Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Berthold Kersting' _publ_contact_author_address ; Leipzig 04103 GERMANY ; _publ_contact_author_email B.KERSTING@UNI-LEIPZIG.DE _publ_section_title ; Preparation and Characterization of Dinuclear Pd(II) Complexes of Binucleating Tetraaza-Thiophenolate Ligands ; loop_ _publ_author_name 'Berthold Kersting' 'Gabriel Siedle' data_2 _database_code_depnum_ccdc_archive 'CCDC 286854' _chemical_formula_structural ; [(L3)Pd2(Cl)2](ClO4)2 ; _chemical_formula_sum 'C20 H33 Cl3 N4 O4 Pd2 S' _chemical_formula_weight 744.71 _chemical_melting_point ? _chemical_compound_source ; Crystals were grown by slow evaporation of a methanolic solution ; #CRYSTAL DATA _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 12.660(3) _cell_length_b 13.313(3) _cell_length_c 16.634(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.47(3) _cell_angle_gamma 90.00 _cell_volume 2773.0(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.784 _exptl_crystal_F_000 1488 _exptl_absorpt_coefficient_mu 1.694 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.82 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ? _diffrn_radiation_type MoK\a _diffrn_ambient_temperature 210(2) _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'BRUKER AXS' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_method hemisphere _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17078 _diffrn_reflns_av_R_equivalents 0.0411 _diffrn_reflns_av_sigmaI/netI 0.0654 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 28.79 _reflns_number_total 6510 _reflns_number_gt 3927 _reflns_threshold_expression >2sigma(I) #REFINEMENT DATA #_reflns_number_total 6510 #_reflns_number_gt 3927 #_reflns_threshold_expression >2sigma(I) _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^)+(0.0600P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6510 _refine_ls_number_parameters 341 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0894 _refine_ls_R_factor_gt 0.0420 _refine_ls_wR_factor_ref 0.1326 _refine_ls_wR_factor_gt 0.0954 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.099 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.901 _diffrn_reflns_theta_full 28.79 _diffrn_measured_fraction_theta_full 0.901 _refine_diff_density_max 0.897 _refine_diff_density_min -1.131 _refine_diff_density_rms 0.224 _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 (FARRUGIA)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; #ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' 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 0.25603(4) -0.51725(4) 0.46473(3) 0.03659(15) Uani 1 1 d . A . Pd2 Pd 0.36503(4) -0.56969(4) 0.25989(3) 0.03472(14) Uani 1 1 d . . . S S 0.29291(13) -0.46244(12) 0.34381(9) 0.0369(4) Uani 1 1 d . . . Cl1 Cl 0.11633(14) -0.60634(16) 0.39517(12) 0.0598(5) Uani 1 1 d . . . Cl2 Cl 0.36046(14) -0.71061(12) 0.33910(11) 0.0497(4) Uani 1 1 d . . . N1 N 0.3646(4) -0.4331(4) 0.5310(3) 0.0396(12) Uani 1 1 d . . . N2 N 0.2213(4) -0.5665(4) 0.5768(3) 0.0574(17) Uani 1 1 d D . . N3 N 0.3746(5) -0.4522(4) 0.1865(3) 0.0439(13) Uani 1 1 d . . . N4 N 0.4195(4) -0.6503(4) 0.1651(3) 0.0468(14) Uani 1 1 d . . . C1 C 0.3849(5) -0.3623(4) 0.3559(4) 0.0344(13) Uani 1 1 d . A . C2 C 0.4124(5) -0.3165(5) 0.2852(4) 0.0408(15) Uani 1 1 d . . . C3 C 0.4688(5) -0.2269(5) 0.2897(4) 0.0442(16) Uani 1 1 d . . . H3 H 0.4821 -0.1970 0.2418 0.053 Uiso 1 1 calc R . . C4 C 0.5060(5) -0.1800(5) 0.3631(4) 0.0416(15) Uani 1 1 d . . . C5 C 0.4850(5) -0.2284(5) 0.4326(4) 0.0409(15) Uani 1 1 d . A . H5 H 0.5112 -0.2001 0.4827 0.049 Uiso 1 1 calc R . . C6 C 0.4257(5) -0.3185(5) 0.4315(4) 0.0372(14) Uani 1 1 d . . . C7 C 0.4167(5) -0.3565(5) 0.5110(4) 0.0421(15) Uani 1 1 d . A . H7 H 0.4540 -0.3207 0.5541 0.051 Uiso 1 1 calc R . . C8A C 0.3834(12) -0.4677(11) 0.6169(8) 0.042(4) Uiso 0.554(19) 1 d P A 1 H8A H 0.4293 -0.5264 0.6225 0.051 Uiso 0.554(19) 1 calc PR A 1 H8B H 0.4170 -0.4151 0.6520 0.051 Uiso 0.554(19) 1 calc PR A 1 C9A C 0.2783(10) -0.4922(9) 0.6380(7) 0.053(4) Uiso 0.554(19) 1 d PD A 1 H9A H 0.2361 -0.4314 0.6381 0.063 Uiso 0.554(19) 1 calc PR A 1 H9B H 0.2864 -0.5211 0.6920 0.063 Uiso 0.554(19) 1 calc PR A 1 C10A C 0.1038(7) -0.5500(10) 0.5814(9) 0.049(4) Uiso 0.554(19) 1 d PD A 1 H10A H 0.0871 -0.5767 0.6316 0.074 Uiso 0.554(19) 1 calc PR A 1 H10B H 0.0615 -0.5835 0.5367 0.074 Uiso 0.554(19) 1 calc PR A 1 H10C H 0.0884 -0.4794 0.5787 0.074 Uiso 0.554(19) 1 calc PR A 1 C11A C 0.2506(10) -0.6694(7) 0.6004(10) 0.062(4) Uiso 0.554(19) 1 d PD A 1 H11A H 0.2356 -0.6816 0.6545 0.093 Uiso 0.554(19) 1 calc PR A 1 H11B H 0.3254 -0.6792 0.5990 0.093 Uiso 0.554(19) 1 calc PR A 1 H11C H 0.2101 -0.7152 0.5634 0.093 Uiso 0.554(19) 1 calc PR A 1 C8B C 0.3498(16) -0.4410(14) 0.6199(10) 0.044(5) Uiso 0.446(19) 1 d P A 2 H8C H 0.4153 -0.4226 0.6547 0.052 Uiso 0.446(19) 1 calc PR A 2 H8D H 0.2934 -0.3962 0.6312 0.052 Uiso 0.446(19) 1 calc PR A 2 C9B C 0.3211(9) -0.5472(12) 0.6352(8) 0.047(5) Uiso 0.446(19) 1 d PD A 2 H9C H 0.3084 -0.5559 0.6909 0.056 Uiso 0.446(19) 1 calc PR A 2 H9D H 0.3777 -0.5925 0.6251 0.056 Uiso 0.446(19) 1 calc PR A 2 C10B C 0.1258(9) -0.5298(11) 0.6063(11) 0.048(5) Uiso 0.446(19) 1 d PD A 2 H10D H 0.1187 -0.5623 0.6567 0.073 Uiso 0.446(19) 1 calc PR A 2 H10E H 0.0643 -0.5444 0.5670 0.073 Uiso 0.446(19) 1 calc PR A 2 H10F H 0.1314 -0.4586 0.6147 0.073 Uiso 0.446(19) 1 calc PR A 2 C11B C 0.2141(13) -0.6809(7) 0.5686(11) 0.057(5) Uiso 0.446(19) 1 d PD A 2 H11D H 0.2008 -0.7095 0.6191 0.086 Uiso 0.446(19) 1 calc PR A 2 H11E H 0.2801 -0.7066 0.5552 0.086 Uiso 0.446(19) 1 calc PR A 2 H11F H 0.1569 -0.6982 0.5264 0.086 Uiso 0.446(19) 1 calc PR A 2 C12 C 0.3903(6) -0.3597(5) 0.2038(4) 0.0455(16) Uani 1 1 d . . . H12 H 0.3872 -0.3153 0.1604 0.055 Uiso 1 1 calc R . . C13 C 0.3687(7) -0.4883(6) 0.1011(4) 0.064(2) Uani 1 1 d . . . H13A H 0.3894 -0.4354 0.0665 0.077 Uiso 1 1 calc R . . H13B H 0.2967 -0.5097 0.0800 0.077 Uiso 1 1 calc R . . C14 C 0.4450(7) -0.5753(6) 0.1041(5) 0.063(2) Uani 1 1 d . . . H14A H 0.4392 -0.6065 0.0509 0.076 Uiso 1 1 calc R . . H14B H 0.5177 -0.5515 0.1189 0.076 Uiso 1 1 calc R . . C15 C 0.5154(7) -0.7131(7) 0.1923(6) 0.082(3) Uani 1 1 d . . . H15A H 0.5360 -0.7478 0.1464 0.123 Uiso 1 1 calc R . . H15B H 0.4991 -0.7612 0.2317 0.123 Uiso 1 1 calc R . . H15C H 0.5731 -0.6709 0.2162 0.123 Uiso 1 1 calc R . . C16 C 0.3306(7) -0.7152(6) 0.1277(5) 0.068(2) Uani 1 1 d . . . H16A H 0.3530 -0.7532 0.0842 0.102 Uiso 1 1 calc R . . H16B H 0.2704 -0.6742 0.1068 0.102 Uiso 1 1 calc R . . H16C H 0.3107 -0.7603 0.1680 0.102 Uiso 1 1 calc R . . C17 C 0.5662(6) -0.0797(5) 0.3637(4) 0.0530(19) Uani 1 1 d . . . C18 C 0.6490(8) -0.0835(7) 0.3058(6) 0.082(3) Uani 1 1 d . . . H18A H 0.7013 -0.1339 0.3239 0.123 Uiso 1 1 calc R . . H18B H 0.6833 -0.0193 0.3050 0.123 Uiso 1 1 calc R . . H18C H 0.6143 -0.0998 0.2521 0.123 Uiso 1 1 calc R . . C19 C 0.6230(7) -0.0539(6) 0.4485(5) 0.073(3) Uani 1 1 d . . . H19A H 0.6757 -0.1043 0.4658 0.109 Uiso 1 1 calc R . . H19B H 0.5718 -0.0517 0.4857 0.109 Uiso 1 1 calc R . . H19C H 0.6571 0.0103 0.4473 0.109 Uiso 1 1 calc R . . C20 C 0.4853(9) 0.0016(6) 0.3354(6) 0.087(3) Uani 1 1 d . . . H20A H 0.5210 0.0652 0.3352 0.130 Uiso 1 1 calc R . . H20B H 0.4329 0.0047 0.3717 0.130 Uiso 1 1 calc R . . H20C H 0.4506 -0.0137 0.2815 0.130 Uiso 1 1 calc R . . Cl3 Cl 0.81515(19) 0.18389(16) 0.37341(13) 0.0661(6) Uani 1 1 d . . . O1A O 0.8783(15) 0.2711(12) 0.3920(14) 0.107(6) Uani 0.65(2) 1 d P B 3 O2A O 0.761(2) 0.199(2) 0.2969(10) 0.160(13) Uani 0.65(2) 1 d P B 3 O3A O 0.8596(13) 0.0952(12) 0.3839(17) 0.125(8) Uani 0.65(2) 1 d P B 3 O4A O 0.7338(13) 0.1894(12) 0.4255(11) 0.107(6) Uani 0.65(2) 1 d P B 3 O1B O 0.890(4) 0.238(3) 0.418(2) 0.17(2) Uani 0.35(2) 1 d P B 4 O2B O 0.719(3) 0.198(3) 0.335(4) 0.18(3) Uani 0.35(2) 1 d P B 4 O3B O 0.872(2) 0.132(4) 0.315(2) 0.164(18) Uani 0.35(2) 1 d P B 4 O4B O 0.820(4) 0.099(3) 0.4237(19) 0.15(2) Uani 0.35(2) 1 d P B 4 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 0.0342(3) 0.0436(3) 0.0332(3) -0.0034(2) 0.0090(2) -0.0008(2) Pd2 0.0373(3) 0.0384(3) 0.0290(2) -0.0035(2) 0.00635(19) -0.0021(2) S 0.0394(9) 0.0419(9) 0.0298(8) -0.0044(7) 0.0066(6) -0.0018(7) Cl1 0.0499(10) 0.0767(13) 0.0543(11) -0.0221(10) 0.0123(8) -0.0215(9) Cl2 0.0580(11) 0.0415(9) 0.0498(10) 0.0054(8) 0.0083(8) -0.0003(8) N1 0.042(3) 0.051(3) 0.026(3) -0.001(2) 0.005(2) -0.002(3) N2 0.047(4) 0.087(5) 0.039(3) 0.006(3) 0.007(3) -0.027(3) N3 0.058(4) 0.047(3) 0.026(3) -0.002(2) 0.003(2) -0.005(3) N4 0.050(3) 0.053(4) 0.040(3) -0.015(3) 0.016(3) -0.010(3) C1 0.038(3) 0.035(3) 0.031(3) -0.001(3) 0.008(3) 0.004(3) C2 0.053(4) 0.041(4) 0.027(3) 0.001(3) 0.001(3) 0.001(3) C3 0.057(4) 0.039(4) 0.036(4) 0.005(3) 0.005(3) 0.002(3) C4 0.051(4) 0.032(3) 0.041(4) 0.003(3) 0.004(3) 0.000(3) C5 0.048(4) 0.041(4) 0.033(3) -0.003(3) 0.002(3) 0.000(3) C6 0.040(4) 0.039(3) 0.033(3) 0.000(3) 0.005(3) 0.002(3) C7 0.044(4) 0.048(4) 0.034(3) -0.004(3) 0.005(3) -0.009(3) C12 0.065(5) 0.046(4) 0.025(3) 0.008(3) 0.004(3) -0.006(3) C13 0.104(7) 0.062(5) 0.025(4) -0.009(3) 0.009(4) -0.025(5) C14 0.080(6) 0.068(5) 0.049(5) -0.024(4) 0.031(4) -0.028(4) C15 0.073(6) 0.092(7) 0.086(7) -0.029(5) 0.030(5) 0.028(5) C16 0.089(6) 0.069(5) 0.051(5) -0.022(4) 0.026(4) -0.030(5) C17 0.076(5) 0.041(4) 0.040(4) 0.002(3) 0.004(4) -0.012(4) C18 0.111(8) 0.071(6) 0.070(6) -0.011(5) 0.035(5) -0.041(5) C19 0.097(7) 0.061(5) 0.056(5) 0.002(4) -0.001(5) -0.037(5) C20 0.138(9) 0.045(5) 0.070(6) -0.002(4) -0.008(6) -0.004(5) Cl3 0.0823(16) 0.0571(13) 0.0603(13) 0.0031(10) 0.0147(11) -0.0151(11) O1A 0.123(11) 0.058(9) 0.147(18) 0.012(9) 0.039(11) -0.050(7) O2A 0.22(3) 0.194(19) 0.053(8) 0.025(9) -0.019(11) 0.00(2) O3A 0.099(11) 0.082(11) 0.19(3) 0.001(13) 0.023(13) 0.040(8) O4A 0.117(11) 0.106(11) 0.112(12) -0.033(9) 0.061(9) -0.015(8) O1B 0.29(4) 0.10(3) 0.09(2) 0.035(18) -0.02(2) -0.14(3) O2B 0.052(17) 0.13(3) 0.33(9) -0.02(5) -0.08(3) 0.033(17) O3B 0.11(2) 0.28(5) 0.11(3) -0.06(3) 0.05(2) -0.01(3) O4B 0.22(5) 0.17(4) 0.063(17) 0.05(2) -0.02(2) -0.11(4) _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 1.977(5) . ? Pd1 N2 2.084(6) . ? Pd1 S 2.2522(17) . ? Pd1 Cl1 2.2958(18) . ? Pd2 N3 1.998(5) . ? Pd2 N4 2.105(5) . ? Pd2 S 2.2797(16) . ? Pd2 Cl2 2.2982(18) . ? S C1 1.763(6) . ? N1 C7 1.285(8) . ? N1 C8A 1.486(14) . ? N1 C8B 1.521(17) . ? N2 C10B 1.454(8) . ? N2 C11A 1.458(8) . ? N2 C9B 1.498(8) . ? N2 C10A 1.517(8) . ? N2 C9A 1.522(8) . ? N2 C11B 1.530(8) . ? N3 C12 1.274(8) . ? N3 C13 1.492(8) . ? N4 C16 1.482(9) . ? N4 C15 1.489(10) . ? N4 C14 1.493(9) . ? C1 C6 1.412(8) . ? C1 C2 1.413(8) . ? C2 C3 1.386(9) . ? C2 C12 1.459(9) . ? C3 C4 1.389(9) . ? C4 C5 1.384(9) . ? C4 C17 1.537(9) . ? C5 C6 1.414(8) . ? C6 C7 1.437(8) . ? C8A C9A 1.46(2) . ? C8B C9B 1.49(2) . ? C13 C14 1.504(11) . ? C17 C20 1.516(11) . ? C17 C18 1.524(11) . ? C17 C19 1.525(10) . ? Cl3 O2B 1.29(3) . ? Cl3 O3A 1.309(14) . ? Cl3 O1B 1.33(4) . ? Cl3 O2A 1.367(17) . ? Cl3 O4B 1.40(3) . ? Cl3 O1A 1.417(17) . ? Cl3 O4A 1.443(11) . ? Cl3 O3B 1.47(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 N1 Pd1 N2 84.3(2) . . ? N1 Pd1 S 95.49(15) . . ? N2 Pd1 S 179.40(16) . . ? N1 Pd1 Cl1 173.66(16) . . ? N2 Pd1 Cl1 92.29(14) . . ? S Pd1 Cl1 87.88(7) . . ? N3 Pd2 N4 83.4(2) . . ? N3 Pd2 S 87.12(17) . . ? N4 Pd2 S 169.31(17) . . ? N3 Pd2 Cl2 176.28(17) . . ? N4 Pd2 Cl2 92.99(17) . . ? S Pd2 Cl2 96.55(6) . . ? C1 S Pd1 111.3(2) . . ? C1 S Pd2 103.1(2) . . ? Pd1 S Pd2 119.89(7) . . ? C7 N1 C8A 118.6(7) . . ? C7 N1 C8B 116.6(8) . . ? C8A N1 C8B 21.5(7) . . ? C7 N1 Pd1 130.3(4) . . ? C8A N1 Pd1 111.1(6) . . ? C8B N1 Pd1 109.1(7) . . ? C10B N2 C11A 114.6(10) . . ? C10B N2 C9B 112.8(6) . . ? C11A N2 C9B 80.2(7) . . ? C10B N2 C10A 20.7(7) . . ? C11A N2 C10A 109.6(6) . . ? C9B N2 C10A 133.1(8) . . ? C10B N2 C9A 83.8(7) . . ? C11A N2 C9A 110.7(6) . . ? C9B N2 C9A 35.3(6) . . ? C10A N2 C9A 104.2(6) . . ? C10B N2 C11B 108.8(6) . . ? C11A N2 C11B 25.6(7) . . ? C9B N2 C11B 105.2(6) . . ? C10A N2 C11B 95.9(8) . . ? C9A N2 C11B 136.2(8) . . ? C10B N2 Pd1 119.4(8) . . ? C11A N2 Pd1 117.2(7) . . ? C9B N2 Pd1 104.9(6) . . ? C10A N2 Pd1 109.7(6) . . ? C9A N2 Pd1 104.5(6) . . ? C11B N2 Pd1 104.5(8) . . ? C12 N3 C13 120.7(6) . . ? C12 N3 Pd2 129.8(4) . . ? C13 N3 Pd2 109.3(4) . . ? C16 N4 C15 109.6(6) . . ? C16 N4 C14 109.4(6) . . ? C15 N4 C14 109.5(6) . . ? C16 N4 Pd2 107.4(4) . . ? C15 N4 Pd2 113.7(5) . . ? C14 N4 Pd2 107.2(4) . . ? C6 C1 C2 117.4(6) . . ? C6 C1 S 124.2(5) . . ? C2 C1 S 118.1(5) . . ? C3 C2 C1 120.9(6) . . ? C3 C2 C12 114.6(6) . . ? C1 C2 C12 124.4(6) . . ? C2 C3 C4 122.7(6) . . ? C5 C4 C3 116.3(6) . . ? C5 C4 C17 123.7(6) . . ? C3 C4 C17 120.0(6) . . ? C4 C5 C6 123.4(6) . . ? C1 C6 C5 119.1(6) . . ? C1 C6 C7 127.3(6) . . ? C5 C6 C7 113.7(6) . . ? N1 C7 C6 129.1(6) . . ? C9A C8A N1 106.1(11) . . ? C8A C9A N2 110.1(10) . . ? C9B C8B N1 107.4(13) . . ? C8B C9B N2 104.7(12) . . ? N3 C12 C2 126.3(6) . . ? N3 C13 C14 105.9(6) . . ? N4 C14 C13 109.6(6) . . ? C20 C17 C18 108.9(7) . . ? C20 C17 C19 109.3(7) . . ? C18 C17 C19 108.5(7) . . ? C20 C17 C4 107.8(7) . . ? C18 C17 C4 110.6(6) . . ? C19 C17 C4 111.5(6) . . ? O2B Cl3 O3A 123(2) . . ? O2B Cl3 O1B 137(3) . . ? O3A Cl3 O1B 99(2) . . ? O2B Cl3 O2A 39(3) . . ? O3A Cl3 O2A 113.6(16) . . ? O1B Cl3 O2A 131.5(19) . . ? O2B Cl3 O4B 111(3) . . ? O3A Cl3 O4B 38.1(18) . . ? O1B Cl3 O4B 98(2) . . ? O2A Cl3 O4B 129.9(19) . . ? O2B Cl3 O1A 117(2) . . ? O3A Cl3 O1A 119.5(12) . . ? O1B Cl3 O1A 25.8(17) . . ? O2A Cl3 O1A 106.0(16) . . ? O4B Cl3 O1A 123.8(16) . . ? O2B Cl3 O4A 66(3) . . ? O3A Cl3 O4A 107.3(10) . . ? O1B Cl3 O4A 99(2) . . ? O2A Cl3 O4A 104.3(12) . . ? O4B Cl3 O4A 70(2) . . ? O1A Cl3 O4A 104.9(9) . . ? O2B Cl3 O3B 105(3) . . ? O3A Cl3 O3B 54.5(18) . . ? O1B Cl3 O3B 105(3) . . ? O2A Cl3 O3B 71.2(17) . . ? O4B Cl3 O3B 92(2) . . ? O1A Cl3 O3B 102.5(17) . . ? O4A Cl3 O3B 152.4(17) . . ? #===END # Attachment 'CCDC_286855_n.CIF' data_3 _database_code_depnum_ccdc_archive 'CCDC 286855' _chemical_formula_structural ; [(L4)Pd2(Cl)](ClO4)2(MeOH) ; _chemical_formula_sum 'C21 H41 Cl3 N4 O9 Pd2 S' _chemical_formula_weight 844.79 _chemical_melting_point ? _chemical_compound_source ; Crystals were grown by slow evaporation of a methanolic solution ; #CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pca2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 17.285(4) _cell_length_b 14.357(3) _cell_length_c 12.751(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3164.1(11) _cell_formula_units_Z 4 _cell_measurement_temperature 210(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.773 _exptl_crystal_F_000 1704 _exptl_absorpt_coefficient_mu 1.507 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.87 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ? _diffrn_radiation_type MoK\a _diffrn_ambient_temperature 210(2) _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'BRUKER AXS' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_method hemisphere _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19240 _diffrn_reflns_av_R_equivalents 0.0591 _diffrn_reflns_av_sigmaI/netI 0.1057 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 28.89 #REFINEMENT DATA _reflns_number_total 7209 _reflns_number_gt 4239 _reflns_threshold_expression >2sigma(I) _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^)+(0.0659P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.03(6) _refine_ls_number_reflns 7209 _refine_ls_number_parameters 325 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1133 _refine_ls_R_factor_gt 0.0540 _refine_ls_wR_factor_ref 0.1554 _refine_ls_wR_factor_gt 0.1178 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.919 _diffrn_reflns_theta_full 28.89 _diffrn_measured_fraction_theta_full 0.919 _refine_diff_density_max 1.035 _refine_diff_density_min -1.111 _refine_diff_density_rms 0.211 _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 (FARRUGIA)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; #ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' 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 0.46751(4) 0.97147(5) 0.76895(6) 0.03256(18) Uani 1 1 d . . . Pd2 Pd 0.40716(4) 0.77179(6) 0.73203(6) 0.03388(19) Uani 1 1 d . . . S S 0.52554(14) 0.83918(18) 0.7145(2) 0.0327(6) Uani 1 1 d . . . Cl1 Cl 0.36545(16) 0.9169(2) 0.6626(2) 0.0460(7) Uani 1 1 d . . . Cl2 Cl 0.5517(2) 0.3904(2) 0.9383(3) 0.0572(9) Uani 1 1 d . . . Cl3 Cl 0.6308(2) 1.0753(3) 0.5624(3) 0.0674(10) Uani 1 1 d . . . N1 N 0.5495(5) 0.9999(6) 0.8766(7) 0.037(2) Uani 1 1 d . . . H1 H 0.5311 0.9763 0.9380 0.044 Uiso 1 1 calc R . . N2 N 0.4224(5) 1.1044(6) 0.8084(7) 0.036(2) Uani 1 1 d . . . N3 N 0.4503(4) 0.6529(6) 0.7957(6) 0.032(2) Uani 1 1 d . . . H3A H 0.4467 0.6597 0.8665 0.039 Uiso 1 1 calc R . . N4 N 0.3011(5) 0.7045(6) 0.7435(8) 0.043(2) Uani 1 1 d . . . C1 C 0.5817(5) 0.7974(7) 0.8172(8) 0.029(2) Uani 1 1 d . . . C2 C 0.5851(6) 0.6999(7) 0.8353(8) 0.032(2) Uani 1 1 d . . . C3 C 0.6349(6) 0.6641(8) 0.9098(8) 0.035(2) Uani 1 1 d . . . H3B H 0.6357 0.6000 0.9203 0.043 Uiso 1 1 calc R . . C4 C 0.6833(5) 0.7190(7) 0.9693(8) 0.028(2) Uani 1 1 d . . . C5 C 0.6778(6) 0.8143(7) 0.9539(8) 0.032(2) Uani 1 1 d . . . H5 H 0.7083 0.8538 0.9945 0.038 Uiso 1 1 calc R . . C6 C 0.6271(6) 0.8539(7) 0.8783(8) 0.033(2) Uani 1 1 d . . . C7 C 0.6273(6) 0.9588(7) 0.8638(9) 0.035(2) Uani 1 1 d . . . H7A H 0.6622 0.9865 0.9146 0.042 Uiso 1 1 calc R . . H7B H 0.6466 0.9735 0.7943 0.042 Uiso 1 1 calc R . . C8 C 0.5498(6) 1.1039(8) 0.8910(10) 0.042(3) Uani 1 1 d . . . H8A H 0.5777 1.1204 0.9544 0.051 Uiso 1 1 calc R . . H8B H 0.5749 1.1338 0.8319 0.051 Uiso 1 1 calc R . . C9 C 0.4669(6) 1.1354(8) 0.8989(10) 0.043(3) Uani 1 1 d . . . H9A H 0.4440 1.1105 0.9624 0.052 Uiso 1 1 calc R . . H9B H 0.4652 1.2028 0.9031 0.052 Uiso 1 1 calc R . . C10 C 0.4360(8) 1.1643(9) 0.7181(12) 0.063(4) Uani 1 1 d . . . H10A H 0.4285 1.2282 0.7380 0.095 Uiso 1 1 calc R . . H10B H 0.4004 1.1484 0.6631 0.095 Uiso 1 1 calc R . . H10C H 0.4881 1.1559 0.6937 0.095 Uiso 1 1 calc R . . C11 C 0.3378(6) 1.1050(9) 0.8295(10) 0.050(3) Uani 1 1 d . . . H11A H 0.3245 1.0524 0.8724 0.075 Uiso 1 1 calc R . . H11B H 0.3101 1.1015 0.7644 0.075 Uiso 1 1 calc R . . H11C H 0.3241 1.1614 0.8654 0.075 Uiso 1 1 calc R . . C12 C 0.5324(5) 0.6342(6) 0.7727(10) 0.038(2) Uani 1 1 d . . . H12A H 0.5418 0.6424 0.6983 0.046 Uiso 1 1 calc R . . H12B H 0.5444 0.5701 0.7906 0.046 Uiso 1 1 calc R . . C13 C 0.3964(6) 0.5782(8) 0.7669(11) 0.052(3) Uani 1 1 d . . . H13A H 0.4088 0.5216 0.8050 0.062 Uiso 1 1 calc R . . H13B H 0.3996 0.5653 0.6923 0.062 Uiso 1 1 calc R . . C14 C 0.3171(6) 0.6111(8) 0.7949(12) 0.056(4) Uani 1 1 d . . . H14A H 0.3128 0.6172 0.8705 0.068 Uiso 1 1 calc R . . H14B H 0.2791 0.5659 0.7717 0.068 Uiso 1 1 calc R . . C15 C 0.2690(7) 0.6911(9) 0.6370(10) 0.055(3) Uani 1 1 d . . . H15A H 0.2221 0.6555 0.6413 0.083 Uiso 1 1 calc R . . H15B H 0.3060 0.6585 0.5944 0.083 Uiso 1 1 calc R . . H15C H 0.2582 0.7507 0.6061 0.083 Uiso 1 1 calc R . . C16 C 0.2431(7) 0.7560(9) 0.8105(11) 0.060(4) Uani 1 1 d . . . H16A H 0.2313 0.8149 0.7788 0.091 Uiso 1 1 calc R . . H16B H 0.2645 0.7660 0.8791 0.091 Uiso 1 1 calc R . . H16C H 0.1967 0.7197 0.8164 0.091 Uiso 1 1 calc R . . C17 C 0.7420(7) 0.6750(8) 1.0442(9) 0.042(3) Uani 1 1 d . . . C18 C 0.7023(8) 0.6148(10) 1.1203(11) 0.064(4) Uani 1 1 d . . . H18A H 0.6739 0.6527 1.1690 0.096 Uiso 1 1 calc R . . H18B H 0.7397 0.5782 1.1576 0.096 Uiso 1 1 calc R . . H18C H 0.6672 0.5743 1.0839 0.096 Uiso 1 1 calc R . . C19 C 0.7864(8) 0.7462(9) 1.1056(12) 0.069(5) Uani 1 1 d . . . H19A H 0.7510 0.7845 1.1444 0.104 Uiso 1 1 calc R . . H19B H 0.8158 0.7844 1.0584 0.104 Uiso 1 1 calc R . . H19C H 0.8208 0.7153 1.1534 0.104 Uiso 1 1 calc R . . C20 C 0.7988(8) 0.6196(11) 0.9762(12) 0.074(5) Uani 1 1 d . . . H20A H 0.8413 0.5988 1.0185 0.111 Uiso 1 1 calc R . . H20B H 0.8179 0.6587 0.9208 0.111 Uiso 1 1 calc R . . H20C H 0.7728 0.5667 0.9465 0.111 Uiso 1 1 calc R . . O1 O 0.4969(8) 0.3785(10) 0.8580(11) 0.117(4) Uiso 1 1 d . . . O2 O 0.6215(9) 0.4250(11) 0.9075(13) 0.128(5) Uiso 1 1 d . . . O3 O 0.5571(9) 0.3151(12) 1.0044(12) 0.125(5) Uiso 1 1 d . . . O4 O 0.5291(11) 0.4575(14) 1.0080(17) 0.172(8) Uiso 1 1 d . . . O5 O 0.6355(6) 1.1299(8) 0.6536(9) 0.087(3) Uiso 1 1 d . . . O6 O 0.5495(8) 1.0450(10) 0.5523(12) 0.112(4) Uiso 1 1 d . . . O7 O 0.6690(9) 0.9855(11) 0.5850(12) 0.129(5) Uiso 1 1 d . . . O8 O 0.6563(12) 1.1118(14) 0.4711(18) 0.191(8) Uiso 1 1 d . . . O9A O 0.4157(9) 0.6851(13) 1.0116(12) 0.063(6) Uiso 0.62(3) 1 d P A 1 H9A1 H 0.3659 0.7093 1.0307 0.076 Uiso 0.62(3) 1 d PR A 1 C21A C 0.4479(17) 0.629(2) 1.108(2) 0.075(9) Uiso 0.62(3) 1 d P A 1 H21A H 0.5033 0.6248 1.1038 0.112 Uiso 0.62(3) 1 calc PR A 1 H21B H 0.4265 0.5668 1.1078 0.112 Uiso 0.62(3) 1 calc PR A 1 H21C H 0.4336 0.6595 1.1721 0.112 Uiso 0.62(3) 1 calc PR A 1 O9B O 0.4269(15) 0.602(2) 1.0080(19) 0.063(10) Uiso 0.38(3) 1 d P A 2 H9B1 H 0.4484 0.5520 1.0179 0.095 Uiso 0.38(3) 1 calc PR A 2 C21B C 0.454(2) 0.671(3) 1.087(3) 0.044(9) Uiso 0.38(3) 1 d P A 2 H21D H 0.4412 0.6489 1.1561 0.067 Uiso 0.38(3) 1 calc PR A 2 H21E H 0.4293 0.7296 1.0748 0.067 Uiso 0.38(3) 1 calc PR A 2 H21F H 0.5091 0.6779 1.0814 0.067 Uiso 0.38(3) 1 calc PR A 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 0.0328(4) 0.0315(4) 0.0333(4) 0.0031(4) 0.0004(4) 0.0035(4) Pd2 0.0323(4) 0.0351(4) 0.0343(4) 0.0000(4) -0.0045(4) -0.0003(4) S 0.0324(13) 0.0318(14) 0.0338(15) 0.0009(11) 0.0012(12) 0.0021(11) Cl1 0.0419(15) 0.0456(18) 0.0506(18) -0.0004(14) -0.0150(14) 0.0063(14) Cl2 0.071(2) 0.0395(18) 0.061(2) 0.0004(16) -0.0029(17) -0.0053(17) Cl3 0.088(3) 0.062(2) 0.052(2) -0.0116(18) 0.0054(19) -0.028(2) N1 0.052(6) 0.026(5) 0.032(5) 0.005(4) 0.011(4) 0.007(4) N2 0.032(5) 0.039(5) 0.039(5) 0.003(4) 0.012(4) 0.006(4) N3 0.034(5) 0.029(5) 0.034(5) -0.004(4) 0.002(4) -0.007(4) N4 0.036(4) 0.049(6) 0.045(6) -0.006(5) -0.003(4) 0.001(4) C1 0.023(5) 0.031(6) 0.032(5) 0.000(4) 0.000(4) -0.001(4) C2 0.035(6) 0.025(5) 0.035(6) 0.000(4) 0.011(5) -0.004(5) C3 0.033(6) 0.032(6) 0.041(6) 0.003(5) -0.007(5) 0.004(5) C4 0.023(5) 0.031(6) 0.030(5) 0.002(4) 0.006(4) 0.002(4) C5 0.032(6) 0.026(6) 0.037(6) -0.001(5) 0.003(4) -0.004(5) C6 0.028(5) 0.028(6) 0.042(6) 0.008(5) 0.003(5) 0.001(5) C7 0.028(5) 0.037(6) 0.040(6) 0.002(5) -0.002(5) -0.001(5) C8 0.050(7) 0.034(6) 0.042(7) -0.005(5) 0.002(5) -0.003(6) C9 0.049(7) 0.033(6) 0.047(7) 0.001(5) 0.000(6) -0.003(6) C10 0.075(9) 0.045(7) 0.069(10) 0.029(8) -0.004(8) -0.003(6) C11 0.045(7) 0.051(8) 0.054(8) 0.004(6) 0.003(6) 0.019(6) C12 0.040(5) 0.029(5) 0.047(6) 0.000(6) -0.010(6) 0.010(5) C13 0.042(6) 0.045(7) 0.069(9) -0.005(7) -0.016(7) -0.009(5) C14 0.053(7) 0.032(6) 0.085(11) -0.006(7) -0.009(7) -0.012(6) C15 0.056(8) 0.056(8) 0.054(8) -0.016(7) -0.018(7) 0.003(7) C16 0.039(7) 0.084(10) 0.058(8) 0.000(7) -0.003(6) 0.002(7) C17 0.039(6) 0.039(6) 0.049(8) -0.002(5) -0.012(6) 0.000(6) C18 0.061(9) 0.070(10) 0.062(9) 0.024(8) -0.023(7) -0.015(8) C19 0.082(10) 0.043(8) 0.083(11) 0.008(7) -0.051(9) -0.009(7) C20 0.054(9) 0.080(12) 0.088(12) -0.012(9) -0.015(8) 0.044(8) _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 2.014(9) . ? Pd1 N2 2.123(9) . ? Pd1 S 2.257(3) . ? Pd1 Cl1 2.359(3) . ? Pd1 Pd2 3.0867(12) . ? Pd2 N3 2.031(8) . ? Pd2 N4 2.077(8) . ? Pd2 S 2.274(3) . ? Pd2 Cl1 2.375(3) . ? S C1 1.736(10) . ? Cl2 O2 1.362(15) . ? Cl2 O4 1.37(2) . ? Cl2 O3 1.373(16) . ? Cl2 O1 1.405(14) . ? Cl3 O8 1.35(2) . ? Cl3 O5 1.404(12) . ? Cl3 O7 1.477(15) . ? Cl3 O6 1.477(14) . ? N1 C7 1.478(13) . ? N1 C8 1.505(13) . ? N2 C9 1.456(14) . ? N2 C10 1.456(14) . ? N2 C11 1.487(12) . ? N3 C13 1.467(12) . ? N3 C12 1.474(11) . ? N4 C15 1.480(15) . ? N4 C16 1.510(15) . ? N4 C14 1.518(14) . ? C1 C6 1.372(13) . ? C1 C2 1.420(14) . ? C2 C3 1.381(14) . ? C2 C12 1.536(14) . ? C3 C4 1.379(14) . ? C4 C5 1.386(14) . ? C4 C17 1.530(15) . ? C5 C6 1.421(14) . ? C6 C7 1.517(14) . ? C8 C9 1.505(15) . ? C13 C14 1.494(15) . ? C17 C18 1.469(17) . ? C17 C19 1.499(16) . ? C17 C20 1.532(17) . ? O9A C21A 1.58(3) . ? O9B C21B 1.49(5) . ? 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 N2 85.1(3) . . ? N1 Pd1 S 93.9(2) . . ? N2 Pd1 S 173.2(2) . . ? N1 Pd1 Cl1 170.0(3) . . ? N2 Pd1 Cl1 99.2(3) . . ? S Pd1 Cl1 82.88(10) . . ? N1 Pd1 Pd2 122.0(2) . . ? N2 Pd1 Pd2 138.3(2) . . ? S Pd1 Pd2 47.29(7) . . ? Cl1 Pd1 Pd2 49.54(7) . . ? N3 Pd2 N4 84.5(3) . . ? N3 Pd2 S 93.8(2) . . ? N4 Pd2 S 177.1(3) . . ? N3 Pd2 Cl1 175.5(2) . . ? N4 Pd2 Cl1 99.6(3) . . ? S Pd2 Cl1 82.16(10) . . ? N3 Pd2 Pd1 126.5(2) . . ? N4 Pd2 Pd1 136.0(2) . . ? S Pd2 Pd1 46.83(7) . . ? Cl1 Pd2 Pd1 49.08(7) . . ? C1 S Pd1 107.9(3) . . ? C1 S Pd2 106.4(3) . . ? Pd1 S Pd2 85.88(9) . . ? Pd1 Cl1 Pd2 81.38(9) . . ? O2 Cl2 O4 100.5(11) . . ? O2 Cl2 O3 113.8(10) . . ? O4 Cl2 O3 100.1(11) . . ? O2 Cl2 O1 115.6(9) . . ? O4 Cl2 O1 111.5(10) . . ? O3 Cl2 O1 113.4(9) . . ? O8 Cl3 O5 118.6(10) . . ? O8 Cl3 O7 111.2(11) . . ? O5 Cl3 O7 107.5(8) . . ? O8 Cl3 O6 110.4(11) . . ? O5 Cl3 O6 107.0(8) . . ? O7 Cl3 O6 100.7(8) . . ? C7 N1 C8 114.0(8) . . ? C7 N1 Pd1 118.9(7) . . ? C8 N1 Pd1 106.7(7) . . ? C9 N2 C10 111.1(9) . . ? C9 N2 C11 112.0(9) . . ? C10 N2 C11 107.4(9) . . ? C9 N2 Pd1 105.6(6) . . ? C10 N2 Pd1 106.5(7) . . ? C11 N2 Pd1 114.1(7) . . ? C13 N3 C12 115.3(8) . . ? C13 N3 Pd2 106.4(6) . . ? C12 N3 Pd2 115.3(6) . . ? C15 N4 C16 109.5(9) . . ? C15 N4 C14 110.5(10) . . ? C16 N4 C14 108.0(9) . . ? C15 N4 Pd2 109.0(7) . . ? C16 N4 Pd2 113.5(7) . . ? C14 N4 Pd2 106.3(6) . . ? C6 C1 C2 117.8(9) . . ? C6 C1 S 123.0(8) . . ? C2 C1 S 119.1(8) . . ? C3 C2 C1 120.4(10) . . ? C3 C2 C12 119.8(9) . . ? C1 C2 C12 119.8(9) . . ? C4 C3 C2 122.9(10) . . ? C3 C4 C5 116.5(9) . . ? C3 C4 C17 120.7(10) . . ? C5 C4 C17 122.8(10) . . ? C4 C5 C6 122.2(10) . . ? C1 C6 C5 120.2(9) . . ? C1 C6 C7 121.2(9) . . ? C5 C6 C7 118.6(9) . . ? N1 C7 C6 112.4(8) . . ? C9 C8 N1 107.6(9) . . ? N2 C9 C8 111.0(9) . . ? N3 C12 C2 110.8(8) . . ? N3 C13 C14 106.9(9) . . ? C13 C14 N4 110.1(10) . . ? C18 C17 C19 107.2(11) . . ? C18 C17 C4 110.2(10) . . ? C19 C17 C4 112.6(9) . . ? C18 C17 C20 111.6(11) . . ? C19 C17 C20 108.8(12) . . ? C4 C17 C20 106.6(9) . . ? #===END # Attachment 'CCDC_286856_n.CIF' data_5 _database_code_depnum_ccdc_archive 'CCDC 286856' _chemical_formula_structural ; [(L3)Pd2(SCN)2]BPh4MeCN ; _chemical_formula_sum 'C48 H59 B N7 Pd2 S3' _chemical_formula_weight 1053.81 _chemical_melting_point ? _chemical_compound_source ; Crystals were taken from the reaction mixture (acetonitrile) ; #CRYSTAL DATA _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 12.459(3) _cell_length_b 13.980(3) _cell_length_c 15.412(3) _cell_angle_alpha 103.97(3) _cell_angle_beta 96.68(3) _cell_angle_gamma 109.90(3) _cell_volume 2390.7(8) _cell_formula_units_Z 2 _cell_measurement_temperature 210(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.464 _exptl_crystal_F_000 1082 _exptl_absorpt_coefficient_mu 0.924 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.85 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ? _diffrn_radiation_type MoK\a _diffrn_ambient_temperature 210(2) _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'BRUKER AXS' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_method hemisphere _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20729 _diffrn_reflns_av_R_equivalents 0.0387 _diffrn_reflns_av_sigmaI/netI 0.0694 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 28.65 #REFINEMENT DATA _reflns_number_total 10883 _reflns_number_gt 6872 _reflns_threshold_expression >2sigma(I) _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^)+(0.0686P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10883 _refine_ls_number_parameters 543 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0881 _refine_ls_R_factor_gt 0.0487 _refine_ls_wR_factor_ref 0.1315 _refine_ls_wR_factor_gt 0.1134 _refine_ls_goodness_of_fit_ref 0.976 _refine_ls_restrained_S_all 0.976 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.884 _diffrn_reflns_theta_full 28.65 _diffrn_measured_fraction_theta_full 0.884 _refine_diff_density_max 1.423 _refine_diff_density_min -0.964 _refine_diff_density_rms 0.107 _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 (FARRUGIA)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; #ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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' B B 0.0013 0.0007 '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' S S 0.1246 0.1234 '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' 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 -0.21704(3) 0.76614(3) 0.60750(3) 0.03846(11) Uani 1 1 d . . . Pd2 Pd 0.07356(3) 0.73969(3) 0.69332(2) 0.03354(11) Uani 1 1 d . . . S1 S -0.06016(10) 0.81401(9) 0.72130(8) 0.0353(3) Uani 1 1 d . . . S2 S -0.28286(15) 0.60165(12) 0.63312(13) 0.0721(5) Uani 1 1 d . . . S3 S -0.02758(12) 0.62839(10) 0.54773(9) 0.0527(3) Uani 1 1 d . . . N1 N -0.1583(3) 0.9030(3) 0.5771(3) 0.0398(9) Uani 1 1 d . . . N2 N -0.3627(3) 0.7253(3) 0.5007(3) 0.0519(11) Uani 1 1 d . . . N3 N 0.1684(3) 0.8361(3) 0.8187(2) 0.0355(8) Uani 1 1 d . . . N4 N 0.2009(3) 0.6715(3) 0.6984(3) 0.0410(9) Uani 1 1 d . . . N5 N -0.4606(6) 0.6053(6) 0.7338(5) 0.137(3) Uani 1 1 d . . . N6 N -0.0268(4) 0.7749(5) 0.4512(3) 0.0700(14) Uani 1 1 d . . . C1 C 0.0254(3) 0.9516(3) 0.7511(3) 0.0318(9) Uani 1 1 d . . . C2 C 0.1231(4) 0.9940(3) 0.8250(3) 0.0330(9) Uani 1 1 d . . . C3 C 0.1806(4) 1.1041(4) 0.8623(3) 0.0391(11) Uani 1 1 d . . . H3 H 0.2416 1.1304 0.9134 0.047 Uiso 1 1 calc R . . C4 C 0.1516(4) 1.1764(4) 0.8272(3) 0.0410(11) Uani 1 1 d . . . C5 C 0.0622(4) 1.1328(4) 0.7495(3) 0.0411(11) Uani 1 1 d . . . H5 H 0.0434 1.1787 0.7216 0.049 Uiso 1 1 calc R . . C6 C -0.0011(4) 1.0226(3) 0.7109(3) 0.0344(10) Uani 1 1 d . . . C7 C -0.0844(4) 0.9939(4) 0.6254(3) 0.0398(11) Uani 1 1 d . . . H7 H -0.0832 1.0503 0.6030 0.048 Uiso 1 1 calc R . . C8 C -0.2224(5) 0.8904(4) 0.4858(4) 0.0575(14) Uani 1 1 d . . . H8A H -0.1928 0.8539 0.4384 0.069 Uiso 1 1 calc R . . H8B H -0.2131 0.9596 0.4785 0.069 Uiso 1 1 calc R . . C9 C -0.3488(5) 0.8261(4) 0.4787(4) 0.0601(15) Uani 1 1 d . . . H9A H -0.3802 0.8676 0.5207 0.072 Uiso 1 1 calc R . . H9B H -0.3925 0.8097 0.4170 0.072 Uiso 1 1 calc R . . C10 C -0.3573(5) 0.6454(5) 0.4219(4) 0.0660(16) Uani 1 1 d . . . H10A H -0.3751 0.5786 0.4349 0.099 Uiso 1 1 calc R . . H10B H -0.2801 0.6686 0.4099 0.099 Uiso 1 1 calc R . . H10C H -0.4131 0.6368 0.3691 0.099 Uiso 1 1 calc R . . C11 C -0.4777(5) 0.6854(5) 0.5258(5) 0.0755(19) Uani 1 1 d . . . H11A H -0.5388 0.6734 0.4755 0.113 Uiso 1 1 calc R . . H11B H -0.4798 0.7373 0.5786 0.113 Uiso 1 1 calc R . . H11C H -0.4888 0.6197 0.5396 0.113 Uiso 1 1 calc R . . C12 C 0.1772(4) 0.9305(4) 0.8611(3) 0.0365(10) Uani 1 1 d . . . H12 H 0.2225 0.9610 0.9205 0.044 Uiso 1 1 calc R . . C13 C 0.2428(5) 0.7871(4) 0.8572(3) 0.0524(14) Uani 1 1 d . . . H13A H 0.1964 0.7290 0.8778 0.063 Uiso 1 1 calc R . . H13B H 0.3036 0.8395 0.9087 0.063 Uiso 1 1 calc R . . C14 C 0.2958(5) 0.7460(4) 0.7800(4) 0.0560(14) Uani 1 1 d . . . H14A H 0.3468 0.8054 0.7634 0.067 Uiso 1 1 calc R . . H14B H 0.3423 0.7088 0.7999 0.067 Uiso 1 1 calc R . . C15 C 0.2543(5) 0.6576(4) 0.6171(4) 0.0550(14) Uani 1 1 d . . . H15A H 0.2891 0.7254 0.6066 0.083 Uiso 1 1 calc R . . H15B H 0.1949 0.6090 0.5643 0.083 Uiso 1 1 calc R . . H15C H 0.3133 0.6296 0.6279 0.083 Uiso 1 1 calc R . . C16 C 0.1459(5) 0.5647(4) 0.7114(4) 0.0541(13) Uani 1 1 d . . . H16A H 0.2047 0.5364 0.7220 0.081 Uiso 1 1 calc R . . H16B H 0.0877 0.5175 0.6574 0.081 Uiso 1 1 calc R . . H16C H 0.1098 0.5715 0.7631 0.081 Uiso 1 1 calc R . . C17 C 0.2195(5) 1.2963(4) 0.8662(4) 0.0584(15) Uani 1 1 d . . . C18 C 0.2489(7) 1.3279(5) 0.9703(5) 0.102(3) Uani 1 1 d . . . H18A H 0.3027 1.2978 0.9898 0.153 Uiso 1 1 calc R . . H18B H 0.1787 1.3015 0.9920 0.153 Uiso 1 1 calc R . . H18C H 0.2840 1.4042 0.9949 0.153 Uiso 1 1 calc R . . C19 C 0.1510(7) 1.3589(5) 0.8400(6) 0.112(3) Uani 1 1 d . . . H19A H 0.1926 1.4333 0.8725 0.169 Uiso 1 1 calc R . . H19B H 0.0759 1.3345 0.8554 0.169 Uiso 1 1 calc R . . H19C H 0.1406 1.3489 0.7753 0.169 Uiso 1 1 calc R . . C20 C 0.3325(7) 1.3241(6) 0.8351(7) 0.131(4) Uani 1 1 d . . . H20A H 0.3180 1.3210 0.7717 0.196 Uiso 1 1 calc R . . H20B H 0.3675 1.2742 0.8425 0.196 Uiso 1 1 calc R . . H20C H 0.3846 1.3949 0.8711 0.196 Uiso 1 1 calc R . . C21 C -0.3866(7) 0.6088(5) 0.6935(5) 0.078(2) Uani 1 1 d . . . C22 C -0.0269(4) 0.7171(4) 0.4921(3) 0.0473(12) Uani 1 1 d . . . B B -0.3933(5) 1.1163(4) 0.7970(4) 0.0405(12) Uani 1 1 d . . . C101 C -0.5087(4) 1.0350(4) 0.7156(3) 0.0378(10) Uani 1 1 d . . . C102 C -0.6245(4) 1.0200(4) 0.7194(3) 0.0396(11) Uani 1 1 d . . . H102 H -0.6397 1.0548 0.7733 0.048 Uiso 1 1 calc R . . C103 C -0.7178(4) 0.9556(4) 0.6466(3) 0.0446(12) Uani 1 1 d . . . H103 H -0.7934 0.9483 0.6527 0.053 Uiso 1 1 calc R . . C104 C -0.7002(4) 0.9020(4) 0.5647(3) 0.0437(11) Uani 1 1 d . . . H104 H -0.7629 0.8573 0.5163 0.052 Uiso 1 1 calc R . . C105 C -0.5870(4) 0.9170(4) 0.5575(3) 0.0474(12) Uani 1 1 d . . . H105 H -0.5723 0.8838 0.5028 0.057 Uiso 1 1 calc R . . C106 C -0.4950(4) 0.9808(4) 0.6308(3) 0.0487(12) Uani 1 1 d . . . H106 H -0.4197 0.9885 0.6236 0.058 Uiso 1 1 calc R . . C201 C -0.3236(4) 1.2072(4) 0.7518(3) 0.0411(11) Uani 1 1 d . . . C202 C -0.3713(5) 1.2784(4) 0.7322(4) 0.0526(13) Uani 1 1 d . . . H202 H -0.4415 1.2753 0.7489 0.063 Uiso 1 1 calc R . . C203 C -0.3202(5) 1.3538(5) 0.6891(4) 0.0671(17) Uani 1 1 d . . . H203 H -0.3558 1.3996 0.6778 0.080 Uiso 1 1 calc R . . C204 C -0.2165(5) 1.3600(5) 0.6634(4) 0.0683(17) Uani 1 1 d . . . H204 H -0.1809 1.4106 0.6353 0.082 Uiso 1 1 calc R . . C205 C -0.1667(5) 1.2918(5) 0.6795(4) 0.0602(15) Uani 1 1 d . . . H205 H -0.0976 1.2943 0.6611 0.072 Uiso 1 1 calc R . . C206 C -0.2195(4) 1.2175(4) 0.7239(3) 0.0484(12) Uani 1 1 d . . . H206 H -0.1826 1.1727 0.7353 0.058 Uiso 1 1 calc R . . C301 C -0.3089(4) 1.0559(4) 0.8283(3) 0.0404(11) Uani 1 1 d . . . C302 C -0.3347(5) 0.9472(4) 0.7996(3) 0.0469(12) Uani 1 1 d . . . H302 H -0.4029 0.9026 0.7561 0.056 Uiso 1 1 calc R . . C303 C -0.2602(5) 0.9027(5) 0.8347(4) 0.0552(14) Uani 1 1 d . . . H303 H -0.2810 0.8292 0.8150 0.066 Uiso 1 1 calc R . . C304 C -0.1593(5) 0.9647(5) 0.8962(4) 0.0592(15) Uani 1 1 d . . . H304 H -0.1101 0.9344 0.9179 0.071 Uiso 1 1 calc R . . C305 C -0.1296(5) 1.0730(5) 0.9268(4) 0.0577(14) Uani 1 1 d . . . H305 H -0.0605 1.1167 0.9695 0.069 Uiso 1 1 calc R . . C306 C -0.2048(5) 1.1169(4) 0.8927(3) 0.0496(12) Uani 1 1 d . . . H306 H -0.1840 1.1903 0.9142 0.059 Uiso 1 1 calc R . . C401 C -0.4316(4) 1.1654(4) 0.8914(3) 0.0409(11) Uani 1 1 d . . . C402 C -0.3973(5) 1.2732(4) 0.9368(4) 0.0533(13) Uani 1 1 d . . . H402 H -0.3484 1.3230 0.9137 0.064 Uiso 1 1 calc R . . C403 C -0.4338(5) 1.3090(5) 1.0162(4) 0.0612(15) Uani 1 1 d . . . H403 H -0.4084 1.3819 1.0451 0.073 Uiso 1 1 calc R . . C404 C -0.5065(5) 1.2387(5) 1.0522(3) 0.0553(15) Uani 1 1 d . . . H404 H -0.5328 1.2627 1.1040 0.066 Uiso 1 1 calc R . . C405 C -0.5392(4) 1.1329(5) 1.0103(3) 0.0530(14) Uani 1 1 d . . . H405 H -0.5870 1.0836 1.0345 0.064 Uiso 1 1 calc R . . C406 C -0.5021(4) 1.0975(4) 0.9317(3) 0.0448(12) Uani 1 1 d . . . H406 H -0.5259 1.0244 0.9049 0.054 Uiso 1 1 calc R . . C23 C -0.035(2) 0.5633(14) 0.9035(12) 0.188(6) Uiso 1 1 d . . . C24 C -0.1186(14) 0.4620(13) 0.9066(10) 0.216(6) Uiso 1 1 d . . . N5A N 0.060(2) 0.6024(17) 0.9312(14) 0.132(10) Uiso 0.42(2) 1 d P . . N5B N -0.059(2) 0.627(2) 0.8714(17) 0.231(13) Uiso 0.58(2) 1 d P . . 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 0.0320(2) 0.0305(2) 0.0507(2) 0.00936(16) 0.00456(16) 0.01263(15) Pd2 0.0385(2) 0.03031(19) 0.03514(19) 0.01199(15) 0.00397(14) 0.01704(15) S1 0.0337(6) 0.0313(6) 0.0440(6) 0.0151(5) 0.0088(5) 0.0136(5) S2 0.0687(10) 0.0449(9) 0.0931(12) 0.0252(8) 0.0122(9) 0.0087(7) S3 0.0649(9) 0.0406(7) 0.0480(7) 0.0024(6) -0.0063(6) 0.0280(7) N1 0.035(2) 0.041(2) 0.046(2) 0.0152(19) 0.0026(17) 0.0195(18) N2 0.034(2) 0.047(3) 0.061(3) 0.000(2) -0.003(2) 0.0143(19) N3 0.037(2) 0.037(2) 0.0331(19) 0.0136(17) 0.0012(16) 0.0152(17) N4 0.047(2) 0.037(2) 0.046(2) 0.0173(18) 0.0074(19) 0.0224(19) N5 0.099(5) 0.100(5) 0.133(6) -0.048(4) 0.064(5) -0.013(4) N6 0.075(3) 0.107(4) 0.062(3) 0.046(3) 0.029(3) 0.057(3) C1 0.029(2) 0.034(2) 0.037(2) 0.0122(19) 0.0104(18) 0.0160(19) C2 0.035(2) 0.035(2) 0.031(2) 0.0078(19) 0.0095(18) 0.016(2) C3 0.036(2) 0.042(3) 0.037(2) 0.005(2) 0.006(2) 0.018(2) C4 0.039(3) 0.033(2) 0.050(3) 0.007(2) 0.008(2) 0.017(2) C5 0.040(3) 0.036(3) 0.054(3) 0.017(2) 0.010(2) 0.020(2) C6 0.032(2) 0.034(2) 0.040(2) 0.011(2) 0.0083(19) 0.016(2) C7 0.038(3) 0.039(3) 0.053(3) 0.022(2) 0.010(2) 0.021(2) C8 0.059(3) 0.053(3) 0.056(3) 0.017(3) -0.009(3) 0.022(3) C9 0.051(3) 0.060(4) 0.066(4) 0.011(3) -0.009(3) 0.029(3) C10 0.065(4) 0.057(4) 0.068(4) 0.003(3) 0.001(3) 0.027(3) C11 0.038(3) 0.089(5) 0.086(5) 0.020(4) 0.000(3) 0.017(3) C12 0.041(3) 0.043(3) 0.025(2) 0.014(2) 0.0053(19) 0.013(2) C13 0.064(3) 0.039(3) 0.051(3) 0.011(2) -0.010(3) 0.025(3) C14 0.050(3) 0.053(3) 0.068(4) 0.014(3) -0.006(3) 0.033(3) C15 0.060(3) 0.064(4) 0.057(3) 0.024(3) 0.022(3) 0.036(3) C16 0.072(4) 0.043(3) 0.059(3) 0.023(3) 0.013(3) 0.031(3) C17 0.047(3) 0.032(3) 0.082(4) 0.004(3) -0.005(3) 0.013(2) C18 0.121(6) 0.047(4) 0.102(6) -0.018(4) -0.029(5) 0.033(4) C19 0.120(6) 0.034(3) 0.147(7) 0.001(4) -0.059(5) 0.032(4) C20 0.098(6) 0.053(5) 0.196(10) 0.002(5) 0.055(7) -0.009(4) C21 0.093(5) 0.039(3) 0.071(4) 0.006(3) 0.015(4) -0.004(3) C22 0.047(3) 0.062(3) 0.043(3) 0.012(3) 0.010(2) 0.034(3) B 0.044(3) 0.044(3) 0.040(3) 0.017(3) 0.014(2) 0.021(3) C101 0.045(3) 0.038(3) 0.040(3) 0.020(2) 0.016(2) 0.020(2) C102 0.050(3) 0.049(3) 0.037(2) 0.024(2) 0.020(2) 0.028(2) C103 0.043(3) 0.057(3) 0.052(3) 0.030(3) 0.020(2) 0.027(2) C104 0.049(3) 0.042(3) 0.048(3) 0.023(2) 0.012(2) 0.020(2) C105 0.049(3) 0.055(3) 0.042(3) 0.013(2) 0.019(2) 0.023(3) C106 0.045(3) 0.057(3) 0.054(3) 0.021(3) 0.022(2) 0.025(3) C201 0.042(3) 0.048(3) 0.039(2) 0.018(2) 0.009(2) 0.019(2) C202 0.048(3) 0.059(3) 0.065(3) 0.032(3) 0.016(3) 0.027(3) C203 0.059(4) 0.073(4) 0.086(4) 0.052(4) 0.012(3) 0.027(3) C204 0.071(4) 0.081(4) 0.063(4) 0.048(3) 0.023(3) 0.021(3) C205 0.050(3) 0.074(4) 0.064(4) 0.030(3) 0.029(3) 0.020(3) C206 0.055(3) 0.059(3) 0.047(3) 0.022(3) 0.023(2) 0.033(3) C301 0.047(3) 0.049(3) 0.037(2) 0.019(2) 0.018(2) 0.026(2) C302 0.053(3) 0.051(3) 0.050(3) 0.022(2) 0.027(2) 0.026(3) C303 0.074(4) 0.058(3) 0.063(4) 0.033(3) 0.041(3) 0.043(3) C304 0.069(4) 0.086(5) 0.060(3) 0.041(3) 0.032(3) 0.055(4) C305 0.063(4) 0.082(4) 0.047(3) 0.030(3) 0.015(3) 0.043(3) C306 0.057(3) 0.050(3) 0.048(3) 0.016(3) 0.011(3) 0.027(3) C401 0.042(3) 0.051(3) 0.038(2) 0.014(2) 0.010(2) 0.027(2) C402 0.062(3) 0.050(3) 0.054(3) 0.017(3) 0.019(3) 0.027(3) C403 0.071(4) 0.062(4) 0.052(3) 0.005(3) 0.000(3) 0.040(3) C404 0.052(3) 0.092(5) 0.031(3) 0.012(3) 0.006(2) 0.043(3) C405 0.047(3) 0.085(4) 0.035(3) 0.023(3) 0.009(2) 0.030(3) C406 0.049(3) 0.055(3) 0.033(2) 0.017(2) 0.007(2) 0.021(2) _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 1.994(4) . ? Pd1 N2 2.115(4) . ? Pd1 S1 2.2561(15) . ? Pd1 S2 2.3121(17) . ? Pd2 N3 2.018(4) . ? Pd2 N4 2.113(4) . ? Pd2 S1 2.2739(13) . ? Pd2 S3 2.3163(17) . ? S1 C1 1.764(4) . ? S2 C21 1.694(8) . ? S3 C22 1.668(6) . ? N1 C7 1.266(6) . ? N1 C8 1.474(6) . ? N2 C10 1.463(7) . ? N2 C11 1.485(7) . ? N2 C9 1.487(7) . ? N3 C12 1.283(5) . ? N3 C13 1.478(5) . ? N4 C15 1.488(6) . ? N4 C16 1.489(6) . ? N4 C14 1.499(6) . ? N5 C21 1.165(8) . ? N6 C22 1.139(6) . ? C1 C6 1.397(6) . ? C1 C2 1.412(6) . ? C2 C3 1.393(6) . ? C2 C12 1.454(6) . ? C3 C4 1.382(6) . ? C4 C5 1.386(6) . ? C4 C17 1.523(7) . ? C5 C6 1.403(6) . ? C6 C7 1.455(6) . ? C8 C9 1.499(7) . ? C13 C14 1.515(7) . ? C17 C20 1.496(9) . ? C17 C19 1.503(8) . ? C17 C18 1.521(9) . ? B C201 1.634(7) . ? B C101 1.646(7) . ? B C401 1.648(7) . ? B C301 1.654(7) . ? C101 C102 1.397(6) . ? C101 C106 1.405(6) . ? C102 C103 1.384(7) . ? C103 C104 1.387(7) . ? C104 C105 1.376(7) . ? C105 C106 1.378(7) . ? C201 C206 1.386(6) . ? C201 C202 1.394(6) . ? C202 C203 1.392(7) . ? C203 C204 1.376(8) . ? C204 C205 1.355(8) . ? C205 C206 1.401(7) . ? C301 C302 1.384(7) . ? C301 C306 1.391(7) . ? C302 C303 1.407(7) . ? C303 C304 1.347(8) . ? C304 C305 1.372(8) . ? C305 C306 1.400(7) . ? C401 C406 1.380(6) . ? C401 C402 1.387(7) . ? C402 C403 1.394(7) . ? C403 C404 1.367(8) . ? C404 C405 1.355(8) . ? C405 C406 1.386(7) . ? C23 N5A 1.10(2) . ? C23 N5B 1.22(2) . ? C23 C24 1.459(18) . ? N5A N5B 1.83(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 N1 Pd1 N2 84.38(16) . . ? N1 Pd1 S1 94.19(11) . . ? N2 Pd1 S1 178.55(12) . . ? N1 Pd1 S2 176.00(12) . . ? N2 Pd1 S2 94.25(14) . . ? S1 Pd1 S2 87.20(6) . . ? N3 Pd2 N4 83.99(15) . . ? N3 Pd2 S1 86.22(11) . . ? N4 Pd2 S1 167.17(11) . . ? N3 Pd2 S3 177.41(11) . . ? N4 Pd2 S3 93.76(11) . . ? S1 Pd2 S3 96.19(5) . . ? C1 S1 Pd1 111.25(15) . . ? C1 S1 Pd2 102.31(14) . . ? Pd1 S1 Pd2 117.70(6) . . ? C21 S2 Pd1 102.8(2) . . ? C22 S3 Pd2 101.14(19) . . ? C7 N1 C8 119.7(4) . . ? C7 N1 Pd1 130.1(3) . . ? C8 N1 Pd1 110.0(3) . . ? C10 N2 C11 109.9(4) . . ? C10 N2 C9 110.6(5) . . ? C11 N2 C9 108.1(4) . . ? C10 N2 Pd1 108.6(3) . . ? C11 N2 Pd1 114.4(4) . . ? C9 N2 Pd1 105.1(3) . . ? C12 N3 C13 120.5(4) . . ? C12 N3 Pd2 129.6(3) . . ? C13 N3 Pd2 109.7(3) . . ? C15 N4 C16 107.9(4) . . ? C15 N4 C14 108.3(4) . . ? C16 N4 C14 110.8(4) . . ? C15 N4 Pd2 116.5(3) . . ? C16 N4 Pd2 108.1(3) . . ? C14 N4 Pd2 105.2(3) . . ? C6 C1 C2 117.7(4) . . ? C6 C1 S1 124.7(3) . . ? C2 C1 S1 117.4(3) . . ? C3 C2 C1 119.7(4) . . ? C3 C2 C12 115.7(4) . . ? C1 C2 C12 124.3(4) . . ? C4 C3 C2 123.4(4) . . ? C3 C4 C5 115.8(4) . . ? C3 C4 C17 122.4(4) . . ? C5 C4 C17 121.6(4) . . ? C4 C5 C6 123.1(4) . . ? C1 C6 C5 119.8(4) . . ? C1 C6 C7 126.0(4) . . ? C5 C6 C7 114.0(4) . . ? N1 C7 C6 129.2(4) . . ? N1 C8 C9 107.2(4) . . ? N2 C9 C8 110.7(4) . . ? N3 C12 C2 126.0(4) . . ? N3 C13 C14 105.6(4) . . ? N4 C14 C13 110.0(4) . . ? C20 C17 C19 111.3(6) . . ? C20 C17 C18 107.5(6) . . ? C19 C17 C18 107.2(6) . . ? C20 C17 C4 108.6(5) . . ? C19 C17 C4 112.4(5) . . ? C18 C17 C4 109.7(5) . . ? N5 C21 S2 174.7(7) . . ? N6 C22 S3 177.5(5) . . ? C201 B C101 104.2(4) . . ? C201 B C401 113.4(4) . . ? C101 B C401 111.3(4) . . ? C201 B C301 110.7(4) . . ? C101 B C301 112.7(4) . . ? C401 B C301 104.8(4) . . ? C102 C101 C106 114.1(4) . . ? C102 C101 B 125.3(4) . . ? C106 C101 B 120.4(4) . . ? C103 C102 C101 122.9(4) . . ? C102 C103 C104 120.9(4) . . ? C105 C104 C103 117.8(5) . . ? C104 C105 C106 120.6(5) . . ? C105 C106 C101 123.6(5) . . ? C206 C201 C202 113.8(4) . . ? C206 C201 B 125.4(4) . . ? C202 C201 B 120.7(4) . . ? C203 C202 C201 123.9(5) . . ? C204 C203 C202 119.3(5) . . ? C205 C204 C203 119.5(5) . . ? C204 C205 C206 120.0(5) . . ? C201 C206 C205 123.6(5) . . ? C302 C301 C306 115.5(4) . . ? C302 C301 B 125.9(4) . . ? C306 C301 B 118.6(4) . . ? C301 C302 C303 121.6(5) . . ? C304 C303 C302 121.1(5) . . ? C303 C304 C305 119.6(5) . . ? C304 C305 C306 119.1(5) . . ? C301 C306 C305 123.1(5) . . ? C406 C401 C402 114.9(4) . . ? C406 C401 B 120.0(4) . . ? C402 C401 B 125.1(5) . . ? C401 C402 C403 122.0(5) . . ? C404 C403 C402 121.0(5) . . ? C405 C404 C403 118.2(5) . . ? C404 C405 C406 120.6(5) . . ? C401 C406 C405 123.2(5) . . ? N5A C23 N5B 104(2) . . ? N5A C23 C24 130(2) . . ? N5B C23 C24 126(3) . . ? C23 N5A N5B 40.1(14) . . ? C23 N5B N5A 35.7(13) . . ? #===END # Attachment 'CCDC_286857_n.CIF' data_6 _database_code_depnum_ccdc_archive 'CCDC 286857' _chemical_formula_structural ; [(L3)Pd2(N3)2]BPh4(MeCN) ; _chemical_formula_sum 'C46 H56 B N11 Pd2 S' _chemical_formula_weight 1018.69 _chemical_melting_point ? _chemical_compound_source ; Crystals were grown by slwo evaporation from a mixed acetonitrile/ethanol solvent system ; #CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/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 11.646(2) _cell_length_b 19.717(3) _cell_length_c 20.203(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.976(3) _cell_angle_gamma 90.00 _cell_volume 4621.3(14) _cell_formula_units_Z 4 _cell_measurement_temperature 210(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.464 _exptl_crystal_F_000 2088 _exptl_absorpt_coefficient_mu 0.869 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.78 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ? _diffrn_radiation_type MoK\a _diffrn_ambient_temperature 210(2) _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'BRUKER AXS' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_method hemisphere _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41364 _diffrn_reflns_av_R_equivalents 0.0637 _diffrn_reflns_av_sigmaI/netI 0.0731 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 28.96 #REFINEMENT DATA _reflns_number_total 11258 _reflns_number_gt 6150 _reflns_threshold_expression >2sigma(I) _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^)+(0.0072P)^2^+22.0185P] 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 11258 _refine_ls_number_parameters 554 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1226 _refine_ls_R_factor_gt 0.0548 _refine_ls_wR_factor_ref 0.1188 _refine_ls_wR_factor_gt 0.0928 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.919 _diffrn_reflns_theta_full 28.96 _diffrn_measured_fraction_theta_full 0.919 _refine_diff_density_max 1.187 _refine_diff_density_min -1.355 _refine_diff_density_rms 0.123 _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 (FARRUGIA)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; #ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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' B B 0.0013 0.0007 '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' S S 0.1246 0.1234 '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' 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 0.85599(4) -0.02624(2) 0.20630(2) 0.04097(12) Uani 1 1 d . . . Pd2 Pd 0.77119(4) 0.05650(2) 0.02959(2) 0.03701(11) Uani 1 1 d . . . S S 0.90224(12) 0.02029(7) 0.11075(7) 0.0379(3) Uani 1 1 d . . . N1 N 0.9392(4) 0.0426(2) 0.2616(2) 0.0470(12) Uani 1 1 d . . . N2 N 0.8261(5) -0.0710(3) 0.2969(2) 0.0593(15) Uani 1 1 d . . . N3 N 0.9005(4) 0.0870(2) -0.0221(2) 0.0377(10) Uani 1 1 d . . . N4 N 0.6687(4) 0.0745(2) -0.0593(2) 0.0412(11) Uani 1 1 d . . . N5 N 0.7653(6) -0.1025(3) 0.1621(3) 0.088(2) Uani 1 1 d . . . N6 N 0.7472(4) -0.1127(3) 0.1048(3) 0.0558(14) Uani 1 1 d . . . N7 N 0.7247(5) -0.1261(4) 0.0504(3) 0.087(2) Uani 1 1 d . . . N8 N 0.6310(4) 0.0327(3) 0.0761(3) 0.0555(14) Uani 1 1 d . . . N9 N 0.6255(4) 0.0432(3) 0.1335(3) 0.0537(14) Uani 1 1 d . . . N10 N 0.6107(5) 0.0522(4) 0.1879(3) 0.089(2) Uani 1 1 d . . . C1 C 1.0081(4) 0.0828(3) 0.1231(3) 0.0336(11) Uani 1 1 d . . . C2 C 1.0611(5) 0.1005(3) 0.1855(3) 0.0381(12) Uani 1 1 d . . . C3 C 1.1549(5) 0.1453(3) 0.1904(3) 0.0416(13) Uani 1 1 d . . . H3 H 1.1897 0.1560 0.2328 0.050 Uiso 1 1 calc R . . C4 C 1.1985(5) 0.1743(3) 0.1355(3) 0.0407(13) Uani 1 1 d . . . C5 C 1.1432(5) 0.1569(3) 0.0749(3) 0.0407(13) Uani 1 1 d . . . H5 H 1.1706 0.1757 0.0365 0.049 Uiso 1 1 calc R . . C6 C 1.0493(4) 0.1132(3) 0.0671(3) 0.0364(12) Uani 1 1 d . . . C7 C 1.0205(5) 0.0831(3) 0.2494(3) 0.0507(15) Uani 1 1 d . . . H7 H 1.0590 0.1044 0.2866 0.061 Uiso 1 1 calc R . . C8 C 0.9071(8) 0.0378(4) 0.3308(3) 0.089(3) Uani 1 1 d . . . H8A H 0.9671 0.0589 0.3611 0.106 Uiso 1 1 calc R . . H8B H 0.8347 0.0621 0.3349 0.106 Uiso 1 1 calc R . . C9 C 0.8942(8) -0.0312(5) 0.3481(3) 0.097(3) Uani 1 1 d . . . H9A H 0.8568 -0.0337 0.3897 0.116 Uiso 1 1 calc R . . H9B H 0.9708 -0.0518 0.3561 0.116 Uiso 1 1 calc R . . C10 C 0.7038(7) -0.0700(5) 0.3058(4) 0.103(3) Uani 1 1 d . . . H10A H 0.6621 -0.0946 0.2698 0.155 Uiso 1 1 calc R . . H10B H 0.6769 -0.0234 0.3058 0.155 Uiso 1 1 calc R . . H10C H 0.6907 -0.0912 0.3478 0.155 Uiso 1 1 calc R . . C11 C 0.8669(9) -0.1414(4) 0.3014(4) 0.110(3) Uani 1 1 d . . . H11A H 0.8557 -0.1593 0.3450 0.165 Uiso 1 1 calc R . . H11B H 0.9482 -0.1428 0.2943 0.165 Uiso 1 1 calc R . . H11C H 0.8237 -0.1685 0.2677 0.165 Uiso 1 1 calc R . . C12 C 1.0002(5) 0.1073(3) -0.0011(3) 0.0394(13) Uani 1 1 d . . . H12 H 1.0485 0.1201 -0.0339 0.047 Uiso 1 1 calc R . . C13 C 0.8631(5) 0.0907(3) -0.0937(3) 0.0470(15) Uani 1 1 d . . . H13A H 0.8667 0.0458 -0.1140 0.056 Uiso 1 1 calc R . . H13B H 0.9132 0.1216 -0.1161 0.056 Uiso 1 1 calc R . . C14 C 0.7420(5) 0.1165(3) -0.0998(3) 0.0457(14) Uani 1 1 d . . . H14A H 0.7409 0.1637 -0.0848 0.055 Uiso 1 1 calc R . . H14B H 0.7112 0.1151 -0.1465 0.055 Uiso 1 1 calc R . . C15 C 0.6463(5) 0.0068(3) -0.0903(3) 0.0520(16) Uani 1 1 d . . . H15A H 0.5993 -0.0200 -0.0627 0.078 Uiso 1 1 calc R . . H15B H 0.7189 -0.0163 -0.0943 0.078 Uiso 1 1 calc R . . H15C H 0.6060 0.0124 -0.1340 0.078 Uiso 1 1 calc R . . C16 C 0.5568(5) 0.1083(3) -0.0532(3) 0.0545(17) Uani 1 1 d . . . H16A H 0.5698 0.1520 -0.0317 0.082 Uiso 1 1 calc R . . H16B H 0.5096 0.0803 -0.0269 0.082 Uiso 1 1 calc R . . H16C H 0.5176 0.1150 -0.0971 0.082 Uiso 1 1 calc R . . C17 C 1.3016(5) 0.2225(3) 0.1404(3) 0.0491(15) Uani 1 1 d . . . C18 C 1.4082(6) 0.1836(5) 0.1279(5) 0.113(4) Uani 1 1 d . . . H18A H 1.3978 0.1623 0.0845 0.169 Uiso 1 1 calc R . . H18B H 1.4224 0.1490 0.1618 0.169 Uiso 1 1 calc R . . H18C H 1.4734 0.2144 0.1293 0.169 Uiso 1 1 calc R . . C19 C 1.2831(8) 0.2785(4) 0.0885(4) 0.099(3) Uani 1 1 d . . . H19A H 1.2728 0.2585 0.0445 0.149 Uiso 1 1 calc R . . H19B H 1.3497 0.3082 0.0913 0.149 Uiso 1 1 calc R . . H19C H 1.2149 0.3044 0.0967 0.149 Uiso 1 1 calc R . . C20 C 1.3180(6) 0.2565(4) 0.2080(4) 0.081(2) Uani 1 1 d . . . H20A H 1.3839 0.2866 0.2093 0.121 Uiso 1 1 calc R . . H20B H 1.3309 0.2222 0.2422 0.121 Uiso 1 1 calc R . . H20C H 1.2495 0.2824 0.2156 0.121 Uiso 1 1 calc R . . B B 0.7301(6) -0.1610(4) 0.5351(3) 0.0446(16) Uani 1 1 d . . . C101 C 0.7394(5) -0.0794(3) 0.5164(3) 0.0434(14) Uani 1 1 d . . . C102 C 0.6470(6) -0.0449(3) 0.4841(3) 0.0608(18) Uani 1 1 d . . . H102 H 0.5788 -0.0692 0.4725 0.073 Uiso 1 1 calc R . . C103 C 0.6492(7) 0.0224(4) 0.4681(4) 0.068(2) Uani 1 1 d . . . H103 H 0.5838 0.0427 0.4457 0.082 Uiso 1 1 calc R . . C104 C 0.7454(7) 0.0606(3) 0.4844(4) 0.0666(19) Uani 1 1 d . . . H104 H 0.7474 0.1069 0.4736 0.080 Uiso 1 1 calc R . . C105 C 0.8385(7) 0.0293(4) 0.5168(4) 0.074(2) Uani 1 1 d . . . H105 H 0.9058 0.0543 0.5288 0.089 Uiso 1 1 calc R . . C106 C 0.8344(6) -0.0387(3) 0.5318(3) 0.0599(18) Uani 1 1 d . . . H106 H 0.9004 -0.0586 0.5538 0.072 Uiso 1 1 calc R . . C201 C 0.7037(5) -0.2058(3) 0.4662(3) 0.0434(14) Uani 1 1 d . . . C202 C 0.6001(5) -0.1995(3) 0.4265(3) 0.0557(17) Uani 1 1 d . . . H202 H 0.5433 -0.1702 0.4404 0.067 Uiso 1 1 calc R . . C203 C 0.5776(6) -0.2343(4) 0.3679(3) 0.0638(19) Uani 1 1 d . . . H203 H 0.5065 -0.2281 0.3429 0.077 Uiso 1 1 calc R . . C204 C 0.6561(7) -0.2776(4) 0.3455(3) 0.0629(19) Uani 1 1 d . . . H204 H 0.6408 -0.3004 0.3048 0.076 Uiso 1 1 calc R . . C205 C 0.7583(6) -0.2874(3) 0.3834(3) 0.0606(18) Uani 1 1 d . . . H205 H 0.8128 -0.3182 0.3694 0.073 Uiso 1 1 calc R . . C206 C 0.7813(6) -0.2517(3) 0.4425(3) 0.0506(15) Uani 1 1 d . . . H206 H 0.8522 -0.2589 0.4674 0.061 Uiso 1 1 calc R . . C301 C 0.8502(5) -0.1877(3) 0.5765(3) 0.0438(14) Uani 1 1 d . . . C302 C 0.9578(6) -0.1830(3) 0.5515(3) 0.0552(16) Uani 1 1 d . . . H302 H 0.9621 -0.1620 0.5100 0.066 Uiso 1 1 calc R . . C303 C 1.0580(6) -0.2073(3) 0.5840(4) 0.0628(19) Uani 1 1 d . . . H303 H 1.1283 -0.2030 0.5648 0.075 Uiso 1 1 calc R . . C304 C 1.0549(7) -0.2379(4) 0.6446(4) 0.068(2) Uani 1 1 d . . . H304 H 1.1230 -0.2544 0.6674 0.082 Uiso 1 1 calc R . . C305 C 0.9528(7) -0.2443(3) 0.6716(3) 0.0627(19) Uani 1 1 d . . . H305 H 0.9503 -0.2654 0.7132 0.075 Uiso 1 1 calc R . . C306 C 0.8520(6) -0.2199(3) 0.6383(3) 0.0479(15) Uani 1 1 d . . . H306 H 0.7823 -0.2252 0.6580 0.057 Uiso 1 1 calc R . . C401 C 0.6227(5) -0.1685(3) 0.5823(3) 0.0481(15) Uani 1 1 d . . . C402 C 0.6103(6) -0.1236(4) 0.6341(3) 0.0622(18) Uani 1 1 d . . . H402 H 0.6654 -0.0891 0.6421 0.075 Uiso 1 1 calc R . . C403 C 0.5209(8) -0.1273(4) 0.6744(4) 0.080(2) Uani 1 1 d . . . H403 H 0.5156 -0.0951 0.7083 0.097 Uiso 1 1 calc R . . C404 C 0.4406(8) -0.1768(5) 0.6656(5) 0.095(3) Uani 1 1 d . . . H404 H 0.3791 -0.1790 0.6928 0.114 Uiso 1 1 calc R . . C405 C 0.4505(7) -0.2230(5) 0.6171(5) 0.100(3) Uani 1 1 d . . . H405 H 0.3970 -0.2587 0.6114 0.120 Uiso 1 1 calc R . . C406 C 0.5394(6) -0.2183(4) 0.5754(4) 0.070(2) Uani 1 1 d . . . H406 H 0.5426 -0.2503 0.5411 0.085 Uiso 1 1 calc R . . N11 N 1.2080(10) -0.0456(6) 0.2634(5) 0.156(4) Uani 1 1 d . . . C21 C 1.2859(11) -0.0510(5) 0.2980(6) 0.106(3) Uani 1 1 d . . . C22 C 1.3834(9) -0.0589(5) 0.3448(6) 0.136(4) Uani 1 1 d . . . H22A H 1.3961 -0.0174 0.3701 0.204 Uiso 1 1 calc R . . H22B H 1.4508 -0.0689 0.3215 0.204 Uiso 1 1 calc R . . H22C H 1.3698 -0.0960 0.3748 0.204 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 0.0456(3) 0.0402(2) 0.0373(2) 0.00285(19) 0.00450(19) -0.0080(2) Pd2 0.0323(2) 0.0421(2) 0.0368(2) -0.00015(19) 0.00412(17) -0.00196(19) S 0.0377(7) 0.0414(8) 0.0346(7) 0.0008(6) 0.0023(6) -0.0071(6) N1 0.058(3) 0.051(3) 0.032(2) -0.001(2) 0.007(2) -0.010(3) N2 0.075(4) 0.063(4) 0.040(3) 0.010(3) 0.007(3) -0.022(3) N3 0.035(2) 0.047(3) 0.032(2) 0.001(2) 0.0034(19) 0.002(2) N4 0.035(2) 0.043(3) 0.045(3) 0.002(2) -0.001(2) -0.001(2) N5 0.134(6) 0.080(5) 0.050(4) 0.001(3) 0.000(4) -0.061(4) N6 0.046(3) 0.054(3) 0.069(4) -0.011(3) 0.017(3) -0.013(3) N7 0.074(4) 0.118(6) 0.070(4) -0.048(4) 0.015(4) -0.013(4) N8 0.040(3) 0.083(4) 0.043(3) -0.001(3) 0.007(2) -0.014(3) N9 0.037(3) 0.068(4) 0.058(4) 0.011(3) 0.012(3) 0.007(3) N10 0.076(4) 0.134(6) 0.062(4) 0.001(4) 0.024(3) 0.023(4) C1 0.031(3) 0.031(3) 0.038(3) 0.002(2) 0.005(2) 0.002(2) C2 0.039(3) 0.040(3) 0.034(3) 0.000(2) 0.000(2) -0.003(3) C3 0.044(3) 0.044(3) 0.036(3) 0.001(3) -0.001(3) -0.002(3) C4 0.038(3) 0.041(3) 0.044(3) 0.000(3) 0.004(3) 0.000(3) C5 0.038(3) 0.043(3) 0.042(3) 0.001(3) 0.009(3) -0.001(3) C6 0.032(3) 0.037(3) 0.041(3) 0.001(2) 0.008(2) 0.003(2) C7 0.058(4) 0.052(4) 0.041(3) -0.005(3) -0.003(3) -0.011(3) C8 0.135(7) 0.100(7) 0.034(4) -0.011(4) 0.023(4) -0.058(6) C9 0.137(8) 0.115(7) 0.037(4) 0.007(4) 0.007(4) -0.056(6) C10 0.098(7) 0.153(9) 0.063(5) 0.022(5) 0.030(5) -0.039(6) C11 0.163(10) 0.076(6) 0.092(7) 0.046(5) 0.015(6) 0.014(6) C12 0.036(3) 0.049(3) 0.035(3) 0.001(2) 0.012(2) 0.001(3) C13 0.047(3) 0.060(4) 0.033(3) 0.001(3) 0.004(3) -0.003(3) C14 0.044(3) 0.047(4) 0.044(3) 0.008(3) -0.005(3) 0.000(3) C15 0.043(3) 0.048(4) 0.063(4) -0.005(3) -0.006(3) -0.007(3) C16 0.032(3) 0.065(4) 0.065(4) 0.006(3) 0.000(3) 0.011(3) C17 0.046(4) 0.050(4) 0.051(4) 0.003(3) 0.001(3) -0.016(3) C18 0.041(4) 0.105(7) 0.195(11) -0.033(7) 0.026(6) -0.016(5) C19 0.117(7) 0.084(6) 0.092(6) 0.028(5) -0.010(5) -0.059(5) C20 0.075(5) 0.093(6) 0.075(5) -0.013(4) 0.005(4) -0.046(5) B 0.046(4) 0.046(4) 0.042(4) -0.002(3) 0.004(3) -0.001(3) C101 0.050(3) 0.041(3) 0.039(3) -0.002(3) 0.004(3) -0.005(3) C102 0.058(4) 0.049(4) 0.073(5) 0.002(3) -0.010(3) -0.006(3) C103 0.078(5) 0.051(4) 0.074(5) 0.003(4) -0.010(4) 0.012(4) C104 0.088(6) 0.040(4) 0.073(5) 0.006(3) 0.016(4) -0.002(4) C105 0.072(5) 0.052(4) 0.097(6) 0.000(4) -0.001(4) -0.014(4) C106 0.062(4) 0.043(4) 0.072(5) 0.004(3) -0.012(3) -0.009(3) C201 0.047(3) 0.038(3) 0.045(3) 0.006(3) 0.004(3) -0.005(3) C202 0.051(4) 0.058(4) 0.056(4) -0.004(3) -0.005(3) -0.005(3) C203 0.063(5) 0.064(5) 0.062(4) 0.000(4) -0.010(4) -0.016(4) C204 0.080(5) 0.066(5) 0.043(4) -0.009(3) 0.006(4) -0.032(4) C205 0.074(5) 0.048(4) 0.063(4) -0.009(3) 0.024(4) -0.009(4) C206 0.056(4) 0.051(4) 0.045(4) 0.002(3) 0.005(3) -0.003(3) C301 0.051(4) 0.039(3) 0.040(3) -0.004(3) -0.003(3) -0.001(3) C302 0.058(4) 0.051(4) 0.057(4) -0.001(3) 0.004(3) -0.002(3) C303 0.048(4) 0.059(5) 0.080(5) -0.009(4) -0.001(4) -0.002(3) C304 0.066(5) 0.064(5) 0.070(5) -0.008(4) -0.020(4) 0.004(4) C305 0.081(5) 0.063(5) 0.040(4) 0.002(3) -0.013(4) 0.007(4) C306 0.062(4) 0.045(4) 0.035(3) -0.002(3) -0.001(3) -0.001(3) C401 0.053(4) 0.049(4) 0.043(3) 0.006(3) 0.005(3) 0.005(3) C402 0.072(5) 0.064(5) 0.053(4) 0.002(3) 0.015(4) 0.007(4) C403 0.103(7) 0.077(6) 0.067(5) 0.017(4) 0.038(5) 0.032(5) C404 0.087(7) 0.112(8) 0.094(7) 0.035(6) 0.049(6) 0.026(6) C405 0.075(6) 0.120(8) 0.109(8) 0.021(6) 0.034(6) -0.025(6) C406 0.074(5) 0.072(5) 0.067(5) -0.002(4) 0.021(4) -0.017(4) N11 0.181(11) 0.149(9) 0.129(9) -0.017(7) -0.034(7) 0.053(8) C21 0.126(10) 0.083(7) 0.106(8) -0.008(6) -0.005(7) 0.017(7) C22 0.125(9) 0.092(8) 0.185(12) 0.008(8) -0.021(9) 0.002(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 1.959(5) . ? Pd1 N5 2.003(6) . ? Pd1 N2 2.088(5) . ? Pd1 S 2.2446(14) . ? Pd2 N3 1.998(4) . ? Pd2 N8 2.009(5) . ? Pd2 N4 2.099(4) . ? Pd2 S 2.2567(14) . ? S C1 1.746(5) . ? N1 C7 1.279(7) . ? N1 C8 1.482(7) . ? N2 C10 1.451(9) . ? N2 C11 1.468(9) . ? N2 C9 1.473(8) . ? N3 C12 1.266(6) . ? N3 C13 1.476(6) . ? N4 C16 1.478(7) . ? N4 C14 1.486(7) . ? N4 C15 1.488(7) . ? N5 N6 1.175(7) . ? N6 N7 1.138(7) . ? N8 N9 1.186(7) . ? N9 N10 1.141(7) . ? C1 C2 1.398(7) . ? C1 C6 1.401(7) . ? C2 C3 1.401(7) . ? C2 C7 1.455(8) . ? C3 C4 1.381(7) . ? C4 C5 1.377(7) . ? C4 C17 1.528(8) . ? C5 C6 1.390(7) . ? C6 C12 1.451(7) . ? C8 C9 1.417(10) . ? C13 C14 1.494(7) . ? C17 C18 1.499(9) . ? C17 C20 1.518(9) . ? C17 C19 1.525(9) . ? B C401 1.644(9) . ? B C301 1.653(9) . ? B C201 1.655(9) . ? B C101 1.657(9) . ? C101 C106 1.380(8) . ? C101 C102 1.389(8) . ? C102 C103 1.366(9) . ? C103 C104 1.366(9) . ? C104 C105 1.365(9) . ? C105 C106 1.375(9) . ? C201 C206 1.393(8) . ? C201 C202 1.395(8) . ? C202 C203 1.373(9) . ? C203 C204 1.357(9) . ? C204 C205 1.371(9) . ? C205 C206 1.392(8) . ? C301 C302 1.394(8) . ? C301 C306 1.399(8) . ? C302 C303 1.376(9) . ? C303 C304 1.368(10) . ? C304 C305 1.356(10) . ? C305 C306 1.387(8) . ? C401 C406 1.378(9) . ? C401 C402 1.388(8) . ? C402 C403 1.379(9) . ? C403 C404 1.352(12) . ? C404 C405 1.351(12) . ? C405 C406 1.393(10) . ? N11 C21 1.101(12) . ? C21 C22 1.422(13) . ? 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 N5 171.8(2) . . ? N1 Pd1 N2 84.5(2) . . ? N5 Pd1 N2 87.3(2) . . ? N1 Pd1 S 93.65(14) . . ? N5 Pd1 S 94.57(17) . . ? N2 Pd1 S 175.71(17) . . ? N3 Pd2 N8 174.1(2) . . ? N3 Pd2 N4 84.33(17) . . ? N8 Pd2 N4 90.82(19) . . ? N3 Pd2 S 88.95(13) . . ? N8 Pd2 S 96.45(15) . . ? N4 Pd2 S 166.87(13) . . ? C1 S Pd1 112.62(18) . . ? C1 S Pd2 107.76(18) . . ? Pd1 S Pd2 123.81(6) . . ? C7 N1 C8 118.2(5) . . ? C7 N1 Pd1 131.4(4) . . ? C8 N1 Pd1 110.0(4) . . ? C10 N2 C11 108.7(7) . . ? C10 N2 C9 112.4(6) . . ? C11 N2 C9 108.0(7) . . ? C10 N2 Pd1 110.1(4) . . ? C11 N2 Pd1 112.0(5) . . ? C9 N2 Pd1 105.7(4) . . ? C12 N3 C13 119.7(5) . . ? C12 N3 Pd2 129.2(4) . . ? C13 N3 Pd2 110.8(3) . . ? C16 N4 C14 110.3(4) . . ? C16 N4 C15 108.4(4) . . ? C14 N4 C15 110.9(5) . . ? C16 N4 Pd2 116.5(4) . . ? C14 N4 Pd2 104.7(3) . . ? C15 N4 Pd2 105.9(3) . . ? N6 N5 Pd1 127.6(5) . . ? N7 N6 N5 175.2(7) . . ? N9 N8 Pd2 122.2(4) . . ? N10 N9 N8 174.4(7) . . ? C2 C1 C6 117.7(5) . . ? C2 C1 S 123.8(4) . . ? C6 C1 S 118.3(4) . . ? C1 C2 C3 120.1(5) . . ? C1 C2 C7 126.1(5) . . ? C3 C2 C7 113.4(5) . . ? C4 C3 C2 122.9(5) . . ? C5 C4 C3 115.7(5) . . ? C5 C4 C17 121.1(5) . . ? C3 C4 C17 123.2(5) . . ? C4 C5 C6 123.8(5) . . ? C5 C6 C1 119.7(5) . . ? C5 C6 C12 113.5(5) . . ? C1 C6 C12 126.8(5) . . ? N1 C7 C2 128.4(5) . . ? C9 C8 N1 109.5(6) . . ? C8 C9 N2 113.6(7) . . ? N3 C12 C6 128.1(5) . . ? N3 C13 C14 107.2(4) . . ? N4 C14 C13 110.4(5) . . ? C18 C17 C20 109.6(6) . . ? C18 C17 C19 108.9(7) . . ? C20 C17 C19 107.3(6) . . ? C18 C17 C4 109.2(5) . . ? C20 C17 C4 111.7(5) . . ? C19 C17 C4 110.1(5) . . ? C401 B C301 109.2(5) . . ? C401 B C201 110.2(5) . . ? C301 B C201 110.1(5) . . ? C401 B C101 106.8(5) . . ? C301 B C101 110.8(5) . . ? C201 B C101 109.8(5) . . ? C106 C101 C102 113.1(6) . . ? C106 C101 B 125.6(5) . . ? C102 C101 B 121.3(5) . . ? C103 C102 C101 123.9(6) . . ? C104 C103 C102 120.6(7) . . ? C105 C104 C103 117.9(7) . . ? C104 C105 C106 120.3(7) . . ? C105 C106 C101 124.1(6) . . ? C206 C201 C202 114.5(6) . . ? C206 C201 B 123.9(5) . . ? C202 C201 B 121.6(5) . . ? C203 C202 C201 122.8(7) . . ? C204 C203 C202 121.2(7) . . ? C203 C204 C205 118.6(6) . . ? C204 C205 C206 120.1(7) . . ? C205 C206 C201 122.7(6) . . ? C302 C301 C306 114.1(6) . . ? C302 C301 B 122.9(5) . . ? C306 C301 B 122.9(5) . . ? C303 C302 C301 123.8(6) . . ? C304 C303 C302 119.6(7) . . ? C305 C304 C303 119.6(7) . . ? C304 C305 C306 120.5(6) . . ? C305 C306 C301 122.5(6) . . ? C406 C401 C402 114.3(6) . . ? C406 C401 B 124.8(6) . . ? C402 C401 B 120.9(6) . . ? C403 C402 C401 123.0(7) . . ? C404 C403 C402 120.6(8) . . ? C405 C404 C403 118.7(8) . . ? C404 C405 C406 120.6(9) . . ? C401 C406 C405 122.7(8) . . ? N11 C21 C22 177.5(15) . . ? #===END # Attachment 'CCDC_286858_n.CIF' data_7 _database_code_depnum_ccdc_archive 'CCDC 286858' _chemical_formula_structural ; [{(L3)Pd2(uCN}2](ClO4)4(CH3CH2CN)2(MeCN) ; _chemical_formula_sum 'C50 H79 Cl4 N13 O16 Pd4 S2' _chemical_formula_weight 1749.78 _chemical_melting_point ? _chemical_compound_source ; Crystals were grown by recrystallization from a mixed acetonitrile/propionitrile solvent system ; #CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.689(5) _cell_length_b 11.289(2) _cell_length_c 27.918(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.71(3) _cell_angle_gamma 90.00 _cell_volume 7466(3) _cell_formula_units_Z 8 _cell_measurement_temperature 210(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.557 _exptl_crystal_F_000 3528 _exptl_absorpt_coefficient_mu 1.212 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.80 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ? _diffrn_radiation_type MoK\a _diffrn_ambient_temperature 210(2) _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'BRUKER AXS' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_method hemisphere _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32483 _diffrn_reflns_av_R_equivalents 0.0695 _diffrn_reflns_av_sigmaI/netI 0.0890 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 28.84 #REFINEMENT DATA _reflns_number_total 9087 _reflns_number_gt 5038 _reflns_threshold_expression >2sigma(I) _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^)+(0.1034P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9087 _refine_ls_number_parameters 429 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1275 _refine_ls_R_factor_gt 0.0581 _refine_ls_wR_factor_ref 0.1893 _refine_ls_wR_factor_gt 0.1493 _refine_ls_goodness_of_fit_ref 0.993 _refine_ls_restrained_S_all 0.993 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.930 _diffrn_reflns_theta_full 28.84 _diffrn_measured_fraction_theta_full 0.930 _refine_diff_density_max 1.612 _refine_diff_density_min -0.673 _refine_diff_density_rms 0.175 _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 (FARRUGIA)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; #ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' 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 1.08776(2) 1.00771(4) 0.307453(17) 0.03173(16) Uani 1 1 d . . . Pd2 Pd 0.97077(2) 0.76829(5) 0.339433(17) 0.03294(16) Uani 1 1 d . . . S S 1.05868(8) 0.84892(14) 0.35038(6) 0.0340(4) Uani 1 1 d . . . Cl1 Cl 0.91024(10) 0.6267(2) 0.52227(8) 0.0605(6) Uani 1 1 d . . . Cl2 Cl 1.25007(11) 0.8853(2) 0.31271(11) 0.0736(7) Uani 1 1 d . . . N1 N 1.1089(2) 1.1033(5) 0.36460(19) 0.0351(13) Uani 1 1 d . . . N2 N 1.1236(3) 1.1471(5) 0.2685(2) 0.0419(15) Uani 1 1 d . . . N3 N 0.9893(3) 0.6555(5) 0.39251(19) 0.0366(14) Uani 1 1 d . . . N4 N 0.8978(3) 0.6647(6) 0.3306(2) 0.0449(15) Uani 1 1 d . . . C1 C 1.0660(3) 0.8702(6) 0.4127(2) 0.0326(15) Uani 1 1 d . . . C2 C 1.0503(3) 0.7780(6) 0.4434(2) 0.0366(16) Uani 1 1 d . . . C3 C 1.0620(3) 0.7856(6) 0.4924(2) 0.0384(17) Uani 1 1 d . . . H3 H 1.0525 0.7218 0.5118 0.046 Uiso 1 1 calc R . . C4 C 1.0869(3) 0.8833(6) 0.5135(2) 0.0387(16) Uani 1 1 d . A . C5 C 1.1003(3) 0.9740(6) 0.4831(2) 0.0387(16) Uani 1 1 d . . . H5 H 1.1161 1.0421 0.4963 0.046 Uiso 1 1 calc R . . C6 C 1.0916(3) 0.9711(6) 0.4330(2) 0.0356(16) Uani 1 1 d . . . C7 C 1.1099(3) 1.0785(6) 0.4087(2) 0.0384(16) Uani 1 1 d . . . H7 H 1.1244 1.1374 0.4286 0.046 Uiso 1 1 calc R . . C8 C 1.1261(4) 1.2239(7) 0.3501(3) 0.050(2) Uani 1 1 d . . . H8A H 1.1506 1.2585 0.3744 0.060 Uiso 1 1 calc R . . H8B H 1.0931 1.2741 0.3462 0.060 Uiso 1 1 calc R . . C9 C 1.1566(4) 1.2147(7) 0.3038(3) 0.048(2) Uani 1 1 d . . . H9A H 1.1637 1.2935 0.2915 0.058 Uiso 1 1 calc R . . H9B H 1.1927 1.1761 0.3092 0.058 Uiso 1 1 calc R . . C10 C 1.0792(4) 1.2222(7) 0.2464(3) 0.058(2) Uani 1 1 d . . . H10A H 1.0621 1.2702 0.2706 0.088 Uiso 1 1 calc R . . H10B H 1.0510 1.1728 0.2316 0.088 Uiso 1 1 calc R . . H10C H 1.0957 1.2724 0.2226 0.088 Uiso 1 1 calc R . . C11 C 1.1602(4) 1.1033(8) 0.2291(3) 0.057(2) Uani 1 1 d . . . H11A H 1.1372 1.0669 0.2047 0.086 Uiso 1 1 calc R . . H11B H 1.1865 1.0462 0.2417 0.086 Uiso 1 1 calc R . . H11C H 1.1805 1.1686 0.2156 0.086 Uiso 1 1 calc R . . C12 C 1.0193(3) 0.6702(6) 0.4295(2) 0.0377(17) Uani 1 1 d . . . H12 H 1.0222 0.6062 0.4504 0.045 Uiso 1 1 calc R . . C13 C 0.9575(4) 0.5467(6) 0.3851(3) 0.048(2) Uani 1 1 d . . . H13A H 0.9581 0.4992 0.4140 0.057 Uiso 1 1 calc R . . H13B H 0.9739 0.5008 0.3594 0.057 Uiso 1 1 calc R . . C14 C 0.8976(4) 0.5814(7) 0.3722(3) 0.052(2) Uani 1 1 d . . . H14A H 0.8759 0.5113 0.3641 0.063 Uiso 1 1 calc R . . H14B H 0.8801 0.6193 0.3994 0.063 Uiso 1 1 calc R . . C15 C 0.8459(4) 0.7297(9) 0.3288(4) 0.077(3) Uani 1 1 d . . . H15A H 0.8151 0.6761 0.3230 0.115 Uiso 1 1 calc R . . H15B H 0.8473 0.7870 0.3035 0.115 Uiso 1 1 calc R . . H15C H 0.8405 0.7694 0.3588 0.115 Uiso 1 1 calc R . . C16 C 0.9045(4) 0.5970(7) 0.2850(3) 0.060(2) Uani 1 1 d . . . H16A H 0.8722 0.5470 0.2799 0.090 Uiso 1 1 calc R . . H16B H 0.9379 0.5491 0.2870 0.090 Uiso 1 1 calc R . . H16C H 0.9077 0.6514 0.2587 0.090 Uiso 1 1 calc R . . C17 C 1.0974(3) 0.8902(7) 0.5675(2) 0.0432(18) Uani 1 1 d . . . C21 C 1.0666(3) 0.9220(5) 0.2483(2) 0.0263(13) Uani 1 1 d . . . N5 N 0.9471(3) 0.8722(5) 0.2850(2) 0.0444(15) Uani 1 1 d . . . C18A C 1.0386(7) 0.868(2) 0.5938(6) 0.056(6) Uani 0.51(3) 1 d P A 1 H18A H 1.0450 0.8640 0.6278 0.084 Uiso 0.51(3) 1 calc PR A 1 H18B H 1.0223 0.7954 0.5827 0.084 Uiso 0.51(3) 1 calc PR A 1 H18C H 1.0133 0.9326 0.5867 0.084 Uiso 0.51(3) 1 calc PR A 1 C19A C 1.1363(10) 0.791(2) 0.5811(8) 0.070(8) Uani 0.51(3) 1 d P A 1 H19A H 1.1614 0.8163 0.6063 0.105 Uiso 0.51(3) 1 calc PR A 1 H19B H 1.1579 0.7679 0.5537 0.105 Uiso 0.51(3) 1 calc PR A 1 H19C H 1.1146 0.7244 0.5918 0.105 Uiso 0.51(3) 1 calc PR A 1 C20A C 1.1217(11) 1.0086(18) 0.5843(6) 0.064(7) Uani 0.51(3) 1 d P A 1 H20A H 1.0983 1.0719 0.5725 0.096 Uiso 0.51(3) 1 calc PR A 1 H20B H 1.1593 1.0177 0.5723 0.096 Uiso 0.51(3) 1 calc PR A 1 H20C H 1.1228 1.0107 0.6187 0.096 Uiso 0.51(3) 1 calc PR A 1 C18B C 1.0542(15) 0.973(3) 0.5854(8) 0.114(17) Uani 0.49(3) 1 d P A 2 H18D H 1.0195 0.9611 0.5679 0.171 Uiso 0.49(3) 1 calc PR A 2 H18E H 1.0669 1.0529 0.5811 0.171 Uiso 0.49(3) 1 calc PR A 2 H18F H 1.0481 0.9583 0.6188 0.171 Uiso 0.49(3) 1 calc PR A 2 C19B C 1.089(3) 0.772(3) 0.5926(9) 0.22(4) Uani 0.49(3) 1 d P A 2 H19D H 1.0983 0.7802 0.6259 0.336 Uiso 0.49(3) 1 calc PR A 2 H19E H 1.1119 0.7131 0.5783 0.336 Uiso 0.49(3) 1 calc PR A 2 H19F H 1.0496 0.7495 0.5895 0.336 Uiso 0.49(3) 1 calc PR A 2 C20B C 1.1582(14) 0.925(5) 0.5754(9) 0.17(3) Uani 0.49(3) 1 d P A 2 H20D H 1.1615 1.0095 0.5746 0.249 Uiso 0.49(3) 1 calc PR A 2 H20E H 1.1808 0.8910 0.5506 0.249 Uiso 0.49(3) 1 calc PR A 2 H20F H 1.1710 0.8960 0.6060 0.249 Uiso 0.49(3) 1 calc PR A 2 O1 O 0.9173(4) 0.5224(6) 0.4953(3) 0.102(3) Uani 1 1 d . . . O2 O 0.9561(3) 0.6421(9) 0.5542(3) 0.109(3) Uani 1 1 d . . . O3 O 0.9069(5) 0.7231(7) 0.4909(3) 0.116(3) Uani 1 1 d . . . O4 O 0.8610(3) 0.6238(10) 0.5489(3) 0.124(4) Uani 1 1 d . . . O5 O 1.2187(5) 0.8166(11) 0.2834(4) 0.167(5) Uani 1 1 d . . . O6 O 1.2893(7) 0.8309(13) 0.3389(5) 0.233(9) Uani 1 1 d . . . O7 O 1.2238(7) 0.9684(14) 0.3348(4) 0.226(9) Uani 1 1 d . . . O8 O 1.2810(8) 0.9468(18) 0.2807(7) 0.278(10) Uani 1 1 d . . . N6 N 0.9265(5) 0.4937(9) 0.1800(3) 0.081(3) Uani 1 1 d . . . C22 C 0.8890(6) 0.5328(10) 0.1640(5) 0.081(4) Uani 1 1 d . . . C23 C 0.8407(7) 0.5875(14) 0.1406(7) 0.145(7) Uani 1 1 d . . . H23A H 0.8378 0.6688 0.1515 0.173 Uiso 1 1 calc R . . H23B H 0.8471 0.5893 0.1064 0.173 Uiso 1 1 calc R . . C24 C 0.7898(8) 0.5306(15) 0.1488(7) 0.152(7) Uani 1 1 d . . . H24A H 0.7941 0.4472 0.1433 0.227 Uiso 1 1 calc R . . H24B H 0.7613 0.5617 0.1275 0.227 Uiso 1 1 calc R . . H24C H 0.7787 0.5436 0.1814 0.227 Uiso 1 1 calc R . . N7 N 1.2340(12) 0.514(2) 0.5368(10) 0.136(9) Uiso 0.50 1 d P . . C25 C 1.2446(14) 0.405(3) 0.5586(12) 0.128(10) Uiso 0.50 1 d P . . C26 C 1.2467(12) 0.298(2) 0.5715(9) 0.103(8) Uiso 0.50 1 d P . . H26A H 1.2099 0.2728 0.5809 0.154 Uiso 0.50 1 calc PR . . H26B H 1.2725 0.2906 0.5981 0.154 Uiso 0.50 1 calc PR . . H26C H 1.2595 0.2504 0.5454 0.154 Uiso 0.50 1 calc PR . . 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 0.0390(3) 0.0325(3) 0.0237(2) 0.0010(2) -0.0003(2) -0.0059(2) Pd2 0.0435(3) 0.0317(3) 0.0235(2) 0.0020(2) -0.0025(2) -0.0062(2) S 0.0463(11) 0.0296(8) 0.0259(8) 0.0013(6) -0.0034(7) -0.0074(8) Cl1 0.0628(15) 0.0675(14) 0.0512(12) -0.0029(10) 0.0040(11) 0.0100(11) Cl2 0.0553(15) 0.0604(14) 0.105(2) -0.0121(14) -0.0102(14) 0.0067(12) N1 0.043(4) 0.032(3) 0.030(3) 0.003(2) 0.002(3) -0.008(3) N2 0.048(4) 0.048(4) 0.030(3) 0.007(3) 0.006(3) -0.008(3) N3 0.052(4) 0.028(3) 0.029(3) 0.006(2) -0.004(3) -0.006(3) N4 0.049(4) 0.051(4) 0.035(3) 0.005(3) -0.008(3) -0.012(3) C1 0.040(4) 0.032(3) 0.026(3) 0.001(3) -0.002(3) -0.001(3) C2 0.050(5) 0.035(4) 0.025(3) 0.004(3) -0.008(3) -0.001(3) C3 0.043(4) 0.043(4) 0.029(3) 0.005(3) -0.004(3) 0.003(3) C4 0.041(4) 0.046(4) 0.030(3) -0.001(3) -0.004(3) 0.003(3) C5 0.040(4) 0.042(4) 0.033(4) -0.002(3) -0.007(3) -0.007(3) C6 0.046(4) 0.033(4) 0.028(3) 0.001(3) -0.003(3) -0.005(3) C7 0.042(4) 0.039(4) 0.034(4) -0.001(3) -0.010(3) -0.006(3) C8 0.073(6) 0.039(4) 0.037(4) 0.005(3) -0.003(4) -0.018(4) C9 0.056(5) 0.049(5) 0.040(4) 0.000(3) 0.001(4) -0.016(4) C10 0.071(6) 0.050(5) 0.053(5) 0.015(4) -0.007(4) -0.007(4) C11 0.065(6) 0.063(5) 0.045(4) 0.000(4) 0.020(4) -0.021(5) C12 0.054(5) 0.027(3) 0.032(4) 0.007(3) -0.002(3) -0.002(3) C13 0.072(6) 0.033(4) 0.037(4) 0.004(3) -0.007(4) -0.011(4) C14 0.067(6) 0.054(5) 0.035(4) 0.007(3) -0.001(4) -0.035(4) C15 0.053(6) 0.080(7) 0.097(8) 0.020(6) -0.013(6) -0.011(5) C16 0.084(7) 0.057(5) 0.040(4) -0.006(4) -0.004(4) -0.033(5) C17 0.041(4) 0.061(5) 0.027(3) 0.001(3) -0.008(3) 0.000(4) C21 0.035(4) 0.027(3) 0.016(3) -0.003(2) -0.001(2) -0.003(3) N5 0.051(4) 0.044(4) 0.039(3) -0.003(3) 0.000(3) -0.004(3) C18A 0.053(11) 0.084(17) 0.032(8) 0.004(9) 0.017(7) -0.002(10) C19A 0.075(16) 0.073(16) 0.060(13) 0.017(11) -0.017(11) 0.018(12) C20A 0.078(18) 0.084(15) 0.030(8) -0.008(8) -0.009(9) -0.014(12) C18B 0.16(3) 0.15(3) 0.038(11) -0.016(15) 0.002(14) 0.09(3) C19B 0.50(11) 0.14(3) 0.032(14) 0.045(17) -0.08(3) -0.14(5) C20B 0.10(2) 0.36(8) 0.039(13) 0.03(2) -0.040(14) -0.12(4) O1 0.168(9) 0.066(5) 0.072(5) -0.011(4) 0.018(5) 0.030(5) O2 0.082(6) 0.151(8) 0.094(6) 0.000(6) -0.021(5) -0.011(5) O3 0.201(11) 0.068(5) 0.080(5) 0.013(4) 0.010(6) 0.036(6) O4 0.073(6) 0.207(10) 0.091(6) -0.055(6) 0.032(5) -0.022(6) O5 0.172(11) 0.136(9) 0.190(11) -0.001(8) -0.093(9) -0.039(8) O6 0.305(18) 0.215(14) 0.173(11) -0.107(11) -0.147(12) 0.176(14) O7 0.251(16) 0.300(17) 0.128(9) -0.063(11) -0.008(10) 0.207(15) O8 0.229(19) 0.29(2) 0.31(2) 0.028(19) 0.060(17) -0.144(17) N6 0.089(8) 0.082(7) 0.073(6) 0.003(5) 0.021(6) -0.016(6) C22 0.088(10) 0.056(7) 0.101(9) -0.029(6) 0.019(8) -0.001(6) C23 0.111(13) 0.095(11) 0.23(2) -0.046(12) 0.035(14) 0.001(10) C24 0.139(16) 0.117(13) 0.20(2) 0.007(13) 0.026(14) 0.036(12) _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 C21 1.973(6) . ? Pd1 N1 1.985(5) . ? Pd1 N2 2.097(6) . ? Pd1 S 2.2683(17) . ? Pd2 N5 1.994(6) . ? Pd2 N3 1.998(5) . ? Pd2 N4 2.099(6) . ? Pd2 S 2.2898(19) . ? S C1 1.763(6) . ? Cl1 O4 1.392(7) . ? Cl1 O3 1.399(7) . ? Cl1 O2 1.407(8) . ? Cl1 O1 1.409(7) . ? Cl2 O7 1.288(10) . ? Cl2 O6 1.326(10) . ? Cl2 O5 1.345(10) . ? Cl2 O8 1.354(16) . ? N1 C7 1.262(8) . ? N1 C8 1.479(9) . ? N2 C9 1.465(9) . ? N2 C10 1.480(10) . ? N2 C11 1.496(9) . ? N3 C12 1.259(8) . ? N3 C13 1.454(9) . ? N4 C15 1.432(11) . ? N4 C16 1.495(9) . ? N4 C14 1.495(9) . ? C1 C2 1.400(9) . ? C1 C6 1.406(9) . ? C2 C3 1.396(9) . ? C2 C12 1.471(10) . ? C3 C4 1.379(10) . ? C4 C5 1.370(10) . ? C4 C17 1.528(9) . ? C5 C6 1.411(9) . ? C6 C7 1.459(9) . ? C8 C9 1.490(11) . ? C13 C14 1.511(12) . ? C17 C18B 1.48(2) . ? C17 C19A 1.50(2) . ? C17 C20B 1.50(3) . ? C17 C19B 1.52(3) . ? C17 C20A 1.53(2) . ? C17 C18A 1.602(17) . ? C21 N5 1.131(8) 2_755 ? N5 C21 1.131(8) 2_755 ? N6 C22 1.084(15) . ? C22 C23 1.45(2) . ? C23 C24 1.39(2) . ? N7 C25 1.40(4) . ? C25 C26 1.25(4) . ? 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 C21 Pd1 N1 176.4(2) . . ? C21 Pd1 N2 92.0(2) . . ? N1 Pd1 N2 84.8(2) . . ? C21 Pd1 S 88.81(18) . . ? N1 Pd1 S 94.61(16) . . ? N2 Pd1 S 173.77(19) . . ? N5 Pd2 N3 175.4(2) . . ? N5 Pd2 N4 90.9(2) . . ? N3 Pd2 N4 84.6(2) . . ? N5 Pd2 S 96.58(19) . . ? N3 Pd2 S 87.90(18) . . ? N4 Pd2 S 169.55(19) . . ? C1 S Pd1 112.8(2) . . ? C1 S Pd2 105.3(2) . . ? Pd1 S Pd2 121.68(8) . . ? O4 Cl1 O3 108.1(6) . . ? O4 Cl1 O2 108.1(5) . . ? O3 Cl1 O2 109.7(6) . . ? O4 Cl1 O1 111.8(6) . . ? O3 Cl1 O1 108.8(5) . . ? O2 Cl1 O1 110.2(6) . . ? O7 Cl2 O6 114.4(8) . . ? O7 Cl2 O5 116.4(10) . . ? O6 Cl2 O5 116.5(8) . . ? O7 Cl2 O8 102.2(12) . . ? O6 Cl2 O8 102.7(12) . . ? O5 Cl2 O8 101.2(10) . . ? C7 N1 C8 118.0(6) . . ? C7 N1 Pd1 131.6(5) . . ? C8 N1 Pd1 110.3(4) . . ? C9 N2 C10 110.7(6) . . ? C9 N2 C11 110.9(6) . . ? C10 N2 C11 107.3(6) . . ? C9 N2 Pd1 105.0(4) . . ? C10 N2 Pd1 110.9(5) . . ? C11 N2 Pd1 112.1(5) . . ? C12 N3 C13 121.0(6) . . ? C12 N3 Pd2 129.9(5) . . ? C13 N3 Pd2 108.9(4) . . ? C15 N4 C16 109.5(7) . . ? C15 N4 C14 109.8(7) . . ? C16 N4 C14 110.0(6) . . ? C15 N4 Pd2 115.1(5) . . ? C16 N4 Pd2 106.8(5) . . ? C14 N4 Pd2 105.6(4) . . ? C2 C1 C6 118.1(6) . . ? C2 C1 S 118.6(5) . . ? C6 C1 S 123.0(5) . . ? C3 C2 C1 120.3(6) . . ? C3 C2 C12 113.6(6) . . ? C1 C2 C12 126.1(6) . . ? C4 C3 C2 123.0(7) . . ? C5 C4 C3 115.8(6) . . ? C5 C4 C17 122.5(7) . . ? C3 C4 C17 121.7(7) . . ? C4 C5 C6 124.3(7) . . ? C1 C6 C5 118.4(6) . . ? C1 C6 C7 128.0(6) . . ? C5 C6 C7 113.6(6) . . ? N1 C7 C6 129.5(6) . . ? N1 C8 C9 108.1(6) . . ? N2 C9 C8 111.0(6) . . ? N3 C12 C2 126.9(6) . . ? N3 C13 C14 107.3(6) . . ? N4 C14 C13 109.6(6) . . ? C18B C17 C19A 144.6(14) . . ? C18B C17 C20B 117(2) . . ? C19A C17 C20B 65(2) . . ? C18B C17 C19B 107(3) . . ? C19A C17 C19B 47(3) . . ? C20B C17 C19B 107(3) . . ? C18B C17 C20A 66.6(17) . . ? C19A C17 C20A 110.6(13) . . ? C20B C17 C20A 51(2) . . ? C19B C17 C20A 132.8(14) . . ? C18B C17 C4 105.1(10) . . ? C19A C17 C4 107.7(11) . . ? C20B C17 C4 107.6(11) . . ? C19B C17 C4 112.9(12) . . ? C20A C17 C4 113.8(9) . . ? C18B C17 C18A 48.1(15) . . ? C19A C17 C18A 107.8(13) . . ? C20B C17 C18A 144.0(13) . . ? C19B C17 C18A 62(3) . . ? C20A C17 C18A 108.7(12) . . ? C4 C17 C18A 108.2(8) . . ? N5 C21 Pd1 177.8(6) 2_755 . ? C21 N5 Pd2 173.7(6) 2_755 . ? N6 C22 C23 176.9(16) . . ? C24 C23 C22 114.2(16) . . ? C26 C25 N7 168(4) . . ? #===END # Attachment 'CCDC_286859_n.CIF' data_9 _database_code_depnum_ccdc_archive 'CCDC 286859' _chemical_formula_structural ; [(L3)Pd2(OAc)](ClO4)2 ; _chemical_formula_sum 'C22 H36 Cl2 N4 O10 Pd2 S' _chemical_formula_weight 832.31 _chemical_melting_point ? _chemical_compound_source ; Crystals were grown by recrystallization from a mixed acetone/methanol solvent system ; #CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/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 11.410(3) _cell_length_b 12.245(2) _cell_length_c 22.395(4) _cell_angle_alpha 90.00 _cell_angle_beta 102.20(3) _cell_angle_gamma 90.00 _cell_volume 3058.2(11) _cell_formula_units_Z 4 _cell_measurement_temperature 210(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour pale-yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.808 _exptl_crystal_F_000 1672 _exptl_absorpt_coefficient_mu 1.476 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.82 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ? _diffrn_radiation_type MoK\a _diffrn_ambient_temperature 210(2) _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'BRUKER AXS' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_method hemisphere _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26837 _diffrn_reflns_av_R_equivalents 0.1677 _diffrn_reflns_av_sigmaI/netI 0.1194 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 28.77 #REFINEMENT DATA _reflns_number_total 7412 _reflns_number_gt 4259 _reflns_threshold_expression >2sigma(I) _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^)+(0.0491P)^2^+1.8932P] 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 7412 _refine_ls_number_parameters 370 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1105 _refine_ls_R_factor_gt 0.0563 _refine_ls_wR_factor_ref 0.1464 _refine_ls_wR_factor_gt 0.1187 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.931 _diffrn_reflns_theta_full 28.77 _diffrn_measured_fraction_theta_full 0.931 _refine_diff_density_max 1.288 _refine_diff_density_min -1.158 _refine_diff_density_rms 0.163 _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 (FARRUGIA)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; #ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' 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 1.12458(4) 0.76735(4) 0.90397(2) 0.03494(15) Uani 1 1 d . . . Pd2 Pd 0.86818(4) 0.83557(4) 0.97322(2) 0.03587(15) Uani 1 1 d . . . S S 1.01329(14) 0.90355(12) 0.92947(6) 0.0331(3) Uani 1 1 d . . . O1 O 1.1460(5) 0.7076(5) 0.9902(2) 0.0687(15) Uani 1 1 d . . . O2 O 0.9507(5) 0.6918(5) 0.9991(3) 0.0697(16) Uani 1 1 d . . . N1 N 1.1146(5) 0.8200(4) 0.8195(2) 0.0342(11) Uani 1 1 d . . . N2 N 1.2341(5) 0.6442(4) 0.8803(2) 0.0422(13) Uani 1 1 d . . . N3 N 0.7729(5) 0.9725(4) 0.9553(2) 0.0382(12) Uani 1 1 d . . . N4 N 0.7343(5) 0.7882(5) 1.0190(2) 0.0450(14) Uani 1 1 d . . . C1 C 0.9446(5) 0.9808(4) 0.8661(2) 0.0303(13) Uani 1 1 d . . . C2 C 0.8473(6) 1.0510(5) 0.8697(3) 0.0346(14) Uani 1 1 d . . . C3 C 0.8062(6) 1.1272(5) 0.8241(3) 0.0420(16) Uani 1 1 d . . . H3 H 0.7452 1.1747 0.8289 0.050 Uiso 1 1 calc R . . C4 C 0.8528(6) 1.1356(5) 0.7714(3) 0.0402(15) Uani 1 1 d . . . C5 C 0.9433(6) 1.0623(5) 0.7678(3) 0.0385(15) Uani 1 1 d . . . H5 H 0.9765 1.0654 0.7333 0.046 Uiso 1 1 calc R . . C6 C 0.9881(6) 0.9852(5) 0.8115(3) 0.0355(14) Uani 1 1 d . . . C7 C 1.0692(5) 0.9061(5) 0.7934(3) 0.0348(14) Uani 1 1 d . . . H7 H 1.0913 0.9216 0.7566 0.042 Uiso 1 1 calc R . . C8 C 1.1755(8) 0.7435(6) 0.7841(3) 0.057(2) Uani 1 1 d . . . H8A H 1.1173 0.6925 0.7618 0.068 Uiso 1 1 calc R . . H8B H 1.2095 0.7843 0.7548 0.068 Uiso 1 1 calc R . . C9 C 1.2684(9) 0.6847(7) 0.8242(4) 0.079(3) Uani 1 1 d . . . H9A H 1.3378 0.7319 0.8358 0.094 Uiso 1 1 calc R . . H9B H 1.2919 0.6230 0.8022 0.094 Uiso 1 1 calc R . . C10 C 1.1675(9) 0.5401(7) 0.8687(5) 0.088(3) Uani 1 1 d . . . H10A H 1.2190 0.4848 0.8579 0.132 Uiso 1 1 calc R . . H10B H 1.0993 0.5497 0.8357 0.132 Uiso 1 1 calc R . . H10C H 1.1410 0.5183 0.9048 0.132 Uiso 1 1 calc R . . C11 C 1.3493(8) 0.6296(9) 0.9256(4) 0.091(3) Uani 1 1 d . . . H11A H 1.3949 0.5720 0.9122 0.136 Uiso 1 1 calc R . . H11B H 1.3328 0.6111 0.9646 0.136 Uiso 1 1 calc R . . H11C H 1.3945 0.6963 0.9290 0.136 Uiso 1 1 calc R . . C12 C 0.7758(6) 1.0476(5) 0.9167(3) 0.0386(15) Uani 1 1 d . . . H12 H 0.7268 1.1077 0.9186 0.046 Uiso 1 1 calc R . . C13 C 0.6876(7) 0.9824(6) 0.9968(3) 0.0519(19) Uani 1 1 d . . . H13A H 0.6241 1.0335 0.9802 0.062 Uiso 1 1 calc R . . H13B H 0.7288 1.0083 1.0367 0.062 Uiso 1 1 calc R . . C14 C 0.6371(6) 0.8707(6) 1.0018(3) 0.0518(18) Uani 1 1 d . . . H14A H 0.5881 0.8715 1.0323 0.062 Uiso 1 1 calc R . . H14B H 0.5862 0.8506 0.9629 0.062 Uiso 1 1 calc R . . C15 C 0.6869(8) 0.6777(6) 1.0020(4) 0.062(2) Uani 1 1 d . . . H15A H 0.6263 0.6604 1.0244 0.093 Uiso 1 1 calc R . . H15B H 0.7509 0.6255 1.0116 0.093 Uiso 1 1 calc R . . H15C H 0.6528 0.6755 0.9590 0.093 Uiso 1 1 calc R . . C16 C 0.7873(8) 0.7903(7) 1.0859(3) 0.064(2) Uani 1 1 d . . . H16A H 0.7276 0.7689 1.1081 0.095 Uiso 1 1 calc R . . H16B H 0.8145 0.8629 1.0978 0.095 Uiso 1 1 calc R . . H16C H 0.8538 0.7406 1.0949 0.095 Uiso 1 1 calc R . . C17 C 0.8025(7) 1.2187(6) 0.7224(3) 0.055(2) Uani 1 1 d . . . C18 C 0.8143(9) 1.3320(6) 0.7485(4) 0.077(3) Uani 1 1 d . . . H18A H 0.7738 1.3360 0.7819 0.116 Uiso 1 1 calc R . . H18B H 0.7789 1.3833 0.7175 0.116 Uiso 1 1 calc R . . H18C H 0.8976 1.3491 0.7628 0.116 Uiso 1 1 calc R . . C19 C 0.8684(10) 1.2153(7) 0.6697(4) 0.087(3) Uani 1 1 d . . . H19A H 0.8613 1.1437 0.6518 0.130 Uiso 1 1 calc R . . H19B H 0.9515 1.2322 0.6848 0.130 Uiso 1 1 calc R . . H19C H 0.8338 1.2680 0.6393 0.130 Uiso 1 1 calc R . . C20 C 0.6691(9) 1.1923(9) 0.6984(4) 0.096(3) Uani 1 1 d . . . H20A H 0.6279 1.1951 0.7316 0.144 Uiso 1 1 calc R . . H20B H 0.6614 1.1205 0.6808 0.144 Uiso 1 1 calc R . . H20C H 0.6347 1.2449 0.6679 0.144 Uiso 1 1 calc R . . C21 C 1.0635(7) 0.6747(6) 1.0176(3) 0.0462(17) Uani 1 1 d . . . C22 C 1.0974(8) 0.6088(9) 1.0743(4) 0.090(3) Uani 1 1 d . . . H22A H 1.0265 0.5900 1.0888 0.134 Uiso 1 1 calc R . . H22B H 1.1504 0.6504 1.1050 0.134 Uiso 1 1 calc R . . H22C H 1.1370 0.5432 1.0659 0.134 Uiso 1 1 calc R . . Cl1 Cl 1.4092(2) 0.99021(18) 0.82924(10) 0.0708(6) Uani 1 1 d . . . Cl2 Cl 1.44735(17) 0.63874(15) 1.11366(8) 0.0521(5) Uani 1 1 d . . . O3 O 1.5082(8) 1.0523(10) 0.8315(6) 0.190(5) Uani 1 1 d . . . O4 O 1.3915(8) 0.9180(7) 0.7794(3) 0.127(3) Uani 1 1 d . . . O5 O 1.4111(9) 0.9294(7) 0.8825(3) 0.132(3) Uani 1 1 d . . . O6 O 1.3071(8) 1.0562(7) 0.8195(4) 0.129(3) Uani 1 1 d . . . O7 O 1.4023(7) 0.5429(6) 1.0833(4) 0.110(2) Uani 1 1 d . . . O8 O 1.3906(6) 0.6617(6) 1.1624(3) 0.099(2) Uani 1 1 d . . . O9 O 1.5723(5) 0.6272(6) 1.1364(3) 0.0841(19) Uani 1 1 d . . . O10 O 1.4223(7) 0.7275(5) 1.0716(3) 0.088(2) Uani 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 0.0305(3) 0.0403(3) 0.0350(2) 0.0038(2) 0.0091(2) 0.0060(2) Pd2 0.0314(3) 0.0442(3) 0.0335(2) 0.0029(2) 0.0102(2) 0.0021(2) S 0.0299(9) 0.0399(8) 0.0303(7) -0.0001(6) 0.0080(6) 0.0029(7) O1 0.070(4) 0.080(4) 0.057(3) 0.012(3) 0.017(3) 0.011(3) O2 0.054(4) 0.068(3) 0.092(4) 0.032(3) 0.027(3) 0.008(3) N1 0.032(3) 0.038(3) 0.035(2) -0.001(2) 0.012(2) 0.012(2) N2 0.043(4) 0.034(3) 0.051(3) 0.005(2) 0.014(3) 0.011(3) N3 0.026(3) 0.051(3) 0.041(3) -0.002(2) 0.012(2) 0.002(3) N4 0.040(3) 0.064(4) 0.036(3) 0.000(3) 0.018(3) -0.005(3) C1 0.029(3) 0.028(3) 0.035(3) -0.002(2) 0.010(3) 0.001(3) C2 0.031(3) 0.038(3) 0.037(3) -0.005(3) 0.011(3) -0.002(3) C3 0.040(4) 0.039(3) 0.049(4) -0.004(3) 0.014(3) 0.005(3) C4 0.038(4) 0.040(3) 0.043(3) 0.007(3) 0.010(3) 0.009(3) C5 0.036(4) 0.043(3) 0.038(3) 0.007(3) 0.011(3) 0.007(3) C6 0.031(4) 0.037(3) 0.041(3) -0.001(3) 0.012(3) 0.003(3) C7 0.027(3) 0.045(4) 0.035(3) 0.003(3) 0.013(3) 0.004(3) C8 0.078(6) 0.053(4) 0.048(4) 0.005(3) 0.033(4) 0.029(4) C9 0.098(8) 0.081(6) 0.064(5) 0.014(4) 0.033(5) 0.047(6) C10 0.099(8) 0.051(5) 0.127(8) -0.022(5) 0.054(7) -0.009(5) C11 0.057(6) 0.134(9) 0.075(6) -0.014(6) 0.000(5) 0.044(6) C12 0.032(4) 0.040(3) 0.045(3) -0.002(3) 0.011(3) 0.009(3) C13 0.056(5) 0.055(4) 0.055(4) 0.000(3) 0.035(4) 0.001(4) C14 0.037(4) 0.071(5) 0.054(4) -0.004(4) 0.023(3) -0.002(4) C15 0.069(6) 0.049(4) 0.073(5) 0.000(4) 0.027(5) -0.011(4) C16 0.068(6) 0.083(6) 0.042(4) 0.007(4) 0.017(4) -0.003(5) C17 0.055(5) 0.058(5) 0.054(4) 0.019(3) 0.019(4) 0.020(4) C18 0.108(8) 0.061(5) 0.071(5) 0.020(4) 0.037(6) 0.028(5) C19 0.138(10) 0.080(6) 0.057(5) 0.032(4) 0.054(6) 0.049(6) C20 0.066(7) 0.124(8) 0.088(7) 0.041(6) -0.009(5) 0.015(7) C21 0.035(4) 0.056(4) 0.049(4) 0.009(3) 0.013(3) 0.005(4) C22 0.054(6) 0.150(9) 0.064(5) 0.040(6) 0.011(5) 0.009(6) Cl1 0.0804(17) 0.0614(12) 0.0707(13) 0.0016(10) 0.0161(12) 0.0079(13) Cl2 0.0463(11) 0.0624(11) 0.0516(10) 0.0023(8) 0.0194(9) 0.0096(9) O3 0.092(7) 0.203(11) 0.265(13) -0.002(10) 0.015(8) -0.065(8) O4 0.174(8) 0.133(7) 0.083(5) -0.016(5) 0.047(5) -0.007(6) O5 0.190(9) 0.128(7) 0.066(4) 0.024(4) 0.003(5) 0.017(6) O6 0.115(7) 0.121(6) 0.155(7) 0.028(5) 0.039(6) 0.049(6) O7 0.098(6) 0.072(4) 0.154(7) -0.020(4) 0.012(5) 0.002(4) O8 0.078(5) 0.147(6) 0.088(5) 0.015(4) 0.052(4) 0.034(5) O9 0.047(4) 0.131(5) 0.075(4) 0.000(4) 0.014(3) 0.023(4) O10 0.113(6) 0.080(4) 0.069(4) 0.023(3) 0.013(4) 0.012(4) _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 1.979(5) . ? Pd1 O1 2.031(5) . ? Pd1 N2 2.097(5) . ? Pd1 S 2.2421(15) . ? Pd2 N3 1.993(5) . ? Pd2 O2 2.022(5) . ? Pd2 N4 2.093(5) . ? Pd2 S 2.2538(16) . ? S C1 1.747(6) . ? O1 C21 1.292(8) . ? O2 C21 1.283(8) . ? N1 C7 1.262(7) . ? N1 C8 1.490(7) . ? N2 C9 1.478(9) . ? N2 C10 1.478(10) . ? N2 C11 1.491(10) . ? N3 C12 1.267(7) . ? N3 C13 1.486(7) . ? N4 C15 1.477(9) . ? N4 C14 1.491(9) . ? N4 C16 1.494(8) . ? C1 C6 1.415(7) . ? C1 C2 1.420(8) . ? C2 C3 1.390(9) . ? C2 C12 1.462(8) . ? C3 C4 1.399(8) . ? C4 C5 1.382(8) . ? C4 C17 1.517(9) . ? C5 C6 1.379(8) . ? C6 C7 1.455(8) . ? C8 C9 1.431(11) . ? C13 C14 1.497(10) . ? C17 C18 1.501(11) . ? C17 C19 1.528(9) . ? C17 C20 1.537(13) . ? C21 C22 1.487(10) . ? Cl1 O3 1.354(9) . ? Cl1 O6 1.396(8) . ? Cl1 O5 1.402(7) . ? Cl1 O4 1.405(7) . ? Cl2 O7 1.399(7) . ? Cl2 O8 1.410(5) . ? Cl2 O9 1.416(6) . ? Cl2 O10 1.427(6) . ? 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 O1 175.8(2) . . ? N1 Pd1 N2 84.83(19) . . ? O1 Pd1 N2 91.3(2) . . ? N1 Pd1 S 94.58(14) . . ? O1 Pd1 S 89.24(16) . . ? N2 Pd1 S 177.81(16) . . ? N3 Pd2 O2 172.47(19) . . ? N3 Pd2 N4 84.7(2) . . ? O2 Pd2 N4 87.8(2) . . ? N3 Pd2 S 91.21(15) . . ? O2 Pd2 S 96.06(15) . . ? N4 Pd2 S 173.87(16) . . ? C1 S Pd1 112.15(18) . . ? C1 S Pd2 108.0(2) . . ? Pd1 S Pd2 110.10(7) . . ? C21 O1 Pd1 127.6(5) . . ? C21 O2 Pd2 127.5(5) . . ? C7 N1 C8 118.1(5) . . ? C7 N1 Pd1 130.5(4) . . ? C8 N1 Pd1 111.3(4) . . ? C9 N2 C10 111.0(7) . . ? C9 N2 C11 105.3(7) . . ? C10 N2 C11 111.3(7) . . ? C9 N2 Pd1 104.6(4) . . ? C10 N2 Pd1 110.6(5) . . ? C11 N2 Pd1 113.6(5) . . ? C12 N3 C13 118.8(5) . . ? C12 N3 Pd2 131.0(4) . . ? C13 N3 Pd2 110.1(4) . . ? C15 N4 C14 110.0(6) . . ? C15 N4 C16 108.9(6) . . ? C14 N4 C16 111.7(5) . . ? C15 N4 Pd2 113.1(4) . . ? C14 N4 Pd2 105.4(4) . . ? C16 N4 Pd2 107.7(4) . . ? C6 C1 C2 116.6(5) . . ? C6 C1 S 122.9(4) . . ? C2 C1 S 120.3(4) . . ? C3 C2 C1 120.7(5) . . ? C3 C2 C12 113.3(5) . . ? C1 C2 C12 125.8(5) . . ? C2 C3 C4 122.7(6) . . ? C5 C4 C3 115.1(6) . . ? C5 C4 C17 124.5(6) . . ? C3 C4 C17 120.4(6) . . ? C6 C5 C4 124.9(5) . . ? C5 C6 C1 119.7(5) . . ? C5 C6 C7 114.9(5) . . ? C1 C6 C7 125.1(5) . . ? N1 C7 C6 130.6(5) . . ? C9 C8 N1 110.5(6) . . ? C8 C9 N2 114.1(7) . . ? N3 C12 C2 127.6(6) . . ? N3 C13 C14 106.6(5) . . ? N4 C14 C13 111.2(6) . . ? C18 C17 C4 110.4(6) . . ? C18 C17 C19 107.9(7) . . ? C4 C17 C19 111.6(6) . . ? C18 C17 C20 109.3(8) . . ? C4 C17 C20 107.9(6) . . ? C19 C17 C20 109.7(8) . . ? O2 C21 O1 125.3(6) . . ? O2 C21 C22 115.3(6) . . ? O1 C21 C22 119.4(7) . . ? O3 Cl1 O6 110.1(7) . . ? O3 Cl1 O5 113.8(7) . . ? O6 Cl1 O5 107.6(5) . . ? O3 Cl1 O4 111.2(6) . . ? O6 Cl1 O4 105.4(6) . . ? O5 Cl1 O4 108.3(5) . . ? O7 Cl2 O8 111.2(5) . . ? O7 Cl2 O9 109.2(4) . . ? O8 Cl2 O9 109.5(4) . . ? O7 Cl2 O10 108.5(4) . . ? O8 Cl2 O10 107.4(4) . . ? O9 Cl2 O10 111.1(4) . . ? #===END # Attachment 'CCDC_286860_n.CIF' data_10 _database_code_depnum_ccdc_archive 'CCDC 286860' _chemical_formula_structural ; [(L3)Pd2(uCH2ClCONH)](ClO4)2 ; _chemical_formula_sum 'C22 H36 Cl3 N5 O9 Pd2 S' _chemical_formula_weight 865.77 _chemical_melting_point ? _chemical_compound_source ; Crystals were grown by slow evaporation of a mixed chloroacetonitrile/methanol solvent system ; #CRYSTAL DATA _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 11.351(2) _cell_length_b 11.518(2) _cell_length_c 12.189(2) _cell_angle_alpha 85.70(3) _cell_angle_beta 84.74(3) _cell_angle_gamma 83.01(3) _cell_volume 1571.8(5) _cell_formula_units_Z 2 _cell_measurement_temperature 210(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.829 _exptl_crystal_F_000 868 _exptl_absorpt_coefficient_mu 1.521 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.85 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ? _diffrn_radiation_type MoK\a _diffrn_ambient_temperature 210(2) _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'BRUKER AXS' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_method hemisphere _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13926 _diffrn_reflns_av_R_equivalents 0.0187 _diffrn_reflns_av_sigmaI/netI 0.0353 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 28.78 #REFINEMENT DATA _reflns_number_total 7300 _reflns_number_gt 5548 _reflns_threshold_expression >2sigma(I) _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^)+(0.0824P)^2^+2.2797P] 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 7300 _refine_ls_number_parameters 442 _refine_ls_number_restraints 114 _refine_ls_R_factor_all 0.0623 _refine_ls_R_factor_gt 0.0440 _refine_ls_wR_factor_ref 0.1396 _refine_ls_wR_factor_gt 0.1262 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.890 _diffrn_reflns_theta_full 28.78 _diffrn_measured_fraction_theta_full 0.890 _refine_diff_density_max 1.029 _refine_diff_density_min -2.115 _refine_diff_density_rms 0.138 _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 (FARRUGIA)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; #ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' 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 1.04855(3) 0.67072(3) 0.60524(3) 0.02926(12) Uani 1 1 d . . . Pd2 Pd 0.87249(3) 0.88918(3) 0.43073(3) 0.02818(11) Uani 1 1 d . . . S S 1.05772(11) 0.82664(10) 0.48295(9) 0.0275(2) Uani 1 1 d . . . N1 N 1.1836(4) 0.5724(4) 0.5288(3) 0.0344(9) Uani 1 1 d . . . N2 N 1.0476(5) 0.5265(4) 0.7217(4) 0.0392(10) Uani 1 1 d . . . N3 N 0.9382(4) 0.9698(3) 0.2935(3) 0.0297(8) Uani 1 1 d . . . N4 N 0.7071(4) 0.9542(4) 0.3725(4) 0.0363(10) Uani 1 1 d . . . N5 N 0.9145(4) 0.7615(4) 0.6951(3) 0.0366(10) Uani 1 1 d . . . H1 H 0.9282 0.7699 0.7621 0.044 Uiso 1 1 calc R . . O1 O 0.7805(4) 0.8267(4) 0.5681(3) 0.0483(10) Uani 1 1 d . . . C21 C 0.8121(5) 0.8084(5) 0.6676(4) 0.0374(11) Uani 1 1 d . . . C22 C 0.7162(6) 0.8372(8) 0.7600(6) 0.070(2) Uani 1 1 d . . . H22A H 0.7564 0.8457 0.8253 0.084 Uiso 1 1 calc R . . H22B H 0.6734 0.7691 0.7753 0.084 Uiso 1 1 calc R . . Cl1 Cl 0.6200(4) 0.9474(4) 0.7475(3) 0.1519(15) Uani 1 1 d . . . C1 C 1.1481(4) 0.7897(4) 0.3621(4) 0.0280(9) Uani 1 1 d . . . C2 C 1.1378(4) 0.8614(4) 0.2640(4) 0.0313(10) Uani 1 1 d . . . C3 C 1.2224(5) 0.8448(5) 0.1743(4) 0.0400(12) Uani 1 1 d . . . H3 H 1.2141 0.8940 0.1107 0.048 Uiso 1 1 calc R . . C4 C 1.3186(5) 0.7574(5) 0.1761(5) 0.0418(13) Uani 1 1 d . A . C5 C 1.3264(5) 0.6837(5) 0.2706(4) 0.0384(12) Uani 1 1 d . . . H5 H 1.3889 0.6236 0.2734 0.046 Uiso 1 1 calc R . . C6 C 1.2422(5) 0.6969(4) 0.3634(4) 0.0330(11) Uani 1 1 d . . . C7 C 1.2560(5) 0.5989(5) 0.4452(4) 0.0375(12) Uani 1 1 d . . . H7 H 1.3262 0.5485 0.4362 0.045 Uiso 1 1 calc R . . C8 C 1.2137(6) 0.4568(5) 0.5895(5) 0.0483(15) Uani 1 1 d . . . H8A H 1.2758 0.4618 0.6380 0.058 Uiso 1 1 calc R . . H8B H 1.2419 0.3975 0.5379 0.058 Uiso 1 1 calc R . . C9 C 1.1023(6) 0.4257(5) 0.6556(5) 0.0472(14) Uani 1 1 d . . . H9A H 1.0459 0.4068 0.6064 0.057 Uiso 1 1 calc R . . H9B H 1.1213 0.3572 0.7049 0.057 Uiso 1 1 calc R . . C10 C 1.1215(7) 0.5437(6) 0.8137(5) 0.0543(16) Uani 1 1 d . . . H10A H 1.1210 0.4774 0.8663 0.081 Uiso 1 1 calc R . . H10B H 1.0890 0.6135 0.8493 0.081 Uiso 1 1 calc R . . H10C H 1.2018 0.5512 0.7843 0.081 Uiso 1 1 calc R . . C11 C 0.9277(6) 0.4992(6) 0.7709(6) 0.0551(16) Uani 1 1 d . . . H11A H 0.9369 0.4322 0.8225 0.083 Uiso 1 1 calc R . . H11B H 0.8810 0.4826 0.7134 0.083 Uiso 1 1 calc R . . H11C H 0.8881 0.5653 0.8084 0.083 Uiso 1 1 calc R . . C12 C 1.0399(5) 0.9523(4) 0.2402(4) 0.0323(10) Uani 1 1 d . . . H12 H 1.0536 1.0033 0.1788 0.039 Uiso 1 1 calc R . . C13 C 0.8461(5) 1.0610(5) 0.2510(4) 0.0371(11) Uani 1 1 d . . . H13A H 0.8688 1.0863 0.1751 0.045 Uiso 1 1 calc R . . H13B H 0.8365 1.1286 0.2953 0.045 Uiso 1 1 calc R . . C14 C 0.7320(5) 1.0052(5) 0.2584(4) 0.0394(12) Uani 1 1 d . . . H14A H 0.6667 1.0635 0.2393 0.047 Uiso 1 1 calc R . . H14B H 0.7391 0.9442 0.2066 0.047 Uiso 1 1 calc R . . C15 C 0.6282(5) 0.8602(6) 0.3731(6) 0.0505(15) Uani 1 1 d . . . H15A H 0.5535 0.8927 0.3463 0.076 Uiso 1 1 calc R . . H15B H 0.6147 0.8268 0.4471 0.076 Uiso 1 1 calc R . . H15C H 0.6655 0.8003 0.3265 0.076 Uiso 1 1 calc R . . C16 C 0.6480(5) 1.0462(6) 0.4449(5) 0.0468(14) Uani 1 1 d . . . H16A H 0.5722 1.0765 0.4189 0.070 Uiso 1 1 calc R . . H16B H 0.6971 1.1086 0.4433 0.070 Uiso 1 1 calc R . . H16C H 0.6363 1.0130 0.5191 0.070 Uiso 1 1 calc R . . C17 C 1.4063(6) 0.7356(6) 0.0736(5) 0.061(2) Uani 1 1 d D . . C18A C 1.3764(15) 0.6166(12) 0.0319(14) 0.085(5) Uiso 0.56(2) 1 d PD A 1 H18A H 1.2919 0.6197 0.0285 0.127 Uiso 0.56(2) 1 calc PR A 1 H18B H 1.4033 0.5527 0.0821 0.127 Uiso 0.56(2) 1 calc PR A 1 H18C H 1.4159 0.6053 -0.0402 0.127 Uiso 0.56(2) 1 calc PR A 1 C19A C 1.3875(13) 0.8308(11) -0.0192(11) 0.062(4) Uiso 0.56(2) 1 d PD A 1 H19A H 1.4504 0.8192 -0.0769 0.093 Uiso 0.56(2) 1 calc PR A 1 H19B H 1.3878 0.9063 0.0091 0.093 Uiso 0.56(2) 1 calc PR A 1 H19C H 1.3123 0.8267 -0.0482 0.093 Uiso 0.56(2) 1 calc PR A 1 C20A C 1.5346(11) 0.7193(16) 0.1064(13) 0.074(4) Uiso 0.56(2) 1 d PD A 1 H20A H 1.5418 0.6613 0.1670 0.111 Uiso 0.56(2) 1 calc PR A 1 H20B H 1.5548 0.7923 0.1281 0.111 Uiso 0.56(2) 1 calc PR A 1 H20C H 1.5877 0.6940 0.0446 0.111 Uiso 0.56(2) 1 calc PR A 1 C18B C 1.341(2) 0.678(2) -0.006(2) 0.113(9) Uiso 0.44(2) 1 d PD A 2 H18D H 1.2792 0.7337 -0.0347 0.170 Uiso 0.44(2) 1 calc PR A 2 H18E H 1.3059 0.6125 0.0312 0.170 Uiso 0.44(2) 1 calc PR A 2 H18F H 1.3957 0.6511 -0.0663 0.170 Uiso 0.44(2) 1 calc PR A 2 C19B C 1.4394(19) 0.8584(14) 0.0229(19) 0.087(7) Uiso 0.44(2) 1 d PD A 2 H19D H 1.4967 0.8474 -0.0396 0.131 Uiso 0.44(2) 1 calc PR A 2 H19E H 1.4727 0.8975 0.0775 0.131 Uiso 0.44(2) 1 calc PR A 2 H19F H 1.3690 0.9052 -0.0003 0.131 Uiso 0.44(2) 1 calc PR A 2 C20B C 1.5256(11) 0.6626(15) 0.0985(13) 0.053(4) Uiso 0.44(2) 1 d PD A 2 H20D H 1.5118 0.5834 0.1211 0.080 Uiso 0.44(2) 1 calc PR A 2 H20E H 1.5593 0.6960 0.1565 0.080 Uiso 0.44(2) 1 calc PR A 2 H20F H 1.5799 0.6630 0.0332 0.080 Uiso 0.44(2) 1 calc PR A 2 Cl2 Cl 0.90505(16) 0.80003(13) 0.02297(11) 0.0498(4) Uani 1 1 d D . . O3A O 0.866(4) 0.775(2) 0.1341(11) 0.132(17) Uani 0.35(5) 1 d PD B 1 O4A O 1.0291(12) 0.789(3) 0.014(4) 0.132(15) Uani 0.35(5) 1 d PD B 1 O5A O 0.858(3) 0.9103(12) -0.012(2) 0.104(13) Uani 0.35(5) 1 d PD B 1 O3B O 0.8275(18) 0.9040(10) 0.0076(14) 0.091(5) Uani 0.65(5) 1 d PD B 2 O4B O 0.909(2) 0.7660(10) 0.1316(7) 0.086(5) Uani 0.65(5) 1 d PD B 2 O5B O 1.0166(13) 0.8211(19) -0.0267(18) 0.209(14) Uani 0.65(5) 1 d PD B 2 O6 O 0.8677(8) 0.7135(6) -0.0374(6) 0.125(3) Uani 1 1 d D B 2 Cl3 Cl 1.47539(18) 0.63899(16) 0.66167(17) 0.0657(5) Uani 1 1 d D . . O7A O 1.5992(12) 0.6310(13) 0.676(2) 0.173(12) Uani 0.59(2) 1 d PD C 1 O8A O 1.413(2) 0.7214(14) 0.7212(12) 0.192(14) Uani 0.59(2) 1 d PD C 1 O9A O 1.4687(19) 0.6697(13) 0.5480(10) 0.122(7) Uani 0.59(2) 1 d PD C 1 O10A O 1.4448(13) 0.5286(11) 0.6829(19) 0.118(8) Uani 0.59(2) 1 d PD C 1 O7B O 1.5384(18) 0.6223(17) 0.7600(13) 0.113(8) Uani 0.41(2) 1 d PD C 2 O8B O 1.3534(11) 0.6895(12) 0.6866(16) 0.075(6) Uani 0.41(2) 1 d PD C 2 O9B O 1.5328(18) 0.7004(16) 0.5758(18) 0.118(11) Uani 0.41(2) 1 d PD C 2 O10B O 1.4664(16) 0.5198(13) 0.6296(19) 0.087(8) Uani 0.41(2) 1 d PD C 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 0.0389(2) 0.02759(19) 0.02064(19) 0.00030(13) -0.00130(14) -0.00319(15) Pd2 0.0303(2) 0.0301(2) 0.02230(19) 0.00011(14) 0.00145(14) -0.00002(14) S 0.0328(6) 0.0264(5) 0.0221(5) -0.0011(4) 0.0008(4) -0.0011(4) N1 0.044(2) 0.029(2) 0.029(2) 0.0057(17) -0.0058(18) -0.0002(18) N2 0.058(3) 0.030(2) 0.029(2) 0.0007(17) 0.000(2) -0.008(2) N3 0.035(2) 0.0264(19) 0.025(2) 0.0007(15) -0.0007(16) 0.0038(16) N4 0.034(2) 0.040(2) 0.032(2) 0.0002(18) 0.0030(18) 0.0030(18) N5 0.047(3) 0.039(2) 0.022(2) -0.0015(17) 0.0005(18) 0.001(2) O1 0.040(2) 0.067(3) 0.034(2) 0.0092(19) 0.0040(17) -0.008(2) C21 0.040(3) 0.040(3) 0.031(3) -0.003(2) 0.008(2) -0.006(2) C22 0.047(4) 0.111(7) 0.052(4) -0.032(4) 0.014(3) -0.006(4) Cl1 0.144(3) 0.185(4) 0.111(3) -0.016(3) 0.005(2) 0.036(3) C1 0.033(2) 0.026(2) 0.024(2) -0.0014(17) 0.0018(18) -0.0020(18) C2 0.033(2) 0.032(2) 0.027(2) 0.0007(19) 0.0022(19) 0.000(2) C3 0.046(3) 0.042(3) 0.029(3) 0.004(2) 0.007(2) -0.002(2) C4 0.040(3) 0.049(3) 0.032(3) 0.000(2) 0.011(2) 0.002(2) C5 0.037(3) 0.038(3) 0.035(3) 0.001(2) 0.004(2) 0.010(2) C6 0.037(3) 0.035(3) 0.024(2) 0.0033(19) 0.000(2) 0.001(2) C7 0.042(3) 0.036(3) 0.031(3) 0.000(2) -0.005(2) 0.009(2) C8 0.065(4) 0.034(3) 0.039(3) 0.011(2) 0.002(3) 0.008(3) C9 0.075(4) 0.031(3) 0.034(3) 0.004(2) -0.007(3) -0.004(3) C10 0.083(5) 0.052(4) 0.030(3) 0.006(3) -0.016(3) -0.013(3) C11 0.065(4) 0.047(3) 0.052(4) 0.008(3) 0.009(3) -0.020(3) C12 0.039(3) 0.030(2) 0.026(2) 0.0041(19) 0.000(2) -0.001(2) C13 0.039(3) 0.035(3) 0.033(3) 0.003(2) 0.001(2) 0.006(2) C14 0.041(3) 0.043(3) 0.031(3) -0.001(2) -0.003(2) 0.008(2) C15 0.042(3) 0.048(3) 0.062(4) 0.001(3) -0.011(3) -0.005(3) C16 0.045(3) 0.052(3) 0.038(3) -0.005(3) 0.007(2) 0.008(3) C17 0.059(4) 0.071(4) 0.041(3) 0.008(3) 0.022(3) 0.019(3) Cl2 0.0739(10) 0.0452(8) 0.0284(6) 0.0005(5) 0.0014(6) -0.0048(7) O3A 0.22(3) 0.077(17) 0.064(16) 0.033(12) 0.08(2) 0.045(18) O4A 0.084(19) 0.12(2) 0.20(4) -0.03(2) -0.04(2) -0.014(14) O5A 0.18(3) 0.043(11) 0.067(16) 0.045(11) 0.046(16) 0.009(13) O3B 0.142(12) 0.066(8) 0.049(7) 0.004(6) 0.002(8) 0.038(8) O4B 0.184(14) 0.046(6) 0.026(5) -0.002(4) -0.031(7) 0.011(7) O5B 0.138(16) 0.19(2) 0.25(2) 0.11(2) 0.108(17) 0.002(14) O6 0.204(9) 0.085(5) 0.094(5) -0.043(4) -0.056(6) 0.010(5) Cl3 0.0748(12) 0.0515(9) 0.0669(12) -0.0063(8) 0.0097(9) -0.0022(8) O7A 0.131(15) 0.118(13) 0.29(3) -0.078(17) 0.012(17) -0.057(11) O8A 0.36(3) 0.084(12) 0.083(10) -0.002(9) 0.065(17) 0.107(17) O9A 0.171(18) 0.101(11) 0.098(10) -0.025(8) 0.038(11) -0.048(11) O10A 0.078(9) 0.052(7) 0.21(2) 0.040(9) 0.021(11) 0.007(6) O7B 0.104(16) 0.17(2) 0.069(12) -0.025(12) -0.006(10) -0.046(14) O8B 0.061(9) 0.046(8) 0.113(16) -0.013(8) 0.031(8) -0.009(6) O9B 0.111(17) 0.084(13) 0.131(19) 0.051(13) 0.079(14) -0.002(11) O10B 0.045(9) 0.077(12) 0.145(19) -0.055(12) -0.016(10) 0.004(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 1.994(4) . ? Pd1 N5 2.022(4) . ? Pd1 N2 2.103(4) . ? Pd1 S 2.2524(14) . ? Pd2 N3 1.981(4) . ? Pd2 O1 2.023(4) . ? Pd2 N4 2.100(4) . ? Pd2 S 2.2700(14) . ? S C1 1.764(5) . ? N1 C7 1.291(7) . ? N1 C8 1.491(6) . ? N2 C11 1.496(8) . ? N2 C10 1.499(8) . ? N2 C9 1.502(7) . ? N3 C12 1.273(6) . ? N3 C13 1.488(6) . ? N4 C14 1.485(7) . ? N4 C15 1.486(7) . ? N4 C16 1.487(7) . ? N5 C21 1.283(7) . ? O1 C21 1.292(7) . ? C21 C22 1.519(8) . ? C22 Cl1 1.578(9) . ? C1 C2 1.408(6) . ? C1 C6 1.416(7) . ? C2 C3 1.396(7) . ? C2 C12 1.465(7) . ? C3 C4 1.393(8) . ? C4 C5 1.382(8) . ? C4 C17 1.540(7) . ? C5 C6 1.417(7) . ? C6 C7 1.454(7) . ? C8 C9 1.502(9) . ? C13 C14 1.508(8) . ? C17 C18B 1.515(14) . ? C17 C19A 1.526(11) . ? C17 C20A 1.531(11) . ? C17 C20B 1.547(12) . ? C17 C19B 1.576(13) . ? C17 C18A 1.581(12) . ? Cl2 O4B 1.357(8) . ? Cl2 O5A 1.371(13) . ? Cl2 O4A 1.393(13) . ? Cl2 O5B 1.393(10) . ? Cl2 O3A 1.405(13) . ? Cl2 O3B 1.409(9) . ? Cl2 O6 1.409(6) . ? Cl3 O8A 1.333(11) . ? Cl3 O10A 1.359(11) . ? Cl3 O9B 1.377(12) . ? Cl3 O9A 1.410(12) . ? Cl3 O7A 1.423(12) . ? Cl3 O7B 1.440(13) . ? Cl3 O8B 1.450(12) . ? Cl3 O10B 1.473(13) . ? 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 N5 174.91(17) . . ? N1 Pd1 N2 84.09(18) . . ? N5 Pd1 N2 91.14(18) . . ? N1 Pd1 S 94.89(12) . . ? N5 Pd1 S 89.80(13) . . ? N2 Pd1 S 177.38(14) . . ? N3 Pd2 O1 170.25(17) . . ? N3 Pd2 N4 84.02(17) . . ? O1 Pd2 N4 87.09(17) . . ? N3 Pd2 S 91.74(13) . . ? O1 Pd2 S 97.11(12) . . ? N4 Pd2 S 175.74(12) . . ? C1 S Pd1 111.43(16) . . ? C1 S Pd2 106.88(17) . . ? Pd1 S Pd2 109.28(6) . . ? C7 N1 C8 116.5(4) . . ? C7 N1 Pd1 130.1(4) . . ? C8 N1 Pd1 112.8(3) . . ? C11 N2 C10 108.4(5) . . ? C11 N2 C9 108.0(5) . . ? C10 N2 C9 111.4(5) . . ? C11 N2 Pd1 116.0(4) . . ? C10 N2 Pd1 109.9(3) . . ? C9 N2 Pd1 103.1(3) . . ? C12 N3 C13 119.9(4) . . ? C12 N3 Pd2 130.3(3) . . ? C13 N3 Pd2 109.7(3) . . ? C14 N4 C15 110.5(5) . . ? C14 N4 C16 110.4(4) . . ? C15 N4 C16 108.7(5) . . ? C14 N4 Pd2 106.8(3) . . ? C15 N4 Pd2 111.6(3) . . ? C16 N4 Pd2 108.9(3) . . ? C21 N5 Pd1 130.0(4) . . ? C21 O1 Pd2 129.1(4) . . ? N5 C21 O1 125.8(5) . . ? N5 C21 C22 117.5(5) . . ? O1 C21 C22 116.5(5) . . ? C21 C22 Cl1 121.0(6) . . ? C2 C1 C6 117.6(4) . . ? C2 C1 S 120.2(4) . . ? C6 C1 S 121.7(4) . . ? C3 C2 C1 120.4(5) . . ? C3 C2 C12 113.0(4) . . ? C1 C2 C12 126.5(4) . . ? C4 C3 C2 122.6(5) . . ? C5 C4 C3 117.2(5) . . ? C5 C4 C17 120.8(5) . . ? C3 C4 C17 121.7(5) . . ? C4 C5 C6 122.0(5) . . ? C1 C6 C5 120.0(4) . . ? C1 C6 C7 127.0(4) . . ? C5 C6 C7 112.4(4) . . ? N1 C7 C6 128.6(5) . . ? N1 C8 C9 107.5(5) . . ? N2 C9 C8 110.1(5) . . ? N3 C12 C2 127.8(4) . . ? N3 C13 C14 106.4(4) . . ? N4 C14 C13 109.4(4) . . ? C18B C17 C19A 76.9(10) . . ? C18B C17 C20A 134.0(12) . . ? C19A C17 C20A 112.1(7) . . ? C18B C17 C4 106.5(12) . . ? C19A C17 C4 112.6(7) . . ? C20A C17 C4 110.1(8) . . ? C18B C17 C20B 111.9(10) . . ? C19A C17 C20B 126.4(9) . . ? C20A C17 C20B 25.8(7) . . ? C4 C17 C20B 114.4(7) . . ? C18B C17 C19B 110.6(10) . . ? C19A C17 C19B 34.3(8) . . ? C20A C17 C19B 83.8(9) . . ? C4 C17 C19B 107.5(9) . . ? C20B C17 C19B 105.9(8) . . ? C18B C17 C18A 33.4(9) . . ? C19A C17 C18A 108.0(8) . . ? C20A C17 C18A 109.0(8) . . ? C4 C17 C18A 104.7(8) . . ? C20B C17 C18A 83.5(8) . . ? C19B C17 C18A 138.3(11) . . ? O4B Cl2 O5A 121.9(13) . . ? O4B Cl2 O4A 88.0(17) . . ? O5A Cl2 O4A 111.5(11) . . ? O4B Cl2 O5B 111.8(8) . . ? O5A Cl2 O5B 90.6(16) . . ? O4A Cl2 O5B 25.3(18) . . ? O4B Cl2 O3A 20.3(17) . . ? O5A Cl2 O3A 110.0(10) . . ? O4A Cl2 O3A 108.2(10) . . ? O5B Cl2 O3A 131.1(16) . . ? O4B Cl2 O3B 111.4(7) . . ? O5A Cl2 O3B 16.8(17) . . ? O4A Cl2 O3B 126.7(15) . . ? O5B Cl2 O3B 107.3(8) . . ? O3A Cl2 O3B 96.3(16) . . ? O4B Cl2 O6 112.2(6) . . ? O5A Cl2 O6 111.6(10) . . ? O4A Cl2 O6 108.7(9) . . ? O5B Cl2 O6 105.6(8) . . ? O3A Cl2 O6 106.6(10) . . ? O3B Cl2 O6 108.3(7) . . ? O8A Cl3 O10A 116.0(9) . . ? O8A Cl3 O9B 104.6(11) . . ? O10A Cl3 O9B 136.8(11) . . ? O8A Cl3 O9A 110.2(8) . . ? O10A Cl3 O9A 108.4(8) . . ? O9B Cl3 O9A 39.6(9) . . ? O8A Cl3 O7A 111.6(10) . . ? O10A Cl3 O7A 105.9(8) . . ? O9B Cl3 O7A 69.9(10) . . ? O9A Cl3 O7A 104.0(8) . . ? O8A Cl3 O7B 80.3(11) . . ? O10A Cl3 O7B 88.1(11) . . ? O9B Cl3 O7B 113.7(9) . . ? O9A Cl3 O7B 152.2(9) . . ? O7A Cl3 O7B 49.0(9) . . ? O8A Cl3 O8B 39.7(11) . . ? O10A Cl3 O8B 91.5(9) . . ? O9B Cl3 O8B 112.4(9) . . ? O9A Cl3 O8B 91.5(11) . . ? O7A Cl3 O8B 151.3(8) . . ? O7B Cl3 O8B 110.7(8) . . ? O8A Cl3 O10B 139.4(11) . . ? O10A Cl3 O10B 27.5(10) . . ? O9B Cl3 O10B 109.4(9) . . ? O9A Cl3 O10B 83.9(10) . . ? O7A Cl3 O10B 100.6(9) . . ? O7B Cl3 O10B 105.0(9) . . ? O8B Cl3 O10B 105.0(7) . . ? #===END # Attachment 'CCDC_286861_n.CIF' data_11 _database_code_depnum_ccdc_archive 'CCDC 286861' _chemical_formula_structural ; [(L3)Pd2(Ph)2]BPh4 ; _chemical_formula_sum 'C56 H63 B N4 Pd2 S' _chemical_formula_weight 1047.77 _chemical_melting_point ? _chemical_compound_source ; Crystals were grown by recrystallization from a mixed acetonitrile/ethanol solvent system ; #CRYSTAL DATA _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 12.375(2) _cell_length_b 13.557(3) _cell_length_c 17.310(3) _cell_angle_alpha 74.396(3) _cell_angle_beta 78.886(3) _cell_angle_gamma 62.886(3) _cell_volume 2481.1(8) _cell_formula_units_Z 2 _cell_measurement_temperature 210(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.402 _exptl_crystal_F_000 1080 _exptl_absorpt_coefficient_mu 0.808 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.88 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ? _diffrn_radiation_type MoK\a _diffrn_ambient_temperature 210(2) _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'BRUKER AXS' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_method hemisphere _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21123 _diffrn_reflns_av_R_equivalents 0.0401 _diffrn_reflns_av_sigmaI/netI 0.0871 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.23 _diffrn_reflns_theta_max 28.89 #REFINEMENT DATA _reflns_number_total 11263 _reflns_number_gt 6367 _reflns_threshold_expression >2sigma(I) _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^)+(0.0439P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11263 _refine_ls_number_parameters 577 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1002 _refine_ls_R_factor_gt 0.0483 _refine_ls_wR_factor_ref 0.1174 _refine_ls_wR_factor_gt 0.0905 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.862 _diffrn_reflns_theta_full 28.89 _diffrn_measured_fraction_theta_full 0.862 _refine_diff_density_max 1.185 _refine_diff_density_min -1.217 _refine_diff_density_rms 0.113 _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 (FARRUGIA)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; #ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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' B B 0.0013 0.0007 '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' S S 0.1246 0.1234 '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' 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 0.63125(3) 0.53029(3) 0.07407(2) 0.03365(11) Uani 1 1 d . . . Pd2 Pd 0.68916(3) 0.32407(3) 0.28554(2) 0.03603(11) Uani 1 1 d . . . S S 0.57572(10) 0.41879(10) 0.17852(7) 0.0337(3) Uani 1 1 d . . . N1 N 0.5051(4) 0.6777(3) 0.1077(2) 0.0411(10) Uani 1 1 d . . . N2 N 0.6745(3) 0.6415(3) -0.0259(2) 0.0383(9) Uani 1 1 d . . . N3 N 0.5582(4) 0.2653(3) 0.3344(2) 0.0376(9) Uani 1 1 d . . . N4 N 0.7816(4) 0.2068(4) 0.3873(2) 0.0461(11) Uani 1 1 d . . . C1 C 0.4349(4) 0.4971(4) 0.2285(3) 0.0320(10) Uani 1 1 d . . . C2 C 0.3807(4) 0.4359(4) 0.2884(3) 0.0347(11) Uani 1 1 d . . . C3 C 0.2613(4) 0.4901(4) 0.3200(3) 0.0398(12) Uani 1 1 d . . . H3 H 0.2266 0.4466 0.3571 0.048 Uiso 1 1 calc R . . C4 C 0.1921(4) 0.6055(4) 0.2986(3) 0.0403(12) Uani 1 1 d . . . C5 C 0.2496(4) 0.6651(4) 0.2446(3) 0.0406(12) Uani 1 1 d . . . H5 H 0.2071 0.7435 0.2310 0.049 Uiso 1 1 calc R . . C6 C 0.3675(4) 0.6155(4) 0.2090(3) 0.0330(10) Uani 1 1 d . . . C7 C 0.4096(4) 0.6969(4) 0.1562(3) 0.0417(12) Uani 1 1 d . . . H7 H 0.3606 0.7726 0.1582 0.050 Uiso 1 1 calc R . . C8 C 0.5273(5) 0.7745(4) 0.0575(3) 0.0599(16) Uani 1 1 d . . . H8A H 0.5895 0.7820 0.0788 0.072 Uiso 1 1 calc R . . H8B H 0.4532 0.8441 0.0568 0.072 Uiso 1 1 calc R . . C9 C 0.5683(5) 0.7518(4) -0.0255(3) 0.0544(15) Uani 1 1 d . . . H9A H 0.5018 0.7529 -0.0482 0.065 Uiso 1 1 calc R . . H9B H 0.5893 0.8114 -0.0591 0.065 Uiso 1 1 calc R . . C10 C 0.7862(5) 0.6484(5) -0.0132(3) 0.0587(15) Uani 1 1 d . . . H10A H 0.8569 0.5851 -0.0285 0.088 Uiso 1 1 calc R . . H10B H 0.7860 0.6471 0.0425 0.088 Uiso 1 1 calc R . . H10C H 0.7877 0.7176 -0.0455 0.088 Uiso 1 1 calc R . . C11 C 0.6914(5) 0.6124(5) -0.1051(3) 0.0526(14) Uani 1 1 d . . . H11A H 0.6227 0.6018 -0.1122 0.079 Uiso 1 1 calc R . . H11B H 0.7642 0.5438 -0.1076 0.079 Uiso 1 1 calc R . . H11C H 0.6984 0.6727 -0.1469 0.079 Uiso 1 1 calc R . . C13 C 0.6127(5) 0.1559(4) 0.3898(3) 0.0510(14) Uani 1 1 d . . . H13A H 0.6615 0.0963 0.3602 0.061 Uiso 1 1 calc R . . H13B H 0.5499 0.1373 0.4242 0.061 Uiso 1 1 calc R . . C14 C 0.6914(5) 0.1689(5) 0.4394(3) 0.0497(14) Uani 1 1 d . . . H14A H 0.6403 0.2238 0.4724 0.060 Uiso 1 1 calc R . . H14B H 0.7340 0.0970 0.4749 0.060 Uiso 1 1 calc R . . C15 C 0.8850(5) 0.1095(5) 0.3606(3) 0.0743(19) Uani 1 1 d . . . H15A H 0.9188 0.0514 0.4067 0.111 Uiso 1 1 calc R . . H15B H 0.9461 0.1329 0.3305 0.111 Uiso 1 1 calc R . . H15C H 0.8578 0.0804 0.3272 0.111 Uiso 1 1 calc R . . C16 C 0.8261(6) 0.2535(6) 0.4354(3) 0.0754(19) Uani 1 1 d . . . H16A H 0.8519 0.2003 0.4850 0.113 Uiso 1 1 calc R . . H16B H 0.7618 0.3233 0.4468 0.113 Uiso 1 1 calc R . . H16C H 0.8936 0.2673 0.4058 0.113 Uiso 1 1 calc R . . C17 C 0.0627(4) 0.6678(4) 0.3353(3) 0.0486(13) Uani 1 1 d . . . C18 C 0.0091(5) 0.5856(5) 0.3823(3) 0.0641(17) Uani 1 1 d . . . H18A H -0.0759 0.6273 0.3971 0.096 Uiso 1 1 calc R . . H18B H 0.0510 0.5428 0.4301 0.096 Uiso 1 1 calc R . . H18C H 0.0183 0.5349 0.3495 0.096 Uiso 1 1 calc R . . C19 C -0.0218(5) 0.7490(5) 0.2693(4) 0.0747(19) Uani 1 1 d . . . H19A H -0.0201 0.7076 0.2316 0.112 Uiso 1 1 calc R . . H19B H 0.0051 0.8065 0.2419 0.112 Uiso 1 1 calc R . . H19C H -0.1034 0.7837 0.2931 0.112 Uiso 1 1 calc R . . C20 C 0.0677(6) 0.7366(6) 0.3908(4) 0.090(2) Uani 1 1 d . . . H20A H 0.1021 0.7877 0.3606 0.135 Uiso 1 1 calc R . . H20B H 0.1173 0.6861 0.4339 0.135 Uiso 1 1 calc R . . H20C H -0.0132 0.7791 0.4126 0.135 Uiso 1 1 calc R . . C21 C 0.7512(4) 0.3909(4) 0.0345(3) 0.0364(11) Uani 1 1 d . . . C22 C 0.7132(5) 0.3259(4) 0.0085(3) 0.0471(13) Uani 1 1 d . . . H22 H 0.6304 0.3443 0.0137 0.057 Uiso 1 1 calc R . . C23 C 0.7934(5) 0.2334(5) -0.0252(3) 0.0563(15) Uani 1 1 d . . . H23 H 0.7639 0.1909 -0.0416 0.068 Uiso 1 1 calc R . . C24 C 0.9160(6) 0.2051(5) -0.0343(3) 0.0608(16) Uani 1 1 d . . . H24 H 0.9705 0.1438 -0.0572 0.073 Uiso 1 1 calc R . . C25 C 0.9563(5) 0.2690(5) -0.0089(3) 0.0611(16) Uani 1 1 d . . . H25 H 1.0390 0.2514 -0.0154 0.073 Uiso 1 1 calc R . . C26 C 0.8766(5) 0.3589(4) 0.0261(3) 0.0496(13) Uani 1 1 d . . . H26 H 0.9069 0.3991 0.0445 0.060 Uiso 1 1 calc R . . C27 C 0.8052(4) 0.3937(4) 0.2459(3) 0.0417(12) Uani 1 1 d . . . C28 C 0.7641(5) 0.5075(5) 0.2502(3) 0.0553(15) Uani 1 1 d . . . H28 H 0.6845 0.5471 0.2700 0.066 Uiso 1 1 calc R . . C29 C 0.8396(6) 0.5609(5) 0.2255(4) 0.0703(18) Uani 1 1 d . . . H29 H 0.8114 0.6357 0.2299 0.084 Uiso 1 1 calc R . . C30 C 0.9574(6) 0.5044(6) 0.1941(4) 0.0694(18) Uani 1 1 d . . . H30 H 1.0079 0.5413 0.1754 0.083 Uiso 1 1 calc R . . C31 C 0.9978(5) 0.3943(6) 0.1912(3) 0.0636(17) Uani 1 1 d . . . H31 H 1.0781 0.3547 0.1723 0.076 Uiso 1 1 calc R . . C32 C 0.9221(5) 0.3392(5) 0.2157(3) 0.0556(15) Uani 1 1 d . . . H32 H 0.9517 0.2641 0.2115 0.067 Uiso 1 1 calc R . . B B 0.4078(5) 0.9639(5) 0.2873(3) 0.0388(13) Uani 1 1 d . . . C12 C 0.4437(5) 0.3183(4) 0.3294(3) 0.0434(12) Uani 1 1 d . . . H12 H 0.3967 0.2791 0.3537 0.052 Uiso 1 1 calc R . . C101 C 0.4606(4) 0.8341(4) 0.3419(3) 0.0401(12) Uani 1 1 d . . . C102 C 0.5638(5) 0.7912(4) 0.3850(3) 0.0493(13) Uani 1 1 d . . . H102 H 0.6018 0.8379 0.3813 0.059 Uiso 1 1 calc R . . C103 C 0.6116(5) 0.6841(5) 0.4324(3) 0.0609(16) Uani 1 1 d . . . H103 H 0.6789 0.6606 0.4606 0.073 Uiso 1 1 calc R . . C104 C 0.5590(6) 0.6116(5) 0.4379(3) 0.0617(17) Uani 1 1 d . . . H104 H 0.5903 0.5392 0.4700 0.074 Uiso 1 1 calc R . . C105 C 0.4603(6) 0.6476(5) 0.3957(3) 0.0580(16) Uani 1 1 d . . . H105 H 0.4254 0.5988 0.3978 0.070 Uiso 1 1 calc R . . C106 C 0.4126(5) 0.7564(4) 0.3501(3) 0.0461(13) Uani 1 1 d . . . H106 H 0.3443 0.7791 0.3231 0.055 Uiso 1 1 calc R . . C201 C 0.5256(4) 0.9833(4) 0.2366(3) 0.0374(11) Uani 1 1 d . . . C202 C 0.5429(5) 1.0801(4) 0.2256(3) 0.0439(12) Uani 1 1 d . . . H202 H 0.4842 1.1393 0.2489 0.053 Uiso 1 1 calc R . . C203 C 0.6430(5) 1.0937(5) 0.1816(3) 0.0570(15) Uani 1 1 d . . . H203 H 0.6517 1.1595 0.1780 0.068 Uiso 1 1 calc R . . C204 C 0.7286(5) 1.0113(5) 0.1437(3) 0.0626(17) Uani 1 1 d . . . H204 H 0.7945 1.0212 0.1127 0.075 Uiso 1 1 calc R . . C205 C 0.7161(5) 0.9131(5) 0.1521(3) 0.0593(16) Uani 1 1 d . . . H205 H 0.7743 0.8555 0.1271 0.071 Uiso 1 1 calc R . . C206 C 0.6168(5) 0.9002(4) 0.1977(3) 0.0507(14) Uani 1 1 d . . . H206 H 0.6105 0.8329 0.2029 0.061 Uiso 1 1 calc R . . C301 C 0.3348(4) 1.0577(4) 0.3446(3) 0.0388(12) Uani 1 1 d . . . C302 C 0.3650(5) 1.0442(4) 0.4209(3) 0.0477(13) Uani 1 1 d . . . H302 H 0.4314 0.9787 0.4412 0.057 Uiso 1 1 calc R . . C303 C 0.3009(6) 1.1241(5) 0.4686(3) 0.0602(16) Uani 1 1 d . . . H303 H 0.3242 1.1105 0.5198 0.072 Uiso 1 1 calc R . . C304 C 0.2047(6) 1.2217(5) 0.4411(4) 0.0581(16) Uani 1 1 d . . . H304 H 0.1615 1.2747 0.4734 0.070 Uiso 1 1 calc R . . C305 C 0.1720(5) 1.2413(5) 0.3658(4) 0.0585(15) Uani 1 1 d . . . H305 H 0.1068 1.3083 0.3460 0.070 Uiso 1 1 calc R . . C306 C 0.2364(5) 1.1605(5) 0.3185(3) 0.0534(14) Uani 1 1 d . . . H306 H 0.2127 1.1756 0.2672 0.064 Uiso 1 1 calc R . . C401 C 0.3120(5) 0.9816(4) 0.2258(3) 0.0417(12) Uani 1 1 d . . . C402 C 0.3304(5) 1.0077(4) 0.1425(3) 0.0483(14) Uani 1 1 d . . . H402 H 0.4027 1.0125 0.1194 0.058 Uiso 1 1 calc R . . C403 C 0.2437(6) 1.0270(4) 0.0922(4) 0.0634(17) Uani 1 1 d . . . H403 H 0.2581 1.0465 0.0367 0.076 Uiso 1 1 calc R . . C404 C 0.1386(6) 1.0175(5) 0.1239(4) 0.0673(18) Uani 1 1 d . . . H404 H 0.0823 1.0280 0.0903 0.081 Uiso 1 1 calc R . . C405 C 0.1162(5) 0.9924(5) 0.2056(4) 0.0646(17) Uani 1 1 d . . . H405 H 0.0444 0.9861 0.2279 0.078 Uiso 1 1 calc R . . C406 C 0.2000(5) 0.9766(4) 0.2546(3) 0.0522(14) Uani 1 1 d . . . H406 H 0.1817 0.9618 0.3100 0.063 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 0.0369(2) 0.0369(2) 0.0301(2) -0.00561(16) 0.00141(16) -0.02058(18) Pd2 0.0350(2) 0.0398(2) 0.0319(2) -0.00330(17) -0.00152(16) -0.01751(18) S 0.0335(6) 0.0342(6) 0.0314(6) -0.0043(5) 0.0001(5) -0.0152(5) N1 0.048(3) 0.036(2) 0.044(2) -0.0084(19) 0.002(2) -0.024(2) N2 0.043(2) 0.047(2) 0.033(2) -0.0064(19) 0.0005(18) -0.029(2) N3 0.046(3) 0.039(2) 0.032(2) -0.0023(18) -0.0039(19) -0.024(2) N4 0.040(2) 0.054(3) 0.039(2) -0.002(2) -0.0039(19) -0.020(2) C1 0.032(2) 0.037(3) 0.029(2) -0.006(2) -0.0027(19) -0.016(2) C2 0.036(3) 0.035(3) 0.036(3) -0.007(2) -0.003(2) -0.018(2) C3 0.040(3) 0.045(3) 0.039(3) -0.010(2) 0.002(2) -0.024(3) C4 0.039(3) 0.051(3) 0.037(3) -0.015(2) 0.003(2) -0.024(3) C5 0.038(3) 0.037(3) 0.046(3) -0.014(2) 0.002(2) -0.015(2) C6 0.035(3) 0.035(3) 0.030(2) -0.008(2) 0.001(2) -0.018(2) C7 0.045(3) 0.036(3) 0.044(3) -0.013(2) 0.002(2) -0.017(2) C8 0.072(4) 0.043(3) 0.068(4) -0.011(3) 0.021(3) -0.038(3) C9 0.059(4) 0.040(3) 0.056(4) 0.002(3) 0.010(3) -0.027(3) C10 0.065(4) 0.078(4) 0.052(3) -0.008(3) 0.002(3) -0.052(4) C11 0.063(4) 0.068(4) 0.035(3) -0.005(3) 0.002(3) -0.041(3) C13 0.055(3) 0.043(3) 0.044(3) 0.009(3) -0.006(3) -0.021(3) C14 0.052(3) 0.064(4) 0.029(3) 0.003(2) -0.006(2) -0.027(3) C15 0.053(4) 0.065(4) 0.065(4) 0.007(3) -0.003(3) -0.003(3) C16 0.079(5) 0.106(5) 0.055(4) 0.002(4) -0.026(3) -0.053(4) C17 0.038(3) 0.054(3) 0.054(3) -0.021(3) 0.011(3) -0.019(3) C18 0.040(3) 0.074(4) 0.074(4) -0.021(3) 0.015(3) -0.025(3) C19 0.046(4) 0.070(4) 0.087(5) -0.008(4) -0.001(3) -0.012(3) C20 0.072(5) 0.119(6) 0.112(6) -0.085(5) 0.042(4) -0.055(5) C21 0.039(3) 0.042(3) 0.029(2) -0.004(2) -0.001(2) -0.020(2) C22 0.043(3) 0.051(3) 0.046(3) -0.009(3) 0.000(2) -0.021(3) C23 0.066(4) 0.053(4) 0.053(3) -0.016(3) -0.010(3) -0.024(3) C24 0.063(4) 0.047(3) 0.050(3) -0.012(3) -0.005(3) -0.002(3) C25 0.043(3) 0.065(4) 0.066(4) -0.016(3) 0.003(3) -0.017(3) C26 0.050(3) 0.048(3) 0.049(3) -0.010(3) -0.001(3) -0.021(3) C27 0.041(3) 0.056(3) 0.035(3) -0.012(2) 0.000(2) -0.027(3) C28 0.052(3) 0.067(4) 0.062(4) -0.022(3) 0.007(3) -0.037(3) C29 0.067(4) 0.069(4) 0.086(5) -0.020(4) -0.002(4) -0.038(4) C30 0.065(4) 0.086(5) 0.071(4) -0.008(4) -0.001(3) -0.050(4) C31 0.043(3) 0.095(5) 0.053(4) -0.013(4) 0.008(3) -0.035(4) C32 0.055(4) 0.061(4) 0.047(3) -0.013(3) 0.005(3) -0.024(3) B 0.046(3) 0.039(3) 0.034(3) -0.010(3) -0.005(3) -0.018(3) C12 0.050(3) 0.048(3) 0.040(3) -0.006(2) 0.001(2) -0.032(3) C101 0.048(3) 0.038(3) 0.029(3) -0.010(2) 0.003(2) -0.015(2) C102 0.051(3) 0.044(3) 0.047(3) -0.002(3) -0.006(3) -0.019(3) C103 0.053(4) 0.060(4) 0.047(3) 0.005(3) -0.009(3) -0.012(3) C104 0.072(4) 0.041(3) 0.050(4) 0.007(3) 0.001(3) -0.017(3) C105 0.078(4) 0.044(3) 0.051(3) -0.005(3) 0.007(3) -0.033(3) C106 0.056(3) 0.042(3) 0.041(3) -0.007(2) -0.006(2) -0.022(3) C201 0.046(3) 0.038(3) 0.027(2) 0.000(2) -0.010(2) -0.018(2) C202 0.050(3) 0.042(3) 0.040(3) -0.007(2) -0.003(2) -0.021(3) C203 0.066(4) 0.053(4) 0.055(4) -0.003(3) -0.007(3) -0.032(3) C204 0.053(4) 0.070(4) 0.050(4) 0.004(3) 0.003(3) -0.026(3) C205 0.054(4) 0.058(4) 0.048(3) -0.007(3) 0.001(3) -0.013(3) C206 0.061(4) 0.045(3) 0.044(3) -0.010(3) 0.000(3) -0.023(3) C301 0.041(3) 0.044(3) 0.035(3) -0.008(2) 0.003(2) -0.024(3) C302 0.064(4) 0.048(3) 0.033(3) -0.006(2) 0.003(3) -0.030(3) C303 0.098(5) 0.063(4) 0.033(3) -0.013(3) 0.008(3) -0.049(4) C304 0.068(4) 0.063(4) 0.058(4) -0.031(3) 0.028(3) -0.043(4) C305 0.046(3) 0.051(4) 0.080(4) -0.024(3) 0.004(3) -0.021(3) C306 0.056(4) 0.055(4) 0.055(3) -0.020(3) -0.008(3) -0.023(3) C401 0.051(3) 0.023(2) 0.046(3) -0.007(2) -0.009(2) -0.010(2) C402 0.066(4) 0.026(3) 0.048(3) -0.005(2) -0.013(3) -0.014(3) C403 0.093(5) 0.040(3) 0.051(4) -0.001(3) -0.031(4) -0.018(3) C404 0.064(4) 0.045(3) 0.096(5) -0.017(4) -0.039(4) -0.011(3) C405 0.056(4) 0.050(4) 0.094(5) -0.026(4) -0.018(4) -0.016(3) C406 0.051(3) 0.043(3) 0.067(4) -0.018(3) -0.011(3) -0.017(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 C21 1.998(5) . ? Pd1 N1 2.050(4) . ? Pd1 N2 2.128(4) . ? Pd1 S 2.2413(12) . ? Pd2 C27 1.983(5) . ? Pd2 N3 2.065(4) . ? Pd2 N4 2.133(4) . ? Pd2 S 2.2652(12) . ? S C1 1.772(4) . ? N1 C7 1.274(5) . ? N1 C8 1.474(6) . ? N2 C9 1.475(6) . ? N2 C11 1.477(6) . ? N2 C10 1.488(6) . ? N3 C12 1.271(6) . ? N3 C13 1.465(6) . ? N4 C15 1.467(6) . ? N4 C16 1.477(6) . ? N4 C14 1.485(6) . ? C1 C6 1.408(6) . ? C1 C2 1.410(6) . ? C2 C3 1.392(6) . ? C2 C12 1.458(6) . ? C3 C4 1.381(6) . ? C4 C5 1.377(6) . ? C4 C17 1.531(6) . ? C5 C6 1.394(6) . ? C6 C7 1.457(6) . ? C8 C9 1.493(7) . ? C13 C14 1.509(7) . ? C17 C18 1.525(7) . ? C17 C19 1.531(7) . ? C17 C20 1.534(7) . ? C21 C22 1.367(6) . ? C21 C26 1.397(6) . ? C22 C23 1.391(7) . ? C23 C24 1.372(7) . ? C24 C25 1.370(8) . ? C25 C26 1.377(7) . ? C27 C32 1.362(7) . ? C27 C28 1.405(7) . ? C28 C29 1.370(7) . ? C29 C30 1.381(8) . ? C30 C31 1.353(8) . ? C31 C32 1.389(7) . ? B C401 1.641(7) . ? B C201 1.642(7) . ? B C301 1.644(7) . ? B C101 1.647(7) . ? C101 C106 1.392(6) . ? C101 C102 1.409(7) . ? C102 C103 1.377(7) . ? C103 C104 1.380(8) . ? C104 C105 1.369(8) . ? C105 C106 1.381(7) . ? C201 C202 1.382(6) . ? C201 C206 1.397(6) . ? C202 C203 1.384(7) . ? C203 C204 1.359(7) . ? C204 C205 1.376(7) . ? C205 C206 1.382(7) . ? C301 C302 1.385(6) . ? C301 C306 1.398(7) . ? C302 C303 1.389(7) . ? C303 C304 1.356(8) . ? C304 C305 1.361(7) . ? C305 C306 1.393(7) . ? C401 C402 1.389(6) . ? C401 C406 1.405(7) . ? C402 C403 1.400(7) . ? C403 C404 1.360(8) . ? C404 C405 1.367(8) . ? C405 C406 1.371(7) . ? 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 C21 Pd1 N1 176.53(17) . . ? C21 Pd1 N2 93.69(16) . . ? N1 Pd1 N2 83.80(15) . . ? C21 Pd1 S 88.28(13) . . ? N1 Pd1 S 94.14(11) . . ? N2 Pd1 S 177.11(11) . . ? C27 Pd2 N3 173.59(18) . . ? C27 Pd2 N4 97.32(18) . . ? N3 Pd2 N4 82.68(15) . . ? C27 Pd2 S 94.23(14) . . ? N3 Pd2 S 86.51(11) . . ? N4 Pd2 S 166.96(12) . . ? C1 S Pd1 111.69(15) . . ? C1 S Pd2 99.56(15) . . ? Pd1 S Pd2 121.16(5) . . ? C7 N1 C8 118.9(4) . . ? C7 N1 Pd1 130.6(3) . . ? C8 N1 Pd1 110.0(3) . . ? C9 N2 C11 108.8(4) . . ? C9 N2 C10 110.1(4) . . ? C11 N2 C10 108.6(4) . . ? C9 N2 Pd1 103.8(3) . . ? C11 N2 Pd1 115.5(3) . . ? C10 N2 Pd1 110.0(3) . . ? C12 N3 C13 121.7(4) . . ? C12 N3 Pd2 127.9(3) . . ? C13 N3 Pd2 109.6(3) . . ? C15 N4 C16 108.7(5) . . ? C15 N4 C14 109.6(4) . . ? C16 N4 C14 108.2(4) . . ? C15 N4 Pd2 109.4(3) . . ? C16 N4 Pd2 115.1(3) . . ? C14 N4 Pd2 105.8(3) . . ? C6 C1 C2 116.9(4) . . ? C6 C1 S 125.2(3) . . ? C2 C1 S 117.7(3) . . ? C3 C2 C1 120.6(4) . . ? C3 C2 C12 113.7(4) . . ? C1 C2 C12 125.4(4) . . ? C4 C3 C2 122.9(4) . . ? C5 C4 C3 115.6(4) . . ? C5 C4 C17 120.4(4) . . ? C3 C4 C17 123.9(4) . . ? C4 C5 C6 124.2(4) . . ? C5 C6 C1 119.5(4) . . ? C5 C6 C7 113.8(4) . . ? C1 C6 C7 126.7(4) . . ? N1 C7 C6 128.3(4) . . ? N1 C8 C9 107.2(4) . . ? N2 C9 C8 111.9(4) . . ? N3 C13 C14 106.0(4) . . ? N4 C14 C13 111.3(4) . . ? C18 C17 C19 107.4(4) . . ? C18 C17 C4 111.6(4) . . ? C19 C17 C4 110.6(4) . . ? C18 C17 C20 110.2(5) . . ? C19 C17 C20 108.9(5) . . ? C4 C17 C20 108.1(4) . . ? C22 C21 C26 116.3(5) . . ? C22 C21 Pd1 121.0(4) . . ? C26 C21 Pd1 122.5(4) . . ? C21 C22 C23 122.8(5) . . ? C24 C23 C22 119.8(5) . . ? C25 C24 C23 118.5(5) . . ? C24 C25 C26 121.3(5) . . ? C25 C26 C21 121.3(5) . . ? C32 C27 C28 117.5(5) . . ? C32 C27 Pd2 124.9(4) . . ? C28 C27 Pd2 117.5(4) . . ? C29 C28 C27 121.0(5) . . ? C28 C29 C30 120.4(6) . . ? C31 C30 C29 118.6(6) . . ? C30 C31 C32 121.5(6) . . ? C27 C32 C31 120.8(5) . . ? C401 B C201 110.5(4) . . ? C401 B C301 107.4(4) . . ? C201 B C301 109.8(4) . . ? C401 B C101 110.9(4) . . ? C201 B C101 107.1(4) . . ? C301 B C101 111.1(4) . . ? N3 C12 C2 124.9(4) . . ? C106 C101 C102 113.4(4) . . ? C106 C101 B 125.7(4) . . ? C102 C101 B 120.8(4) . . ? C103 C102 C101 123.7(5) . . ? C102 C103 C104 119.6(6) . . ? C105 C104 C103 119.3(5) . . ? C104 C105 C106 119.8(5) . . ? C105 C106 C101 124.1(5) . . ? C202 C201 C206 114.2(5) . . ? C202 C201 B 125.2(4) . . ? C206 C201 B 120.5(4) . . ? C201 C202 C203 123.5(5) . . ? C204 C203 C202 120.2(5) . . ? C203 C204 C205 119.0(5) . . ? C204 C205 C206 119.9(6) . . ? C205 C206 C201 123.2(5) . . ? C302 C301 C306 114.2(5) . . ? C302 C301 B 124.1(5) . . ? C306 C301 B 121.7(4) . . ? C301 C302 C303 123.0(5) . . ? C304 C303 C302 120.6(5) . . ? C303 C304 C305 119.3(5) . . ? C304 C305 C306 119.8(6) . . ? C305 C306 C301 123.1(5) . . ? C402 C401 C406 114.6(5) . . ? C402 C401 B 123.9(5) . . ? C406 C401 B 121.5(5) . . ? C401 C402 C403 122.1(6) . . ? C404 C403 C402 120.5(6) . . ? C403 C404 C405 119.5(6) . . ? C404 C405 C406 119.8(6) . . ? C405 C406 C401 123.6(6) . . ? #===END