# Electronic Supplementary Material (ESI) for Polymer Chemistry # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Polym.Chem. _journal_coden_cambridge 1478 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name _publ_author_address P.W.Roesky ; Karlsruher Institut f\"ur Technologie (KIT) Institut f\"ur Anorganische Chemie Engesserstr. 15, Geb. 30.45 76131 Karlsruhe Bundesrepublik Deutschland ; C.Kiefer ; Karlsruher Institut f\"ur Technologie (KIT) Institut f\"ur Anorganische Chemie Engesserstr. 15, Geb. 30.45 76131 Karlsruhe Bundesrepublik Deutschland ; _publ_contact_author ; Prof. Dr. Peter W. Roesky Karlsruher Institut f\"ur Technologie (KIT) Institut f\"ur Anorganische Chemie Engesserstr. 15, Geb. 30.45 76131 Karlsruhe Bundesrepublik Deutschland ; _publ_contact_author_email roesky@kit.edu _publ_contact_author_fax '+49 721 608 44854' _publ_contact_author_phone '+49 721 608 46117' _publ_contact_letter ; ; _publ_requested_coeditor_name ? _publ_section_title ; ; _publ_contact_author_name 'Prof. Dr. Peter W. Roesky' data_Ligand _database_code_depnum_ccdc_archive 'CCDC 873652' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H12 N4' _chemical_formula_weight 236.28 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' _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 5.8594(12) _cell_length_b 19.801(4) _cell_length_c 10.253(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.18(3) _cell_angle_gamma 90.00 _cell_volume 1180.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.373 _exptl_crystal_size_mid 0.088 _exptl_crystal_size_min 0.071 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.330 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 496 _exptl_absorpt_coefficient_mu 0.084 _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 200(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 'STOE IPDS 2' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18147 _diffrn_reflns_av_R_equivalents 0.0617 _diffrn_reflns_av_sigmaI/netI 0.0465 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 29.18 _reflns_number_total 3164 _reflns_number_gt 2105 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA, PLATON (A.L.Spek, 2005)' _computing_data_reduction 'STOE X-RED, PLATON (A.L.Spek, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e/3' _computing_publication_material 'X-STEP32, Microsoft Word' _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^)+(0.0591P)^2^+0.0791P] 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 3164 _refine_ls_number_parameters 200 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0945 _refine_ls_R_factor_gt 0.0548 _refine_ls_wR_factor_ref 0.1242 _refine_ls_wR_factor_gt 0.1114 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _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 N1 N 0.8129(3) 0.20248(8) -0.09833(14) 0.0390(4) Uani 1 1 d . . . N2 N 0.4097(3) 0.09599(9) 0.05139(16) 0.0446(4) Uani 1 1 d . . . N3 N 0.4604(3) 0.05020(9) 0.14302(16) 0.0454(4) Uani 1 1 d . . . N4 N 0.6930(2) 0.04424(7) 0.16275(14) 0.0341(3) Uani 1 1 d . . . C1 C 0.8216(3) 0.24602(10) -0.19770(19) 0.0421(4) Uani 1 1 d . . . H1 H 0.970(4) 0.2699(11) -0.200(2) 0.046(6) Uiso 1 1 d . . . C2 C 0.6393(4) 0.25901(10) -0.29439(18) 0.0418(4) Uani 1 1 d . . . H2 H 0.658(4) 0.2905(11) -0.363(2) 0.047(6) Uiso 1 1 d . . . C3 C 0.4334(3) 0.22598(10) -0.28573(18) 0.0418(4) Uani 1 1 d . . . H3 H 0.296(4) 0.2336(10) -0.3512(19) 0.041(5) Uiso 1 1 d . . . C4 C 0.4170(3) 0.18155(9) -0.18354(18) 0.0382(4) Uani 1 1 d . . . H4 H 0.278(3) 0.1573(10) -0.1723(18) 0.038(5) Uiso 1 1 d . . . C5 C 0.6120(3) 0.17052(8) -0.09274(16) 0.0339(4) Uani 1 1 d . . . C6 C 0.6093(3) 0.12006(9) 0.01256(16) 0.0346(4) Uani 1 1 d . . . C7 C 0.7907(3) 0.08714(9) 0.08329(16) 0.0340(4) Uani 1 1 d . . . H7 H 0.955(3) 0.0919(9) 0.0831(18) 0.033(5) Uiso 1 1 d . . . C8 C 0.7991(3) -0.00394(8) 0.25572(16) 0.0325(4) Uani 1 1 d . . . C9 C 0.6896(3) -0.02167(9) 0.36310(18) 0.0377(4) Uani 1 1 d . . . H9 H 0.548(4) -0.0013(12) 0.375(2) 0.048(6) Uiso 1 1 d . . . C10 C 0.7923(3) -0.06842(9) 0.45254(18) 0.0393(4) Uani 1 1 d . . . H10 H 0.718(4) -0.0814(11) 0.527(2) 0.047(6) Uiso 1 1 d . . . C11 C 1.0039(3) -0.09766(9) 0.43689(16) 0.0365(4) Uani 1 1 d . . . C12 C 1.1082(3) -0.07881(9) 0.32789(18) 0.0365(4) Uani 1 1 d . . . H12 H 1.253(4) -0.0965(11) 0.3147(19) 0.045(6) Uiso 1 1 d . . . C13 C 1.0074(3) -0.03253(9) 0.23640(17) 0.0357(4) Uani 1 1 d . . . H13 H 1.084(3) -0.0208(10) 0.1601(19) 0.039(5) Uiso 1 1 d . . . C14 C 1.1166(4) -0.14787(10) 0.53503(19) 0.0495(5) Uani 1 1 d . . . H14A H 1.0767 -0.1371 0.6227 0.074 Uiso 1 1 calc R . . H14B H 1.2840 -0.1457 0.5361 0.074 Uiso 1 1 calc R . . H14C H 1.0626 -0.1935 0.5101 0.074 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 0.0371(8) 0.0396(8) 0.0393(8) -0.0009(6) 0.0012(6) -0.0021(6) N2 0.0346(8) 0.0503(9) 0.0489(9) 0.0069(7) 0.0052(7) 0.0022(7) N3 0.0308(7) 0.0538(9) 0.0517(9) 0.0100(8) 0.0055(7) 0.0004(7) N4 0.0297(7) 0.0366(7) 0.0362(7) 0.0004(6) 0.0050(6) -0.0014(6) C1 0.0411(10) 0.0390(9) 0.0463(10) 0.0005(8) 0.0063(8) -0.0021(8) C2 0.0499(11) 0.0373(9) 0.0386(9) 0.0020(8) 0.0069(8) 0.0047(8) C3 0.0434(10) 0.0405(9) 0.0390(9) -0.0008(8) -0.0039(8) 0.0061(8) C4 0.0349(9) 0.0370(9) 0.0414(9) -0.0032(7) -0.0006(7) 0.0001(7) C5 0.0356(8) 0.0326(8) 0.0330(8) -0.0055(7) 0.0023(6) 0.0015(7) C6 0.0339(8) 0.0348(8) 0.0348(8) -0.0050(7) 0.0032(6) -0.0014(7) C7 0.0317(8) 0.0359(8) 0.0342(8) -0.0018(7) 0.0036(7) -0.0047(7) C8 0.0329(8) 0.0313(8) 0.0332(8) -0.0022(6) 0.0039(6) -0.0042(6) C9 0.0357(9) 0.0374(9) 0.0416(9) -0.0019(7) 0.0115(7) -0.0005(7) C10 0.0448(10) 0.0389(9) 0.0364(9) -0.0002(7) 0.0134(8) -0.0056(7) C11 0.0424(9) 0.0314(8) 0.0349(8) -0.0031(7) 0.0014(7) -0.0044(7) C12 0.0338(9) 0.0353(9) 0.0403(9) -0.0027(7) 0.0048(7) 0.0003(7) C13 0.0325(8) 0.0401(9) 0.0355(8) -0.0007(7) 0.0086(7) -0.0044(7) C14 0.0591(12) 0.0437(10) 0.0445(10) 0.0061(8) 0.0021(9) 0.0029(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 C1 1.341(2) . ? N1 C5 1.344(2) . ? N2 N3 1.313(2) . ? N2 C6 1.367(2) . ? N3 N4 1.358(2) . ? N4 C7 1.353(2) . ? N4 C8 1.434(2) . ? C1 C2 1.388(3) . ? C2 C3 1.385(3) . ? C3 C4 1.381(3) . ? C4 C5 1.398(2) . ? C5 C6 1.473(2) . ? C6 C7 1.374(2) . ? C8 C13 1.382(2) . ? C8 C9 1.387(2) . ? C9 C10 1.386(3) . ? C10 C11 1.396(3) . ? C11 C12 1.390(3) . ? C11 C14 1.507(3) . ? C12 C13 1.389(3) . ? 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 N1 C5 116.88(15) . . ? N3 N2 C6 108.92(15) . . ? N2 N3 N4 107.43(15) . . ? C7 N4 N3 110.38(14) . . ? C7 N4 C8 129.58(15) . . ? N3 N4 C8 120.03(15) . . ? N1 C1 C2 124.27(18) . . ? C3 C2 C1 117.76(18) . . ? C4 C3 C2 119.58(17) . . ? C3 C4 C5 118.42(18) . . ? N1 C5 C4 123.06(16) . . ? N1 C5 C6 116.15(14) . . ? C4 C5 C6 120.74(16) . . ? N2 C6 C7 108.32(15) . . ? N2 C6 C5 122.57(15) . . ? C7 C6 C5 129.05(16) . . ? N4 C7 C6 104.95(15) . . ? C13 C8 C9 120.96(16) . . ? C13 C8 N4 119.63(15) . . ? C9 C8 N4 119.40(16) . . ? C10 C9 C8 119.26(17) . . ? C9 C10 C11 121.27(18) . . ? C12 C11 C10 117.86(16) . . ? C12 C11 C14 120.90(17) . . ? C10 C11 C14 121.24(17) . . ? C13 C12 C11 121.81(17) . . ? C8 C13 C12 118.82(17) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 29.18 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.181 _refine_diff_density_min -0.165 _refine_diff_density_rms 0.035 #============================================================================== data_LPdCl2 _database_code_depnum_ccdc_archive 'CCDC 873653' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C14 H12 Cl2 N4 Pd), C2 H6 O S' _chemical_formula_sum 'C30 H30 Cl4 N8 O Pd2 S' _chemical_formula_weight 905.28 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_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.907(2) _cell_length_b 10.194(2) _cell_length_c 19.177(4) _cell_angle_alpha 79.28(3) _cell_angle_beta 76.22(3) _cell_angle_gamma 62.50(3) _cell_volume 1661.8(6) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 28428 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 29.53 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.385 _exptl_crystal_size_mid 0.223 _exptl_crystal_size_min 0.080 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.809 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 900 _exptl_absorpt_coefficient_mu 1.506 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.5644 _exptl_absorpt_correction_T_max 0.8396 _exptl_absorpt_process_details 'STOE X-RED & X-SHAPE' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'STOE IPDS 2' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15613 _diffrn_reflns_av_R_equivalents 0.0643 _diffrn_reflns_av_sigmaI/netI 0.0544 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 25.25 _reflns_number_total 6018 _reflns_number_gt 4807 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA, PLATON (A.L.Spek, 2005)' _computing_data_reduction 'STOE X-RED, PLATON (A.L.Spek, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e/3' _computing_publication_material 'Olex2, Microsoft Word' _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^)+(0.1491P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6018 _refine_ls_number_parameters 457 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0805 _refine_ls_R_factor_gt 0.0691 _refine_ls_wR_factor_ref 0.1950 _refine_ls_wR_factor_gt 0.1856 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _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 0.48557(6) 0.70596(5) 0.15263(3) 0.0327(2) Uani 1 1 d . . . Pd2 Pd 0.82905(6) 0.79862(5) 0.34810(3) 0.0321(2) Uani 1 1 d . . . Cl1 Cl 0.3588(2) 0.8890(2) 0.07030(10) 0.0439(4) Uani 1 1 d . . . Cl2 Cl 0.3008(2) 0.6226(2) 0.17696(10) 0.0402(4) Uani 1 1 d . . . Cl3 Cl 0.7994(2) 0.6185(2) 0.43175(10) 0.0427(4) Uani 1 1 d . . . Cl4 Cl 0.5884(2) 0.87959(19) 0.32326(10) 0.0401(4) Uani 1 1 d . . . SA S 1.2756(3) 1.1921(3) 0.26082(16) 0.0449(6) Uani 0.70 1 d P A 1 SB S 1.2302(8) 1.3064(6) 0.2392(3) 0.0367(13) Uani 0.30 1 d P B 2 OA O 1.1273(10) 1.3000(12) 0.2379(5) 0.053(2) Uani 0.70 1 d P A 1 OB O 1.157(3) 1.200(3) 0.2624(11) 0.051(5) Uani 0.30 1 d P B 2 N1 N 0.6708(7) 0.7548(6) 0.1337(3) 0.0324(12) Uani 1 1 d . . . N2 N 0.6051(7) 0.5617(6) 0.2272(3) 0.0349(13) Uani 1 1 d . . . N3 N 0.5813(7) 0.4632(6) 0.2755(3) 0.0362(13) Uani 1 1 d . . . N4 N 0.7005(7) 0.4091(6) 0.3119(3) 0.0338(12) Uani 1 1 d . . . N5 N 1.0420(7) 0.7477(7) 0.3664(3) 0.0370(14) Uani 1 1 d . . . N6 N 0.8798(7) 0.9413(6) 0.2730(3) 0.0354(13) Uani 1 1 d . . . N7 N 0.8065(7) 1.0436(6) 0.2247(3) 0.0361(13) Uani 1 1 d . . . N8 N 0.9085(7) 1.0940(6) 0.1873(3) 0.0331(12) Uani 1 1 d . . . C1 C 0.7043(9) 0.8427(8) 0.0788(4) 0.0372(15) Uani 1 1 d . . . H1 H 0.6319 0.8979 0.0473 0.045 Uiso 1 1 calc R . . C1A C 1.277(5) 1.331(5) 0.322(3) 0.049(11) Uani 0.30 1 d PU B 2 H1AA H 1.1875 1.3488 0.3614 0.073 Uiso 0.30 1 calc PR B 2 H1AB H 1.3013 1.4159 0.3138 0.073 Uiso 0.30 1 calc PR B 2 H1AC H 1.3658 1.2410 0.3359 0.073 Uiso 0.30 1 calc PR B 2 C2 C 0.8425(9) 0.8562(8) 0.0660(4) 0.0403(16) Uani 1 1 d . . . H2 H 0.8628 0.9205 0.0268 0.048 Uiso 1 1 calc R . . C3 C 0.9485(9) 0.7755(8) 0.1106(4) 0.0387(16) Uani 1 1 d . . . H3 H 1.0443 0.7809 0.1023 0.046 Uiso 1 1 calc R . . C4 C 0.9114(9) 0.6840(8) 0.1695(4) 0.0367(15) Uani 1 1 d . . . H4 H 0.9809 0.6305 0.2025 0.044 Uiso 1 1 calc R . . C5 C 0.7764(8) 0.6727(7) 0.1790(3) 0.0330(15) Uani 1 1 d . . . C6 C 0.7332(8) 0.5732(8) 0.2310(4) 0.0341(15) Uani 1 1 d . . . C7 C 0.7967(8) 0.4724(8) 0.2867(4) 0.0354(15) Uani 1 1 d . . . H7 H 0.8879 0.4526 0.3033 0.042 Uiso 1 1 calc R . . C8 C 0.7131(9) 0.2924(8) 0.3689(4) 0.0365(15) Uani 1 1 d . . . C9 C 0.5840(9) 0.2847(8) 0.4109(4) 0.0383(15) Uani 1 1 d . . . H9 H 0.4841 0.3580 0.4035 0.046 Uiso 1 1 calc R . . C10 C 0.6001(9) 0.1674(8) 0.4652(4) 0.0373(15) Uani 1 1 d . . . H10 H 0.5103 0.1621 0.4944 0.045 Uiso 1 1 calc R . . C11 C 0.7468(9) 0.0578(7) 0.4770(4) 0.0352(15) Uani 1 1 d . . . C12 C 0.8727(9) 0.0743(8) 0.4345(4) 0.0351(15) Uani 1 1 d . . . H12 H 0.9729 0.0031 0.4427 0.042 Uiso 1 1 calc R . . C13 C 0.8618(8) 0.1890(7) 0.3803(4) 0.0336(14) Uani 1 1 d . . . H13 H 0.9513 0.1967 0.3523 0.040 Uiso 1 1 calc R . . C14 C 0.7605(9) -0.0662(8) 0.5344(4) 0.0389(16) Uani 1 1 d . . . H14A H 0.7314 -0.1348 0.5190 0.058 Uiso 1 1 calc R . . H14B H 0.6915 -0.0260 0.5790 0.058 Uiso 1 1 calc R . . H14C H 0.8674 -0.1193 0.5428 0.058 Uiso 1 1 calc R . . C15 C 1.1136(9) 0.6588(7) 0.4209(4) 0.0360(15) Uani 1 1 d . . . H15 H 1.0666 0.6023 0.4527 0.043 Uiso 1 1 calc R . . C16 C 1.2502(9) 0.6457(7) 0.4327(4) 0.0356(15) Uani 1 1 d . . . H16 H 1.2937 0.5845 0.4730 0.043 Uiso 1 1 calc R . . C17 C 1.3244(9) 0.7215(8) 0.3862(4) 0.0373(15) Uani 1 1 d . . . H17 H 1.4211 0.7111 0.3926 0.045 Uiso 1 1 calc R . . C18 C 1.2522(9) 0.8162(7) 0.3279(4) 0.0354(15) Uani 1 1 d . . . H18 H 1.2992 0.8716 0.2951 0.042 Uiso 1 1 calc R . . C19 C 1.1174(8) 0.8258(7) 0.3201(4) 0.0337(15) Uani 1 1 d . . . C20 C 1.0247(8) 0.9276(7) 0.2682(4) 0.0327(14) Uani 1 1 d . . . C21 C 1.0451(8) 1.0249(8) 0.2107(4) 0.0348(15) Uani 1 1 d . . . H21 H 1.1352 1.0397 0.1919 0.042 Uiso 1 1 calc R . . C22 C 0.8648(8) 1.2116(7) 0.1301(4) 0.0346(15) Uani 1 1 d . . . C23 C 0.7608(9) 1.2227(8) 0.0898(4) 0.0376(15) Uani 1 1 d . . . H23 H 0.7193 1.1526 0.0987 0.045 Uiso 1 1 calc R . . C24 C 0.7185(9) 1.3381(8) 0.0362(4) 0.0358(15) Uani 1 1 d . . . H24 H 0.6484 1.3461 0.0076 0.043 Uiso 1 1 calc R . . C25 C 0.7772(8) 1.4427(7) 0.0235(3) 0.0342(15) Uani 1 1 d . . . C26 C 0.8797(8) 1.4279(7) 0.0652(4) 0.0334(14) Uani 1 1 d . . . H26 H 0.9199 1.4989 0.0570 0.040 Uiso 1 1 calc R . . C27 C 0.9264(9) 1.3120(7) 0.1190(3) 0.0336(14) Uani 1 1 d . . . H27 H 0.9982 1.3026 0.1470 0.040 Uiso 1 1 calc R . . C28 C 0.7272(9) 1.5706(8) -0.0345(4) 0.0387(16) Uani 1 1 d . . . H28A H 0.7352 1.5322 -0.0793 0.058 Uiso 1 1 calc R . . H28B H 0.7941 1.6208 -0.0429 0.058 Uiso 1 1 calc R . . H28C H 0.6199 1.6413 -0.0188 0.058 Uiso 1 1 calc R . . C29A C 1.328(2) 1.287(2) 0.3095(10) 0.052(4) Uani 0.70 1 d P A 1 H29A H 1.3262 1.3779 0.2808 0.077 Uiso 0.70 1 calc PR A 1 H29B H 1.4323 1.2232 0.3199 0.077 Uiso 0.70 1 calc PR A 1 H29C H 1.2547 1.3130 0.3548 0.077 Uiso 0.70 1 calc PR A 1 C30A C 1.422(2) 1.1766(19) 0.1841(8) 0.046(4) Uani 0.70 1 d P A 1 H30D H 1.4069 1.1342 0.1464 0.069 Uiso 0.70 1 calc PR A 1 H30E H 1.5236 1.1119 0.1975 0.069 Uiso 0.70 1 calc PR A 1 H30F H 1.4162 1.2752 0.1661 0.069 Uiso 0.70 1 calc PR A 1 C30B C 1.420(8) 1.229(7) 0.193(4) 0.10(3) Uani 0.30 1 d P B 2 H30A H 1.4713 1.1239 0.2094 0.150 Uiso 0.30 1 calc PR B 2 H30B H 1.4753 1.2810 0.2023 0.150 Uiso 0.30 1 calc PR B 2 H30C H 1.4194 1.2400 0.1411 0.150 Uiso 0.30 1 calc PR 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 0.0402(3) 0.0301(3) 0.0232(3) 0.0095(2) -0.0095(2) -0.0140(2) Pd2 0.0440(3) 0.0287(3) 0.0231(3) 0.0098(2) -0.0053(2) -0.0201(2) Cl1 0.0470(10) 0.0440(10) 0.0333(9) 0.0179(7) -0.0159(7) -0.0173(8) Cl2 0.0468(10) 0.0410(9) 0.0336(9) 0.0095(7) -0.0128(7) -0.0218(8) Cl3 0.0586(11) 0.0401(9) 0.0333(9) 0.0187(7) -0.0114(8) -0.0313(8) Cl4 0.0433(9) 0.0392(9) 0.0366(9) 0.0095(7) -0.0071(7) -0.0216(7) SA 0.0486(16) 0.0510(18) 0.0417(15) 0.0077(13) -0.0117(12) -0.0298(13) SB 0.049(4) 0.031(3) 0.025(3) 0.019(2) -0.010(2) -0.019(3) OA 0.047(5) 0.064(6) 0.047(5) -0.003(5) -0.013(4) -0.023(5) OB 0.060(13) 0.053(12) 0.050(12) 0.008(10) 0.003(9) -0.043(11) N1 0.036(3) 0.022(3) 0.030(3) 0.013(2) -0.011(2) -0.009(2) N2 0.046(3) 0.030(3) 0.026(3) 0.009(2) -0.009(2) -0.017(3) N3 0.043(3) 0.034(3) 0.028(3) 0.009(2) -0.009(2) -0.017(3) N4 0.039(3) 0.029(3) 0.029(3) 0.005(2) -0.013(2) -0.010(2) N5 0.052(4) 0.036(3) 0.029(3) -0.003(2) 0.005(3) -0.029(3) N6 0.048(3) 0.029(3) 0.026(3) 0.010(2) -0.010(2) -0.017(3) N7 0.044(3) 0.034(3) 0.029(3) 0.008(2) -0.008(2) -0.019(3) N8 0.049(3) 0.030(3) 0.021(3) 0.012(2) -0.008(2) -0.022(3) C1 0.046(4) 0.032(3) 0.028(4) 0.005(3) -0.011(3) -0.014(3) C1A 0.051(18) 0.053(19) 0.035(16) -0.011(13) 0.011(12) -0.023(14) C2 0.041(4) 0.039(4) 0.035(4) 0.005(3) -0.003(3) -0.018(3) C3 0.046(4) 0.033(3) 0.033(4) 0.004(3) -0.004(3) -0.018(3) C4 0.047(4) 0.038(4) 0.025(3) 0.014(3) -0.011(3) -0.023(3) C5 0.047(4) 0.033(3) 0.010(3) 0.010(2) -0.012(3) -0.011(3) C6 0.039(4) 0.032(3) 0.026(3) 0.003(3) -0.010(3) -0.011(3) C7 0.043(4) 0.036(4) 0.028(3) 0.010(3) -0.010(3) -0.020(3) C8 0.047(4) 0.034(3) 0.030(4) 0.008(3) -0.015(3) -0.019(3) C9 0.041(4) 0.040(4) 0.030(4) 0.006(3) -0.012(3) -0.015(3) C10 0.040(4) 0.039(4) 0.031(4) 0.007(3) -0.008(3) -0.019(3) C11 0.054(4) 0.026(3) 0.021(3) 0.013(3) -0.010(3) -0.018(3) C12 0.045(4) 0.032(3) 0.024(3) 0.002(3) -0.008(3) -0.014(3) C13 0.043(4) 0.031(3) 0.023(3) 0.008(3) -0.009(3) -0.016(3) C14 0.053(4) 0.037(4) 0.024(3) 0.010(3) -0.005(3) -0.023(3) C15 0.048(4) 0.026(3) 0.029(3) 0.014(3) -0.005(3) -0.019(3) C16 0.054(4) 0.025(3) 0.027(3) 0.005(3) -0.010(3) -0.018(3) C17 0.044(4) 0.035(4) 0.030(4) 0.006(3) -0.008(3) -0.017(3) C18 0.051(4) 0.025(3) 0.029(4) 0.011(3) -0.016(3) -0.017(3) C19 0.048(4) 0.022(3) 0.027(3) 0.013(2) 0.000(3) -0.021(3) C20 0.039(4) 0.028(3) 0.028(3) 0.003(3) -0.002(3) -0.016(3) C21 0.044(4) 0.037(4) 0.022(3) 0.006(3) -0.003(3) -0.022(3) C22 0.042(4) 0.029(3) 0.027(3) 0.010(3) -0.007(3) -0.015(3) C23 0.048(4) 0.033(3) 0.033(4) 0.007(3) -0.005(3) -0.022(3) C24 0.051(4) 0.034(3) 0.024(3) 0.006(3) -0.009(3) -0.022(3) C25 0.042(4) 0.031(3) 0.020(3) 0.011(3) -0.003(3) -0.014(3) C26 0.039(4) 0.029(3) 0.027(3) 0.004(3) 0.000(3) -0.015(3) C27 0.050(4) 0.030(3) 0.022(3) 0.010(3) -0.010(3) -0.021(3) C28 0.056(4) 0.035(4) 0.021(3) 0.006(3) -0.007(3) -0.020(3) C29A 0.074(13) 0.051(10) 0.038(9) 0.007(8) -0.019(9) -0.033(9) C30A 0.040(7) 0.056(9) 0.027(6) 0.013(7) -0.008(6) -0.014(7) C30B 0.06(3) 0.11(5) 0.12(5) -0.08(4) 0.00(3) -0.01(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 N2 2.006(6) . ? Pd1 N1 2.051(6) . ? Pd1 Cl2 2.275(2) . ? Pd1 Cl1 2.288(2) . ? Pd2 N6 1.998(6) . ? Pd2 N5 2.029(7) . ? Pd2 Cl4 2.274(2) . ? Pd2 Cl3 2.2823(18) . ? SA OA 1.483(9) . ? SA C29A 1.76(2) . ? SA C30A 1.775(16) . ? SB OB 1.516(19) . ? SB C30B 1.74(6) . ? SB C1A 1.85(5) . ? N1 C1 1.334(10) . ? N1 C5 1.380(8) . ? N2 N3 1.300(8) . ? N2 C6 1.348(10) . ? N3 N4 1.354(8) . ? N4 C7 1.339(9) . ? N4 C8 1.438(9) . ? N5 C15 1.351(10) . ? N5 C19 1.396(8) . ? N6 N7 1.318(8) . ? N6 C20 1.358(10) . ? N7 N8 1.340(8) . ? N8 C21 1.349(10) . ? N8 C22 1.444(8) . ? C1 C2 1.398(11) . ? C2 C3 1.371(11) . ? C3 C4 1.417(10) . ? C4 C5 1.362(11) . ? C5 C6 1.423(10) . ? C6 C7 1.381(10) . ? C8 C9 1.368(11) . ? C8 C13 1.400(10) . ? C9 C10 1.406(10) . ? C10 C11 1.405(10) . ? C11 C12 1.380(11) . ? C11 C14 1.491(9) . ? C12 C13 1.394(9) . ? C15 C16 1.367(11) . ? C16 C17 1.374(10) . ? C17 C18 1.427(10) . ? C18 C19 1.336(11) . ? C19 C20 1.443(10) . ? C20 C21 1.382(9) . ? C22 C27 1.379(10) . ? C22 C23 1.382(11) . ? C23 C24 1.384(10) . ? C24 C25 1.395(10) . ? C25 C26 1.375(11) . ? C25 C28 1.520(9) . ? C26 C27 1.394(9) . ? 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 N2 Pd1 N1 80.2(2) . . ? N2 Pd1 Cl2 93.97(18) . . ? N1 Pd1 Cl2 172.97(15) . . ? N2 Pd1 Cl1 173.42(18) . . ? N1 Pd1 Cl1 94.46(16) . . ? Cl2 Pd1 Cl1 91.62(7) . . ? N6 Pd2 N5 80.8(2) . . ? N6 Pd2 Cl4 93.95(19) . . ? N5 Pd2 Cl4 174.05(17) . . ? N6 Pd2 Cl3 173.69(19) . . ? N5 Pd2 Cl3 93.92(18) . . ? Cl4 Pd2 Cl3 91.52(8) . . ? OA SA C29A 107.2(8) . . ? OA SA C30A 106.3(6) . . ? C29A SA C30A 95.8(9) . . ? OB SB C30B 115(2) . . ? OB SB C1A 105.3(19) . . ? C30B SB C1A 96(2) . . ? C1 N1 C5 119.2(6) . . ? C1 N1 Pd1 126.5(5) . . ? C5 N1 Pd1 113.9(5) . . ? N3 N2 C6 112.4(6) . . ? N3 N2 Pd1 133.5(5) . . ? C6 N2 Pd1 114.0(4) . . ? N2 N3 N4 104.2(6) . . ? C7 N4 N3 112.6(6) . . ? C7 N4 C8 128.2(6) . . ? N3 N4 C8 119.1(6) . . ? C15 N5 C19 116.2(6) . . ? C15 N5 Pd2 128.5(5) . . ? C19 N5 Pd2 115.1(5) . . ? N7 N6 C20 111.6(6) . . ? N7 N6 Pd2 134.6(5) . . ? C20 N6 Pd2 113.8(4) . . ? N6 N7 N8 104.9(6) . . ? N7 N8 C21 112.5(5) . . ? N7 N8 C22 119.9(6) . . ? C21 N8 C22 127.6(6) . . ? N1 C1 C2 122.2(7) . . ? C3 C2 C1 119.3(7) . . ? C2 C3 C4 118.3(7) . . ? C5 C4 C3 120.1(7) . . ? C4 C5 N1 120.8(6) . . ? C4 C5 C6 125.6(6) . . ? N1 C5 C6 113.5(6) . . ? N2 C6 C7 106.6(6) . . ? N2 C6 C5 118.2(6) . . ? C7 C6 C5 135.1(7) . . ? N4 C7 C6 104.2(6) . . ? C9 C8 C13 121.5(7) . . ? C9 C8 N4 120.9(6) . . ? C13 C8 N4 117.6(7) . . ? C8 C9 C10 119.6(7) . . ? C11 C10 C9 121.0(7) . . ? C12 C11 C10 116.7(6) . . ? C12 C11 C14 123.4(7) . . ? C10 C11 C14 119.9(7) . . ? C11 C12 C13 124.0(7) . . ? C12 C13 C8 117.1(7) . . ? N5 C15 C16 123.5(6) . . ? C15 C16 C17 119.8(7) . . ? C16 C17 C18 118.1(7) . . ? C19 C18 C17 119.0(7) . . ? C18 C19 N5 123.4(6) . . ? C18 C19 C20 124.7(6) . . ? N5 C19 C20 111.6(6) . . ? N6 C20 C21 106.4(6) . . ? N6 C20 C19 118.5(6) . . ? C21 C20 C19 135.1(7) . . ? N8 C21 C20 104.7(6) . . ? C27 C22 C23 122.2(6) . . ? C27 C22 N8 118.0(6) . . ? C23 C22 N8 119.8(6) . . ? C22 C23 C24 118.7(7) . . ? C23 C24 C25 121.0(7) . . ? C26 C25 C24 118.4(6) . . ? C26 C25 C28 121.2(7) . . ? C24 C25 C28 120.4(7) . . ? C25 C26 C27 122.2(7) . . ? C22 C27 C26 117.6(7) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 5.104 _refine_diff_density_min -1.462 _refine_diff_density_rms 0.195 _publ_section_abstract ; ; _publ_section_experimental ; ; _publ_section_comment ; ; _publ_section_references ; ; _publ_section_figure_captions ; ; #==============================================================================