# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Miss Dan Yuan' _publ_contact_author_email chmhhv@nus.edu.sg loop_ _publ_author_name 'Dan Yuan' 'Han Vinh Huynh' data_8583a _database_code_depnum_ccdc_archive 'CCDC 824213' #TrackingRef '- ReCrystal.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H40 Br2 N4 O Pd2 S2' _chemical_formula_weight 921.41 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.718(2) _cell_length_b 12.4490(18) _cell_length_c 15.964(2) _cell_angle_alpha 90.00 _cell_angle_beta 103.858(3) _cell_angle_gamma 90.00 _cell_volume 3418.7(8) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4391 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 27.09 _exptl_crystal_description PLATE _exptl_crystal_colour YELLOW _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.790 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1824 _exptl_absorpt_coefficient_mu 3.542 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3969 _exptl_absorpt_correction_T_max 0.7648 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23754 _diffrn_reflns_av_R_equivalents 0.0483 _diffrn_reflns_av_sigmaI/netI 0.0551 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.18 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7836 _reflns_number_gt 6263 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0570P)^2^+5.4351P] 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 7836 _refine_ls_number_parameters 387 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0596 _refine_ls_R_factor_gt 0.0445 _refine_ls_wR_factor_ref 0.1159 _refine_ls_wR_factor_gt 0.1082 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.67261(2) 0.38435(3) 0.47678(2) 0.01361(10) Uani 1 1 d . . . Pd2 Pd 0.77734(2) 0.57256(3) 0.55641(2) 0.01435(10) Uani 1 1 d . . . Br1 Br 0.60717(3) 0.37195(5) 0.32361(3) 0.02764(14) Uani 1 1 d . . . Br2 Br 0.73859(3) 0.70597(5) 0.64945(4) 0.03262(15) Uani 1 1 d . . . S1 S 0.73098(7) 0.42091(10) 0.61793(7) 0.0178(2) Uani 1 1 d . . . S2 S 0.79460(7) 0.44488(9) 0.45905(7) 0.0158(2) Uani 1 1 d . . . N1 N 0.5379(2) 0.2429(3) 0.4973(3) 0.0183(8) Uani 1 1 d . . . N2 N 0.5434(2) 0.3945(3) 0.5631(3) 0.0186(8) Uani 1 1 d . . . N3 N 0.8815(2) 0.7539(3) 0.5243(2) 0.0165(8) Uani 1 1 d . . . N4 N 0.8060(2) 0.6940(3) 0.4081(2) 0.0160(8) Uani 1 1 d . . . C1 C 0.5789(3) 0.3357(4) 0.5131(3) 0.0153(9) Uani 1 1 d . . . C2 C 0.4769(3) 0.2445(4) 0.5375(3) 0.0243(11) Uani 1 1 d . . . H2 H 0.4397 0.1891 0.5362 0.029 Uiso 1 1 calc R . . C3 C 0.4802(3) 0.3394(4) 0.5789(3) 0.0251(11) Uani 1 1 d . . . H3 H 0.4459 0.3638 0.6124 0.030 Uiso 1 1 calc R . . C4 C 0.5645(3) 0.1480(4) 0.4614(3) 0.0193(10) Uani 1 1 d . . . C5 C 0.5249(3) 0.1110(4) 0.3802(3) 0.0187(10) Uani 1 1 d . . . C6 C 0.5538(3) 0.0193(4) 0.3480(3) 0.0234(11) Uani 1 1 d . . . H6 H 0.5282 -0.0072 0.2927 0.028 Uiso 1 1 calc R . . C7 C 0.6189(3) -0.0338(4) 0.3947(3) 0.0223(11) Uani 1 1 d . . . C8 C 0.6544(3) 0.0029(4) 0.4773(3) 0.0241(11) Uani 1 1 d . . . H8 H 0.6978 -0.0351 0.5105 0.029 Uiso 1 1 calc R . . C9 C 0.6284(3) 0.0924(4) 0.5119(3) 0.0219(11) Uani 1 1 d . . . C10 C 0.4539(3) 0.1672(5) 0.3288(4) 0.0314(13) Uani 1 1 d . . . H10A H 0.4150 0.1720 0.3632 0.047 Uiso 1 1 calc R . . H10B H 0.4324 0.1267 0.2759 0.047 Uiso 1 1 calc R . . H10C H 0.4680 0.2396 0.3139 0.047 Uiso 1 1 calc R . . C11 C 0.6507(4) -0.1320(4) 0.3594(4) 0.0303(13) Uani 1 1 d . . . H11A H 0.6950 -0.1112 0.3361 0.045 Uiso 1 1 calc R . . H11B H 0.6101 -0.1638 0.3135 0.045 Uiso 1 1 calc R . . H11C H 0.6677 -0.1845 0.4058 0.045 Uiso 1 1 calc R . . C12 C 0.6656(4) 0.1265(5) 0.6032(3) 0.0347(14) Uani 1 1 d . . . H12A H 0.6993 0.0687 0.6328 0.052 Uiso 1 1 calc R . . H12B H 0.6251 0.1415 0.6339 0.052 Uiso 1 1 calc R . . H12C H 0.6967 0.1914 0.6022 0.052 Uiso 1 1 calc R . . C13 C 0.5787(3) 0.4904(4) 0.6090(3) 0.0216(10) Uani 1 1 d . . . H13A H 0.5430 0.5223 0.6412 0.026 Uiso 1 1 calc R . . H13B H 0.5882 0.5443 0.5671 0.026 Uiso 1 1 calc R . . C14 C 0.6548(3) 0.4607(4) 0.6710(3) 0.0210(10) Uani 1 1 d . . . H14A H 0.6453 0.4007 0.7079 0.025 Uiso 1 1 calc R . . H14B H 0.6733 0.5229 0.7089 0.025 Uiso 1 1 calc R . . C15 C 0.8239(3) 0.6814(4) 0.4942(3) 0.0160(9) Uani 1 1 d . . . C16 C 0.8992(3) 0.8104(4) 0.4557(3) 0.0209(10) Uani 1 1 d . . . H16 H 0.9372 0.8653 0.4596 0.025 Uiso 1 1 calc R . . C17 C 0.8520(3) 0.7720(4) 0.3829(3) 0.0209(10) Uani 1 1 d . . . H17 H 0.8505 0.7940 0.3256 0.025 Uiso 1 1 calc R . . C18 C 0.9276(3) 0.7597(4) 0.6117(3) 0.0173(10) Uani 1 1 d . . . C19 C 0.9187(3) 0.8448(4) 0.6645(3) 0.0214(10) Uani 1 1 d . . . C20 C 0.9649(3) 0.8464(4) 0.7478(3) 0.0220(11) Uani 1 1 d . . . H20 H 0.9592 0.9039 0.7849 0.026 Uiso 1 1 calc R . . C21 C 1.0192(3) 0.7669(4) 0.7788(3) 0.0221(11) Uani 1 1 d . . . C22 C 1.0276(3) 0.6847(4) 0.7233(3) 0.0198(10) Uani 1 1 d . . . H22 H 1.0654 0.6306 0.7436 0.024 Uiso 1 1 calc R . . C23 C 0.9829(3) 0.6781(4) 0.6390(3) 0.0176(10) Uani 1 1 d . . . C24 C 0.8619(3) 0.9342(4) 0.6312(4) 0.0292(12) Uani 1 1 d . . . H24A H 0.8826 0.9798 0.5919 0.044 Uiso 1 1 calc R . . H24B H 0.8542 0.9774 0.6798 0.044 Uiso 1 1 calc R . . H24C H 0.8121 0.9034 0.6003 0.044 Uiso 1 1 calc R . . C25 C 1.0705(3) 0.7713(5) 0.8692(3) 0.0310(13) Uani 1 1 d . . . H25A H 1.0603 0.8379 0.8973 0.047 Uiso 1 1 calc R . . H25B H 1.1252 0.7694 0.8666 0.047 Uiso 1 1 calc R . . H25C H 1.0594 0.7096 0.9023 0.047 Uiso 1 1 calc R . . C26 C 0.9945(3) 0.5903(4) 0.5795(3) 0.0232(11) Uani 1 1 d . . . H26A H 1.0437 0.5534 0.6040 0.035 Uiso 1 1 calc R . . H26B H 0.9959 0.6209 0.5234 0.035 Uiso 1 1 calc R . . H26C H 0.9515 0.5388 0.5721 0.035 Uiso 1 1 calc R . . C27 C 0.7515(3) 0.6234(4) 0.3498(3) 0.0184(10) Uani 1 1 d . . . H27A H 0.7427 0.6506 0.2900 0.022 Uiso 1 1 calc R . . H27B H 0.7010 0.6231 0.3661 0.022 Uiso 1 1 calc R . . C28 C 0.7835(3) 0.5091(4) 0.3542(3) 0.0171(10) Uani 1 1 d . . . H28A H 0.8348 0.5108 0.3397 0.021 Uiso 1 1 calc R . . H28B H 0.7483 0.4649 0.3100 0.021 Uiso 1 1 calc R . . O1S O 0.0744(3) 0.9129(4) 0.5439(3) 0.0532(13) Uani 1 1 d . . . C1S C 0.1243(4) 0.9084(5) 0.6107(4) 0.0357(14) Uani 1 1 d . . . C2S C 0.1178(4) 0.9728(5) 0.6875(4) 0.0377(14) Uani 1 1 d . . . H2S1 H 0.0697 1.0149 0.6735 0.057 Uiso 1 1 calc R . . H2S2 H 0.1625 1.0214 0.7037 0.057 Uiso 1 1 calc R . . H2S3 H 0.1171 0.9245 0.7357 0.057 Uiso 1 1 calc R . . C3S C 0.1943(5) 0.8408(7) 0.6215(6) 0.068(2) Uani 1 1 d . . . H3S1 H 0.1929 0.8022 0.5677 0.102 Uiso 1 1 calc R . . H3S2 H 0.1957 0.7890 0.6681 0.102 Uiso 1 1 calc R . . H3S3 H 0.2407 0.8862 0.6360 0.102 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 0.01312(18) 0.01685(18) 0.01153(17) -0.00047(13) 0.00429(13) -0.00073(13) Pd2 0.01331(18) 0.01783(19) 0.01193(17) -0.00192(13) 0.00305(13) -0.00069(14) Br1 0.0230(3) 0.0420(3) 0.0174(2) 0.0007(2) 0.0037(2) -0.0040(2) Br2 0.0329(3) 0.0364(3) 0.0302(3) -0.0107(2) 0.0107(2) -0.0014(2) S1 0.0179(6) 0.0228(6) 0.0131(5) -0.0001(4) 0.0042(5) -0.0014(5) S2 0.0147(6) 0.0185(6) 0.0148(5) -0.0012(4) 0.0052(4) -0.0006(4) N1 0.017(2) 0.020(2) 0.019(2) -0.0008(16) 0.0055(16) -0.0035(16) N2 0.016(2) 0.025(2) 0.0158(19) -0.0009(16) 0.0067(16) -0.0037(17) N3 0.016(2) 0.017(2) 0.0152(19) -0.0008(15) 0.0011(16) 0.0002(16) N4 0.014(2) 0.017(2) 0.0159(19) 0.0011(15) 0.0018(16) 0.0019(16) C1 0.013(2) 0.018(2) 0.015(2) 0.0011(18) 0.0037(18) 0.0024(18) C2 0.019(3) 0.029(3) 0.028(3) 0.001(2) 0.011(2) -0.007(2) C3 0.021(3) 0.032(3) 0.028(3) -0.004(2) 0.015(2) -0.004(2) C4 0.019(2) 0.019(2) 0.022(2) 0.0026(19) 0.007(2) -0.0041(19) C5 0.018(2) 0.021(2) 0.018(2) 0.0022(19) 0.006(2) -0.0020(19) C6 0.030(3) 0.023(3) 0.017(2) -0.003(2) 0.005(2) -0.001(2) C7 0.025(3) 0.021(3) 0.024(3) 0.003(2) 0.013(2) -0.001(2) C8 0.022(3) 0.020(3) 0.027(3) 0.005(2) -0.001(2) 0.003(2) C9 0.026(3) 0.021(3) 0.017(2) 0.0060(19) 0.003(2) -0.003(2) C10 0.023(3) 0.035(3) 0.030(3) -0.006(2) -0.006(2) 0.003(2) C11 0.036(3) 0.028(3) 0.031(3) 0.002(2) 0.017(3) 0.005(2) C12 0.046(4) 0.027(3) 0.023(3) 0.003(2) -0.007(3) 0.000(3) C13 0.025(3) 0.024(3) 0.020(2) -0.001(2) 0.012(2) -0.002(2) C14 0.024(3) 0.027(3) 0.014(2) -0.0054(19) 0.009(2) -0.005(2) C15 0.018(2) 0.015(2) 0.014(2) -0.0031(17) 0.0023(18) 0.0034(18) C16 0.021(3) 0.019(2) 0.021(2) 0.0033(19) 0.003(2) -0.005(2) C17 0.023(3) 0.021(3) 0.019(2) 0.0070(19) 0.003(2) -0.001(2) C18 0.015(2) 0.019(2) 0.015(2) -0.0009(18) -0.0004(18) -0.0027(19) C19 0.017(2) 0.022(3) 0.024(3) -0.003(2) 0.004(2) -0.003(2) C20 0.019(3) 0.024(3) 0.023(3) -0.009(2) 0.004(2) -0.005(2) C21 0.018(3) 0.028(3) 0.018(2) 0.002(2) -0.002(2) -0.005(2) C22 0.016(2) 0.021(3) 0.020(2) 0.0039(19) 0.0014(19) 0.0006(19) C23 0.017(2) 0.015(2) 0.022(2) 0.0012(19) 0.008(2) -0.0027(19) C24 0.028(3) 0.020(3) 0.032(3) -0.009(2) -0.006(2) 0.008(2) C25 0.030(3) 0.038(3) 0.024(3) -0.002(2) 0.004(2) -0.002(3) C26 0.019(3) 0.023(3) 0.025(3) -0.002(2) 0.001(2) 0.004(2) C27 0.019(2) 0.021(3) 0.015(2) -0.0001(18) 0.0051(19) -0.0027(19) C28 0.019(2) 0.021(2) 0.011(2) -0.0004(18) 0.0040(19) -0.0066(19) O1S 0.054(3) 0.047(3) 0.046(3) -0.004(2) -0.013(2) -0.007(2) C1S 0.034(3) 0.024(3) 0.042(3) 0.005(2) -0.004(3) -0.012(2) C2S 0.034(3) 0.036(3) 0.042(3) 0.015(3) 0.007(3) -0.007(3) C3S 0.067(6) 0.052(5) 0.075(6) -0.015(4) -0.002(5) 0.011(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 C1 1.980(5) . ? Pd1 S1 2.2887(12) . ? Pd1 S2 2.3691(12) . ? Pd1 Br1 2.4472(7) . ? Pd1 Pd2 3.0690(6) . ? Pd2 C15 1.973(5) . ? Pd2 S2 2.2944(12) . ? Pd2 S1 2.3642(13) . ? Pd2 Br2 2.4340(7) . ? S1 C14 1.826(5) . ? S2 C28 1.823(4) . ? N1 C1 1.355(6) . ? N1 C2 1.383(6) . ? N1 C4 1.442(6) . ? N2 C1 1.346(6) . ? N2 C3 1.388(6) . ? N2 C13 1.460(6) . ? N3 C15 1.361(6) . ? N3 C16 1.400(6) . ? N3 C18 1.440(6) . ? N4 C15 1.344(6) . ? N4 C17 1.388(6) . ? N4 C27 1.463(6) . ? C2 C3 1.348(7) . ? C4 C5 1.396(7) . ? C4 C9 1.404(7) . ? C5 C6 1.399(7) . ? C5 C10 1.500(7) . ? C6 C7 1.381(7) . ? C7 C8 1.396(7) . ? C7 C11 1.510(7) . ? C8 C9 1.371(7) . ? C9 C12 1.510(7) . ? C13 C14 1.515(7) . ? C16 C17 1.346(7) . ? C18 C19 1.386(7) . ? C18 C23 1.406(7) . ? C19 C20 1.384(7) . ? C19 C24 1.509(7) . ? C20 C21 1.387(7) . ? C21 C22 1.385(7) . ? C21 C25 1.510(7) . ? C22 C23 1.392(7) . ? C23 C26 1.495(7) . ? C27 C28 1.526(7) . ? O1S C1S 1.213(7) . ? C1S C3S 1.474(10) . ? C1S C2S 1.492(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pd1 S1 89.17(13) . . ? C1 Pd1 S2 170.15(13) . . ? S1 Pd1 S2 81.05(4) . . ? C1 Pd1 Br1 92.49(13) . . ? S1 Pd1 Br1 172.10(4) . . ? S2 Pd1 Br1 97.36(3) . . ? C1 Pd1 Pd2 125.34(13) . . ? S1 Pd1 Pd2 49.80(3) . . ? S2 Pd1 Pd2 47.80(3) . . ? Br1 Pd1 Pd2 123.83(2) . . ? C15 Pd2 S2 89.72(13) . . ? C15 Pd2 S1 170.37(13) . . ? S2 Pd2 S1 81.04(4) . . ? C15 Pd2 Br2 92.95(13) . . ? S2 Pd2 Br2 171.50(4) . . ? S1 Pd2 Br2 96.58(4) . . ? C15 Pd2 Pd1 126.85(13) . . ? S2 Pd2 Pd1 49.90(3) . . ? S1 Pd2 Pd1 47.68(3) . . ? Br2 Pd2 Pd1 122.88(2) . . ? C14 S1 Pd1 107.49(16) . . ? C14 S1 Pd2 110.20(17) . . ? Pd1 S1 Pd2 82.52(4) . . ? C28 S2 Pd2 108.39(16) . . ? C28 S2 Pd1 110.41(16) . . ? Pd2 S2 Pd1 82.29(4) . . ? C1 N1 C2 110.2(4) . . ? C1 N1 C4 124.1(4) . . ? C2 N1 C4 124.2(4) . . ? C1 N2 C3 110.6(4) . . ? C1 N2 C13 122.5(4) . . ? C3 N2 C13 125.5(4) . . ? C15 N3 C16 110.3(4) . . ? C15 N3 C18 125.4(4) . . ? C16 N3 C18 123.4(4) . . ? C15 N4 C17 111.5(4) . . ? C15 N4 C27 122.6(4) . . ? C17 N4 C27 125.5(4) . . ? N2 C1 N1 105.5(4) . . ? N2 C1 Pd1 123.4(3) . . ? N1 C1 Pd1 131.0(3) . . ? C3 C2 N1 107.1(4) . . ? C2 C3 N2 106.6(4) . . ? C5 C4 C9 121.8(5) . . ? C5 C4 N1 120.0(4) . . ? C9 C4 N1 118.1(4) . . ? C4 C5 C6 117.6(5) . . ? C4 C5 C10 121.5(5) . . ? C6 C5 C10 120.9(5) . . ? C7 C6 C5 121.6(5) . . ? C6 C7 C8 118.8(5) . . ? C6 C7 C11 121.6(5) . . ? C8 C7 C11 119.5(5) . . ? C9 C8 C7 121.8(5) . . ? C8 C9 C4 118.2(5) . . ? C8 C9 C12 120.3(5) . . ? C4 C9 C12 121.4(5) . . ? N2 C13 C14 109.6(4) . . ? C13 C14 S1 113.8(3) . . ? N4 C15 N3 104.9(4) . . ? N4 C15 Pd2 124.8(3) . . ? N3 C15 Pd2 130.2(3) . . ? C17 C16 N3 106.7(4) . . ? C16 C17 N4 106.6(4) . . ? C19 C18 C23 122.4(4) . . ? C19 C18 N3 120.5(4) . . ? C23 C18 N3 117.1(4) . . ? C20 C19 C18 117.9(5) . . ? C20 C19 C24 121.3(5) . . ? C18 C19 C24 120.8(4) . . ? C19 C20 C21 122.2(5) . . ? C22 C21 C20 118.0(4) . . ? C22 C21 C25 120.4(5) . . ? C20 C21 C25 121.5(5) . . ? C21 C22 C23 122.6(5) . . ? C22 C23 C18 116.8(4) . . ? C22 C23 C26 121.6(4) . . ? C18 C23 C26 121.6(4) . . ? N4 C27 C28 110.5(4) . . ? C27 C28 S2 114.1(3) . . ? O1S C1S C3S 123.0(7) . . ? O1S C1S C2S 121.0(6) . . ? C3S C1S C2S 116.0(6) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.395 _refine_diff_density_min -1.757 _refine_diff_density_rms 0.165 #==End data_8149 _database_code_depnum_ccdc_archive 'CCDC 824214' #TrackingRef '- ReCrystal.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H38 Br2 Cl4 N4 Pd2 S2' _chemical_formula_weight 1033.18 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 16.9381(14) _cell_length_b 8.9830(7) _cell_length_c 24.9425(19) _cell_angle_alpha 90.00 _cell_angle_beta 91.468(2) _cell_angle_gamma 90.00 _cell_volume 3793.9(5) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 1845 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 21.26 _exptl_crystal_description PLATE _exptl_crystal_colour YELLOW _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.809 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2032 _exptl_absorpt_coefficient_mu 3.473 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6420 _exptl_absorpt_correction_T_max 0.8187 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20763 _diffrn_reflns_av_R_equivalents 0.1048 _diffrn_reflns_av_sigmaI/netI 0.1125 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6686 _reflns_number_gt 4137 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. There are two disordered dichloromethane solvents. One was disordered with one of the Cl atom occupied two different positions with occupancy ratio=75:25. The other dichloromethane was disordered with the whole molecule occupied two differnt positions with occupancy ratio=75:25. Restraints in bond lengths and thermal parameters were applied to the disordered solvents so that the refinement became convergent the structure remained reasonable. ; _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^)+(0.0530P)^2^+13.6108P] 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 6686 _refine_ls_number_parameters 433 _refine_ls_number_restraints 35 _refine_ls_R_factor_all 0.1321 _refine_ls_R_factor_gt 0.0776 _refine_ls_wR_factor_ref 0.1591 _refine_ls_wR_factor_gt 0.1432 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.095 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.69246(5) 0.64183(9) 0.89657(3) 0.0271(2) Uani 1 1 d . . . Pd2 Pd 0.55354(5) 0.65818(10) 0.81505(3) 0.0309(2) Uani 1 1 d . . . Br1 Br 0.67843(7) 0.60100(15) 0.99284(5) 0.0448(4) Uani 1 1 d . . . Br2 Br 0.52906(9) 0.52224(19) 0.73115(5) 0.0637(5) Uani 1 1 d . . . S1 S 0.69240(17) 0.6797(3) 0.80548(11) 0.0363(7) Uani 1 1 d . . . S2 S 0.58452(17) 0.8048(3) 0.88643(11) 0.0318(7) Uani 1 1 d . . . N1 N 0.8546(5) 0.5026(12) 0.9186(4) 0.042(3) Uani 1 1 d . . . N2 N 0.7913(7) 0.3985(12) 0.8547(4) 0.053(3) Uani 1 1 d . . . N3 N 0.3108(5) 0.6032(10) 0.8396(4) 0.033(2) Uani 1 1 d . . . N4 N 0.4163(5) 0.6304(10) 0.8885(3) 0.035(2) Uani 1 1 d . . . C1 C 0.7858(7) 0.5084(13) 0.8920(4) 0.037(3) Uani 1 1 d . . . C2 C 0.9003(8) 0.3889(17) 0.8994(6) 0.060(4) Uani 1 1 d . . . H2 H 0.9507 0.3619 0.9127 0.072 Uiso 1 1 calc R . . C3 C 0.8616(8) 0.3239(16) 0.8591(5) 0.054(4) Uani 1 1 d . . . H3 H 0.8787 0.2440 0.8380 0.065 Uiso 1 1 calc R . . C4 C 0.8775(6) 0.6073(16) 0.9607(5) 0.046(3) Uani 1 1 d . . . C5 C 0.8931(7) 0.7521(19) 0.9470(5) 0.056(4) Uani 1 1 d . . . C6 C 0.9119(7) 0.8523(18) 0.9872(6) 0.063(4) Uani 1 1 d . . . H6 H 0.9239 0.9512 0.9782 0.076 Uiso 1 1 calc R . . C7 C 0.9135(7) 0.8101(18) 1.0409(5) 0.053(4) Uani 1 1 d . . . C8 C 0.9016(7) 0.665(2) 1.0525(5) 0.061(4) Uani 1 1 d . . . H8 H 0.9058 0.6341 1.0885 0.073 Uiso 1 1 calc R . . C9 C 0.8835(7) 0.5581(17) 1.0138(5) 0.048(4) Uani 1 1 d . . . C10 C 0.8949(9) 0.7979(17) 0.8888(5) 0.069(4) Uani 1 1 d . . . H10A H 0.8415 0.7990 0.8738 0.103 Uiso 1 1 calc R . . H10B H 0.9265 0.7275 0.8692 0.103 Uiso 1 1 calc R . . H10C H 0.9177 0.8965 0.8861 0.103 Uiso 1 1 calc R . . C11 C 0.9286(8) 0.924(2) 1.0845(6) 0.078(5) Uani 1 1 d . . . H11A H 0.9071 0.8883 1.1179 0.116 Uiso 1 1 calc R . . H11B H 0.9034 1.0172 1.0745 0.116 Uiso 1 1 calc R . . H11C H 0.9850 0.9395 1.0893 0.116 Uiso 1 1 calc R . . C12 C 0.8676(9) 0.3980(18) 1.0295(6) 0.074(5) Uani 1 1 d . . . H12A H 0.8193 0.3639 1.0116 0.110 Uiso 1 1 calc R . . H12B H 0.8619 0.3918 1.0680 0.110 Uiso 1 1 calc R . . H12C H 0.9113 0.3358 1.0189 0.110 Uiso 1 1 calc R . . C13 C 0.7300(7) 0.3788(14) 0.8119(5) 0.049(4) Uani 1 1 d . . . H13A H 0.6782 0.3685 0.8280 0.059 Uiso 1 1 calc R . . H13B H 0.7407 0.2875 0.7918 0.059 Uiso 1 1 calc R . . C14 C 0.7289(7) 0.5074(14) 0.7747(5) 0.047(3) Uani 1 1 d . . . H14A H 0.6952 0.4833 0.7434 0.056 Uiso 1 1 calc R . . H14B H 0.7825 0.5246 0.7622 0.056 Uiso 1 1 calc R . . C15 C 0.4412(6) 0.6359(13) 0.8354(4) 0.034(3) Uani 1 1 d . . . C16 C 0.3739(7) 0.6244(12) 0.8069(4) 0.035(3) Uani 1 1 d . . . H16 H 0.3701 0.6299 0.7693 0.042 Uiso 1 1 calc R . . C17 C 0.3395(6) 0.6093(13) 0.8896(4) 0.034(3) Uani 1 1 d . . . H17 H 0.3097 0.6000 0.9207 0.041 Uiso 1 1 calc R . . C18 C 0.2276(6) 0.5852(13) 0.8231(4) 0.035(3) Uani 1 1 d . . . C19 C 0.1830(7) 0.7122(14) 0.8104(4) 0.040(3) Uani 1 1 d . . . C20 C 0.1082(7) 0.6914(14) 0.7922(4) 0.040(3) Uani 1 1 d . . . H20 H 0.0776 0.7744 0.7819 0.048 Uiso 1 1 calc R . . C21 C 0.0750(8) 0.5479(16) 0.7882(5) 0.049(3) Uani 1 1 d . . . C22 C 0.1197(7) 0.4283(14) 0.8014(4) 0.038(3) Uani 1 1 d . . . H22 H 0.0973 0.3328 0.7984 0.045 Uiso 1 1 calc R . . C23 C 0.1966(7) 0.4415(14) 0.8191(4) 0.037(3) Uani 1 1 d . . . C24 C 0.2194(8) 0.8645(14) 0.8149(5) 0.055(4) Uani 1 1 d . . . H24A H 0.1791 0.9394 0.8081 0.083 Uiso 1 1 calc R . . H24B H 0.2605 0.8744 0.7887 0.083 Uiso 1 1 calc R . . H24C H 0.2420 0.8781 0.8506 0.083 Uiso 1 1 calc R . . C25 C -0.0107(7) 0.5280(18) 0.7674(5) 0.064(4) Uani 1 1 d . . . H25A H -0.0107 0.4922 0.7307 0.096 Uiso 1 1 calc R . . H25B H -0.0380 0.6229 0.7686 0.096 Uiso 1 1 calc R . . H25C H -0.0374 0.4565 0.7897 0.096 Uiso 1 1 calc R . . C26 C 0.2466(8) 0.3073(15) 0.8352(5) 0.058(4) Uani 1 1 d . . . H26A H 0.2966 0.3115 0.8172 0.087 Uiso 1 1 calc R . . H26B H 0.2189 0.2167 0.8251 0.087 Uiso 1 1 calc R . . H26C H 0.2562 0.3082 0.8738 0.087 Uiso 1 1 calc R . . C27 C 0.4696(7) 0.6369(14) 0.9357(4) 0.039(3) Uani 1 1 d . . . H27A H 0.5079 0.5554 0.9340 0.047 Uiso 1 1 calc R . . H27B H 0.4390 0.6235 0.9682 0.047 Uiso 1 1 calc R . . C28 C 0.5126(7) 0.7817(14) 0.9390(4) 0.042(3) Uani 1 1 d . . . H28A H 0.5400 0.7888 0.9740 0.051 Uiso 1 1 calc R . . H28B H 0.4742 0.8631 0.9365 0.051 Uiso 1 1 calc R . . C1S C 0.7117(10) 0.0018(15) 0.9774(5) 0.087(6) Uani 1 1 d D . . H1S1 H 0.7320 -0.1004 0.9777 0.104 Uiso 1 1 calc R A 1 H1S2 H 0.6572 -0.0019 0.9632 0.104 Uiso 1 1 calc R A 1 Cl1A Cl 0.7095(4) 0.0632(7) 1.0422(2) 0.130(2) Uani 1 1 d D B . Cl1B Cl 0.7660(6) 0.1029(9) 0.9346(3) 0.128(3) Uani 0.75 1 d PD B 1 Cl1C Cl 0.695(3) 0.170(3) 0.9409(9) 0.23(2) Uani 0.25 1 d PD B 2 C2S C 0.5094(13) 0.247(3) 0.8592(8) 0.117(9) Uani 0.75 1 d PDU C 3 H2S1 H 0.4916 0.3453 0.8468 0.140 Uiso 0.75 1 calc PR C 3 H2S2 H 0.5359 0.1976 0.8296 0.140 Uiso 0.75 1 calc PR C 3 Cl2A Cl 0.4298(6) 0.1432(17) 0.8782(6) 0.235(6) Uani 0.75 1 d PDU C 3 Cl2B Cl 0.5764(6) 0.2678(12) 0.9145(4) 0.153(4) Uani 0.75 1 d PDU C 3 C3S C 0.437(2) 0.239(3) 0.877(2) 0.047(15) Uani 0.25 1 d PDU D 4 H3S1 H 0.4372 0.3112 0.8474 0.057 Uiso 0.25 1 calc PR D 4 H3S2 H 0.3991 0.2734 0.9033 0.057 Uiso 0.25 1 calc PR D 4 Cl3A Cl 0.5306(10) 0.2255(19) 0.9064(9) 0.069(4) Uani 0.25 1 d PD D 4 Cl3B Cl 0.4080(11) 0.0617(18) 0.8521(8) 0.069(4) Uani 0.25 1 d PD D 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 0.0314(5) 0.0301(5) 0.0199(5) -0.0004(4) 0.0031(3) -0.0005(4) Pd2 0.0371(5) 0.0368(5) 0.0188(5) -0.0011(4) 0.0021(4) -0.0049(4) Br1 0.0490(8) 0.0550(8) 0.0307(7) 0.0081(6) 0.0050(6) 0.0066(6) Br2 0.0602(9) 0.0963(12) 0.0353(8) -0.0262(8) 0.0121(7) -0.0285(9) S1 0.0395(17) 0.0468(19) 0.0228(16) 0.0028(13) 0.0054(12) -0.0027(14) S2 0.0395(17) 0.0288(16) 0.0270(16) -0.0032(12) -0.0022(13) 0.0061(13) N1 0.033(6) 0.065(8) 0.030(6) 0.002(5) 0.010(5) 0.008(5) N2 0.067(8) 0.057(7) 0.037(7) -0.003(5) 0.023(6) 0.001(6) N3 0.033(5) 0.041(6) 0.024(6) 0.001(4) -0.008(4) 0.006(4) N4 0.043(6) 0.040(6) 0.022(5) 0.000(4) -0.001(4) 0.000(5) C1 0.038(7) 0.045(8) 0.028(7) 0.002(6) 0.008(5) 0.010(6) C2 0.038(8) 0.097(12) 0.045(9) 0.013(8) 0.006(7) 0.021(8) C3 0.049(8) 0.071(10) 0.043(9) -0.001(7) 0.016(7) 0.034(8) C4 0.021(6) 0.080(11) 0.037(8) -0.001(7) 0.002(5) 0.010(7) C5 0.041(8) 0.102(13) 0.025(8) 0.002(8) -0.008(6) -0.026(8) C6 0.046(8) 0.088(12) 0.055(10) 0.000(9) 0.007(7) -0.025(8) C7 0.033(7) 0.087(12) 0.040(9) -0.006(8) -0.008(6) -0.009(7) C8 0.032(7) 0.116(14) 0.035(8) 0.004(9) 0.000(6) 0.000(9) C9 0.027(7) 0.085(11) 0.033(8) 0.001(7) 0.006(6) 0.002(7) C10 0.068(10) 0.086(12) 0.053(10) 0.019(8) 0.001(8) -0.033(9) C11 0.053(9) 0.129(15) 0.052(10) -0.026(9) 0.010(7) -0.023(10) C12 0.067(10) 0.097(13) 0.058(10) 0.016(9) 0.025(8) 0.033(9) C13 0.053(8) 0.061(9) 0.033(8) -0.029(7) 0.001(6) 0.015(7) C14 0.053(8) 0.065(9) 0.022(7) 0.000(6) 0.002(6) 0.011(7) C15 0.033(6) 0.045(7) 0.025(7) -0.006(5) 0.001(5) -0.008(6) C16 0.045(7) 0.041(7) 0.020(6) 0.001(5) 0.006(5) 0.002(6) C17 0.031(7) 0.049(8) 0.023(7) 0.001(5) 0.004(5) 0.005(6) C18 0.033(7) 0.045(7) 0.027(7) -0.004(5) 0.003(5) -0.003(6) C19 0.048(8) 0.055(8) 0.018(6) -0.001(6) 0.006(5) 0.007(7) C20 0.041(7) 0.048(8) 0.031(7) 0.009(6) -0.011(6) 0.011(6) C21 0.050(8) 0.072(10) 0.025(7) 0.001(6) 0.006(6) 0.001(8) C22 0.045(8) 0.044(8) 0.024(7) -0.009(5) 0.010(6) -0.009(6) C23 0.034(7) 0.047(8) 0.031(7) -0.001(6) 0.009(5) 0.008(6) C24 0.080(10) 0.043(8) 0.042(8) 0.005(6) -0.011(7) 0.002(7) C25 0.049(9) 0.099(12) 0.044(9) -0.003(8) -0.013(7) -0.012(8) C26 0.052(9) 0.064(10) 0.056(10) 0.001(7) -0.016(7) -0.005(7) C27 0.040(7) 0.060(8) 0.018(6) -0.004(6) -0.001(5) 0.005(6) C28 0.045(8) 0.053(8) 0.029(7) -0.016(6) -0.001(6) 0.003(6) C1S 0.138(16) 0.068(11) 0.053(11) -0.010(8) -0.015(10) -0.035(11) Cl1A 0.156(5) 0.145(5) 0.089(4) -0.041(3) 0.016(4) 0.009(4) Cl1B 0.188(9) 0.081(6) 0.115(6) 0.030(5) 0.017(6) 0.001(5) Cl1C 0.42(7) 0.066(19) 0.21(4) 0.08(2) -0.13(4) -0.05(3) C2S 0.160(17) 0.131(16) 0.060(13) -0.011(12) 0.022(13) -0.084(14) Cl2A 0.140(9) 0.293(15) 0.275(14) 0.156(12) 0.045(9) 0.095(10) Cl2B 0.191(10) 0.139(8) 0.129(8) -0.029(6) 0.024(7) 0.000(7) C3S 0.045(17) 0.045(17) 0.052(18) 0.000(10) -0.004(10) 0.011(10) Cl3A 0.079(9) 0.050(7) 0.077(9) -0.006(6) -0.032(7) 0.024(6) Cl3B 0.079(9) 0.050(7) 0.077(9) -0.006(6) -0.032(7) 0.024(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C1 1.990(11) . ? Pd1 S1 2.297(3) . ? Pd1 S2 2.351(3) . ? Pd1 Br1 2.4466(14) . ? Pd1 Pd2 3.0738(12) . ? Pd2 C15 1.992(11) . ? Pd2 S2 2.266(3) . ? Pd2 S1 2.378(3) . ? Pd2 Br2 2.4490(15) . ? S1 C14 1.841(13) . ? S2 C28 1.824(12) . ? N1 C1 1.328(14) . ? N1 C2 1.376(16) . ? N1 C4 1.453(16) . ? N2 C1 1.361(15) . ? N2 C3 1.369(15) . ? N2 C13 1.481(15) . ? N3 C17 1.326(13) . ? N3 C16 1.374(13) . ? N3 C18 1.467(13) . ? N4 C17 1.317(13) . ? N4 C15 1.402(13) . ? N4 C27 1.466(13) . ? C2 C3 1.322(18) . ? C4 C5 1.373(19) . ? C4 C9 1.397(17) . ? C5 C6 1.380(19) . ? C5 C10 1.508(17) . ? C6 C7 1.392(18) . ? C7 C8 1.355(19) . ? C7 C11 1.510(19) . ? C8 C9 1.387(19) . ? C9 C12 1.517(19) . ? C13 C14 1.481(17) . ? C15 C16 1.331(14) . ? C18 C23 1.397(16) . ? C18 C19 1.399(16) . ? C19 C20 1.349(16) . ? C19 C24 1.504(17) . ? C20 C21 1.408(17) . ? C21 C22 1.351(17) . ? C21 C25 1.540(17) . ? C22 C23 1.370(15) . ? C23 C26 1.522(16) . ? C27 C28 1.492(16) . ? C1S Cl1B 1.693(13) . ? C1S Cl1A 1.709(12) . ? C1S Cl1C 1.783(16) . ? C2S Cl2A 1.717(16) . ? C2S Cl2B 1.773(16) . ? C3S Cl3A 1.74(2) . ? C3S Cl3B 1.77(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pd1 S1 90.7(3) . . ? C1 Pd1 S2 170.4(3) . . ? S1 Pd1 S2 79.67(10) . . ? C1 Pd1 Br1 93.6(3) . . ? S1 Pd1 Br1 174.40(9) . . ? S2 Pd1 Br1 95.98(8) . . ? C1 Pd1 Pd2 125.9(3) . . ? S1 Pd1 Pd2 50.04(8) . . ? S2 Pd1 Pd2 47.08(7) . . ? Br1 Pd1 Pd2 124.36(5) . . ? C15 Pd2 S2 93.5(3) . . ? C15 Pd2 S1 170.9(3) . . ? S2 Pd2 S1 79.73(10) . . ? C15 Pd2 Br2 91.5(3) . . ? S2 Pd2 Br2 172.82(9) . . ? S1 Pd2 Br2 95.80(8) . . ? C15 Pd2 Pd1 123.2(3) . . ? S2 Pd2 Pd1 49.45(7) . . ? S1 Pd2 Pd1 47.77(7) . . ? Br2 Pd2 Pd1 130.65(5) . . ? C14 S1 Pd1 107.2(4) . . ? C14 S1 Pd2 108.5(4) . . ? Pd1 S1 Pd2 82.19(9) . . ? C28 S2 Pd2 110.7(4) . . ? C28 S2 Pd1 112.5(4) . . ? Pd2 S2 Pd1 83.47(10) . . ? C1 N1 C2 110.4(11) . . ? C1 N1 C4 123.4(10) . . ? C2 N1 C4 126.2(10) . . ? C1 N2 C3 112.0(11) . . ? C1 N2 C13 121.4(11) . . ? C3 N2 C13 126.2(11) . . ? C17 N3 C16 106.3(9) . . ? C17 N3 C18 126.4(9) . . ? C16 N3 C18 127.2(9) . . ? C17 N4 C15 110.2(9) . . ? C17 N4 C27 125.4(9) . . ? C15 N4 C27 124.3(9) . . ? N1 C1 N2 103.8(10) . . ? N1 C1 Pd1 133.1(9) . . ? N2 C1 Pd1 123.0(9) . . ? C3 C2 N1 108.7(11) . . ? C2 C3 N2 104.9(12) . . ? C5 C4 C9 121.7(13) . . ? C5 C4 N1 118.9(11) . . ? C9 C4 N1 119.4(13) . . ? C4 C5 C6 118.6(13) . . ? C4 C5 C10 120.4(13) . . ? C6 C5 C10 120.8(14) . . ? C5 C6 C7 121.4(15) . . ? C8 C7 C6 117.9(13) . . ? C8 C7 C11 121.6(14) . . ? C6 C7 C11 120.5(15) . . ? C7 C8 C9 123.2(13) . . ? C8 C9 C4 116.8(14) . . ? C8 C9 C12 120.7(13) . . ? C4 C9 C12 122.4(13) . . ? N2 C13 C14 110.9(11) . . ? C13 C14 S1 113.2(8) . . ? C16 C15 N4 103.2(9) . . ? C16 C15 Pd2 133.0(9) . . ? N4 C15 Pd2 123.8(8) . . ? C15 C16 N3 111.2(10) . . ? N4 C17 N3 109.0(9) . . ? C23 C18 C19 122.5(11) . . ? C23 C18 N3 118.6(10) . . ? C19 C18 N3 118.9(10) . . ? C20 C19 C18 117.4(12) . . ? C20 C19 C24 122.0(12) . . ? C18 C19 C24 120.5(11) . . ? C19 C20 C21 121.4(11) . . ? C22 C21 C20 119.4(12) . . ? C22 C21 C25 120.5(13) . . ? C20 C21 C25 120.1(12) . . ? C21 C22 C23 122.1(12) . . ? C22 C23 C18 117.2(11) . . ? C22 C23 C26 122.3(11) . . ? C18 C23 C26 120.5(11) . . ? N4 C27 C28 111.6(10) . . ? C27 C28 S2 113.2(8) . . ? Cl1B C1S Cl1A 116.7(8) . . ? Cl1B C1S Cl1C 45.9(16) . . ? Cl1A C1S Cl1C 101.7(11) . . ? Cl2A C2S Cl2B 109.5(11) . . ? Cl3A C3S Cl3B 109.0(15) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.011 _refine_diff_density_min -1.009 _refine_diff_density_rms 0.158 #==End data_a783 _database_code_depnum_ccdc_archive 'CCDC 824215' #TrackingRef '- ReCrystal.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C76 H98 B2 F8 N8 Pd4 S6' _chemical_formula_weight 1915.20 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' F F 0.0171 0.0103 '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' _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 15.3906(4) _cell_length_b 24.2174(6) _cell_length_c 24.4807(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.7140(10) _cell_angle_gamma 90.00 _cell_volume 9123.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 7741 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 23.60 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'Not Measured' _exptl_crystal_density_diffrn 1.394 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3888 _exptl_absorpt_coefficient_mu 0.971 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7864 _exptl_absorpt_correction_T_max 0.8295 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 53165 _diffrn_reflns_av_R_equivalents 0.0546 _diffrn_reflns_av_sigmaI/netI 0.0594 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 25.00 _reflns_number_total 16052 _reflns_number_gt 12202 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. F atoms of the two anions were disordered into two positions with occupancy ratio = 62:38. Restraints in bond lengths and thermal parameters were applied to the two anions and solvents so that the refinement became convergent and the structure remained reasonable. The electron density peak heights at these two toluene sites were low and diffused. Full occupation with anisotropic refinement gave poor results. They were therefore kept anisotropic. There is still a void of about 60A3, however, the residual peaks were so low that it was not possible to fit any small solvent in there." ; _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^)+(0.0939P)^2^+35.0186P] 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 16052 _refine_ls_number_parameters 936 _refine_ls_number_restraints 245 _refine_ls_R_factor_all 0.0859 _refine_ls_R_factor_gt 0.0651 _refine_ls_wR_factor_ref 0.1873 _refine_ls_wR_factor_gt 0.1743 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.90575(3) 0.78003(2) 0.26390(2) 0.02817(15) Uani 1 1 d . . . Pd2 Pd 1.06436(3) 0.77246(2) 0.18718(2) 0.02685(15) Uani 1 1 d . . . Pd3 Pd 0.92390(3) 0.74080(2) 0.06758(2) 0.02759(15) Uani 1 1 d . . . Pd4 Pd 0.76493(3) 0.75058(2) 0.14370(2) 0.02865(15) Uani 1 1 d . . . S1 S 0.76148(11) 0.77007(8) 0.23700(7) 0.0339(4) Uani 1 1 d . . . S2 S 1.05345(11) 0.79586(8) 0.27931(7) 0.0330(4) Uani 1 1 d . . . S3 S 1.06826(11) 0.75332(8) 0.09383(7) 0.0333(4) Uani 1 1 d . . . S4 S 0.77644(11) 0.72524(8) 0.05220(7) 0.0339(4) Uani 1 1 d . . . S5 S 0.95528(11) 0.70677(7) 0.20663(7) 0.0306(4) Uani 1 1 d . . . S6 S 0.87372(11) 0.81607(7) 0.12218(7) 0.0318(4) Uani 1 1 d . . . N1 N 0.8084(4) 0.8736(3) 0.3136(3) 0.0436(16) Uani 1 1 d . . . N2 N 0.8752(4) 0.8271(3) 0.3763(3) 0.0429(16) Uani 1 1 d . . . N3 N 1.1363(4) 0.8849(2) 0.1942(3) 0.0385(15) Uani 1 1 d . . . N4 N 1.2291(4) 0.8339(2) 0.1532(2) 0.0322(13) Uani 1 1 d . . . N5 N 1.0197(4) 0.6432(3) 0.0265(2) 0.0393(15) Uani 1 1 d . . . N6 N 0.9519(4) 0.6822(3) -0.0407(2) 0.0405(15) Uani 1 1 d . . . N7 N 0.6982(4) 0.6370(3) 0.1405(3) 0.0425(16) Uani 1 1 d . . . N8 N 0.6026(4) 0.6875(3) 0.1803(2) 0.0384(15) Uani 1 1 d . . . C1 C 0.8642(4) 0.8318(3) 0.3209(3) 0.0350(16) Uani 1 1 d . . . C2 C 0.7830(6) 0.8951(4) 0.3627(4) 0.063(3) Uani 1 1 d . . . H2 H 0.7439 0.9244 0.3678 0.075 Uiso 1 1 calc R . . C3 C 0.8243(6) 0.8667(4) 0.4014(4) 0.070(3) Uani 1 1 d . . . H3 H 0.8198 0.8725 0.4393 0.084 Uiso 1 1 calc R . . C4 C 0.7713(5) 0.8848(3) 0.2593(3) 0.050(2) Uani 1 1 d . . . H4A H 0.8182 0.8881 0.2328 0.060 Uiso 1 1 calc R . . H4B H 0.7396 0.9198 0.2600 0.060 Uiso 1 1 calc R . . C5 C 0.7112(5) 0.8395(3) 0.2422(3) 0.044(2) Uani 1 1 d . . . H5A H 0.6857 0.8491 0.2066 0.053 Uiso 1 1 calc R . . H5B H 0.6637 0.8376 0.2685 0.053 Uiso 1 1 calc R . . C6 C 0.9236(5) 0.7837(4) 0.4030(3) 0.051(2) Uani 1 1 d . . . C7 C 1.0038(6) 0.7964(5) 0.4268(3) 0.057(2) Uani 1 1 d . . . C8 C 1.0505(7) 0.7513(6) 0.4497(4) 0.078(4) Uani 1 1 d . . . H8 H 1.1044 0.7586 0.4667 0.093 Uiso 1 1 calc R . . C9 C 1.0225(9) 0.6991(6) 0.4484(4) 0.084(4) Uani 1 1 d . . . C10 C 0.9402(9) 0.6901(5) 0.4265(4) 0.078(3) Uani 1 1 d . . . H10 H 0.9180 0.6540 0.4272 0.094 Uiso 1 1 calc R . . C11 C 0.8895(6) 0.7305(4) 0.4039(3) 0.052(2) Uani 1 1 d . . . C12 C 1.0408(6) 0.8535(5) 0.4279(4) 0.077(3) Uani 1 1 d . . . H12A H 0.9939 0.8803 0.4258 0.115 Uiso 1 1 calc R . . H12B H 1.0788 0.8585 0.3969 0.115 Uiso 1 1 calc R . . H12C H 1.0737 0.8589 0.4615 0.115 Uiso 1 1 calc R . . C13 C 1.0768(10) 0.6524(6) 0.4716(5) 0.127(6) Uani 1 1 d . . . H13A H 1.1309 0.6671 0.4863 0.190 Uiso 1 1 calc R . . H13B H 1.0892 0.6260 0.4430 0.190 Uiso 1 1 calc R . . H13C H 1.0451 0.6342 0.5005 0.190 Uiso 1 1 calc R . . C14 C 0.7981(7) 0.7194(4) 0.3836(4) 0.067(3) Uani 1 1 d . . . H14A H 0.7796 0.6833 0.3962 0.101 Uiso 1 1 calc R . . H14B H 0.7968 0.7203 0.3440 0.101 Uiso 1 1 calc R . . H14C H 0.7594 0.7475 0.3977 0.101 Uiso 1 1 calc R . . C15 C 1.1498(4) 0.8331(3) 0.1761(3) 0.0327(16) Uani 1 1 d . . . C16 C 1.2073(5) 0.9185(3) 0.1828(4) 0.047(2) Uani 1 1 d . . . H16 H 1.2133 0.9562 0.1911 0.056 Uiso 1 1 calc R . . C17 C 1.2645(5) 0.8868(3) 0.1578(3) 0.0438(19) Uani 1 1 d . . . H17 H 1.3193 0.8979 0.1454 0.053 Uiso 1 1 calc R . . C18 C 1.0600(5) 0.9004(3) 0.2274(4) 0.045(2) Uani 1 1 d . . . H18A H 1.0063 0.8900 0.2080 0.054 Uiso 1 1 calc R . . H18B H 1.0593 0.9404 0.2331 0.054 Uiso 1 1 calc R . . C19 C 1.0652(5) 0.8710(3) 0.2818(3) 0.046(2) Uani 1 1 d . . . H19A H 1.0199 0.8858 0.3054 0.055 Uiso 1 1 calc R . . H19B H 1.1214 0.8796 0.2990 0.055 Uiso 1 1 calc R . . C20 C 1.2729(4) 0.7872(3) 0.1300(3) 0.0324(16) Uani 1 1 d . . . C21 C 1.2995(4) 0.7445(3) 0.1644(3) 0.0337(16) Uani 1 1 d . . . C22 C 1.3408(5) 0.6993(3) 0.1411(3) 0.0381(17) Uani 1 1 d . . . H22 H 1.3584 0.6697 0.1635 0.046 Uiso 1 1 calc R . . C23 C 1.3565(5) 0.6972(3) 0.0853(3) 0.0420(18) Uani 1 1 d . . . C24 C 1.3305(5) 0.7406(3) 0.0531(3) 0.0404(18) Uani 1 1 d . . . H24 H 1.3422 0.7394 0.0155 0.048 Uiso 1 1 calc R . . C25 C 1.2876(5) 0.7863(3) 0.0739(3) 0.0370(17) Uani 1 1 d . . . C26 C 1.2867(5) 0.7454(3) 0.2248(3) 0.0429(19) Uani 1 1 d . . . H26A H 1.3038 0.7812 0.2392 0.064 Uiso 1 1 calc R . . H26B H 1.3220 0.7169 0.2418 0.064 Uiso 1 1 calc R . . H26C H 1.2259 0.7388 0.2327 0.064 Uiso 1 1 calc R . . C27 C 1.4007(7) 0.6475(4) 0.0610(4) 0.068(3) Uani 1 1 d . . . H27A H 1.3572 0.6208 0.0495 0.103 Uiso 1 1 calc R . . H27B H 1.4389 0.6309 0.0882 0.103 Uiso 1 1 calc R . . H27C H 1.4344 0.6589 0.0297 0.103 Uiso 1 1 calc R . . C28 C 1.2568(6) 0.8329(4) 0.0365(3) 0.055(2) Uani 1 1 d . . . H28A H 1.1995 0.8449 0.0475 0.083 Uiso 1 1 calc R . . H28B H 1.2542 0.8198 -0.0009 0.083 Uiso 1 1 calc R . . H28C H 1.2971 0.8636 0.0392 0.083 Uiso 1 1 calc R . . C29 C 0.9654(4) 0.6843(3) 0.0147(3) 0.0333(16) Uani 1 1 d . . . C30 C 1.0441(5) 0.6163(4) -0.0208(3) 0.051(2) Uani 1 1 d . . . H30 H 1.0835 0.5867 -0.0233 0.062 Uiso 1 1 calc R . . C31 C 1.0011(5) 0.6403(4) -0.0621(4) 0.053(2) Uani 1 1 d . . . H31 H 1.0039 0.6303 -0.0992 0.064 Uiso 1 1 calc R . . C32 C 1.0596(5) 0.6378(3) 0.0809(3) 0.0434(19) Uani 1 1 d . . . H32A H 1.0916 0.6028 0.0833 0.052 Uiso 1 1 calc R . . H32B H 1.0144 0.6375 0.1086 0.052 Uiso 1 1 calc R . . C33 C 1.1202(5) 0.6848(3) 0.0911(3) 0.047(2) Uani 1 1 d . . . H33A H 1.1637 0.6852 0.0622 0.056 Uiso 1 1 calc R . . H33B H 1.1510 0.6784 0.1258 0.056 Uiso 1 1 calc R . . C34 C 0.9000(5) 0.7209(3) -0.0714(3) 0.0387(18) Uani 1 1 d . . . C35 C 0.8215(5) 0.7024(4) -0.0951(3) 0.050(2) Uani 1 1 d . . . C36 C 0.7717(6) 0.7430(5) -0.1216(3) 0.063(3) Uani 1 1 d . . . H36 H 0.7180 0.7325 -0.1370 0.075 Uiso 1 1 calc R . . C37 C 0.7970(7) 0.7973(5) -0.1262(4) 0.065(3) Uani 1 1 d . . . C38 C 0.8761(7) 0.8112(4) -0.1047(4) 0.065(3) Uani 1 1 d . . . H38 H 0.8951 0.8479 -0.1087 0.078 Uiso 1 1 calc R . . C39 C 0.9301(6) 0.7746(3) -0.0772(3) 0.049(2) Uani 1 1 d . . . C40 C 0.7907(6) 0.6440(4) -0.0928(4) 0.061(3) Uani 1 1 d . . . H40A H 0.8385 0.6202 -0.0821 0.092 Uiso 1 1 calc R . . H40B H 0.7689 0.6330 -0.1285 0.092 Uiso 1 1 calc R . . H40C H 0.7445 0.6410 -0.0664 0.092 Uiso 1 1 calc R . . C41 C 0.7369(9) 0.8385(6) -0.1542(4) 0.106(5) Uani 1 1 d . . . H41A H 0.7171 0.8653 -0.1278 0.158 Uiso 1 1 calc R . . H41B H 0.6872 0.8191 -0.1698 0.158 Uiso 1 1 calc R . . H41C H 0.7679 0.8572 -0.1831 0.158 Uiso 1 1 calc R . . C42 C 1.0189(6) 0.7913(4) -0.0568(4) 0.061(2) Uani 1 1 d . . . H42A H 1.0173 0.7973 -0.0177 0.092 Uiso 1 1 calc R . . H42B H 1.0365 0.8251 -0.0748 0.092 Uiso 1 1 calc R . . H42C H 1.0602 0.7623 -0.0649 0.092 Uiso 1 1 calc R . . C43 C 0.6819(5) 0.6891(3) 0.1564(3) 0.0366(17) Uani 1 1 d . . . C44 C 0.6293(6) 0.6029(4) 0.1542(4) 0.053(2) Uani 1 1 d . . . H44 H 0.6249 0.5648 0.1476 0.064 Uiso 1 1 calc R . . C45 C 0.5704(6) 0.6347(4) 0.1787(4) 0.057(2) Uani 1 1 d . . . H45 H 0.5167 0.6230 0.1924 0.068 Uiso 1 1 calc R . . C46 C 0.7731(6) 0.6225(3) 0.1072(3) 0.048(2) Uani 1 1 d . . . H46A H 0.7759 0.5824 0.1026 0.058 Uiso 1 1 calc R . . H46B H 0.8268 0.6347 0.1256 0.058 Uiso 1 1 calc R . . C47 C 0.7647(5) 0.6502(3) 0.0520(3) 0.0430(19) Uani 1 1 d . . . H47A H 0.7076 0.6410 0.0363 0.052 Uiso 1 1 calc R . . H47B H 0.8087 0.6346 0.0279 0.052 Uiso 1 1 calc R . . C48 C 0.5589(4) 0.7338(3) 0.2039(3) 0.0365(17) Uani 1 1 d . . . C49 C 0.5454(5) 0.7337(3) 0.2602(3) 0.0426(19) Uani 1 1 d . . . C50 C 0.5030(5) 0.7792(4) 0.2822(3) 0.047(2) Uani 1 1 d . . . H50 H 0.4940 0.7803 0.3201 0.057 Uiso 1 1 calc R . . C51 C 0.4734(5) 0.8231(4) 0.2503(3) 0.045(2) Uani 1 1 d . . . C52 C 0.4886(5) 0.8212(4) 0.1952(3) 0.0429(19) Uani 1 1 d . . . H52 H 0.4700 0.8509 0.1733 0.051 Uiso 1 1 calc R . . C53 C 0.5308(4) 0.7766(4) 0.1705(3) 0.0407(19) Uani 1 1 d . . . C54 C 0.5787(6) 0.6881(4) 0.2967(4) 0.060(2) Uani 1 1 d . . . H54A H 0.5397 0.6567 0.2943 0.090 Uiso 1 1 calc R . . H54B H 0.5817 0.7011 0.3341 0.090 Uiso 1 1 calc R . . H54C H 0.6362 0.6771 0.2851 0.090 Uiso 1 1 calc R . . C55 C 0.5426(5) 0.7768(4) 0.1089(3) 0.047(2) Uani 1 1 d . . . H55A H 0.5006 0.8017 0.0922 0.071 Uiso 1 1 calc R . . H55B H 0.5338 0.7398 0.0947 0.071 Uiso 1 1 calc R . . H55C H 0.6009 0.7891 0.1005 0.071 Uiso 1 1 calc R . . C56 C 0.4280(6) 0.8718(4) 0.2757(4) 0.062(2) Uani 1 1 d . . . H56A H 0.4691 0.8925 0.2979 0.093 Uiso 1 1 calc R . . H56B H 0.3811 0.8587 0.2984 0.093 Uiso 1 1 calc R . . H56C H 0.4045 0.8953 0.2471 0.093 Uiso 1 1 calc R . . C57 C 1.0021(5) 0.6603(3) 0.2593(3) 0.0426(19) Uani 1 1 d . . . H57 H 1.0271 0.6828 0.2894 0.051 Uiso 1 1 calc R . . C58 C 1.0731(6) 0.6258(3) 0.2342(4) 0.056(2) Uani 1 1 d . . . H58A H 1.0985 0.6019 0.2619 0.084 Uiso 1 1 calc R . . H58B H 1.1176 0.6499 0.2198 0.084 Uiso 1 1 calc R . . H58C H 1.0488 0.6035 0.2049 0.084 Uiso 1 1 calc R . . C59 C 0.9298(7) 0.6254(4) 0.2811(4) 0.069(3) Uani 1 1 d . . . H59A H 0.9042 0.6039 0.2517 0.104 Uiso 1 1 calc R . . H59B H 0.8858 0.6491 0.2968 0.104 Uiso 1 1 calc R . . H59C H 0.9526 0.6008 0.3091 0.104 Uiso 1 1 calc R . . C60 C 0.8268(6) 0.8618(3) 0.0690(4) 0.053(2) Uani 1 1 d . . . H60 H 0.8015 0.8382 0.0398 0.064 Uiso 1 1 calc R . . C61 C 0.8987(8) 0.8951(5) 0.0447(5) 0.090(4) Uani 1 1 d . . . H60A H 0.8783 0.9121 0.0111 0.135 Uiso 1 1 calc R . . H60B H 0.9475 0.8711 0.0370 0.135 Uiso 1 1 calc R . . H60C H 0.9167 0.9235 0.0704 0.135 Uiso 1 1 calc R . . C62 C 0.7547(7) 0.8962(4) 0.0925(5) 0.074(3) Uani 1 1 d . . . H62A H 0.7767 0.9166 0.1239 0.112 Uiso 1 1 calc R . . H62B H 0.7077 0.8723 0.1038 0.112 Uiso 1 1 calc R . . H62C H 0.7334 0.9219 0.0651 0.112 Uiso 1 1 calc R . . B1 B 0.8967(7) 0.4957(4) 0.1595(5) 0.092(4) Uani 1 1 d DU . . F1 F 0.8067(5) 0.5058(4) 0.1622(4) 0.084(4) Uani 0.616(14) 1 d PDU A 1 F2 F 0.9362(6) 0.5415(4) 0.1383(5) 0.100(4) Uani 0.616(14) 1 d PDU A 1 F3 F 0.9132(6) 0.4494(3) 0.1325(4) 0.085(4) Uani 0.616(14) 1 d PDU A 1 F4 F 0.9255(8) 0.4904(5) 0.2151(4) 0.172(8) Uani 0.616(14) 1 d PDU A 1 F1A F 0.8242(11) 0.5109(9) 0.1847(9) 0.150(7) Uani 0.384(14) 1 d PDU A 2 F2A F 0.9113(14) 0.4369(6) 0.1686(9) 0.150(7) Uani 0.384(14) 1 d PDU A 2 F3A F 0.8858(14) 0.4998(9) 0.1014(6) 0.150(7) Uani 0.384(14) 1 d PDU A 2 F4A F 0.9698(11) 0.5230(8) 0.1751(9) 0.150(7) Uani 0.384(14) 1 d PDU A 2 B2 B 0.1248(8) 0.0623(5) 0.2505(5) 0.138(7) Uani 1 1 d DU . . F5 F 0.1086(8) 0.1146(4) 0.2547(5) 0.118(4) Uani 0.621(15) 1 d PDU B 1 F6 F 0.0791(9) 0.0289(6) 0.2833(5) 0.166(6) Uani 0.621(15) 1 d PDU B 1 F7 F 0.1091(8) 0.0442(4) 0.1952(4) 0.118(4) Uani 0.621(15) 1 d PDU B 1 F8 F 0.2144(7) 0.0511(6) 0.2586(6) 0.166(6) Uani 0.621(15) 1 d PDU B 1 F5A F 0.1821(13) 0.0379(8) 0.2218(9) 0.151(7) Uani 0.379(15) 1 d PDU B 2 F6A F 0.0956(14) 0.1138(7) 0.2262(9) 0.151(7) Uani 0.379(15) 1 d PDU B 2 F7A F 0.0503(12) 0.0326(9) 0.2623(9) 0.151(7) Uani 0.379(15) 1 d PDU B 2 F8A F 0.1602(13) 0.0804(9) 0.3031(7) 0.151(7) Uani 0.379(15) 1 d PDU B 2 C1S C 0.3601(6) 1.0030(4) 0.0887(5) 0.121(2) Uani 1 1 d GDU . . C2S C 0.3696(6) 1.0127(3) 0.1444(5) 0.120(2) Uani 1 1 d GU . . H2S H 0.3254 1.0308 0.1635 0.144 Uiso 1 1 calc R . . C3S C 0.4446(7) 0.9957(4) 0.1718(3) 0.120(2) Uani 1 1 d GU . . H3S H 0.4511 1.0023 0.2095 0.144 Uiso 1 1 calc R . . C4S C 0.5101(5) 0.9690(4) 0.1435(5) 0.121(2) Uani 1 1 d GU . . H4S H 0.5608 0.9575 0.1620 0.145 Uiso 1 1 calc R . . C5S C 0.5006(6) 0.9592(3) 0.0878(4) 0.121(2) Uani 1 1 d GU . . H5S H 0.5449 0.9412 0.0686 0.145 Uiso 1 1 calc R . . C6S C 0.4256(8) 0.9762(4) 0.0604(3) 0.121(2) Uani 1 1 d GU . . H6S H 0.4192 0.9697 0.0227 0.145 Uiso 1 1 calc R . . C7S C 0.2727(6) 1.0200(5) 0.0655(6) 0.121(2) Uani 1 1 d DU . . H7SA H 0.2390 1.0376 0.0938 0.182 Uiso 1 1 calc R . . H7SC H 0.2420 0.9876 0.0522 0.182 Uiso 1 1 calc R . . H7SB H 0.2810 1.0457 0.0356 0.182 Uiso 1 1 calc R . . C8S C 0.1309(8) 0.9490(7) 0.9109(5) 0.094(3) Uiso 0.50 1 d PGDU . . C9S C 0.0872(7) 0.9607(7) 0.8623(6) 0.094(3) Uiso 0.50 1 d PGDU . . H9S H 0.0264 0.9647 0.8619 0.112 Uiso 0.50 1 calc PR . . C10S C 0.1332(10) 0.9663(7) 0.8141(5) 0.094(3) Uiso 0.50 1 d PGU . . H10S H 0.1036 0.9742 0.7812 0.113 Uiso 0.50 1 calc PR . . C11S C 0.2230(10) 0.9603(7) 0.8146(5) 0.094(3) Uiso 0.50 1 d PGU . . H11S H 0.2542 0.9642 0.7820 0.112 Uiso 0.50 1 calc PR . . C12S C 0.2668(7) 0.9487(7) 0.8632(6) 0.093(3) Uiso 0.50 1 d PGU . . H12S H 0.3276 0.9446 0.8636 0.112 Uiso 0.50 1 calc PR . . C13S C 0.2208(8) 0.9430(7) 0.9114(5) 0.094(3) Uiso 0.50 1 d PGDU . . H13S H 0.2504 0.9351 0.9443 0.112 Uiso 0.50 1 calc PR . . C14S C 0.0817(11) 0.9466(11) 0.9638(6) 0.095(3) Uiso 0.50 1 d PDU . . H14SC H 0.0201 0.9515 0.9563 0.143 Uiso 0.50 1 calc PR . . H14SA H 0.1020 0.9758 0.9879 0.143 Uiso 0.50 1 calc PR . . H14SB H 0.0912 0.9111 0.9811 0.143 Uiso 0.50 1 calc PR . . C15S C 0.7997(12) 0.5014(7) 0.9002(5) 0.102(3) Uiso 0.50 1 d PGDU . . C16S C 0.7126(10) 0.4976(7) 0.9141(6) 0.102(3) Uiso 0.50 1 d PGU . . H16S H 0.6699 0.4933 0.8866 0.122 Uiso 0.50 1 calc PR . . C17S C 0.6886(8) 0.5002(7) 0.9686(7) 0.102(3) Uiso 0.50 1 d PGU . . H17S H 0.6296 0.4976 0.9779 0.122 Uiso 0.50 1 calc PR . . C18S C 0.7517(11) 0.5065(7) 1.0092(5) 0.102(3) Uiso 0.50 1 d PGU . . H18S H 0.7354 0.5082 1.0460 0.122 Uiso 0.50 1 calc PR . . C19S C 0.8388(10) 0.5102(7) 0.9953(6) 0.102(3) Uiso 0.50 1 d PGU . . H19S H 0.8814 0.5145 1.0228 0.123 Uiso 0.50 1 calc PR . . C20S C 0.8628(8) 0.5077(7) 0.9408(7) 0.102(3) Uiso 0.50 1 d PGU . . H20S H 0.9217 0.5102 0.9315 0.122 Uiso 0.50 1 calc PR . . C21S C 0.8394(16) 0.4994(11) 0.8439(7) 0.102(3) Uiso 0.50 1 d PDU . . H21A H 0.7937 0.4955 0.8166 0.153 Uiso 0.50 1 calc PR . . H21B H 0.8787 0.4682 0.8418 0.153 Uiso 0.50 1 calc PR . . H21C H 0.8713 0.5333 0.8375 0.153 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 0.0241(3) 0.0349(3) 0.0256(3) -0.0028(2) 0.0014(2) -0.0003(2) Pd2 0.0232(3) 0.0303(3) 0.0270(3) -0.0037(2) 0.0014(2) -0.0017(2) Pd3 0.0245(3) 0.0334(3) 0.0248(3) -0.0031(2) 0.0016(2) 0.0002(2) Pd4 0.0234(3) 0.0358(3) 0.0267(3) -0.0021(2) 0.0010(2) -0.0015(2) S1 0.0251(9) 0.0470(11) 0.0295(9) -0.0054(8) 0.0008(7) -0.0034(8) S2 0.0271(9) 0.0429(10) 0.0288(9) -0.0074(8) -0.0004(7) -0.0019(7) S3 0.0268(9) 0.0445(11) 0.0287(9) -0.0070(8) 0.0023(7) -0.0023(7) S4 0.0264(9) 0.0462(11) 0.0291(9) -0.0046(8) -0.0018(7) 0.0004(8) S5 0.0286(9) 0.0333(9) 0.0299(9) -0.0029(7) 0.0008(7) -0.0030(7) S6 0.0303(9) 0.0327(9) 0.0323(9) -0.0027(8) 0.0034(7) 0.0001(7) N1 0.039(4) 0.045(4) 0.046(4) -0.017(3) -0.006(3) 0.009(3) N2 0.038(4) 0.059(4) 0.032(3) -0.012(3) -0.003(3) 0.012(3) N3 0.037(3) 0.033(3) 0.045(4) -0.005(3) 0.003(3) -0.005(3) N4 0.027(3) 0.034(3) 0.036(3) 0.001(3) 0.004(3) -0.003(2) N5 0.038(3) 0.045(4) 0.034(3) -0.007(3) -0.008(3) 0.009(3) N6 0.042(4) 0.050(4) 0.030(3) -0.012(3) 0.001(3) 0.002(3) N7 0.048(4) 0.042(4) 0.038(4) -0.003(3) 0.005(3) -0.005(3) N8 0.036(3) 0.046(4) 0.033(3) 0.002(3) -0.001(3) -0.012(3) C1 0.029(4) 0.039(4) 0.037(4) -0.009(3) 0.000(3) -0.002(3) C2 0.062(6) 0.074(7) 0.052(6) -0.026(5) -0.006(5) 0.023(5) C3 0.078(7) 0.088(7) 0.044(5) -0.032(5) -0.005(5) 0.034(6) C4 0.049(5) 0.050(5) 0.051(5) -0.004(4) -0.003(4) 0.013(4) C5 0.033(4) 0.062(5) 0.038(4) -0.010(4) -0.004(3) 0.015(4) C6 0.048(5) 0.078(7) 0.028(4) -0.007(4) 0.005(4) 0.020(5) C7 0.043(5) 0.094(7) 0.035(5) -0.007(5) 0.005(4) 0.013(5) C8 0.052(6) 0.135(11) 0.047(6) 0.002(7) 0.008(5) 0.034(7) C9 0.095(9) 0.125(11) 0.033(5) 0.007(7) 0.008(6) 0.050(9) C10 0.121(10) 0.079(7) 0.034(5) 0.000(5) 0.021(6) 0.021(7) C11 0.064(6) 0.061(6) 0.032(4) -0.011(4) 0.006(4) 0.007(5) C12 0.049(6) 0.131(10) 0.051(6) 0.003(6) -0.003(5) -0.008(6) C13 0.165(14) 0.157(13) 0.058(7) 0.012(8) 0.000(8) 0.108(12) C14 0.086(7) 0.072(7) 0.045(5) 0.000(5) 0.009(5) -0.012(6) C15 0.029(4) 0.039(4) 0.030(4) -0.003(3) 0.006(3) -0.005(3) C16 0.047(5) 0.033(4) 0.061(6) -0.006(4) 0.014(4) -0.013(4) C17 0.041(4) 0.036(4) 0.055(5) 0.000(4) 0.009(4) -0.007(3) C18 0.037(4) 0.033(4) 0.064(6) -0.011(4) 0.014(4) 0.003(3) C19 0.039(4) 0.057(5) 0.042(5) -0.023(4) 0.015(4) -0.016(4) C20 0.029(4) 0.034(4) 0.034(4) -0.002(3) 0.007(3) -0.005(3) C21 0.024(3) 0.043(4) 0.034(4) -0.002(3) 0.001(3) -0.006(3) C22 0.032(4) 0.036(4) 0.046(5) 0.005(4) -0.004(3) -0.001(3) C23 0.036(4) 0.043(5) 0.047(5) -0.006(4) 0.002(3) -0.001(3) C24 0.037(4) 0.047(5) 0.037(4) -0.002(4) 0.011(3) -0.007(3) C25 0.031(4) 0.044(4) 0.036(4) 0.003(3) 0.007(3) -0.001(3) C26 0.027(4) 0.062(5) 0.040(5) 0.015(4) 0.001(3) -0.004(3) C27 0.073(7) 0.070(6) 0.062(6) -0.014(5) 0.004(5) 0.020(5) C28 0.060(6) 0.064(6) 0.042(5) 0.012(4) 0.005(4) 0.006(5) C29 0.029(4) 0.039(4) 0.032(4) -0.003(3) -0.001(3) -0.006(3) C30 0.047(5) 0.059(5) 0.048(5) -0.027(4) -0.003(4) 0.015(4) C31 0.057(5) 0.059(5) 0.043(5) -0.022(4) -0.001(4) 0.018(4) C32 0.048(5) 0.039(4) 0.042(5) -0.006(4) -0.010(4) 0.012(4) C33 0.038(4) 0.056(5) 0.047(5) -0.016(4) -0.002(4) 0.009(4) C34 0.046(4) 0.054(5) 0.016(3) 0.000(3) 0.004(3) 0.012(4) C35 0.046(5) 0.076(6) 0.029(4) -0.009(4) 0.002(4) 0.015(4) C36 0.056(6) 0.108(9) 0.024(4) -0.007(5) -0.013(4) 0.026(6) C37 0.084(7) 0.080(7) 0.032(5) -0.005(5) -0.006(5) 0.034(6) C38 0.105(8) 0.055(6) 0.036(5) -0.008(4) 0.010(5) 0.011(6) C39 0.073(6) 0.046(5) 0.028(4) -0.004(4) 0.008(4) 0.007(4) C40 0.057(6) 0.089(7) 0.037(5) -0.002(5) -0.005(4) -0.019(5) C41 0.135(11) 0.126(11) 0.055(7) 0.011(7) -0.004(7) 0.086(9) C42 0.072(6) 0.065(6) 0.046(5) 0.001(5) 0.003(5) -0.017(5) C43 0.033(4) 0.046(5) 0.030(4) 0.001(3) -0.004(3) -0.009(3) C44 0.062(6) 0.042(5) 0.056(6) 0.002(4) 0.009(5) -0.018(4) C45 0.054(5) 0.063(6) 0.054(6) 0.004(5) 0.011(4) -0.026(5) C46 0.057(5) 0.041(5) 0.047(5) -0.004(4) 0.008(4) -0.004(4) C47 0.039(4) 0.049(5) 0.041(4) -0.013(4) 0.008(3) -0.013(4) C48 0.023(4) 0.049(5) 0.038(4) 0.006(4) 0.004(3) -0.013(3) C49 0.035(4) 0.057(5) 0.036(4) 0.001(4) 0.009(3) -0.005(4) C50 0.038(4) 0.067(6) 0.037(4) 0.001(4) 0.002(4) -0.012(4) C51 0.029(4) 0.059(5) 0.047(5) -0.003(4) 0.004(3) -0.006(4) C52 0.026(4) 0.060(5) 0.042(5) 0.004(4) -0.003(3) -0.001(4) C53 0.020(4) 0.066(5) 0.035(4) 0.003(4) -0.001(3) -0.012(3) C54 0.066(6) 0.070(6) 0.045(5) 0.017(5) 0.012(4) 0.006(5) C55 0.038(4) 0.069(6) 0.034(4) 0.011(4) -0.003(3) -0.006(4) C56 0.054(6) 0.079(7) 0.052(6) -0.010(5) -0.001(4) 0.009(5) C57 0.060(5) 0.034(4) 0.033(4) 0.003(3) -0.003(4) -0.001(4) C58 0.054(5) 0.044(5) 0.070(6) 0.007(4) 0.004(5) 0.009(4) C59 0.097(8) 0.048(5) 0.064(6) 0.024(5) 0.023(6) 0.003(5) C60 0.074(6) 0.035(4) 0.051(5) 0.007(4) 0.003(5) 0.011(4) C61 0.095(9) 0.077(7) 0.100(9) 0.037(7) 0.031(7) 0.012(6) C62 0.076(7) 0.058(6) 0.089(8) 0.010(6) 0.003(6) 0.026(5) B1 0.092(5) 0.091(5) 0.092(5) 0.000(2) -0.001(2) -0.001(2) F1 0.088(5) 0.074(5) 0.090(5) -0.003(3) 0.010(3) 0.006(3) F2 0.095(5) 0.093(5) 0.114(6) 0.008(4) -0.004(4) -0.009(3) F3 0.086(5) 0.080(5) 0.088(5) -0.021(3) 0.011(3) 0.006(3) F4 0.176(8) 0.173(8) 0.167(8) -0.004(4) -0.004(4) 0.007(4) F1A 0.151(7) 0.150(7) 0.149(7) -0.002(2) 0.001(2) 0.000(2) F2A 0.151(7) 0.150(7) 0.149(7) -0.002(2) 0.001(2) 0.000(2) F3A 0.151(7) 0.150(7) 0.149(7) -0.002(2) 0.001(2) 0.000(2) F4A 0.151(7) 0.150(7) 0.149(7) -0.002(2) 0.001(2) 0.000(2) B2 0.138(7) 0.139(7) 0.138(7) 0.000(2) 0.002(2) 0.000(2) F5 0.122(5) 0.113(5) 0.118(5) -0.012(3) 0.006(3) 0.003(3) F6 0.163(6) 0.168(6) 0.166(6) 0.003(3) 0.005(3) 0.003(3) F7 0.122(5) 0.113(5) 0.118(5) -0.012(3) 0.006(3) 0.003(3) F8 0.163(6) 0.168(6) 0.166(6) 0.003(3) 0.005(3) 0.003(3) F5A 0.152(8) 0.149(8) 0.153(8) -0.004(2) 0.003(2) 0.002(2) F6A 0.152(8) 0.149(8) 0.153(8) -0.004(2) 0.003(2) 0.002(2) F7A 0.152(8) 0.149(8) 0.153(8) -0.004(2) 0.003(2) 0.002(2) F8A 0.152(8) 0.149(8) 0.153(8) -0.004(2) 0.003(2) 0.002(2) C1S 0.150(5) 0.075(3) 0.137(5) 0.003(4) 0.019(4) -0.027(4) C2S 0.150(5) 0.074(3) 0.137(5) 0.002(4) 0.019(4) -0.027(4) C3S 0.150(5) 0.074(3) 0.137(5) 0.002(4) 0.019(4) -0.027(4) C4S 0.150(5) 0.075(3) 0.137(5) 0.002(4) 0.019(4) -0.026(4) C5S 0.150(5) 0.076(3) 0.137(5) 0.002(4) 0.019(4) -0.026(4) C6S 0.150(5) 0.076(3) 0.137(5) 0.002(4) 0.019(4) -0.026(4) C7S 0.151(5) 0.076(3) 0.138(5) 0.003(4) 0.018(4) -0.027(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 C1 1.988(7) . ? Pd1 S1 2.3207(18) . ? Pd1 S2 2.3314(18) . ? Pd1 S5 2.3917(18) . ? Pd1 Pd2 3.1039(7) . ? Pd2 C15 1.991(7) . ? Pd2 S3 2.3333(18) . ? Pd2 S2 2.3336(18) . ? Pd2 S5 2.3656(17) . ? Pd3 C29 1.994(7) . ? Pd3 S3 2.3249(18) . ? Pd3 S4 2.3267(18) . ? Pd3 S6 2.3939(18) . ? Pd3 Pd4 3.1030(7) . ? Pd4 C43 1.989(7) . ? Pd4 S4 2.3315(18) . ? Pd4 S1 2.3335(18) . ? Pd4 S6 2.3703(18) . ? S1 C5 1.856(8) . ? S2 C19 1.829(8) . ? S3 C33 1.843(8) . ? S4 C47 1.826(8) . ? S5 C57 1.851(8) . ? S6 C60 1.849(8) . ? N1 C1 1.337(9) . ? N1 C2 1.370(10) . ? N1 C4 1.465(10) . ? N2 C1 1.369(9) . ? N2 C3 1.388(10) . ? N2 C6 1.441(11) . ? N3 C15 1.347(9) . ? N3 C16 1.393(9) . ? N3 C18 1.486(9) . ? N4 C15 1.349(8) . ? N4 C17 1.395(9) . ? N4 C20 1.439(9) . ? N5 C29 1.329(9) . ? N5 C30 1.384(9) . ? N5 C32 1.466(9) . ? N6 C29 1.371(9) . ? N6 C31 1.374(10) . ? N6 C34 1.439(10) . ? N7 C43 1.344(10) . ? N7 C44 1.389(10) . ? N7 C46 1.463(10) . ? N8 C43 1.360(9) . ? N8 C45 1.372(10) . ? N8 C48 1.433(10) . ? C2 C3 1.327(13) . ? C4 C5 1.491(11) . ? C6 C11 1.390(13) . ? C6 C7 1.392(12) . ? C7 C8 1.417(15) . ? C7 C12 1.498(15) . ? C8 C9 1.337(17) . ? C9 C10 1.386(17) . ? C9 C13 1.512(15) . ? C10 C11 1.364(14) . ? C11 C14 1.510(13) . ? C16 C17 1.325(11) . ? C18 C19 1.513(12) . ? C20 C21 1.390(10) . ? C20 C25 1.396(10) . ? C21 C22 1.392(10) . ? C21 C26 1.495(10) . ? C22 C23 1.392(11) . ? C23 C24 1.370(11) . ? C23 C27 1.507(11) . ? C24 C25 1.388(11) . ? C25 C28 1.525(11) . ? C30 C31 1.336(12) . ? C32 C33 1.491(11) . ? C34 C39 1.388(11) . ? C34 C35 1.406(11) . ? C35 C36 1.399(12) . ? C35 C40 1.494(13) . ? C36 C37 1.378(15) . ? C37 C38 1.364(14) . ? C37 C41 1.517(13) . ? C38 C39 1.385(13) . ? C39 C42 1.504(13) . ? C44 C45 1.336(12) . ? C46 C47 1.513(11) . ? C48 C53 1.386(11) . ? C48 C49 1.398(11) . ? C49 C50 1.393(12) . ? C49 C54 1.506(12) . ? C50 C51 1.392(12) . ? C51 C52 1.373(11) . ? C51 C56 1.507(12) . ? C52 C53 1.403(11) . ? C53 C55 1.520(11) . ? C57 C59 1.501(12) . ? C57 C58 1.513(11) . ? C60 C61 1.498(13) . ? C60 C62 1.508(12) . ? B1 F3 1.328(12) . ? B1 F1A 1.334(16) . ? B1 F4A 1.355(15) . ? B1 F2 1.370(12) . ? B1 F1 1.409(13) . ? B1 F3A 1.432(15) . ? B1 F4 1.432(13) . ? B1 F2A 1.460(16) . ? B2 F5A 1.279(16) . ? B2 F5 1.295(14) . ? B2 F6 1.346(15) . ? B2 F7A 1.388(16) . ? B2 F8 1.417(14) . ? B2 F7 1.441(14) . ? B2 F6A 1.450(16) . ? B2 F8A 1.460(16) . ? C1S C2S 1.3900 . ? C1S C6S 1.3900 . ? C1S C7S 1.511(5) . ? C2S C3S 1.3900 . ? C3S C4S 1.3900 . ? C4S C5S 1.3900 . ? C5S C6S 1.3900 . ? C8S C9S 1.3900 . ? C8S C13S 1.3900 . ? C8S C14S 1.509(5) . ? C9S C10S 1.3900 . ? C10S C11S 1.3900 . ? C11S C12S 1.3900 . ? C12S C13S 1.3900 . ? C15S C16S 1.3900 . ? C15S C20S 1.3900 . ? C15S C21S 1.515(5) . ? C16S C17S 1.3900 . ? C17S C18S 1.3900 . ? C18S C19S 1.3900 . ? C19S C20S 1.3900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pd1 S1 87.1(2) . . ? C1 Pd1 S2 96.0(2) . . ? S1 Pd1 S2 172.11(7) . . ? C1 Pd1 S5 170.8(2) . . ? S1 Pd1 S5 93.86(6) . . ? S2 Pd1 S5 84.24(6) . . ? C1 Pd1 Pd2 136.4(2) . . ? S1 Pd1 Pd2 125.38(5) . . ? S2 Pd1 Pd2 48.32(4) . . ? S5 Pd1 Pd2 48.91(4) . . ? C15 Pd2 S3 89.3(2) . . ? C15 Pd2 S2 90.5(2) . . ? S3 Pd2 S2 176.27(7) . . ? C15 Pd2 S5 174.0(2) . . ? S3 Pd2 S5 95.20(6) . . ? S2 Pd2 S5 84.78(6) . . ? C15 Pd2 Pd1 124.4(2) . . ? S3 Pd2 Pd1 129.38(5) . . ? S2 Pd2 Pd1 48.26(4) . . ? S5 Pd2 Pd1 49.64(4) . . ? C29 Pd3 S3 87.5(2) . . ? C29 Pd3 S4 95.9(2) . . ? S3 Pd3 S4 173.08(7) . . ? C29 Pd3 S6 173.2(2) . . ? S3 Pd3 S6 93.45(6) . . ? S4 Pd3 S6 83.85(6) . . ? C29 Pd3 Pd4 134.69(19) . . ? S3 Pd3 Pd4 125.59(5) . . ? S4 Pd3 Pd4 48.30(5) . . ? S6 Pd3 Pd4 49.03(4) . . ? C43 Pd4 S4 90.6(2) . . ? C43 Pd4 S1 88.6(2) . . ? S4 Pd4 S1 175.26(7) . . ? C43 Pd4 S6 173.0(2) . . ? S4 Pd4 S6 84.27(6) . . ? S1 Pd4 S6 96.14(6) . . ? C43 Pd4 Pd3 123.4(2) . . ? S4 Pd4 Pd3 48.17(4) . . ? S1 Pd4 Pd3 129.12(5) . . ? S6 Pd4 Pd3 49.69(4) . . ? C5 S1 Pd1 106.5(3) . . ? C5 S1 Pd4 105.4(3) . . ? Pd1 S1 Pd4 105.39(7) . . ? C19 S2 Pd1 105.4(3) . . ? C19 S2 Pd2 105.4(3) . . ? Pd1 S2 Pd2 83.42(6) . . ? C33 S3 Pd3 106.6(3) . . ? C33 S3 Pd2 103.4(3) . . ? Pd3 S3 Pd2 105.09(7) . . ? C47 S4 Pd3 105.0(3) . . ? C47 S4 Pd4 104.8(3) . . ? Pd3 S4 Pd4 83.54(6) . . ? C57 S5 Pd2 106.1(3) . . ? C57 S5 Pd1 99.6(3) . . ? Pd2 S5 Pd1 81.45(6) . . ? C60 S6 Pd4 106.6(3) . . ? C60 S6 Pd3 100.8(3) . . ? Pd4 S6 Pd3 81.28(6) . . ? C1 N1 C2 111.1(7) . . ? C1 N1 C4 120.2(6) . . ? C2 N1 C4 127.7(7) . . ? C1 N2 C3 108.5(7) . . ? C1 N2 C6 124.6(6) . . ? C3 N2 C6 126.5(7) . . ? C15 N3 C16 110.9(6) . . ? C15 N3 C18 122.7(6) . . ? C16 N3 C18 126.0(6) . . ? C15 N4 C17 109.6(6) . . ? C15 N4 C20 125.6(6) . . ? C17 N4 C20 124.7(6) . . ? C29 N5 C30 110.4(6) . . ? C29 N5 C32 121.3(6) . . ? C30 N5 C32 127.0(6) . . ? C29 N6 C31 109.1(7) . . ? C29 N6 C34 124.7(6) . . ? C31 N6 C34 126.0(6) . . ? C43 N7 C44 110.1(7) . . ? C43 N7 C46 122.5(6) . . ? C44 N7 C46 126.9(7) . . ? C43 N8 C45 109.9(7) . . ? C43 N8 C48 125.4(6) . . ? C45 N8 C48 124.7(6) . . ? N1 C1 N2 105.5(6) . . ? N1 C1 Pd1 126.5(6) . . ? N2 C1 Pd1 127.2(5) . . ? C3 C2 N1 106.8(8) . . ? C2 C3 N2 108.1(8) . . ? N1 C4 C5 110.6(7) . . ? C4 C5 S1 115.3(5) . . ? C11 C6 C7 122.1(9) . . ? C11 C6 N2 119.3(8) . . ? C7 C6 N2 118.6(9) . . ? C6 C7 C8 116.0(10) . . ? C6 C7 C12 123.1(9) . . ? C8 C7 C12 120.9(10) . . ? C9 C8 C7 123.9(11) . . ? C8 C9 C10 116.7(11) . . ? C8 C9 C13 121.5(14) . . ? C10 C9 C13 121.8(15) . . ? C11 C10 C9 124.1(12) . . ? C10 C11 C6 117.1(10) . . ? C10 C11 C14 122.1(10) . . ? C6 C11 C14 120.7(9) . . ? N3 C15 N4 105.4(6) . . ? N3 C15 Pd2 122.5(5) . . ? N4 C15 Pd2 132.1(5) . . ? C17 C16 N3 106.2(7) . . ? C16 C17 N4 108.0(7) . . ? N3 C18 C19 109.2(6) . . ? C18 C19 S2 115.8(5) . . ? C21 C20 C25 122.3(7) . . ? C21 C20 N4 118.8(6) . . ? C25 C20 N4 118.9(6) . . ? C20 C21 C22 118.0(7) . . ? C20 C21 C26 123.2(7) . . ? C22 C21 C26 118.9(7) . . ? C23 C22 C21 121.1(7) . . ? C24 C23 C22 118.9(7) . . ? C24 C23 C27 121.0(8) . . ? C22 C23 C27 120.1(8) . . ? C23 C24 C25 122.5(7) . . ? C24 C25 C20 117.2(7) . . ? C24 C25 C28 121.0(7) . . ? C20 C25 C28 121.7(7) . . ? N5 C29 N6 105.9(6) . . ? N5 C29 Pd3 125.4(5) . . ? N6 C29 Pd3 128.5(5) . . ? C31 C30 N5 106.9(7) . . ? C30 C31 N6 107.6(7) . . ? N5 C32 C33 109.8(7) . . ? C32 C33 S3 115.0(5) . . ? C39 C34 C35 122.9(8) . . ? C39 C34 N6 118.6(7) . . ? C35 C34 N6 118.5(7) . . ? C36 C35 C34 115.5(9) . . ? C36 C35 C40 120.6(9) . . ? C34 C35 C40 123.9(8) . . ? C37 C36 C35 123.7(9) . . ? C38 C37 C36 117.1(9) . . ? C38 C37 C41 123.3(12) . . ? C36 C37 C41 119.6(11) . . ? C37 C38 C39 123.9(10) . . ? C38 C39 C34 116.7(9) . . ? C38 C39 C42 121.8(9) . . ? C34 C39 C42 121.4(8) . . ? N7 C43 N8 105.6(6) . . ? N7 C43 Pd4 122.3(5) . . ? N8 C43 Pd4 132.1(6) . . ? C45 C44 N7 106.8(7) . . ? C44 C45 N8 107.6(7) . . ? N7 C46 C47 109.4(7) . . ? C46 C47 S4 115.5(5) . . ? C53 C48 C49 122.3(8) . . ? C53 C48 N8 119.4(7) . . ? C49 C48 N8 118.2(7) . . ? C50 C49 C48 117.1(8) . . ? C50 C49 C54 120.7(7) . . ? C48 C49 C54 122.2(8) . . ? C51 C50 C49 122.7(8) . . ? C52 C51 C50 117.7(8) . . ? C52 C51 C56 121.1(8) . . ? C50 C51 C56 121.1(8) . . ? C51 C52 C53 122.5(8) . . ? C48 C53 C52 117.6(7) . . ? C48 C53 C55 123.3(8) . . ? C52 C53 C55 119.1(7) . . ? C59 C57 C58 112.1(7) . . ? C59 C57 S5 107.9(6) . . ? C58 C57 S5 109.3(6) . . ? C61 C60 C62 113.8(8) . . ? C61 C60 S6 108.5(7) . . ? C62 C60 S6 110.1(7) . . ? F3 B1 F1A 129.0(12) . . ? F3 B1 F4A 112.9(11) . . ? F1A B1 F4A 115.5(10) . . ? F3 B1 F2 114.1(8) . . ? F1A B1 F2 109.3(12) . . ? F4A B1 F2 48.8(9) . . ? F3 B1 F1 111.3(8) . . ? F1A B1 F1 26.1(10) . . ? F4A B1 F1 135.7(12) . . ? F2 B1 F1 108.6(8) . . ? F3 B1 F3A 65.5(9) . . ? F1A B1 F3A 110.7(9) . . ? F4A B1 F3A 109.4(9) . . ? F2 B1 F3A 67.4(9) . . ? F1 B1 F3A 86.1(10) . . ? F3 B1 F4 109.8(8) . . ? F1A B1 F4 80.4(11) . . ? F4A B1 F4 62.0(10) . . ? F2 B1 F4 107.4(8) . . ? F1 B1 F4 105.2(8) . . ? F3A B1 F4 168.6(11) . . ? F3 B1 F2A 38.9(9) . . ? F1A B1 F2A 109.0(9) . . ? F4A B1 F2A 107.9(9) . . ? F2 B1 F2A 141.3(11) . . ? F1 B1 F2A 108.1(11) . . ? F3A B1 F2A 103.6(8) . . ? F4 B1 F2A 73.8(10) . . ? F5A B2 F5 129.1(14) . . ? F5A B2 F6 114.7(14) . . ? F5 B2 F6 116.0(10) . . ? F5A B2 F7A 116.8(11) . . ? F5 B2 F7A 109.3(14) . . ? F6 B2 F7A 28.9(11) . . ? F5A B2 F8 46.6(10) . . ? F5 B2 F8 111.3(9) . . ? F6 B2 F8 108.4(9) . . ? F7A B2 F8 132.6(13) . . ? F5A B2 F7 56.7(10) . . ? F5 B2 F7 110.0(9) . . ? F6 B2 F7 107.2(9) . . ? F7A B2 F7 84.7(11) . . ? F8 B2 F7 103.1(8) . . ? F5A B2 F6A 112.6(10) . . ? F5 B2 F6A 29.9(10) . . ? F6 B2 F6A 126.9(13) . . ? F7A B2 F6A 106.2(9) . . ? F8 B2 F6A 121.2(13) . . ? F7 B2 F6A 80.1(11) . . ? F5A B2 F8A 111.8(10) . . ? F5 B2 F8A 72.9(10) . . ? F6 B2 F8A 81.1(11) . . ? F7A B2 F8A 105.8(9) . . ? F8 B2 F8A 65.2(9) . . ? F7 B2 F8A 167.7(11) . . ? F6A B2 F8A 102.4(9) . . ? C2S C1S C6S 120.0 . . ? C2S C1S C7S 113.8(10) . . ? C6S C1S C7S 126.0(10) . . ? C1S C2S C3S 120.0 . . ? C4S C3S C2S 120.0 . . ? C3S C4S C5S 120.0 . . ? C6S C5S C4S 120.0 . . ? C5S C6S C1S 120.0 . . ? C9S C8S C13S 120.0 . . ? C9S C8S C14S 119.9(2) . . ? C13S C8S C14S 120.0(2) . . ? C8S C9S C10S 120.0 . . ? C9S C10S C11S 120.0 . . ? C10S C11S C12S 120.0 . . ? C13S C12S C11S 120.0 . . ? C12S C13S C8S 120.0 . . ? C16S C15S C20S 120.0 . . ? C16S C15S C21S 128.4(16) . . ? C20S C15S C21S 111.6(16) . . ? C17S C16S C15S 120.0 . . ? C18S C17S C16S 120.0 . . ? C17S C18S C19S 120.0 . . ? C20S C19S C18S 120.0 . . ? C19S C20S C15S 120.0 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.386 _refine_diff_density_min -0.892 _refine_diff_density_rms 0.156