3 N1 C14 122.2(9) . . ? C14 N1 Pd1 118.9(6) . . ? N3 N2 Pd1 134.9(7) . . ? N3 N2 C4 112.3(8) . . ? C4 N2 Pd1 112.6(7) . . ? N2 N3 N4 104.5(8) . . ? N3 N4 C6 117.6(8) . . ? C5 N4 N3 113.0(8) . . ? C5 N4 C6 129.2(8) . . ? N6 N5 Pd1 136.6(7) . . ? N6 N5 C15 111.3(8) . . ? C15 N5 Pd1 112.1(6) . . ? N5 N6 N7 105.5(8) . . ? N6 N7 C16 112.4(8) . . ? N6 N7 C17 119.7(8) . . ? C16 N7 C17 127.7(9) . . ? C2 C1 C13 120.7(10) . . ? C3 C2 C1 119.4(10) . . ? N1 C3 C2 119.4(10) . . ? N1 C3 C4 110.8(9) . . ? C2 C3 C4 129.8(10) . . ? N2 C4 C3 117.5(9) . . ? N2 C4 C5 104.7(9) . . ? C5 C4 C3 137.7(10) . . ? N4 C5 C4 105.4(8) . . ? C7 C6 N4 118.6(10) . . ? C11 C6 N4 118.1(9) . . ? C11 C6 C7 123.3(11) . . ? C6 C7 C8 116.3(12) . . ? C9 C8 C7 122.1(11) . . ? C8 C9 C10 119.3(10) . . ? C8 C9 C12 121.3(10) . . ? C10 C9 C12 119.4(11) . . ? C9 C10 C11 120.6(11) . . ? C6 C11 C10 118.3(10) . . ? C14 C13 C1 117.7(10) . . ? N1 C14 C13 120.7(9) . . ? N1 C14 C15 110.5(9) . . ? C13 C14 C15 128.8(10) . . ? N5 C15 C14 117.9(9) . . ? C16 C15 N5 106.3(8) . . ? C16 C15 C14 135.8(10) . . ? N7 C16 C15 104.5(9) . . ? C18 C17 N7 118.7(9) . . ? C22 C17 N7 118.3(10) . . ? C22 C17 C18 123.1(10) . . ? C17 C18 C19 117.7(10) . . ? C18 C19 C20 122.8(11) . . ? C19 C20 C21 116.7(10) . . ? C19 C20 C23 122.0(11) . . ? C21 C20 C23 121.3(11) . . ? C22 C21 C20 121.8(11) . . ? C17 C22 C21 117.9(11) . . ? O3A S3A C28A 105.6(13) . . ? O3A S3A C29A 105.2(13) . . ? C28A S3A C29A 100.7(11) . . ? O3B S3B C28B 107(2) . . ? O3B S3B C29B 107(2) . . ? C28B S3B C29B 99.2(18) . . ? _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _shelx_hkl_checksum 6140 #============================================================================== _database_code_depnum_ccdc_archive 'CCDC 939315'