data_d:\pd _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H20 N18 O2 Pd2 S4' _chemical_formula_weight 789.58 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' '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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 26.305(9) _cell_length_b 6.6097(17) _cell_length_c 17.001(7) _cell_angle_alpha 90.00 _cell_angle_beta 116.39(3) _cell_angle_gamma 90.00 _cell_volume 2647.9(16) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 11607 _cell_measurement_theta_min 1.73 _cell_measurement_theta_max 27.00 _exptl_crystal_description Prism _exptl_crystal_colour Orange _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.981 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1560 _exptl_absorpt_coefficient_mu 1.725 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6521 _exptl_absorpt_correction_T_max 0.7001 _exptl_absorpt_process_details 'SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'Bruker APEX II CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11607 _diffrn_reflns_av_R_equivalents 0.0985 _diffrn_reflns_av_sigmaI/netI 0.0845 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 26.99 _reflns_number_total 2896 _reflns_number_gt 2487 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX II' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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^)+(0.0398P)^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 2896 _refine_ls_number_parameters 175 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0450 _refine_ls_R_factor_gt 0.0313 _refine_ls_wR_factor_ref 0.0945 _refine_ls_wR_factor_gt 0.0815 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.001 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 C1 C 0.6023(5) 0.527(2) 0.6441(8) 0.034(3) Uani 1 1 d . . . C2 C 0.6966(7) 0.622(3) 0.7740(9) 0.072(6) Uani 1 1 d . . . H2A H 0.7180 0.7007 0.7516 0.087 Uiso 1 1 calc R . . H2B H 0.7219 0.5374 0.8209 0.087 Uiso 1 1 calc R . . H2C H 0.6769 0.7113 0.7956 0.087 Uiso 1 1 calc R . . C3 C 0.5508(5) 0.657(2) 0.4010(8) 0.033(3) Uani 1 1 d . . . C4 C 0.5947(8) 0.875(2) 0.3223(9) 0.063(5) Uani 1 1 d . . . H4A H 0.6258 0.9400 0.3699 0.076 Uiso 1 1 calc R . . H4B H 0.5624 0.9631 0.2997 0.076 Uiso 1 1 calc R . . H4C H 0.6054 0.8433 0.2765 0.076 Uiso 1 1 calc R . . C5 C 0.7329(5) 0.729(2) 0.5231(8) 0.044(4) Uani 1 1 d . . . C6 C 0.7338(7) 0.525(2) 0.5606(11) 0.072(5) Uani 1 1 d . . . H6A H 0.6957 0.4748 0.5385 0.087 Uiso 1 1 calc R . . H6B H 0.7502 0.5346 0.6235 0.087 Uiso 1 1 calc R . . H6C H 0.7560 0.4349 0.5442 0.087 Uiso 1 1 calc R . . N1 N 0.5921(4) 0.3521(17) 0.5980(7) 0.036(3) Uani 1 1 d . . . N2 N 0.6320(6) 0.2372(19) 0.6242(8) 0.056(4) Uani 1 1 d . . . N3 N 0.6773(5) 0.313(2) 0.6957(9) 0.059(3) Uani 1 1 d . . . N4 N 0.6572(5) 0.501(2) 0.7064(7) 0.056(4) Uani 1 1 d . . . N5 N 0.5507(4) 0.4595(17) 0.4144(7) 0.037(3) Uani 1 1 d . . . N6 N 0.5818(7) 0.366(2) 0.3779(9) 0.076(5) Uani 1 1 d . . . N7 N 0.5991(6) 0.508(2) 0.3415(9) 0.071(4) Uani 1 1 d . . . N8 N 0.5801(5) 0.685(2) 0.3544(7) 0.051(3) Uani 1 1 d . . . N9 N 0.7040(5) 0.876(2) 0.5287(7) 0.051(3) Uani 1 1 d . . . O1 O 0.6726(4) 0.8261(18) 0.5741(6) 0.070(3) Uani 1 1 d . . . H1 H 0.6545 0.9253 0.5762 0.105 Uiso 1 1 calc R . . Pd1 Pd 0.48356(4) 0.69261(16) 0.51505(7) 0.0318(3) Uani 1 1 d . . . S1 S 0.56713(17) 0.7364(6) 0.6393(2) 0.0575(12) Uani 1 1 d . . . S2 S 0.52063(16) 0.8537(5) 0.4321(2) 0.0447(10) 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 C1 0.031(8) 0.048(9) 0.024(7) 0.004(6) 0.013(6) 0.000(7) C2 0.066(11) 0.111(17) 0.032(8) -0.004(9) 0.015(9) -0.019(11) C3 0.023(7) 0.035(9) 0.038(7) -0.001(7) 0.010(6) 0.002(6) C4 0.116(15) 0.043(10) 0.044(9) 0.017(7) 0.048(10) -0.007(9) C5 0.044(9) 0.054(11) 0.037(8) 0.014(7) 0.020(7) 0.014(8) C6 0.074(13) 0.069(14) 0.098(14) 0.012(10) 0.059(12) -0.004(10) N1 0.027(6) 0.041(8) 0.047(7) -0.016(6) 0.022(6) -0.001(6) N2 0.061(9) 0.045(10) 0.066(9) -0.007(7) 0.032(8) -0.013(8) N3 0.035(7) 0.055(9) 0.084(9) 0.008(9) 0.025(7) 0.009(8) N4 0.029(7) 0.102(13) 0.037(8) 0.011(8) 0.014(6) -0.013(8) N5 0.043(7) 0.026(7) 0.052(7) -0.013(6) 0.031(6) -0.001(6) N6 0.131(14) 0.045(10) 0.103(11) 0.008(8) 0.097(11) 0.013(9) N7 0.107(12) 0.061(11) 0.078(10) -0.018(8) 0.073(10) -0.012(9) N8 0.063(8) 0.050(8) 0.055(7) -0.017(7) 0.040(7) -0.013(8) N9 0.040(7) 0.071(10) 0.042(7) -0.001(6) 0.018(6) 0.010(7) O1 0.072(7) 0.091(9) 0.072(7) 0.012(7) 0.054(6) 0.021(7) Pd1 0.0403(6) 0.0288(5) 0.0303(5) -0.0046(6) 0.0193(4) 0.0008(6) S1 0.053(2) 0.059(3) 0.050(2) -0.009(2) 0.014(2) 0.009(2) S2 0.060(3) 0.031(2) 0.058(2) 0.0026(18) 0.040(2) 0.0102(18) _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 C1 N1 1.354(15) . ? C1 N4 1.370(16) . ? C1 S1 1.647(14) . ? C2 N4 1.408(18) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 N5 1.325(15) . ? C3 N8 1.342(14) . ? C3 S2 1.723(13) . ? C4 N8 1.485(17) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 N9 1.263(16) . ? C5 C5 1.46(2) 7_666 ? C5 C6 1.484(19) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? N1 N2 1.210(15) . ? N1 Pd1 2.083(11) 5_666 ? N2 N3 1.364(15) . ? N3 N4 1.396(17) . ? N5 N6 1.373(14) . ? N5 Pd1 2.055(10) 5_666 ? N6 N7 1.309(16) . ? N7 N8 1.331(16) . ? N9 O1 1.398(12) . ? O1 H1 0.8200 . ? Pd1 N5 2.055(10) 5_666 ? Pd1 N1 2.083(11) 5_666 ? Pd1 S1 2.292(4) . ? Pd1 S2 2.302(3) . ? Pd1 Pd1 2.808(2) 5_666 ? 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 C1 N4 102.2(12) . . ? N1 C1 S1 136.6(11) . . ? N4 C1 S1 121.2(11) . . ? N4 C2 H2A 109.5 . . ? N4 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N4 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N5 C3 N8 106.4(11) . . ? N5 C3 S2 130.9(9) . . ? N8 C3 S2 122.7(11) . . ? N8 C4 H4A 109.5 . . ? N8 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N8 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N9 C5 C5 115.3(17) . 7_666 ? N9 C5 C6 123.9(12) . . ? C5 C5 C6 120.8(17) 7_666 . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N2 N1 C1 114.0(12) . . ? N2 N1 Pd1 124.6(10) . 5_666 ? C1 N1 Pd1 121.1(9) . 5_666 ? N1 N2 N3 111.7(12) . . ? N2 N3 N4 102.2(11) . . ? C1 N4 N3 110.0(12) . . ? C1 N4 C2 134.6(16) . . ? N3 N4 C2 115.4(13) . . ? C3 N5 N6 108.6(10) . . ? C3 N5 Pd1 128.0(8) . 5_666 ? N6 N5 Pd1 123.3(9) . 5_666 ? N7 N6 N5 107.2(12) . . ? N6 N7 N8 108.3(11) . . ? N7 N8 C3 109.5(12) . . ? N7 N8 C4 120.3(11) . . ? C3 N8 C4 130.1(12) . . ? C5 N9 O1 112.7(11) . . ? N9 O1 H1 109.5 . . ? N5 Pd1 N1 89.0(4) 5_666 5_666 ? N5 Pd1 S1 90.8(3) 5_666 . ? N1 Pd1 S1 179.1(4) 5_666 . ? N5 Pd1 S2 177.8(3) 5_666 . ? N1 Pd1 S2 89.5(3) 5_666 . ? S1 Pd1 S2 90.72(15) . . ? N5 Pd1 Pd1 85.0(3) 5_666 5_666 ? N1 Pd1 Pd1 87.0(3) 5_666 5_666 ? S1 Pd1 Pd1 92.04(11) . 5_666 ? S2 Pd1 Pd1 93.39(10) . 5_666 ? C1 S1 Pd1 103.1(5) . . ? C3 S2 Pd1 102.5(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 C1 N1 N2 -0.6(13) . . . . ? S1 C1 N1 N2 178.1(10) . . . . ? N4 C1 N1 Pd1 -174.6(7) . . . 5_666 ? S1 C1 N1 Pd1 4.1(16) . . . 5_666 ? C1 N1 N2 N3 1.4(15) . . . . ? Pd1 N1 N2 N3 175.1(8) 5_666 . . . ? N1 N2 N3 N4 -1.5(14) . . . . ? N1 C1 N4 N3 -0.4(12) . . . . ? S1 C1 N4 N3 -179.3(8) . . . . ? N1 C1 N4 C2 176.6(13) . . . . ? S1 C1 N4 C2 -2.3(18) . . . . ? N2 N3 N4 C1 1.1(12) . . . . ? N2 N3 N4 C2 -176.6(10) . . . . ? N8 C3 N5 N6 1.8(14) . . . . ? S2 C3 N5 N6 -178.8(11) . . . . ? N8 C3 N5 Pd1 177.5(8) . . . 5_666 ? S2 C3 N5 Pd1 -3.1(19) . . . 5_666 ? C3 N5 N6 N7 -1.2(17) . . . . ? Pd1 N5 N6 N7 -177.2(10) 5_666 . . . ? N5 N6 N7 N8 0.2(18) . . . . ? N6 N7 N8 C3 0.9(17) . . . . ? N6 N7 N8 C4 178.2(13) . . . . ? N5 C3 N8 N7 -1.7(14) . . . . ? S2 C3 N8 N7 178.9(10) . . . . ? N5 C3 N8 C4 -178.6(13) . . . . ? S2 C3 N8 C4 1.9(19) . . . . ? C5 C5 N9 O1 -179.6(12) 7_666 . . . ? C6 C5 N9 O1 0(2) . . . . ? N1 C1 S1 Pd1 -3.8(13) . . . . ? N4 C1 S1 Pd1 174.7(8) . . . . ? N5 Pd1 S1 C1 86.4(5) 5_666 . . . ? N1 Pd1 S1 C1 11(18) 5_666 . . . ? S2 Pd1 S1 C1 -92.0(4) . . . . ? Pd1 Pd1 S1 C1 1.4(4) 5_666 . . . ? N5 C3 S2 Pd1 4.1(13) . . . . ? N8 C3 S2 Pd1 -176.6(9) . . . . ? N5 Pd1 S2 C3 -45(9) 5_666 . . . ? N1 Pd1 S2 C3 -89.6(5) 5_666 . . . ? S1 Pd1 S2 C3 89.5(4) . . . . ? Pd1 Pd1 S2 C3 -2.6(4) 5_666 . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.99 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.006 _refine_diff_density_min -1.005 _refine_diff_density_rms 0.210